GEOCHRONOMETRIA Vol.

21, pp 1-16, 2002 – Journal on Methods and Applications of Absolute Chronology

PRECISION AND ACCURACY IN THE OPTICALLY

STIMULATED LUMINESCENCE DATING OF SEDIMENTARY
QUARTZ: A STATUS REVIEW
ANDREW S. MURRAY1 and JON M. OLLEY2
1
The Nordic Laboratory for Luminescence Dating, Department of Earth Sciences,
Aarhus University, Risø National Laboratory, DK-4000 Roskilde, Denmark (e-mail: andrew.murray@risoe.dk)
2
CSIRO Water and Land, and Co-operative Centre for Catchment Hydrology, P.O. Box 1666, Canberra, ACT 2601, Australia

Key words
words: Abstract: Optically stimulated luminescence (OSL) dating of light-exposed sediments is used
OSL DATING, increasingly as a mean of establishing a sediment deposition chronology in a wide variety of
AEOLIAN SEDIMENTS, late Quaternary studies. There has been considerable technological development in the last
WATER-LAIN few years – in instrumentation, in the preferred mineral, and in various measurement proto-
SEDIMENTS, cols. New approaches to the latter, especially with the introduction of the single-aliquot
LATE PLEISTOCENE, regenerative-dose (SAR) protocol, have given rise to an increasing number of ages in the li-
HOLOCENE terature based on the OSL signals from quartz. This paper examines the reliability of these
results by reviewing both published and unpublished SAR quartz ages for which some
independent age control exists. It first discusses studies of modern (zero age) sediments,
and the implications of these results for the importance of incomplete bleaching, especially
in water-lain sediments, i.e. sediments for which the initial light exposure is expected to have
been insufficient to reduce the apparent dose at deposition to a negligible fraction of the final
burial dose. It then compares OSL and independent ages derived from various types of sedi-
ments, including aeolian, fluvial/lacustrine, marine and glacio-fluvial/lacustrine. It is concluded
that, in general, the ages are accurate, in that there is no evidence for systematic errors over
an age range from the last century to at least 350 ka. Nevertheless, the published uncertain-
ties of a small fraction of OSL ages are probably underestimated. We conclude that OSL
dating of quartz is a reliable chronological tool; this conclusion is reflected in its growing
popularity in Quaternary studies.

1. INTRODUCTION
Optically stimulated luminescence (OSL) can be used
to estimate the time elapsed since buried sediment grains
were last exposed to daylight. This method of sediment
dating makes use of the fact that daylight releases charge
from light-sensitive traps in the defects in crystals such as
quartz and feldspar. The release of trapped charge by light
resets the OSL signal; this process is commonly referred
to as bleaching. When grains of quartz are buried and
hidden from light, they begin to accumulate a trapped-
charge population due to the effects of ionising radiation,
such as that arising from radionuclides naturally present
in the deposit. This trapped-charge population increases
with burial time in a measurable and predictable way.
As a result, the time elapsed since sediment grains were
buried can be determined by measuring both the OSL
signal and sensitivity from a sample of sediment, and by
estimating the flux of ionising radiation to which it has
been exposed since burial.
Until the late 1990s, the great majority of OSL dates
were based on infrared (IR) stimulation of feldspars
(Wintle, 1997; Aitken, 1998), but over the last few years
both the preferred mineral and the laboratory techniques
used to measure OSL have undergone major changes.
It was always thought that quartz had considerable po-
tential in optical dating, but it was little used because ali-
quot-to-aliquot reproducibility was poor, and because it
was insensitive to IR. It requires visible light stimulation,
which was usually derived from an expensive laser instal-
lation (e.g. Rhodes, 1988). Since then, a readily accessible
measurement technology has become widely available,
with the development of cheap green and blue light
sources (these were at first filtered from the broad-band
emission of an incandescent filament (Bøtter-Jensen and
Duller, 1992); more recently they have been based on
bright blue light emitting diodes (Bøtter-Jensen et al.,
2000). At the same time, measurement protocols have
undergone major development. Until 1997, estimation of
the equivalent dose (i.e. the dose absorbed during burial,
 PRECISION AND ACCURACY IN THE OPTICALLY STIMULATED LUMINESCENCE DATING...
De) for quartz required the use of many aliquots (typi-
cally 50-100, each of about 10 mg). With the development
for quarty of first the single-aliquot additive-dose proto-
col (Murray et al., 1997) and more recently the single-
aliquot regenerative-dose (SAR) protocol (Murray and
Roberts, 1998; Murray and Wintle, 2000), all the measure-
ments for quartz required to estimate the De can now be
made on one aliquot. This has two particular advantages:
(1) the uncertainties on the average De are now based on
external estimates of precision – i.e. the standard uncer-
tainty on the mean is estimated from several independent,
interpolated measurements of De, rather than from the
uncertainties associated with, for example, extrapolating
a single modelled growth curve fitted to the data derived
from many aliquots; and (2), for the first time, the distri-
bution of doses within a sample can be examined explic-
itly (e.g. by making De measurements on single grains).
These developments have resulted in a considerable in-
crease in the number of published quartz dates, almost
all of which are based on the SAR protocol. Age estimates
based on quartz have been now produced by many labo-
ratories over an age range of a few decades to more than
500 ka, and this method has already found considerable
application in the dating of Quaternary sediments.
In this paper, we consider the evidence for the relia-
bility of these SAR quartz OSL ages. The SAR protocol
is first described and some internal checks on performance
outlined. The process of bleaching or resetting the OSL
signal is then discussed, along with the complications of
interpreting the OSL signal when charge transfer is sig-
nificant; the importance of these effects is considered by
examining the reported apparent ages of modern sedi-
ments. We then review both published and unpublished
quartz ages for a variety of sediment types and age ranges.
In some cases these are known to be poorly bleached, but
in all cases some age control exists; this allows the relia-
bility of the OSL ages to be assessed.
2. THE SINGLE ALIQUOT REGENERATIVE DOSE
(SAR) PROTOCOL
There are many published descriptions of the single
aliquot regenerative dose (SAR) protocol and its appli-
cations (e.g. Murray and Olley 1999; Murray and Wintle,
2000; Bailey et al., 2001; Stokes et al., 2001) and it is not
appropriate here to do more than outline its principle
features, and to highlight the main assumptions. Table 1
sets out a typical SAR measurement cycle. The sample is
given a dose (D0) during burial (i.e. before sampling). In
the laboratory, the sample is first preheated to some tem-
perature in the range of 160 to 300o C (usually for 10 s)
and the natural OSL signal (L0) measured. The sample
is then given a test dose (Dt), heated to 160o C and the
test dose OSL signal (T0) is measured; this completes the
first (natural) measurement cycle. To begin the second
cycle, a regenerative dose (D1) is first administered; the
sample is then heated to the same preheat temperature
as in the first cycle and the OSL signal measured (L1).
The sample is then given the same test dose as before (Dt),
heated to 160 o C and the test dose OSL signal (T 1)
2
measured; this regenerative cycle is then repeated as many
times as desired, with the regenerative dose (Di) the only
variable. These regenerative doses are usually chosen
to give values of the sensitivity corrected OSL ratio
(Ri=Li/Ti) which bracket the natural response (N=L0/T0).
The test dose (Dt) is usually a small fraction (~10%) of
the natural dose, although Murray and Wintle (2000) have
shown that this is not a necessary requirement. The natu-
ral dose is then estimated by interpolating the ratio N onto
a plot of Ri against Di (Fig. 1).
For the protocol to be useful, any sensitivity changes
that may occur from one measurement cycle to the next
must be accurately measured by the OSL response to the
test dose (Dt), i.e. Li ∝Ti for constant Di. If this require-
ment is met, the corrected OSL ratio Ri( = Li/Ti) should
be independent of treatment history, i.e. independent of
prior dose or thermal treatment. This is most easily tested
by repeating a particular value of D (e.g. D5 = D1) after
Fig. 1. Typical single-aliquot regenerative-dose growth curve,
showing the natural OSL ratio N(=L0/T0 , see text and Table 1)
interpolated onto the regenerated growth curve, for a single
8 mg aliquot of a glaciofluvial sample from northern Russia
(laboratory code 992528). The recycled value (R 5 at the lowest
regenerated dose is shown as an open circle (R 5/R1=1.02 for
this aliquot), and the recuperated signal for which D 4=0 Gy, as
an open triangle (R 4=1% of the natural signal N).
Table 1. Generalised single-aliquot regenerative-dose protocol
(after Murray and Wintle, 2000).
Step Treatment Observed
1 Give dosea, Di -
2 Preheatb (160-300o C for 10 s) -
3 Stimulatec for ~100 s at 125o C Li
4 Give test dose, Dt -
5 Heatb to 160o C -
6 Stimulatec for ~100 s at 125o C Ti
7 Return to 1
aFor the natural sample, i=0 and Do is the natural dose.
bAliquot cooled to <60o C after heating. In step 5, the TL signal from the test
dose can be observed, but it is not made use of in routine applications.
cThe stimulation time is dependent on the stimulation light intensity and
wavelength (eg. 40 s for blue light diodes, 100 to 125 s for green-light
sources).
dL and T are derived from the stimulation curve, typically the first 1 to 10
i i
seconds of initial OSL signal, minus a background estimated from the last part
of the stimulation curve.
 A.S. Murray and J.M. Olley
various larger values have been used, and comparing the
two OSL ratios (in this case R5 and R1); for the same dose
the two values of R should be the same (R5/R1 = 1, the
so-called recycling ratio). Preheating the sample can also
cause recuperation of the OSL signal (i.e. heating after
OSL measurement can give rise to a new OSL signal, even
in the absence of an ionising radiation dose). To test for
this, a SAR cycle is measured with Di = 0 Gy (usually
i = 4). The ratio R4 should then be zero, but in practice
is usually some small % of N. Rejection criteria can be
proposed based on these two test measurements
(e.g. 0.9 < R5/R1 < 1.1, and R4/N < 5%), but there is little
evidence of how sensitive the value of De is to these
criteria.
The performance of the SAR protocol with respect to
laboratory doses can be checked by the two tests described
above, but it is important to realise that there is no readily
available test that the assumptions hold in the first mea-
surement cycle, in particular that laboratory induced sen-
sitivity variations in L0 are faithfully reflected in variations
in T0. Murray and Wintle (2000; their Figure 3) did test
this assumption using the response of the 110° C TL peak
before and after OSL measurement of the natural signal,
but this approach requires that any sensitivity changes in
the measurement of the OSL signal are reflected in
changes in the 110° C TL peak; this cannot be assumed,
and must be tested from one sample to another.
For feldspar, Wallinga et al. (2001) have suggested the
routine use of a dose recovery test, in which a sample is
first optically zeroed without any heating above room tem-
perature, and then given a known dose using a laboratory
source. This dose is measured as if it were an unknown
natural dose (i.e. beginning with a preheat). The impor-
tant point here is that the first heating of the sample oc-
curs after the administering of the dose to be measured;
at least for feldspar, there is clear evidence that the first
heating of a sample changes its luminescence sensitivity,
probably by changing the rate of charge trapping. Of course,
any useful measurement protocol should be able to mea-
sure this (known) laboratory dose accurately.While this
does not necessarily imply that a natural dose can also be
measured accurately, it does serve to increase confidence
in the measurement procedure. This approach should
probably be made more use of with quartz.
3. RESETTING THE OSL SIGNAL – BLEACHING
If a clean quartz grain is exposed to daylight, the so-
called “fast component” of the OSL signal will be reduced
to a negligible level within a few seconds. However, in
nature this is rarely the case. Quartz sand grains are rarely
“clean”; they usually have iron and manganese oxide sur-
face coatings, and they may have adhering clay grains. The
transport medium is rarely transparent; even during
aeolian transport (usually considered to be the most ideal
bleaching circumstance) other grains can attenuate the
light. Nevertheless, even in aqueous transport, there may
be circumstances where bleaching is complete; sand re-
peatedly washed up and down a lake or marine beach will
receive considerable exposure to light, and sand depos-
3
ited by a high energy event (e.g. a storm or tsunami) is
likely to have been derived from shallow-water deposits
that had already been thoroughly light exposed. In many
freshwater environments, however, turbidity may be the
controlling factor; in some low gradient rivers at low lati-
tudes most of the incident light is absorbed in the first
1 m of water or less (Oliver, 1990).
Predicting the rate of bleaching is complicated further
by the nature of a transport process. Turbulent mixing and
saltation combine to move even coarse sand-sized grains
into and out of the regions of the transport medium which
receive the highest light fluxes. If the flux gradient is steep
(as in a turbid river) this will have the effect of exposing
the grain to light for a short period, before returning it to
effectively complete darkness. It is even possible that the
majority of bleaching in turbid river systems occurs only
during low flow periods when the water is clear and shal-
low, and sand transport has ceased. Then only those sand
grains resting on the surface of the bed will get sufficient
light exposure to fully bleach the OSL signal. As a result
of these various processes, the bleaching history of every
grain will be different, and only when all grains have had
more than sufficient light exposure will a sediment sample
be completely bleached. This is usually assumed to be true
for aeolian transported material, but it is at least ques-
tionable for sediments transported in other ways.
Incomplete bleaching results in grains being deposited
with a heterogeneous distribution of residual trapped
charge. If large sample aliquots (i.e. aliquots made up of
many grains) are used for the measurement of the OSL
signal, these residual trapped charges give rise to an ap-
parent dose that results both from charge trapped during
Fig. 2. (a) Apparent doses from 116 small aliquots of 125-180 µm
diameter grains of quartz (laboratory code ME95002/2)
extracted from a recent sand deposit on the Murrumbidgee River,
New South Wales, Australia. Each aliquot contained between 60
and 100 grains. (b) Apparent doses in 96 aliquots from a modern
aeolian dune sand (125-180 mm diameter), known to be less
than 5 years old, from the east Queensland coast, Australia
(DS1/1; both figures taken from Olley et al., 1998).
 PRECISION AND ACCURACY IN THE OPTICALLY STIMULATED LUMINESCENCE DATING...

burial and the residual trapped charge already present at

the time of burial. The net effect is an overestimate of
the age. However, if small aliquots are used, made up of
only a few grains, or even single grains, a distribution of
apparent doses will be measured, skewed to larger val-
ues. In such cases, the lower values are more likely to give
the true age since burial. Figure 2 illustrates this compari-
son using two modern sediments, one aeolian and one
river sand (Olley et al., 1998), both measured using
aliquots of about 100 grains. Effectively all the aliquots
from the aeolian sand are well bleached, but only about
5% of those taken from the river sand are consistent with
zero dose.
It is possible that during some depositional events none
of the sediment grains would receive sufficient exposure
to fully bleach the OSL signal. Especially in very young
deposits (<100 years) with evidence of heterogeneous
bleaching at deposition, it may be that OSL ages should
be viewed as maximum ages of burial.

4. PREHEATING AND CHARGE TRANSFER

Some heating of the aliquots is always applied before

measurement of any OSL signal. In the SAR protocol
described by Murray and Roberts (1998) and improved
by Murray and Wintle (2000), the OSL signal is measured
while the aliquot is held at 125° C. This is intended to
minimise charge cycling through the 110° C TL trap, and
so increase the rate of decay of the OSL signal, and this
procedure has been adopted widely. Additional heating
prior to OSL measurement is also common. There is a
tendency for younger samples to be measured after heat-
ing to lower temperatures (typically 200 to 220° C for 10 s;
Murray et al., 1995; Olley et al., 1998; Hilgers et al., 2001;
Murray and Clemmensen, 2001; Banerjee et al., 2001;
Wallinga et al., 2001; Stokes et al., 2001) than are used for
older samples. The latter are more usually heated to 260
or 280° C for 10 s prior to measurement (Strickertsson
and Murray, 1999; Strickertsson et al., 2000; Roberts et
al., 1998; 1999; 2001; Wallinga et al., 2001), although there
are several examples of ‘preheat plateaus’ which show that
the apparent dose is insensitive to the temperature of
heating prior to measurement, at least in the range 160
to 300o C (Murray and Olley, 1999; Murray and Wintle,
2000; Roberts et al., 1999).
There are good reasons why younger samples should
be measured with lower preheat temperatures. Thermal
transfer, or the transfer of charge by heating from light-
insensitive but thermally-stable traps into the light-sensi-
tive traps, is probably not important in older samples; this
is shown by the lack of sensitivity of De to preheat tem-
perature mentioned above. This appears not always to be
true for younger samples. Various authors have mentioned
or presented preheat plateaus for young samples which
increase with temperature (Murray and Clemmensen,
2001; Bailey et al., 2001; Rhodes, 2000; Wallinga et al.,
2001; Hilgers et al., unpublished), and Banerjee (2000)
has also discussed this issue. It is likely that this is com-
mon in samples which have received enough light expo-
sure to empty the OSL trap, but insufficient to empty the
Fig. 3. (a) De as a function of preheat temperature for an aeolian
sand sample (age 310±90 years) from the coast of Wales
(redrawn from Figure 3 of Bailey et al., 2001).
(b) Filled circles: preheat plateau for quartz sample F1 of the
dune section “Postdüne”, located north of Berlin in
Brandenburg, Germany (age: 140±10 years). Aliquots were
measured in groups of 3 using 8 different preheat temperatures
from 160° up to 300° C (held for 10 s each; the cycle was
repeated, 48 aliquots were measured in all). Six regeneration
cycles were measured using the following doses for beta-
irradiation 0, 0.38, 0.63, 0.88, 0, 0.38 Gy (test dose: 0.25 Gy),
blue light emitting diodes for optical stimulation (100 s at 125°
C), and a cut heat of 160° C. Each data point shows the average
and standard uncertainty of 6 aliquots, except for 240°C (n=30)
and 260°C (n=24).
Open symbols: Data were obtained for 24 aliquots processed as
described above, but all aliquots were first stimulated for 150 s
with blue diodes at 125° C to remove the natural OSL signal. The
test doses applied were 25 % of the De (0.05 Gy, open square),
160 % (0.31 Gy, open circle) and 1600 % (3.1 Gy, open
triangle). All taken from Hilgers et al. (unpublished).
(c) Apparent values of De resulting from repeated heating of a
single aliquot of 300 year old fluvial bedload from a channel of
the Rhine-Meuse system in the Netherlands (see Wallinga et al.,
2001). The results were checked for the absence of sensitivity
change.

4
 A.S. Murray and J.M. Olley
less light-sensitive and thermally-shallow traps, such as the
TL traps at 160, 240 and 280° C. These traps can be ex-
pected to retain a significant charge population at the time
of deposition, even although the OSL trap was well
bleached (in fact, these TL traps may even contain an
equilibrium trapped-charge population, where rate of
trapping equals rate of thermal release at ambient tem-
perature). If this sample is then heated to a temperature
sufficient to release some or all of this charge in shallow
traps, a fraction of the released charge can be retrapped
by the OSL trap. This gives then rise to a finite OSL sig-
nal from a sample that was, in fact, well bleached at depo-
sition. This phenomenon will become increasingly less
important as the OSL trap stores charge from the ambi-
ent radiation flux after burial, because the retrapping pro-
cess seems to be inefficient. This effect is illustrated in
Fig. 3b,c (open symbols). Here the aliquots were all first
bleached using blue light (at 125° C in Fig. 3b; at room
temperature in Fig. 3c), but without prior heating. This
emptied the OSL trap but left any shallow traps (except
the TL trap at 110° C) relatively untouched. The aliquots
were then subject to the usual SAR protocol, using the
various preheat temperatures shown. At low tempera-
tures, the apparent De is very small, but at higher tem-
peratures there is significant thermal transfer during the
first preheat into the empty OSL trap, and the apparent
De (filled symbols) begins to rise. In both the young
aeolian sample (Fig. 3b, open symbols; Hilgers et al., un-
published data) and in the young fluvial sample (Fig. 3c;
Wallinga et al., unpublished data) the phenomenon is
detectable at temperatures as low as 200° C, and rapidly
becomes significant at temperatures above this. The ef-
fect of this transfer on the variation of De with preheat
temperature is clearly seen in the preheat plateau for the
two aeolian samples (Fig. 3a – Bailey et al., 2001 – and
Fig. 3b, filled circles). It is clearly desirable to use low tem-
perature preheating for young samples, especially those
that are likely to be less well bleached. It is less clear that
there is a compelling reason to use higher temperature
preheating for older samples; as discussed above, all pub-
lished preheat plateaus for older samples appear relatively
flat.
5. MODERN SEDIMENTS
One way to test the hypothesis that samples are well
bleached at the time of deposition is to examine modern
(i.e. zero age) analogues. This is increasingly standard
practice in dating studies, and although such analogues
are not always available at or close to the sampling site of
interest (especially for deposition environments associ-
ated with continental glaciation events) such studies can
be very informative. The following sections summarise
what is known about various classes of modern sediments
using the SAR protocol.
Aeolian – Olley et al. (1998) calculated the average dose
in an Australian aeolian sediment believed to be <5 years
old (using the data of Fig. 2a). They derived an average
De of 0.020±0.006 Gy, using a preheat of 200° C for
10 s; this corresponds to an age of about 20 years, using
5
typical dose rates (note that throughout the symbol ‘±’ is
followed by the standard uncertainty on the mean, and
that the number of significant digits is given as presented
by the original author). Bailey et al. (2001) took a sample
from the top of a parabolic dune, currently subject to wind
erosion, on the coast of north Wales, and obtained an age
of 20±10 years, averaged over the preheat range 160 to
260° C (heated for 10 s). Murray and Clemmensen (2001)
sampled wind-blown sand deposited on concrete on the
west coast of Denmark, and known to have been depo-
sited in the last 35 years; they obtained an age of 36±5
years, using a preheat of 200° C for 10 s. One author
(Murray) has other unpublished examples of ages
~10 years from modern aeolian sediments from this geo-
graphical area.
Fluvial – Murray et al. (1995) used a simplified regen-
eration protocol to examine the residual doses in 4 mod-
ern fluvial sediments, covering catchment scales from a
few hectares up to >100,000 km2. In all these catchments,
flood flows were known to be very turbid. In their ap-
proach only a single regeneration cycle was used, with no
test dose. Their results are considered here, because the
OSL response to dose (the growth curve) at low doses is
known to be linear, and because the sensitivity change at
such low doses will be negligible if the preheat tempera-
ture is kept low (they used 200o C for 10 s). They observed
average doses of between 0.3 Gy and 3 Gy, correspond-
ing to approximate ages of a few hundred up to a thou-
sand years. The lowest apparent age was derived from the
only overbank deposit; the other three were samples of
in-channel deposits. They measured the OSL signals us-
ing small aliquots of only about 150 fine-sand sized grains;
this sample size was chosen to deliberately increase the
scatter in the data, and so increase the probability that
they would observe aliquots containing only well-bleached
grains. In 3 out of the 4 distributions they observed some
aliquots with doses consistent with zero, and in the fourth
sample, the smallest doses were consistent with an age of
about 60 years. This supports the hypothesis that even in
turbid systems there are likely to be some grains that are
well-bleached. Olley et al. (1998) sampled a modern in-
channel sand deposit from the Murrumbidgee River in
eastern Australia, and used a 200o C preheat for 10 s. They
measured an average apparent age of 340±70 years (cal-
culated using their average De and dose rate values). Fur-
ther measurements, using small aliquots of 80 to 100
grains each (see Fig. 2a), demonstrated that not all grains
in this deposit were fully bleached; if they used only the
lowest 5% of aliquots, they derived an age that was con-
sistent with zero (3±4 years). These authors also exam-
ined the grain size dependence of the dose distributions
in sediments from the same river, and found the rather
surprising result that the fraction of well-bleached grains
appeared to increase as the grain size increased (in the
range <63 µm to 250 µm).
Colls et al. (2001) sampled various deposits on the
River Loire in central France. They used a relatively high
temperature preheat (280o C for 10 s), which almost cer-
tainly resulted in some thermal transfer, and probably
contributed to the finite age of 300±60 years they
 PRECISION AND ACCURACY IN THE OPTICALLY STIMULATED LUMINESCENCE DATING...
Fig. 4. Apparent De for bedload samples collected within the
channel of the Loire River in France (after Stokes et al., 2001).
obtained for a modern point-bar deposit. This study
used average estimates of De – no attempt was made to
correct for incomplete bleaching, e.g. by measuring dis-
tributions of dose in small aliquots. Stokes et al. (2001)
conducted a more systematic study of modern sediments
in two river basins, the Colorado (USA) and the Loire
(France). In the Colorado system they collected 4 samples
from the Colombus Point Bar in Texas, and in the Loire
they collected 13 samples along the length of the chan-
nel, from source to mouth. The Colorado study used the
full SAR protocol, whereas that in the Loire used the sim-
plified protocol of Murray et al. (1995). In the Colorado
study they observed average ages between 95 and 648
years. Their data also suggested that the apparently older
samples had not been completely bleached, but their at-
Fig. 5. Schematic cross-sections of (a) the interdune area and modern parabolic dune and (b) aeolian sand stratigraphy at Lake
Coron, on the coast of Wales, UK, derived from ground penetrating radar images. The OSL ages (ka) and sample locations are also
shown (modified by Bailey [pers. comm.] from Bailey et al., 2001).
6
tempt to correct for this only reduced the range to be-
tween 70 and 290 years. However, all their measurements
involved relatively large aliquots (>1000 grains) and so
some averaging was probably unavoidable. In the Loire
study, the average ages decreased with distance from
3.3 ka near the source, to about 80 years at the mouth
(Fig. 4; open circles). If some allowance was made for
incomplete bleaching (filled circles), this pattern changed
to about 1 ka at the source, decreasing to only a few de-
cades within the first 10 km, and staying low thereafter.
Marine – In a study of a possible tsunami deposit on
the Scilly Isles (UK), Banerjee et al. (2001) sampled mo-
dern sub-aqueous coastal sand, from a few centimetres
below the sediment surface and more than 2 m below
water level at low astronomical tide. Using a preheat of
200o C for 10 s, they calculated an average OSL age for
the 180-210 m fraction of 2.0±1.7 years.
6. HOLOCENE AND LATE PLEISTOCENE SEDIMENTS
The effects of incomplete bleaching are most likely to
be obvious in younger samples (e.g. those from the Ho-
locene) and so there have been many studies of aeolian
material from this period, but water-lain deposits tend to
have been avoided. Nevertheless there is an increasing
awareness that incomplete bleaching in fluvial and ma-
rine systems may not be as large a problem as previously
feared, and this has led to an increasing interest in such
sediments.
Aeolian – Strickertsson and Murray (1999) sampled
a sand of historically known (300-400 years) age from the
west coast of Jutland, Denmark, and obtained an OSL age
of 290±20 years, using preheats between 240 and 280° C
for 10 s. Bailey et al. (2001) dated a small dune field on
 A.S. Murray and J.M. Olley
the west coast of north Wales (Fig. 5; note that these ages
have been revised slightly by Bailey, pers. comm., from
those originally published). They obtained an age for the
oldest phase of sand movement of 710±50 years, averaged
over the preheat range 160 to 260° C (heated for 10 s).
This is consistent with the historical evidence that this
dune field began to accumulate in AD 1331. They also
used ground-penetrating radar to identify two deposition
units, which were then sampled from 4 separate boreholes.
This provided 4 samples from the younger unit, of ave-
rage age 328 years (sample standard deviation σ=15), and
3 for the older, of average age 517 years (σ=12). They
assumed that the samples were saturated throughout the
burial period, and do not provide an uncertainty for their
water content values or for other corrections introduced
to compensate for systematic errors. However, these are
presumably not trivial, because their overall combined
standard uncertainty on an individual age varies between
20 and 40 years, significantly in excess of their observed
reproducibility.
7
Murray and Clemmensen (2001) describe a sequence
of 14C dated palaeosols interleaved with aeolian sand units
from a site on the west coast of Jutland in Denmark
(Fig. 6). Their values of De were independent of preheat
temperature (in the range 160 to 280° C, held for 10 s),
and the agreement with 14C over the age range 4500 years
to about 100 years was very satisfactory. Their youngest
results (between 70 and 180 years) were known with con-
siderably better calculated uncertainties (between 9 and
40 years) than the immediately underlying calibrated 14C
ages (±140 years); this illustrates the importance of un-
certainties arising from the shape of the 14C calibration
curve in the last few centuries. (Note that all 14C dates
discussed in this paper are calibrated by the original au-
thors unless otherwise stated.)
Radtke et al. (2001) undertook a comparison of quartz
and feldspar, single- and multiple-aliquot dating of dune
sands immediately above and below the Laacher-See te-
phra layer at a site near the Rhine, close to Mainz, Ger-
many. Using the SAR protocol, and a preheat of 260° C
Fig. 6. Diagrammatic section of the
Lodbjerg site in western Jutland, Denmark
(based on Murray and Clemmensen,
2001), showing relationship between OSL
and calibrated 14C dates. S3 is a complex
and less well-defined palaeosol. The
midpoints of the calibrated 14C ages are
shown, with uncertainties of half the range;
the ages include an additional 40 years to
convert to calendar years.
 PRECISION AND ACCURACY IN THE OPTICALLY STIMULATED LUMINESCENCE DATING...
for 10 s, they obtained quartz ages of 14.6±1.5 ka below
the tephra, 11.9±1.0 ka in the tephra layer, and
13.4±1.2 ka above the tephra. All these ages are consis-
tent with the well-known age for the Laacher-See tephra
of 13.155 ka, based on AMS 14C measurements of decadal
samples of poplar buried by the tephra (Friedrich et al.,
1999). Hilgers et al. (2001) undertook a related study near
Eberswalde, north of Berlin, Germany, at a dune sand site
that contains both the Laacher-See tephra and a well-
described palaeosol, dated by Schlaak (1993) to the
Allerød interstadial (12.9-14 ka). Their study also included
several 14C ages from younger layers, and with one excep-
tion the relevant OSL ages were in good agreement. Ho-
wever, the relative stratigraphy of the earlier 14C samples
compared to the OSL samples in these younger layers was
not unambiguous, and so these comparisons are not con-
sidered here. They used a preheat of 260° C for 10 s; for
the sample immediately overlying the Laacher-See tephra,
they obtained an age of 11.2±1.3 ka, and for the samples
encompassing the palaeosol, they obtained 11.9±1.1 ka
(above) and 15.1±1.4 ka (below). All three of these dates
are in excellent agreement with their respective age
controls.
Rich and Stokes (2001) dated a variety of aeolian
samples from the southern High Plains (between New
Mexico and Texas, USA). The sites were of archaeologi-
cal significance, and many had independent 14C age esti-
mates already available. The reliability of association be-
tween these independent ages and the OSL samples is
unclear, especially since some of the 14C dates were un-
dertaken in the 1950s. Nevertheless for 11 samples for
which a comparison with SAR data can be drawn, the
mean ratio of SAR to independent age is 1.12±0.17.
These samples cover an age range from a few hundred
years to about 11 ka.
Mangerud et al. (2000) report two comparisons of
aeolian OSL dates with 14C from two sites in north west-
ern Russia. One is at the Pymva Shor archaeological site,
where a reindeer bone (uncalibrated 14C age given as
10.27±0.08 ka; after calibration 12.0±0.3 ka) was found
Fig. 7. Radial plots of measured doses for single grains from (a) sample ME95041B and (b) sample WK96008. In each plot,
the shaded region represents the expected burial dose (after Olley et al., 1999).
8
in an aeolian sand unit which provided two OSL dates of
12.0±0.9 and 13.6±1.2 ka. The other is at their Kuya
Bridge site, where they give an uncalibrated 14C age of
12.3±0.06 ka (on organic material extracted from bulk
sediment sample); after calibration this gives 14.3±0.5 ka.
Despite the problems often associated with such samples,
this agrees very well with the OSL age from the same
aeolian sand unit, of 14.6±1.2 ka.
Freshwater sediments – Olley et al. (1998) measured the
apparent age of a flood deposit known to have been de-
posited in 1926. The average apparent age determined
from large aliquots (~2000 grains) was between 400 and
700 years (preheat 200° C for 10 s), but by using small
aliquots (60 to 100 grains), and comparing with the dis-
tribution of a modern analogue (see Fig. 2a) they derived
an age of 67±5 years, in good agreement with the known
age. Olley et al. (1999) later examined the dose distribu-
tion in single grains from this sample and from a sample
with a calibrated 14C age of 1530 years (before 1954) and
a 95% confidence age range of 1400-1690 years. Measured
doses for single grains from each sample are shown in the
form of a radial plots in Fig. 7a, b. The shaded region on
each plot represents the expected burial dose (0.27±0.02
Gy and 5.4±0.6 Gy respectively). The dose measured for
a grain can be read by extrapolating a line from the y-axis
origin through the data point until the line intersects the
radial axis (log scale) on the right-hand side. This gives
the dose estimate in Gy, and its standard uncertainty can
be read by extending a line vertically from the data point
to intersect the x-axis. The x-axis has two scales: one plots
the relative standard uncertainty of the dose (called rela-
tive error by Olley et al., 1999; see Fig. 7) and the other
(precision) plots the reciprocal standard uncertainty of
the log dose estimate. Therefore, values with the highest
precisions and the smallest relative uncertainties plot clos-
est to the radial axis on the right of the diagram, and the
least precise estimates plot furthest to the left (note that
the calculated uncertainties are usually dominated by
counting statistics in this type of study). The y-axis pro-
vides a further aid to data display, by plotting standardised
 A.S. Murray and J.M. Olley

estimates of log dose. These are calculated by subtract-

ing a reference value (such as the pooled log dose for all
aliquots, or another log dose of interest) from each of the
log doses and then dividing each of the differences by the
associated standard uncertainty. Galbraith et al. (1999)
provide further details, and a worked illustration, of how
radial plots may be used to display OSL data. Olley et al.
(1999) concluded on the basis of these data that the popu-
lations of single grains with the lowest doses gave ages
consistent with the expected burial ages.
Olley and Hancock (unpublished data) have compared
210
Pb and OSL ages on two freshwater sediment cores
from south-eastern Australia. In each case the samples
were poorly bleached and the OSL ages were based on
the lowest doses observed in single grains of quartz, mea-
sured with a preheat temperature of 220° C. In the first
example, from the Bega estuary in New South Wales, the
OSL age of 70±8 years at 25 cm compared well with the
210
Pb age of 63±8 years at 24.5 cm. In the second example,
from Blue Lake, one of the highest lakes in Australia,
the 210Pb age of 128±10 years at 52 cm is consistent with
Fig. 8. OSL ages plotted against independent age estimates for
the OSL age of 170±20 years at 60-62 cm if a constant fluvial channel deposits in the Rhine-Meuse system in the
rate of sediment supply is assumed. Olley and Taylor Netherlands (after Wallinga et al., 2001).
(unpublished data) have also produced a similar compari-
son between the first appearance of the fallout nuclide
137
Cs and an OSL age on lake sediments from the Arapiles thermal transfer characteristics of these samples had been
Lake Complex, Wimmera, Australia. The first appearance explicitly studied (those of the youngest sample are shown
of 137Cs in a sediment core from this region occurs at about in Fig. 3c).
AD 1958 (i.e. 44 years ago). The OSL age of the sediments Houmark-Nielsen (unpublished data) has two com-
from this horizon gave an age of 29±15 years. Again parisons of OSL and 14C ages from Late-Glacial lacus-
the sample was poorly bleached and the OSL age was trine deposits in Denmark (Table 2, lines 4 and 5). The
based on the lowest measure doses in single aliquots of OSL ages both used 260° C preheats for 10 s, and the
quartz each consisting of ~10 grains (preheat of 220°C agreement with the independent age is very satisfactory.
for 10 s). Larsen et al. (1999) report one comparison at their
Wallinga et al. (2001) have dated a sequence of aban- Chelmokhta site from northern Russia, where five 14C ages
doned river channels from the Rhine-Meuse system in the (on wood) of between 10.7 and 11.5 ka can be compared
Netherlands. These channels had already been extensively with an OSL age on lacustrine sand of 13.7±1.1 ka.
studied, and the ages of the younger channels are consid- Strickertsson and Murray (1999) took samples from
ered to be well known. Fig. 8 summarises the comparison freshwater Bølling-Allerød (14.1-14.5 ka) and Younger
of OSL ages (preheat 200° C for 10 s using average val- Dryas (11.1-12.9) sediments, from Nørre Lyngby on the
ues of De derived from small aliquots) with the indepen- west coast of Jutland in Denmark (the independent age
dent chronology; the agreement is excellent except for that controls are discussed and referenced in Strickertsson and
from the youngest sample, known from historical sources Murray, 1999). They used preheats of between 240 and
to have been deposited about 300 years ago. The corre- 280° C for 10 s, and obtained SAR ages of 13.6±1.1 ka
sponding OSL age is 920±100 years, and the difference (Bølling-Allerød) and 9.8±0.7 and 8.2±0.6 (Younger
presumably arises from incomplete bleaching, since the Dryas). The latter pair in particular appears to slightly

Table 2. Summary of comparisons between OSL and calibrated 14C ages from various fluvial and lacustrine sites in Denmark (Houmark-
Nielsen, unpublished).
Locality Sample OSL Age [ka] 14C Age [ka] Organic material OSL/14C ratio
Lønstrup 970203 30±2 33±2 plant 0.91±0.08
970204 29±2 32±3 moss 0.91±0.11
Lodbjerg 980203 30±3 33±1 plant 0.91±0.10
980201 13.6±1.0 13.9±0.5 plant 0.98±0.08
Bovbjerg 990205 13.8±0.9 14.0±0.5 plant 0.99±0.06
Møn, Kobbel Gård 990219 26±2 32±2 gyttja 0.81±0.08
990220 29±2 30±2 seed 0.97±0.09
000230 28±2 27±1.0 teeth 1.04±0.08
Average: 0.94±0.03

9
 PRECISION AND ACCURACY IN THE OPTICALLY STIMULATED LUMINESCENCE DATING...
underestimate the independently known age. We do not
consider their Podzol Bh-horizon sample, because the
authors state that this soil was formed on Younger Dryas
sediments, but must have received considerable light ex-
posure at later times, up until the soil was capped by the
300 year old aeolian event discussed earlier.
Marine – Stokes et al. (2001) have reported a set of 5
OSL ages obtained using the silt-sized quartz fraction
from a deep sea core from the Indian Ocean, for which
a well controlled age model already existed. There was
no dependence of De on preheat temperature, in the range
200 to 280° C, and preheat temperatures of 200 and
240° C were employed in routine analysis. Fig. 9 includes
their 2 OSL ages younger than 20 ka; the agreement with
Fig. 9. Chronological models for core 70KL, taken from Stokes
et al. (submitted). OSL dates are based on silt-sized quartz
extracted from a deep sea core in the Indian Ocean. AMS
radiocarbon ages include a 400 year sea water correction and
are calibrated. Other age control includes the Toba Ash (variably
dated to between 68±7 ka by fission track dating and 73-75 ka
by Ar-Ar), a key biostratigraphic marker horizon, LAD G. ruber
(pink) (which provides a maximum age of 120 ka) and
comparison of the oxygen isotope record with the SPECMAP-
Stack (small markers indicate the tie-points; correlation
coefficient=0.94). Details of these independent age controls
are given by Stokes et al. (submitted).
10
the independent age control is excellent. Strickertsson and
Murray (1999) also took marine samples from their Nørre
Lyngby section. These were from the Older and Younger
Yoldia Clay, with independent ages based on calibrated
14
C dating of in-situ shell of about 24 ka, and 17.2±0.4 ka.
Their SAR OSL ages were independent of preheat tem-
peratures in the range 240-280° C (for 10 s), and the one
OSL age (25.3±1.8 ka) from the Older Yoldia Clay was
in good agreement with the expected value of about 24 ka.
However, there was a possible systematic underestima-
tion of the expected ages for the Younger Yoldia Clay,
by about 8% averaged over 4 results. Strickertsson et al.
(2001) report further ages on the Younger Yoldia clay,
from Stensnºs, about 2 km from the earlier site. These
two ages (21.1±0.9 and 26.2±1.4 ka) were significant
overestimates compared to the expected age range, and
the authors suggest that the deposits may have been
misidentified in the field (the Older Yoldia Clay [24 ka]
is very similar to the Younger). The sand layer above the
supposed Younger Yoldia Clay was believed to be Upper
Saxicava in the field, with an expected age of about
12.5 ka. In fact an OSL age of 17.5±1.3 ka was obtained,
also casting doubt on the field identification.
7. OLDER SEDIMENTS
Aeolian – Watanuki et al. (submitted) have examined
the silt-sized (4-11 µm) quartz fraction in loess, depos-
ited on two river terrace sites (Niigata and Tochigi) in
central Japan, using 240 and 260° C preheats. This mate-
rial was blown across from the Chinese mainland, but it
is unusual in that there is age control based on tephra lay-
ers interleaved with the loess; these various tephra layers
have been dated, using 14C and fission tracks, and pro-
vide an independent chronology extending over the age
range 30 to 660 ka. Their data are summarised in Fig. 10.
Despite a very large correction to dose rates arising from
a modern water content of around 100%, the agreement
with the independent evidence is good. The unusually
large age range for such fine-grained sediments can be,
at least in part, attributed to the low dose rate, of about
1 Gy ⋅ ka-1.
In a study of an early human occupation site in south
western Australia, Turney et al. (2001) report a compari-
son of a number of charcoal 14C ages with 5 OSL quartz
ages based on small aliquots (~eighty 100 mm grains per
aliquot; preheats in the range 160 to 300° C). The sedi-
ment is aeolian, but was probably washed into the cave
site during periods of exceptionally heavy rainfall. Only
one pair of ages is in the age range usually regarded as
reliable for 14C (layer 9 at 239 to 249 cm; 24.93±0.34 14C
years BP [28±2 ka after calibration] and OSL 25.5±1.4
ka). Although the older ages obtained using conventional
pretreatments showed clear evidence of the ‘radiocarbon
barrier’ (Roberts et al., 1994), those obtained using a new
acid-base-wet-oxidation pretreatment with stepped com-
bustion (ABOX-SC) provided ages beyond 40 ka. Two of
these, at 41.5±1.3 and 46.7±1.9 14C ka BP, can be directly
compared with OSL ages of 44.4±2.1 and 47.1±2.6 ka.
Turney et al. (2001) suggest that these 14C ages can be
 A.S. Murray and J.M. Olley
calibrated by the addition of 1 to 2 ka, based on Kitagawa
and van der Plicht (1998) and Voelker et al. (1998).
Freshwater – Tanaka et al. (2001) have worked with
river terrace samples from the Kanto Plain in Japan, us-
ing preheating for 10 s at 240° C. At one site age control
was provided by the Nakadaichi tephra (55-60 ka,
Yamagata site), and their SAR age of 55.6±1.3 ka, calcu-
lated using the present day water content, was in good
agreement with this. Roberts et al. (2001) reported an
OSL age of 55±9 ka for sediments from Mammoth cave,
Australia, which were bracketed by flowstones with
230
Th/234U ages of 44.4±1.3 ka (above) and 55.2±2.2 ka
(below). They also reported 230Th/234U ages from two
other sites which were stratigraphically concordant with
OSL dates.
Marine – Larsen et al. (1999) present one comparison
from their Trepuzovo site, where an (uncalibrated) 14C
age on wood (Picea twigs) gave 42.6±1.5 ka BP, compared
with an OSL age of 54±4 ka for the surrounding marine
sand unit.
Stokes et al. (2001) have reported a set of 3 older OSL
ages in their study of a marine core from the Indian Ocean
discussed above. Fig. 9 shows that these older ages are
in good agreement with the independent age model,
although there is a slight systematic tendency to underes-
timate the independent age.
Fig. 10. Comparison of OSL ages from silt-sized quartz grains
with an independent tephra chronology (Watanuki et al.,
submitted). The tephra ages are based on 14C and fission track
dating. Unusually high water contents (around 100%)
contributed to the low dose rates of about 1 Gy.ka-1.
11
Sigaard et al. (unpublished) have obtained two dates
on a mixed pebble and sand unit near Ejby on Zealand,
Denmark; they identified this as an Eemian beach deposit
(assigned an age of between 115 and 129 ka by compari-
son with oxygen isotope stage 5e). The average OSL age
obtained for this unit was 135±8 ka. Mangerud et al.
(2000) discuss two sites in northern Russia with deposits
identified as Eemian. They give three OSL dates, of
111±12, 97±7 and 64±6 ka at site Sula 22, from a shal-
low marine unit 8 to 9 m thick. A similar 3 m thick Eemian
deposit was identified at the adjacent site Sula 21, and this
gave two OSL dates of 104±11 and 91±15 ka. These
two sites are only 4 km apart, and Mangerud et al. (2000)
consider the correlation between the two clear. The
unweighted average OSL age is 93±9 ka (101±5 ka
excluding the 64 ka outlier).
Murray et al. (unpublished data) have sampled an ex-
tensive sequence of Eemian marine sediments near
Gammelmark, in Jutland, Denmark. The sequence is
about 12 m high, and grades from clean sand in the upper
layers to clayey silt at the bottom. Late Saalian freshwa-
ter sediments underlie the sequence. There was no ap-
parent trend in the SAR OSL ages with depth, and all 24
ages are summarised in Fig. 11. The unweighted mean
age (excluding the two outliers, and including uncertain-
ties arising from systematic sources) is 119±7 ka, with an
overall relative sample standard deviation of 8% (these
data are also discussed in Murray et al., 2002). This vari-
ability should be compared with the average relative stan-
dard deviation based on the individual estimates of un-
certainty on each age, of 5% (calculated by averaging the
individual variances), and suggests that the internally
derived uncertainties are slightly underestimated. This
may be connected with the two results (out of 24) which
are clearly anomalous, underestimating the known age by
about 40%. The authors have evidence that this underes-
timate arises from a dose-rate anomaly, possibly because
of radionuclide redeposition occurring as the sand cliff is
Fig. 11. Distribution of dates (obtained using a preheat of
260o C for 10 s) from 24 samples of Eemian coastal marine
sand taken from a coastal cliff section near Gammelmark, south
east Jutland. There was no systematic change in age with depth
in the section, and the unweighted mean is 119±7 ka (n=22,
i.e. excluding the lowest two ages).
 PRECISION AND ACCURACY IN THE OPTICALLY STIMULATED LUMINESCENCE DATING...

eroded back by storm action. It is clearly possible that simi- only a few comparisons in the range between about 50 ka
lar but smaller and undetected variations in dose rate with and 125 ka (because of the lack of reliable independent
time could contribute to the observed scatter in the ac- ages), and the data from beyond about 125 ka are all from
cepted ages. It is also interesting that the gross underesti- one study (Watanuki et al., unpublished). The average
mation observed here is similar to that found for one ratio of the OSL to independent ages is 0.984±0.016
sample by Mangerud et al. (2000) reported above; this (n = 52) unweighted, and 0.978±0.009 weighted (both
sample was also recovered from a retreating sediment omitting the freshwater result of 3.1±0.4 at 300 years).
face. Nevertheless, individual points are not all statistically
Glaciofluvial/glaciolacustrine – As part of his study of consistent with the line of unit slope. This can be seen
the deglaciation history of Denmark, Houmark-Nielsen more readily in the upper part of the figure, where the
has obtained several SAR quartz OSL ages with good 14C OSL/independent age ratios are shown; 5 out of the 53
age control. The samples come from a variety of locations, results lie more than 3 standard deviations from unity.
and all the older samples are from lacustrine muds and Even ignoring the result of 3.1±0.4 at 300 years (because
sands. These results are summarised in Table 2, together the source of error in this case is known to be incomplete
with the two younger samples discussed earlier; the agree- bleaching), it can be concluded that uncertainties in the
ment between OSL and the independent chronology is ratio of OSL to independent age are underestimated in
satisfactory, although there may be a small systematic some cases. Unfortunately it is difficult to deduce where
discrepancy. the error lies – in the measurement of the independent
estimate of age, in the association of this age with that
8. DISCUSSION of the sedimentary horizon, or in the luminescence age
itself.
Fig. 12 and Table 3 summarise all the non-modern age
comparisons discussed above. In order not to bias the data
towards multiple OSL ages with a single independent age
control (e.g. the 22 results from Gammelmark; Murray et
al., unpublished) results from a single horizon at a given
site have been averaged (the number of ages is given in
the column labelled (n) in Table 3). Those comparisons
where the relationship with the age control is poorly de-
fined have also been omitted (e.g. Rich and Stokes, 2001).
The older uncalibrated 14C ages of Turney et al. (2001)
have been calibrated approximately by adding 1.5±1.0 ka
to the uncalibrated data (based on Kitagawa and van der
Plicht, 1998, and Voelker et al., 1998). The data are shown
with logarithmic axes; the inset to the lower graph shows
the same data using linear axes.
Because of the logarithmic axes, the modern results
have been omitted from the figure. However, it is inter-
esting to note that although there are several average De
estimates (i.e. measured using an large number of grains
in each aliquot) from modern freshwater deposits (e.g.
Stokes et al., 2001), many of which show the expected
evidence for incomplete bleaching, there is only one such
estimate from sediment of known finite age (Wallinga
et al., 2001). This reflects the increasing acceptance that
the study of dose distributions using small numbers of
grains, or even single grains, is the standard method if
incomplete bleaching is suspected.
It is also interesting that in none of the dose distribu-
tion studies of modern sediments (or of young non-mo-
dern sediments) using small aliquots or single grains,
is there any suggestion that the dose distribution approach Fig. 12. Summary of age comparisons from all sites discussed
in this paper. Note the logarithmic horizontal axis. The OSL to
overestimates the known age. Thus we conclude that, at independent age ratios are shown in the top part of the figure,
least in the sediment results reviewed here, there were and the inset shows the age data using linear axes. Samples
always some grains that were completely bleached when of known modern (i.e. zero ) age are not shown. One other
compared to a time scale of years to decades. comparison has been omitted – from Larsen et al. (1999) –
Turning now to Fig. 12, it is clear that there is no evi- because the 14C age of 42.6±1.5 ka involved conventional
pretreatment and is uncalibrated. Two other pairs, from Wallinga
dence for any systematic difference between the OSL ages et al. (2001; see Figure 8), are omitted from the upper part of
and the independent age estimates over the entire age the diagram only, because the independent age (1.54±0.84 ka)
range – although it must be acknowledged that there are is poorly known.

12
 A.S. Murray and J.M. Olley

Nevertheless, some comment can be made on the lu-
minescence ages. Combined uncertainties range from
50% (Olley and Taylor, unpublished) to 2.3% (Stokes
et al., submitted). Six out of the 53 results are assigned
combined uncertainties of 3% or less by their authors (not
including the effects of averaging). It is of concern that
only limited information is available on uncertainty analy-
sis in some of the data sets reviewed here; in particular,
a discussion of the analysis of random and systematic
sources of uncertainty is often missing. This is despite two
well-known early publications (Aitken and Alldred, 1972;
Aitken 1976; both summarised in Aitken, 1985) which
outline these contributions, and discuss methods for com-
bining them in the final age. In any comparison of lumi-
nescence ages with independent dating results, it is very
important that the uncertainties on the luminescence ages

Table 3. Summary of all age comparisons used in Figure 12.

Aliquot and Preheat, 10 s OSL Age Independent
Class (n) Reference
grain size [ oC] [ka] Age [ka]
Aeolian l, c 240-280 0.29±0.02 1 0.35±0.03 Strickertsson and Murray, 1999
l, c 160-260 0.71±0.05 1 0.669 Bailey et al., 2001 & pers. comm.
l, c 260 13.00±0.7 3 13.155 Radtke et al., 2001
l, c 260 11.2±1.3 1 13.155 Hilgers et al., 2001
l, c 260 13.1±0.9 2 13.45±0.3 Hilgers et al., 2001
l, c 260 12.6±0.7 1 12.0±0.3* Mangerud et al., 1999
l, c 260 14.6±1.2 1 14.3±0.5* Mangerud et al., 1999
l, c 160-280 4.23±0.1 6 4.31±0.07 Murray and Clemmensen, 2001
l, c 160-280 2.7±0.3 1 2.81±0.02 Murray and Clemmensen, 2001
l, c 160-280 2.0±0.2 1 2.00±0.05 Murray and Clemmensen, 2001
l, c 160-280 0.92±0.04 4 0.87±0.04 Murray and Clemmensen, 2001
l, f 240 93±10 1 98±9 Watanuki et al., 2002
s,c 160-300 25.5±1.4 1 28±2* Turney et al., 2001
s,c 160-300 44.1±2.1 1 43±2* Turney et al., 2001
s,c 160-300 47.1±2.6 1 48±2* Turney et al., 2001
l, f 240 215±22 1 170±20 Watanuki et al., 2002
l, f 240 311±33 1 290±60 Watanuki et al., 2002
l, f 240 296±39 1 290±30 Watanuki et al., 2002
l, f 240 308±36 1 290±70 Watanuki et al., 2002
l, f 260 53±3 1 51±1 Watanuki et al., 2002
l, f 260 145±12 1 135±15 Watanuki et al., 2002
Fluvial s, c 200 67±5 a 1 70 a Olley et al., 1998
l, c 240-280 13.6±1.1 1 14.3±0.1 Strickertsson and Murray, 1999
l, c 240-280 9.0±0.6 2 12±0.3 Strickertsson and Murray, 1999
s, c 200 0.92±0.10 1 0.3 Wallinga et al., 2001
s, c 200 1.49±0.10 1 1.54±0.84 Wallinga et al., 2001
s, c 200 5.62±0.35 1 5.62±0.41 Wallinga et al., 2001
s, c 200 13.26±0.8 1 13.24±0.07 Wallinga et al., 2001
sg 220 70±8 a 1 63±8 a Olley and Hancock (unpub.)
sg 220 170±20 a 1 128±10 a Olley and Hancock (unpub.)
s, c 220 29±15 a 1 42 a Olley and Taylor (unpub.)
l, c 260 13.6±1.0 1 13.9±0.5 Houmark-Nielsen (Table 2)
l, c 260 13.8±0.9 1 14±0.5 Houmark-Nielsen (Table 2)
l, c 260 13.7±1.1 1 11.1±0.3 Larsen et al., 1999
l, c 240 55.6±1.3 1 58±2 Tanaka et al., 2001
s, c 160-300 55±9 1 49.8±4 Roberts et al., 2001
Marine l, c 240-280 25.3±1.8 1 24±2 Strickertsson and Murray, 1999
l, c 240-280 14.9±0.6 3 17.2±0.4 Strickertsson and Murray, 1999
l, c 240-280 17.3±1.5 1 16.2±0.7 Strickertsson and Murray, 1999
l, c 260 119±7 22 122±7 Murray et al. (unpub.)
l, c 260 135±8 2 122±7 Sigaard et al. (unpub.)
l, c 260 101±4 4 122±7 Mangerud et al., 1999
l, f 200, 240 7.31±0.18 1 7.50±0.09 Stokes et al., 2002
l, f 200, 240 22.1±0.4 1 20.0±0.12 Stokes et al., 2002
l, f 200, 240 36.3±0.8 1 43±2 Stokes et al., 2002
l, f 200, 240 67±2 1 71±4 Stokes et al., 2002
l, f 200, 240 117±3 1 128±6 Stokes et al., 2002
Glacial l, c 260 30±2 1 33±2 Houmark-Nielsen (Table 2)
l, c 260 29±2 1 32±3 Houmark-Nielsen (Table 2)
l, c 260 30±3 1 33±1 Houmark-Nielsen (Table 2)
l, c 260 26±2 1 32±2 Houmark-Nielsen (Table 2)
l, c 260 29±2 1 30±2 Houmark-Nielsen (Table 2)
l, c 260 28±2 1 27±1 Houmark-Nielsen (Table 2)
Note: 1. Aliquot size: l - large, s - small, sg - single grain. Grain size, c - coarse, f - silt.
2. (n) is the number of OSL ages included in the average given.
3. * indicates radiocarbon age calibrated by the present authors.

13
 PRECISION AND ACCURACY IN THE OPTICALLY STIMULATED LUMINESCENCE DATING...
include contributions from all known components, includ-
ing uncertainties arising from systematic effects (of course
the same applies to the independent ages, but such pro-
blems are outside the scope of this paper). Some sources
of error that are difficult to avoid (given the methods used
in the papers reviewed here) include conversion from
concentration data to dose rate (estimated at ~3%), abso-
lute calibration of concentration measurements (~3%),
beta source calibration (~2%), and beta attenuation fac-
tor (~2%). These estimated values are of course approxi-
mate, but it should be clear that it is difficult to obtain
a luminescence age with an overall or combined standard
uncertainty of much less than 5%. This is especially true
when it is remembered that other sources of systematic
errors, such as those associated with water content and
cosmic ray contribution, have not been considered in this
discussion because they are site dependent, and that
uncertainties arising from random errors also contribute
to the combined standard uncertainty. It is also intere-
sting to note that if a relative uncertainty of 5% is added
in quadrature to all the OSL ages, only one OSL/inde-
pendent age ratio (0.750±0.065 at 12 ka) lies more than
3 standard uncertainties from unity (again not including
the result of 3.1±0.4 at 300 years, because the source of
error is known).
In the past, any uncertainties arising from systematic
errors have tended to be swamped by those arising from
random errors, especially errors associated with measure-
ment of De. Now that precisions on the mean De of <<5%
are possible using SAR, it is very important that full
attention is given to the uncertainties arising from system-
atic effects – increasingly these will limit the combined
uncertainty in a luminescence date. Only then will it be
possible to determine whether the apparently significant
deviations of the type shown in Fig. 12 are simply
a result of the underestimation of the effects of known
sources of error, or whether they reflect a hitherto uni-
dentified source.
9. CONCLUSIONS
There is now a considerable number of comparisons
available between quartz SAR ages and independent age
control, from a variety of aeolian and water-lain sedi-
ments. These very encouraging results confirm that the
method has a wide application to many classes of trans-
ported material. Incomplete bleaching is very unlikely
to give rise to significant errors in aeolian and coastal
marine sands, but it can be of significance in Holocene
studies of fluvial deposits. However, there is no evidence
for significant systematic effects in ages older than about
20 ka, even from fluvial or glacio-fluvial systems, and this
should be borne in mind when examining dose distribu-
tions in older sediments.
Nevertheless, when due allowance has been made for
incomplete bleaching, there remain two or three indi-
vidual results that are clearly inconsistent with the ex-
pected results, and these point the way to more detailed
future investigations, especially of dose rates. It is clear
that these occasional failures reinforce what is, in any case,
14
good field practice – that several samples, stratigraphically
connected in both horizontal and vertical planes, should
be dated from every site. This minimises the risk of unde-
tected gross errors.
It is also strongly recommended that more detailed
attention should be paid to formal uncertainty analysis.
It has long been recommended good practice in lumine-
scence dating to report both the combined standard
uncertainty, assessed in a justified way, and (separately)
the component arising from systematic effects; unfortu-
nately this is very rare. With the increased precision ava-
ilable from the SAR protocol, such detailed error analy-
sis is essential if the reporting of unreasonably small un-
certainties is to be avoided. We stress that determination
and reporting of the uncertainties associated with an age
estimate is as important as the determination of the age.
ACKNOWLEDGEMENTS
The authors wish to thank all our colleagues who
allowed us access to unpublished data, especially Stephen
Stokes. Andrzej Bluszcz drew our attention to the NIST
Guidelines (Taylor and Kuyatt, 1994) and made several
suggestions for ensuring that our statistical terminology
was consistent with recommended practice. Ann Wintle
and Jakob Wallinga also offered valuable criticism of the
manuscript.
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PRECISION AND ACCURACY IN THE OPTICALLY STIMULATED LUMINESCENCE DATING...

16
 GEOCHRONOMETRIA Vol. 21, pp 17-26, 2002 – Journal on Methods and Applications of Absolute Chronology

ON THE DETECTION OF OSL AGE OVERESTIMATION

USING SINGLE-ALIQUOT TECHNIQUES

JAKOB WALLINGA
Netherlands Centre for Luminescence dating (NCL) IRI Delft University of Technology,
Mekelweg 15, NL-2629 JB Delft, Netherlands
E-mail: j.wallinga@iri.tudelft.nl, Phone: +31 (0)15 278 1056, Fax: +31 (0)15 278 9011

Key words
words: Abstract: Optically stimulated luminescence (OSL) dating is a quantitative dating method
OSL DATING, to determine the time of last exposure of sand and silt to (sun) light. However, insufficient
POOR BLEACHING, resetting of the optically stimulated luminescence signal prior to sediment deposition can
SINGLE ALIQUOTS, result in overestimation of the age of a sample. Therefore detection of so-called poor bleach-
EQUIVALENT DOSE ing is of prime importance in OSL dating. Several methods proposed in the literature for
detection of poor bleaching are based on the scatter in equivalent doses obtained by single-
aliquot methods. In this paper numerical simulations are used to assess the validity of these
methods. The simulations show that scatter in equivalent doses is largely dependent on the
number of grains contributing to the luminescence signal of each aliquot, and proportion of
poorly-bleached grains in the mixture under study. Thresholds for detection of poor bleach-
ing based on inter-aliquot scatter in equivalent doses are therefore not valid. It is concluded
that tight, symmetrical dose distributions obtained on small aliquots (ultimately consisting of
a single grain) provide the best indication that the sample is homogeneously bleached.

1. INTRODUCTION time, as a result of exposure to ionising radiation from

The luminescence properties of quartz and feldspar
grains can be used to determine the timing of the last
exposure of sand and silt to (sun) light. Luminescence dat-
ing has seen major developments over the last decades,
especially since the development of optically stimulated
luminescence (OSL) dating (Huntley et al., 1985). This
dating technique, also known as optical dating, can pro-
vide absolute ages in the range of decades to over a hun-
dred thousand years, and is now widely applied in the
fields of both geomorphology (reviewed in Aitken, 1998;
Stokes, 1999) and archaeology (reviewed in Roberts,
1997). OSL dating is particularly applicable to deposits
for which the light-sensitive OSL signal in all the grains
has been zeroed by the exposure to sunlight during ero-
sion, transportation, and deposition. If the OSL of some
grains is not fully zeroed, an overestimation of the depo-
sitional age will occur. Thus, to have confidence in the
accuracy of an optical age, it should be shown that the
residual signal at the time of deposition was negligible for
all the grains.
The OSL signal given by a grain is the result of the
optical release of charge trapped in the crystal lattice. This
charge is produced at an almost constant rate through
radioactive nuclides in the environment. The radiation
dose is thus a measure of the burial time. For dating, its
magnitude is determined by laboratory measurements of
the OSL from the mineral grains. Thus derived, it is known
as the equivalent dose. Put together with the measured
environmental dose rate, an optical age can be calculated.
The OSL signal is very quickly zeroed by exposure to
(sun) light, much faster than the thermoluminescence
(TL) signal previously used for dating (Godfrey-Smith
et al., 1988). This has opened the possibility of using OSL
dating for materials that have only been exposed to light
for a short period of time, or that have been exposed only
to light of restricted intensity prior to deposition. Conse-
quently, OSL dating has been used in a wide range of
depositional environments, including fluvial, glacio-
fluvial, marine and colluvial. However, although the OSL
signal is reset quickly, this does not imply that it is always
completely reset at the time of deposition. Light exposure
might have been too short in time, too dim, or too re-
stricted in spectrum due to filtering in, for example, a tur-
bid water column. Alternatively, the trapped charge in the
grains prior to erosion might have been very large com-
pared with that resulting from environmental sources
since deposition. In this case, the OSL signal derived from
 ON THE DETECTION OF OSL AGE OVERESTIMATION ...
a small portion of the former, remaining after even quite
extensive light exposure, can have a large influence on the
value obtained for the equivalent dose (Aitken, 1998).
Serious overestimation of age due to poor bleaching
has been shown in several studies using OSL dating on
feldspar separates (Duller et al., 1995; Lamothe, 1996;
Lamothe and Auclair, 1997; Clarke et al., 1999). For quartz
separates, significant residual OSL signals were shown to
be present for samples from modern glaciofluvial sedi-
ments (Rhodes and Pownall, 1994), and to a lesser extent
for modern fluvial sediments (Stokes et al., 2001).
The most rigorous test for poor bleaching is to com-
pare the optical age with independent age control. How-
ever, these tests assume that: 1) the age control is without
problems, and 2) there are no problems other than poor
bleaching in luminescence dating. Especially for feldspar
separates the latter assumption is questionable, because
problems with anomalous fading (Wintle, 1973; Spooner,
1994) and sensitivity changes (Wallinga et al., 2000) can
lead to an underestimation of age. Hence, an overestima-
tion of age caused by poor bleaching can be masked by
an underestimation of age caused by other mechanisms.
To circumvent these problems, several studies have
sampled modern deposits to investigate the remnant dose
at the time of deposition (Stokes, 1992; Rhodes and
Pownall, 1994; Murray et al., 1995; Olley et al., 1998; Bailey
et al., 2001; Porat et al., 2001; Stokes et al., 2001). How-
ever, luminescence dating is most useful when applied to
deposits of unknown age. Therefore methods to detect
poor bleaching are needed and these should be intrinsic
to the luminescence dating measurements.
2. OBJECTIVES
Although differences in micro-dosimetry can cause
different dose rates on a grain-to-grain scale (Murray and
Roberts, 1997; Olley et al., 1997), it is normally assumed
that ionising radiation produced within a sedimentary unit
is uniform (McFee, 1998; Olley et al., 1999). If such is the
case, grains of the same size and mineral type absorb the
same post-depositional dose acquiring an OSL signal that
represents the trapped charge this produces. The effec-
tive absorbed dose of each grain is then the sum of the
grain-dependent remnant dose at deposition and the uni-
form post-depositional dose. Laboratory procedures for
luminescence dating aim at determining this dose; the best
estimate of this dose is normally referred to as the equiva-
lent dose. Assuming that there is no intrusion of grains
from other layers, the grain with the lowest equivalent
dose is expected to have been a well-bleached grain at
deposition and thus provide the post-depositional dose.
In most optical dating procedures, the OSL signal is
derived from a number of grains that form the sub-sample.
A typical sample disc holds ~5 mg of material; this
amounts to ~1000 grains when a 150 µm grain size is used.
If the sub-samples contain grains with different equiva-
lent doses, scatter will be seen for the luminescence data
derived from both single-aliquot dating procedures
(Li, 1994) and multiple-aliquot procedures (Rhodes, 1990;
Duller, 1994a; Huntley and Berger, 1995). In single-
18
aliquot methods, all measurements required for equiva-
lent dose determination are made on a single sub-sample,
thereby allowing comparison of equivalent doses obtained
on different sub-samples (Duller, 1991). Li (1994) sug-
gested that, using single-aliquot procedures, poorly
bleached samples can be identified because they show
a wide range of equivalent-dose values and an increasing
trend of equivalent dose with natural luminescence inten-
sity. His method of assessment of poor bleaching has been
adopted by Duller (1994a; 1995), Duller et al. (1995), and
Wintle et al. (1995).
Clarke (1996) refined Li’s approach by presenting
threshold values for scatter in equivalent dose (both ab-
solute and fractional), indicating different degrees of
bleaching. Clarke et al. (1999) used the same parameters
to determine whether an OSL age can be considered to
be accurate. Based on empirical studies of aeolian and
fluvial sediments, Clarke et al. (1999) concluded that any
luminescence date not showing significant (relative) scat-
ter in equivalent doses is accurate.
Colls et al. (2001) use the correlation between equiva-
lent dose and natural OSL intensity of aliquots as indica-
tion for poor bleaching. They classify samples as poorly
bleached when a statistically significant correlation be-
tween these attributes is found. The statistical significance
of the correlation is tested by a one tailed student’s t-test
on the test statistic
tcalc = R(n-2)/(1-R2), (2.1)
where R is the Pearson’s correlation coefficient for the
normalised equivalent dose and the natural OSL inten-
sity of the aliquots, and n is the number of aliquots.
Samples that do not exhibit an apparent relationship be-
tween signal intensity and equivalent dose are regarded
to be well (or at least uniformly) bleached.
A third indication for poor bleaching based on scatter
in single-aliquot equivalent doses is the asymmetry of dose
distributions. This attribute was first suggested by Murray
et al. (1995) as a way of detecting poorly bleached samples.
In this paper the validity is assessed of poor bleaching
detection methods that are based on characteristics of
single-aliquot equivalent-dose distributions. Three differ-
ent methods, proposed by Clarke et al. (1999), Colls et al.
(2001) and Murray et al. (1995), are tested using numeri-
cal simulations of equivalent-dose distributions of poorly
bleached samples.
3. COMPUTER SIMULATIONS
A simple model was constructed to study the influence
of grain-to-grain variations in equivalent dose on the scat-
ter in equivalent doses obtained for aliquots containing
multiple grains. In this model virtual samples with a char-
acteristic dose distributions are created. Different sub-
samples from this virtual sample are taken, and the model
used to calculate what equivalent dose would be obtained
on this sub-sample when a single-aliquot procedure had
been applied. Three factors control the equivalent dose
that is obtained for each grain. Firstly, its intrinsic sensi-
 J. Wallinga
tivity with regard to luminescence emission per unit dose.
Secondly, the remnant dose that it had at the time of depo-
sition and, lastly, the post-depositional dose (i.e. the dose
that one wishes to obtain as the equivalent dose). Incor-
poration of the three factors in the model is briefly dis-
cussed below.
Sensitivity. Feldspar and quartz grains have been
found with a wide range of intensities (Lamothe et al.,
1994; Murray and Roberts, 1997; McFee and Tite, 1998).
Even for the most uniform sand-sized quartz separates
studied so far, 80% of the signal comes from only 30%
of the grains, thereby being far from the ‘ideal’ of all grains
contributing equally (Duller and Murray, 2000; Duller
et al., 2000). In the current computer simulation, the
brightness distribution of the test-dose response of 891
grains of quartz sample TNE9503 was used (sample de-
scription and methodology can be found in Duller et al.,
2000). The intrinsic OSL response (taken as the initial
signal minus the signal observed at the end of stimula-
tion) of a grain to the test dose is referred to as its bright-
ness index (Bi); the average response was 1089 counts. For
20% of the grains no OSL decay was observed during
stimulation, and it is assumed that these grains do not have
any luminescence sensitivity; their brightness index was
set to zero. Two grains where rejected because the OSL
signal appeared to increase during measurement, which
would result in a negative brightness. Sample TNE9503
was chosen for several reasons: Firstly, the test-dose lu-
minescence response of a large number of grains was
measured. Therefore, the brightness distribution (shown
in Fig. 1) forms a true reflection of the variability of the
sample. Secondly, the brightness distribution of this
sample lies in the middle of those observed for quartz
separates, and is therefore most likely to be representa-
tive for quartz in general (Fig. 1). Finally, the distribu-
tion is similar to that obtained on feldspar sample GDNZ1
Light sum (%)
(Fig. 1, previously described by Duller (1994b)), which
makes the simulations described in this paper relevant to
both quartz and feldspar samples. It should be noted that
the brightness distribution for feldspar separate GDNZ1
was obtained with blue stimulation, but it is assumed that
a similar distribution would be obtained with infrared
stimulation.
Remnant dose. The equivalent dose that would be
obtained if grains had been measured at the time of depo-
sition (remnant dose, Dr,i) is most likely to be highly vari-
able, depending upon the original nature of the deposit
from which the grain was derived and the type and dura-
tion of transport. For the computer simulations, four types
of original deposit were postulated, having received doses
of 5, 50, 100 and 1000 Gy respectively. To allow for varia-
tions in light exposure during transport, it was assumed that
the grains would have had their OSL bleached to some
percentage of the original value. A top hat probability dis-
tribution was used, with equal probability of reducing the
OSL signal by any fraction between 0 and 100%.
Post-depositional dose. All grains were specified to
have received a post-depositional dose of 50 Gy (Dt).
For any particular grain (i), the total absorbed dose
(De,i) will be the sum of the post-depositional dose (Dt)
19
and the remnant dose (Dr,i). In order to use the same lingo
in this paper as in applied studies, the total absorbed dose
is referred to as equivalent dose here, although it is
realised that the latter normally refers to the laboratory
estimate of the former. For every grain in an aliquot, the
natural luminescence intensity (Ii) is calculated by multi-
plying the equivalent dose by the brightness index (Ii =
De,i . Bi). A linear relationship between dose and lumi-
nescence signal is assumed in this calculation. From the
attributes assigned to each grain, it is possible to calcu-
late the equivalent dose that would be obtained for an
aliquot containing a fixed number of grains; the simula-
tion is carried out for aliquots consisting of 1, 5, 10, 100
and 1000 grains. The equivalent dose of an aliquot (a)
holding n grains (De,a), is given by the summed natural
luminescence intensity from all the grains on the aliquot,
divided by the summed brightness index of all the grains
on the aliquot (De,a = Σ I1,n / Σ B1,n). For each sample,
18 aliquots were simulated.
A second computer simulation was carried out, in
which 90% of grains were constrained to have been well
bleached at deposition. The remaining 10% of grains were
assigned a remnant dose as in the previous simulation,
and all grains were assigned a post-depositional dose of
50 Gy as in the previous simulation. Once again grains
were picked at random to produce an aliquot with the
desired number of grains (1 to 1000).
100
80
60
40 Quartz TNE9503 (n = 891)
K-Feldspar GDNZ1 (n= 405)
Quartz BA14 (n = 324)
20 Cal. Quartz (annealed, n= 405)
0
0 20 40 60 80 100
Proportion of grains (%)
Fig. 1. Brightness distribution of single grains of quartz and
feldspar. The OSL response was measured in the Risø TL/OSL
reader with single grain attachment (Bøtter-Jensen et al., 2000),
after administration of a uniform laboratory ionising dose
and subsequent preheating. The data for this graph was kindly
supplied by Geoff Duller of the University of Wales, Aberystwyth
(UK). The brightness distribution of quartz sample TNE9503
is used in the computer simulations described in this paper.
Its brightness distribution is similar to that obtained on feldspar
from sample GDNZ1, and lies in the middle of the range of that
obtained on other quartz samples (BA14 and calibration quartz).
Sample descriptions can be found in Duller et al. (2000) and
Duller (1994b), for the quartz and feldspar samples,
respectively.
 ON THE DETECTION OF OSL AGE OVERESTIMATION ...

4. SIMULATION RESULTS
For each scenario, the simulation described in the pre-
vious section was carried out ten times. Results are pre-
sented in Table 1 for the simulations where all grains are
poorly bleached, and in Table 2 for the simulations where
10% of grains are poorly bleached. The values shown in-
dicate the mean of the ten simulations, and the standard
error on the mean. The percentage offset from the post-
depositional dose (50 Gy) is indicated; samples for which
the contamination with poorly bleached grains results in
an offset in the equivalent dose of less than 7.5% are re-
garded as well bleached. Samples for which the equiva-
lent dose is overestimated with 7.5% or more (De ≥ 53.75)
are interpreted as poorly bleached, and the percentage
offset is printed in bold type-setting in Tables 1 and 2.
Suggested indicators for poor-bleaching are also
summarised in the Tables, where the values above sug-
gested thresholds for poor bleaching are printed in bold
type-setting. The indicators shown are: 1) the fractional
error in the equivalent dose (SN = s/De,av , threshold for
poor bleaching: SN>0.10, Clarke et al., 1999); 2) the
squared Pearson’s correlation coefficient for the trend in
the equivalent dose versus natural aliquot intensity (Colls
et al., 2001, for 18 aliquots the threshold for poor bleach-
ing is R2 > 0.16); 3) the skewness of the equivalent dose
distribution
simulation results (Table 2, Fig. 3) show that this type of
contamination will result in larger scatter between aliquots
for scenarios with a similar offset in equivalent dose.
5. VALIDITY OF POOR-BLEACHING DETECTION
METHODS
Relative scatter in equivalent dose
Using the relative-scatter criterion (S N >0.10;
Clarke et al., 1999), samples from the first simulation (all
grains poorly-bleached) are properly classified as poorly
bleached when aliquots consist of 10 grains or less
(Table 1 and Fig. 2, scenario I-III). However, when
aliquots are larger the method fails because grain-to-grain
variations in equivalent dose are averaged within the
aliquots. When the majority of the grains is well-bleached
the method is slightly more successful, being able to de-
tect severe offsets due to poor bleaching even in relatively
large aliquots (Table 2 and Fig. 3, scenario IV and V).
Some recent publications have suggested that the ab-
sence of scatter in equivalent doses obtained on single
aliquots is a guarantee that the sample under study is well
bleached (Clarke, 1996; Clarke et al., 1999). However, the
simulations discussed in the present paper clearly show

Σ( ) 3
n De, a - De, av
skewness = (n-1)(n-2) s (4.1)

where n is the number of aliquots). No threshold for poor

bleaching based on the skewness of the distribution has
been suggested in the literature. Table 1. Summary of results of poor-bleaching tests for the first
For graphical presentation, the equivalent dose of each simulation (all grains poorly bleached, scatter plots in Fig. 2).
simulated aliquot (De,a) and the natural luminescence No.=number of grains per aliquot.
intensity of each aliquot (Ia) are normalised to the sample No. Scen. Previous dose 5 Gy (Scenario A)
average. The resulting normalised equivalent dose (De,a (N)) Fig.2 Offset De [%] SN R2 Skew
and normalised natural OSL signal (Ia (N)) of a single 1 I 4.5 + 0.1 0.03 + 0.00 0.01 + 0.01 0.25 + 0.11
simulation for each scenario, are presented in a scatter 5 II +
5.3 0.3 0.02 + 0.00 0.00 + 0.01 -0.32 + 0.12
plots as suggested by Clarke (1996) and Clarke et al. 10 III 4.8 + 0.1 0.02 + 0.00 0.02 + 0.00 -0.05 + 0.13
(1999). Results of a single run of the first (all grains poorly 100 IV 5.0 + 0.1 0.01 + 0.00 0.00 + 0.00 0.14 + 0.13
bleached) and second (10% of grains poorly bleached) 1000 V 5.0 + 0.0 0.00 + 0.00 0.00 + 0.00 -0.01 + 0.21
simulation experiment are shown in Figures 2 and 3, Previous dose 50 Gy (Scenario B)
respectively. The group average equivalent dose (De, av) 1 I 48 + 2 0.20 + 0.01 0.01 + 0.01 0.10 + 0.12
and standard deviation (s) are also shown on the plots. 5 II 51 + 2 0.15 + 0.01 0.01 + 0.02 0.03 + 0.15
The influence of the number of grains per aliquot on the 10 III 51 + 2 0.12 + 0.00 0.02 + 0.01 0.00 + 0.17
degree of scatter is shown in scenario I-V displayed down 100 IV 49 + 1 0.06 + 0.00 0.05 + 0.02 0.08 + 0.26
the page in increasing aliquot size, whereas the influence 1000 V 50 + 1 0.02 + 0.00 0.15 + 0.04 0.22 + 0.16
of the value of the previous dose is shown in scenario Previous dose 100 Gy (Scenario C)
A-D. Dose distributions from selected scenarios are also 1 I 96 + 5 0.30 + 0.02 0.01 + 0.01 0.00 + 0.19
presented as weighted histograms in Fig. 4. 5 I 103 + 4 0.23 + 0.02 0.04 + 0.02 -0.12 + 0.16
The first simulation (Table 1, Fig. 2) shows that, for a
10 III 98 + 3 0.19 + 0.01 0.06 + 0.03 -0.07 + 0.09
sample where all the grains are poorly bleached, inaccu-
100 IV 99 + 2 0.11 + 0.01 0.12 + 0.03 -0.02 + 0.19
racy of the equivalent dose as a consequence of poor
1000 V 100 + 1 0.04 + 0.00 0.10 + 0.04 0.14 + 0.19
bleaching will only show as scatter if small aliquots are
Previous dose 1000 Gy (Scenario D)
used, or if the previous dose is large compared to the post-
1 I 950 + 56 0.58 + 0.04 0.02 + 0.02 0.14 + 0.18
depositional dose. When the aliquot consists of 100 or
5 II 976 + 25 0.39 + 0.02 0.08 + 0.03 0.04 + 0.11
more grains (scenario IV and V), the equivalent dose is
10 III 971 + 22 0.36 + 0.02 0.09 + 0.03 -0.14 + 0.14
largely averaged within each aliquot. In the second simu-
lation, the vast majority of the grains are well bleached, 100 IV 975 + 13 0.20 + 0.01 0.09 + 0.03 -0.15 + 0.13
and only 10% of the grains contain a remnant dose. The 1000 V 994 + 9 0.06 + 0.00 0.25 + 0.04 -0.20 + 0.16

20
 J. Wallinga

that the scatter observed is largely dependent upon the the simulations show that the type of mixture of well
number of grains that contribute to the luminescence sig- bleached and poorly bleached grains affects the scatter; a
nal of each aliquot. This result accords with that of previ- lesser abundance of contaminating grains results in
ous studies. When first proposing the use of scatter for greater scatter in equivalent doses obtained. Hence, para-
detection of poor-bleaching, Li (1994) already showed doxically, poor-bleaching is more easily detected when it
that the degree of scatter in equivalent doses obtained for only affects a small percentage of the grains and thereby
single aliquots is dependent on aliquot size. Moreover, has a minor influence on the mean equivalent dose.

Increase in previous dose

A B C D
previous dose 5 Gy previous dose 50Gy previous dose 100Gy previous dose 1000Gy
2.0
De,av = 52.4 + 1.6 De,av = 74.2 + 14.4 De,av = 100 + 36 De,av = 439 + 336
1.5
De (N)

I 1.0

0.5
1 Grain 1 Grain 1 Grain 1 Grain
0.0
2.0
De,av = 53.4 + 1.2 De,av = 82.0 + 10.0 De,av = 96.7 + 27.6 De,av = 554 + 180
Increase in number of grains per aliquot

1.5
De (N)

II 1.0

0.5
5 Grains 5 Grains 5 Grains 5 Grains
0.0
2.0
De,av = 52.1 + 0.9 De,av = 70.9 + 8.6 De,av = 102 + 23 De,av = 492 + 196
1.5
De (N)

III 1.0

0.5
10 Grains 10 Grains 10 Grains 10 Grains
0.0
2.0
De,av = 52.5 + 0.4 De,av = 73.0 + 4.6 De,av = 95.3 + 13.1 De,av = 523 + 95
1.5
De (N)

IV 1.0

0.5
100 Grains 100 Grains 100 Grains 100 Grains
0.0

2.0
De,av = 52.4 + 0.2 De,av = 73.4 + 1.7 De,av = 98.7 + 3.5 De,av = 551 + 23
1.5
De (N)

V 1.0

0.5
1000 Grains 1000 Grains 1000 Grains 1000 Grains
0.0
0.0 0.5 1.0 1.5 2.0 0.0 0.5 1.0 1.5 2.0 0.0 0.5 1.0 1.5 2.0 0.0 0.5 1.0 1.5 2.0
In(N) In(N) In(N) In(N)

Fig. 2. Using the model described in the text, equivalent doses and natural intensities are computed for aliquots consisting of grains
picked at random from a poorly bleached virtual sample. Each grain is assigned the OSL sensitivity, as well as the equivalent dose,
which consists of the post-depositional dose (=50 Gy) plus a random percentage of the previous dose. The previous doses are 5, 10,
100 and 1000 Gy for scenarios A, B, C and D respectively. Both the equivalent dose and the natural intensity obtained on each disc
are normalised to the average from 18 discs, to construct normalised scatter plots (Clarke et al., 1999). The mean equivalent dose
(De,av) of the 18 discs is presented on each plot, as well as the standard deviation on the mean. Data are presented for aliquots consi-
sting of 1, 5, 10, 100 and 1000 grains in scenarios I to V. For grains that have no luminescence response, an equivalent dose could
not be calculated. Therefore, these grains are not plotted on the scatter plots with single-grain data (scenario I). Aliquots for which the
normalised intensity or the normalised equivalent dose is beyond the limits of the graph, are indicated by small arrows. Scatter plots
shown here represent one out of the ten model runs for each scenario. Average results of the ten runs are presented in Table 1.

21
 ON THE DETECTION OF OSL AGE OVERESTIMATION ...

Correlation of OSL intensity versus equivalent dose grains. A strong correlation is only to be expected when
Statistically significant correlation between aliquot the OSL sensitivities of the grains are similar, or when
natural OSL intensity and equivalent dose (R2 > 0.16, for large aliquots with a small percentage of poorly bleached
n = 18; Colls et al., 2001) is only found for the simula- grains are dated.
tions where 10% of the grains is very poorly bleached
(Table 2 and Fig. 3, scenario D) and for the simulation Asymmetry of dose distributions
where all grains are very poorly bleached and aliquots The asymmetry of dose distributions as an indication
contain 1000 grains (Table 1 and Fig. 2, scenario D-V). for poor-bleaching of a sample (Murray et al., 1995) is the
The absence of this correlation in the other scenarios is a third method assessed. In this study, the skewness of the
result of the wide spread in intrinsic OSL sensitivities of distribution is used to characterise the degree of asymme-

Increase in previous dose

A B C D
previous dose 5 Gy previous dose 50Gy previous dose 100Gy previous dose 1000Gy
2.0
De,av = 50.0 + 0.0 De,av = 51.7 + 5.9 De,av = 64.7 + 30.9 De,av = 140 + 240
1.5
De (N)

I 1.0

0.5
1 Grain 1 Grain 1 Grain 1 Grain
0.0
2.0
De,av = 50.2 + 0.7 De,av = 51.8 + 4.3 De,av = 55.1 + 20.7 De,av = 86.4 + 104.0
Increase in number of grains per aliquot

1.5
De (N)

II 1.0

0.5
5 Grains 5 Grains 5 Grains 5 Grains
0.0
2.0
De,av = 50.5 + 1.0 De,av = 51.7 + 3.2 De,av = 57.3 + 14.0 De,av = 67.6 + 34.0
1.5
De (N)

III 1.0

0.5
10 Grains 10 Grains 10 Grains 10 Grains
0.0
2.0
De,av = 50.2 + 0.2 De,av = 51.9 + 1.9 De,av = 55.1 + 7.8 De,av = 89.8 + 31.6
1.5
De (N)

IV 1.0

0.5
100 Grains 100 Grains 100 Grains 100 Grains
0.0

2.0
De,av = 50.2 + 0.1 De,av = 52.8 + 1.9 De,av = 55.8 + 3.7 De,av = 109 + 29
1.5
De (N)

V 1.0

0.5
1000 Grains 1000 Grains 1000 Grains 1000 Grains
0.0
0.0 0.5 1.0 1.5 2.0 0.0 0.5 1.0 1.5 2.0 0.0 0.5 1.0 1.5 2.0 0.0 0.5 1.0 1.5 2.0
In(N) In(N) In(N) In(N)

Fig. 3. A simulation similar to Figure 2, with the difference that 90% of the grains in the virtual sample are well bleached, and thus only
contain the OSL signal resulting from the post-depositional dose of 50 Gy. The remaining 10% of the grains is poorly bleached, and
assigned a random fraction of the previous dose as in Figure 2. While the grains are picked randomly from the sample, not all aliquots
contain exactly 10% of poorly bleached grains. Scatter plots shown here represent one out of the ten model runs for each scenario.
Average results of the ten runs are presented in Table 2.

22
 J. Wallinga

try of the distribution around its mean; positive skewness Table 2. Summary of results of poor-bleaching tests for the
indicates a distribution with an asymmetric tail extending second simulation (10% of grains poorly bleached, scatter plots
in Fig. 3). No.=number of grains per aliquot.
towards more positive values. Lepper et al. (2000) pro-
posed a different quantification for asymmetry of a dose- No. Scen. Previous dose 5 Gy (Scenario A)
distribution Fig. 3 Offset D [%] SN R2 Skew
1 I 0.50 + 0.22 0.01 + 0.00 0.00 + 0.01 1.9 + 0.5
Asymmetry = (De, max – De, mode)/(De, mode – De, min) (5.1)
5 II 0.55 + 0.13 0.01 + 0.00 0.02 + 0.02 2.6 + 0.2
where De, mode is the most frequently occurring equiva- 10 III 0.43 + 0.10 0.01 + 0.00 0.00 + 0.00 2.3 + 0.3
lent dose). However, this quantification was not applicable 100 IV 0.47 + 0.04 0.01 + 0.00 0.00 + 0.00 2.0 + 0.3
for the simulated dataset as the values for De, min and 1000 V 0.50 + 0.03 0.00 + 0.00 0.00 + 0.00 0.77 + 0.15
De, mode were often identical. Previous dose 50 Gy (Scenario B)
The simulations show that the dose distributions are 1 I 4.8 + 0.9 0.14 + 0.02 0.00 + 0.01 3.1 + 0.4
skewed only when the majority of grains in the sample are 5 II 5.2 + 0.8 0.11 + 0.02 0.00 + 0.00 2.7 + 0.2
well bleached (compare results in Table 1 and 2, as well 10 III 4.3 + 0.9 0.08 + 0.02 0.01 + 0.01 2.4 + 0.3
as Fig. 4B and 4C). Moreover, it was found that the skew-
100 IV 4.5 + 0.3 0.04 + 0.01 0.00 + 0.00 1.5 + 0.3
ness of the distribution decreases with aliquot size (see
1000 V 4.9 + 0.2 0.02 + 0.00 0.05 + 0.02 0.8 + 0.2
Table 2). Both findings accord with those made by Olley
Previous dose 100 Gy (Scenario C)
et al. (1999) in their investigation of the use of histograms
1 I 14.0 + 3.0 0.34 + 0.05 0.00 + 0.00 2.8 + 0.4
for detection of poor bleaching. However, where Olley
5 II 8.5 + 1.6 0.21 + 0.04 0.05 + 0.04 2.9 + 0.2
et al. (1999) indicate that the dose distribution will not be
10 III 9.6 + 2.1 0.18 + 0.03 0.01 + 0.02 2.9 + 0.3
skewed when 10% or more of the grains is unbleached,
100 IV 10.7 + 0.7 0.12 + 0.01 0.09 + 0.02 2.4 + 0.2
such contamination is shown to produce skewed distri-
butions in the present simulations. This difference is 1000 V 11.0 + 0.4 0.05 + 0.00 0.06 + 0.03 1.03 + 0.14
caused by the attribution of different OSL sensitivities to Previous dose 1000 Gy (Scenario D)
the grains in the present simulation, where Olley et al. 1 I 109 + 24 1.5 + 0.2 0.21 + 0.08 3.1 + 0.4
(1999) assumed uniform sensitivity for all grains. 5 II 105 + 18 1.2 + 0.1 0.23 + 0.07 2.9 + 0.2
10 III 93 + 16 0.87 + 0.08 0.31 + 0.09 2.4 + 0.1
100 IV 107 + 11 0.52 + 0.06 0.43 + 0.10 1.7 + 0.3
1000 V 97 + 5 0.23 + 0.01 0.71 + 0.03 0.7 + 0.2

16
Frequency

12
8
4
A-1 A-2
0

16
Frequency

12
Fig. 4. Typical equivalent-dose
8 distributions for well bleached
(A) and poorly bleached samples
4 (B and C) presented in histogram
B-1 B-2 plots. The dose distributions used
0 are obtained from the different
simulation scenarios: A) 10% of
16 the grains poorly bleached with a
previous dose of 5 Gy (scenario B
Frequency

in Fig. 3); B) All grains poorly

12 bleached with a previous dose of
50 Gy (scenario B in Fig. 2); C)
8 10% of the grains poorly bleached
with a previous dose of 100 Gy
4
C-1 C-2 (scenario C in Fig. 3). Eighteen
aliquots are used for each
0 histogram; results are shown for
0 25 50 75 100 0 25 50 75 100 aliquots containing 10 (left) and
Equivalent dose (Gy) Equivalent dose (Gy) 100 (right) grains.

23
 ON THE DETECTION OF OSL AGE OVERESTIMATION ...
6. IMPLICATIONS FOR DETECTION OF POOR
BLEACHING
In interpreting the simulation results for suitability of
methods for detection of poor bleaching in real samples,
limitations of the model have to be kept in mind. In the
simulations, the scatter in equivalent doses between
aliquots arises purely from grain-to-grain differences in
the remnant dose. In real samples there will be added
sources for scatter: Firstly, grain-to-grain differences in
micro-dosimetry can result in different post-depositional
doses for the grains. Although these differences are ge-
nerally thought to be small (Olley et al., 1999) they can be
of importance for some samples (Murray and Roberts,
1997; Olley et al., 1997). Especially when small-aliquots
or single-grains are used for equivalent-dose determina-
tion will differences in micro-dosimetry cause added scat-
ter in equivalent doses. Secondly, in real samples there
will be scatter arising from OSL-measurement impreci-
sion resulting from photon-counting statistics. This again
will be particularly the case when small aliquots or single
grains are used. Thirdly, intrusion of grains from other
layers can cause scatter in natural samples.
In ignoring the additive sources for scatter discussed
above, the model provides a minimum estimate for the
scatter in equivalent doses to be found in real samples. In
isolating the scatter caused by poor-bleaching, it fits the
assumptions made in the poor-bleaching detection meth-
ods based on the scatter of equivalent doses resulting from
poor-bleaching. Thereby it creates the ideal circumstances
for the detection of poor-bleaching by these tests. If the
tests are not able to detect such simulated poorly-bleached
samples, they cannot be regarded as reliable tests of poor
bleaching in real samples.
Previous studies have shown it possible to identify
poorly-bleached samples using the scatter in equivalent
doses (Li, 1994; Duller, 1994a; 1995; Clarke, 1996; Clarke
et al., 1999). In view of the results from computer simula-
tions presented in this paper, it is concluded that the
samples investigated in those studies must have fit one
(or both) of the following two criteria: 1) the luminescence
signal from each aliquot was dominated by a small num-
ber of bright grains with different equivalent doses; or 2)
only a small proportion of the grains was poorly bleached.
From the computer simulations it is evident that the ab-
sence of scatter in equivalent doses cannot be interpreted
as an assurance that the sample was well bleached at the
time of deposition.
In applying the correlation method for detecting poor-
bleaching to fluvial quartz separates, Stokes et al. (2001)
found that three out of four samples from the Colorado
River (Texas, USA) showed evidence for partial bleach-
ing, whereas for thirteen samples from the Loire River
(France) only two were classified as poorly bleached.
However, for the Loire River samples, mean equivalent
doses of up to 14 Gy were reported for ‘well-bleached’
samples, whereas a sample from the Colorado River was
classified as poorly bleached, in spite of having an equiva-
lent dose of only 0.23 Gy. Colls et al. (2001) also worked
on Loire samples and found that from 18 samples inves-
24
tigated, five should be classed as poorly bleached. Three
of these were characterised by a single outlier (aliquot
De > 3 SD from the mean) and the remaining two samples
showed extraordinary wide scatter in equivalent doses.
Folz et al. (2001) used a similar method to check for poor-
bleaching in another suite of fluvial quartz from France.
Although OSL ages overestimated the known age by 40%,
no correlation was found between natural aliquot inten-
sity and equivalent dose.
In expecting a correlation between equivalent dose and
natural aliquot OSL signal for poorly bleached samples,
this method assumes that the grains in the sample have
similar OSL sensitivities. This assumption is clearly not
valid (Fig. 1) and it is therefore not surprising that the
method fails to identify poor-bleaching for simulated
(Table 1, 2) and real samples (Stokes et al., 2001). For the
natural samples where the method indicated poor-bleach-
ing, results also showed a wide spread in equivalent doses
or the existence of a single outlier (Colls et al., 2001; Stokes
et al., 2001), which are probably better indications for
poor-bleaching.
Histograms have successfully been used as a means to
visualise the width and the skewness of dose distributions
and to detect poorly bleached samples using small aliquots
(Murray et al., 1995; Olley et al., 1998 and 1999; Lepper
et al., 2000) and single grains (Roberts et al., 2000) of
quartz. Primary limitation of this method is that the dis-
tribution will only be skewed if the majority of the grains
in the sample are well bleached (compare Tables 1 and 2).
Olley et al. (1999), have already pointed this out in their
investigation of the use of this method. Murray and Rob-
erts (1997) found wide, but symmetrical dose distributions
for single-grains from supposedly well-bleached, aeolian
quartz from Australia. The large standard deviation (23%
of the mean) was attributed to differences in micro-do-
simetry. Lepper et al. (2000) discuss ways to deconvolve
the spread in equivalent doses arising from experimental
errors and that from sedimentary processes. They propose
that the correct equivalent dose can be obtained from an
asymmetrical dose distribution after deconvolution.
The dependency of the degree of scatter on the ali-
quot size and on the percentage of poorly bleached grains,
makes the use of thresholds for detecting poor-bleaching
based on inter-aliquot scatter impossible. Although it is
tempting to suggest such thresholds (Clarke, 1996; Clarke
et al., 1999; Colls et al., 2001), they are not generally ap-
plicable, and hence do not provide an objective criterion
for detecting poor bleaching. To improve the chances of
detecting poor-bleaching using methods based on inter-
aliquot scatter in equivalent doses, the aliquot size should
be taken as small as possible, ultimately consisting of a
single grain of sand. One should however keep in mind
that scatter in equivalent doses can also results from other
sources than poor-bleaching, for example differences in
micro-dosimetry. Correlation of aliquot equivalent dose
and natural OSL intensity is the only indicator that per-
forms better for large aliquots; however, it only detects
poor bleaching successfully when poor-bleaching results
in a severe error in the equivalent dose.
 J. Wallinga
A method for visualising scatter in equivalent doses
in relation to its relative error is provided by radial plots
(Galbraith, 1990). This type of plot has recently been used
in studies using small aliquots (Olley et al., 1999) and
single-grains (Roberts et al., 1998; 2000) of quartz. Al-
though a promising method, the validity of radial plots
for detecting poor bleaching is not assessed in this paper
because the simulations do not allow calculation of an
error on individual equivalent-dose determinations.
7. CONCLUSIONS
Scatter in equivalent doses obtained by single-aliquot
OSL dating methods may indicate that the luminescence
signal was not completely zeroed in all grains prior to
deposition. However, the degree of scatter is largely de-
pendent on the number of grains in each aliquot that con-
tribute to the luminescence signal, the percentage of
poorly bleached grains, and the remnant dose in the poorly
bleached grains. For aliquots consisting of a number of
grains, computer simulations indicate that:
1) The absence of scatter in equivalent doses obtained
cannot be taken as assurance that all grains were well
bleached prior to deposition.
2) A correlation of natural aliquot luminescence inten-
sity versus equivalent dose should only be expected for
poorly bleached samples when the luminescence sen-
sitivity of the grains is relatively uniform. Therefore
the absence of such a correlation is not an indication
that the sample was well bleached.
3) Skewed dose distributions are an indication that the
sample contains a small percentage of poorly bleached
grains. A non-skewed distribution can indicate that the
sample is well bleached or that a relatively large per-
centage of grains from the sample are poorly bleached.
The best method to check whether the equivalent dose
of a sample might be overestimated as a consequence of
poor-bleaching is to use small aliquots (ultimately con-
sisting of a single grain), and to look at both the spread in
the equivalent doses and the symmetry of the dose distri-
bution. Tight, symmetrical dose distributions on very small
aliquots indicate that the sample is homogeneously
bleached, but even this does not necessarily mean that its
OSL signal was completely reset during the last transpor-
tation event.
8. ACKNOWLEDGEMENTS
This is a contribution to the NEESDI (Netherlands
Environmental Earth System Dynamics Initiative)
programme, partly funded by the Netherlands Organiza-
tion for Scientific Research (NWO-Grant 750.296.01).
The author is grateful to Geoff Duller for providing the
single-grain brightness distributions, and to Andrzej
Bluszcz for his critical and helpful review. Ann Wintle and
Eddy Rhodes are acknowledged for their useful comments
on earlier versions of the manuscript.
25
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 GEOCHRONOMETRIA Vol. 21, pp 27-32, 2002 – Journal on Methods and Applications of Absolute Chronology

DIVERGENCE IN THE TL DATING RESULTING FROM

DIFFERENT METHODS OF EQUIVALENT DOSE
DETERMINATION

JAROS£AW KUSIAK1, MARIA £ANCZONT1, ANDRZEJ BOGUCKYJ2,

and JÓZEF WOJTANOWICZ1
1
Department of Physical Geography and Palaeogeography, Maria Curie-Sk³odowska University, Akademicka 19,
20-033 Lublin, Poland (e-mail: paleog@biotop.umcs.lublin.pl)
2
Department of Geomorphology and Palaeogeography, Ivan Franko National University,
Doroszenka 41, 290 000 Lviv, Ukraine

Key words
words: Abstract: This paper focuses on problems connected with equivalent dose (ED) estimation.
THERMOLUMINES- The ED results obtained by using two methods: regeneration (R) and total-bleach (TB) were
CENCE DATING, compared. To this end, ten loess samples were taken from about 20 m thick Zahvizdja profile
REGENERATION (western Ukraine).
METHOD, The obtained results show that the ED values are strongly dependent on the applied tech-
TOTAL-BLEACH nique. When using the regeneration method, the maximum ED value observed is 1051±158
METHOD, LOESS, Gy. The total-bleach procedure gives considerably different results, because the gradual
UKRAINE increase of ED values is recorded up to 2833±896 Gy. TL ages obtained by the TB method
were confirmed by palaeomagnetic investigations.

1. INTRODUCTION 2. LOCATION AND DESCRIPTION OF THE

Aeolian sediments such as loess are particularly sui-
table for the application of thermoluminescence dating
method, enabling determination of time passed since the
last exposure to sunlight. Wintle and Huntley (1980) used
this method for the first time in dating of detrital mine-
rals. Since that time several research groups have con-
ducted tests on accuracy, using different techniques of
equivalent dose (ED) determination. The published
materials contain conflicting reports on the reliability of
TL dating and the upper dating limit (e.g. Berger et al.,
1992. Pillans et al., 1996; Frechen et al., 1997 and 1999).
Nowadays, this method also arouses controversies among
the Quaternary geologists, and research works are still
continued to establish a reliable TL sediment-dating
procedure.
In this paper we present the TL dating results for
10 samples from the Zahvizdja loess profile (western
Ukraine). We compare their TL ages obtained by using
two methods of equivalent dose determination: regenera-
tion (R) and total-bleach (TB) methods.
ZAHVIZDJA PROFILE
The studied loess site occurs in the central part of the
East Carpathian Foreland. It is situated to SSE of Lviv,
near Ivano-Frankivs’k (Fig. 1). The East Carpathian
Foreland extends between the Carpathian margin in SW
and the Dnister river valley in NE. Rivers draining this
area rise in the Carpathians. They dissect the Carpathian
Foreland on quite a few flat and wast plateau-ridges which
are mostly covered by fluvial gravels, evidencing old flows
of the Dnister River during the Early Quaternary
(Villafranchien), i.e. when the Dnister valley was form-
ing. These plateau-ridges covered by gravels are termed
the Lojova planation surface. Valley-sides of the Dnister
River and its tributaries have a typical step like arrange-
ment because the Pleistocene terraces occur at different
altitudes. Both the interfluve plateau-ridges and the val-
ley sides are covered with loesses.
The Zahvizdja profile is exposed in a large brickyard
excavation, so spatial extension of its particular elements
could be studied in detail. The profile is connected with
 DIVERGENCE IN THE TL DATING RESULTING FROM DIFFERENT METHODS ...
a high terrace rising about 80 m above the valley floor of
the Bystrycja Solotvyns’ka River. This terrace was formed
as a result of dissection of the Lojova planation surface,
reaching 360-380 m a.s.l.
The profile is about 22 m thick and it is built mainly of
loesses and silty-clayey deposits overlying the marine
Krakowiec clays from the Miocene. Three main litholo-
gical units can be distinguished in the profile. The upper
unit (0-14.5 m) consists of loesses and loess-like deposits;
a paleosol occurs just near the ground surface, because of
exploitation works. The middle unit (14.5-19.0 m) is silty-
clayey, and the lower unit (19.0-20.5 m) is built of fluvial
deposits of channel facies (gravels and sands), and flood
facies (muds). All these sediments are carbonate-free.
A series of eight paleosols of high stratigraphic rank
occurs in the Zahvizdja profile. They represent the Up-
per Eopleistocene and Mesopleistocene (£anczont et al.,
in press).
The upper unit is built of several loess layers separated
by paleosols of forest type, usually with traces of denuda-
tion in their top parts. Stratigraphy of this part of the
Zahvizdja profile was preliminarily defined on the basis
of paleopedological criterion and geomorphologic situa-
tion, and also in relation to the typical loess profiles in
the Podillia (Boguckyj, 1987; Boguckyj et al., 1999). The
stratigraphy of the discussed unit is rather complex. First
two soils from the top of the profile are single ones; they
were connected with the Lublinian (= Rügen) and
Mazovian sensu lato (= Holstein) Interglacials. In the
Ukrainian stratigraphic scheme these paleosols are named
the Korshov = Kaydaki and Sokal = Zavadovka soils.
A very complicated pedocomplex occurs at a depth of 8 m.
It consists of two forest paleosols, the lower of which is
better developed and distinguishable by red illuvial hori-
zon; a thin loess layer or a series of fluvial deposits sepa-
rates these paleosols. This pedocomplex can be correlated
with the Ferdynandowian (= Voigtstedt) Interglacial,
BYELORUSSIA
D
P O L A N
Bu
Kiev
L’viv
Zahvizdja
D nister
M
OL
DO
VIA
ROMANIA
0 100 km Black Sea
28
and it corresponds to the Solotvin = Lubny soil in the
Ukraine.
Nature of the middle unit is different. It is almost
wholly transformed by soil-forming processes, and con-
sists of four paleosols lying in direct succession; the low-
est one is formed on fluvial deposits (flood muds) of the
lower unit. Genetic profiles of these paleosols are well
developed, and their features indicate that they were
formed in wet climate, warmer than the modern one.
However, development periods of the successive soils
were interrupted by cool stages during which strong cry-
ogenic disturbances affected their A and E horizons.
Brunhes/Matuyama paleomagnetic boundary was found
within the illuvial horizon of the third paleosol from the
top of this pedocomplex (Nawrocki et al., in press).
3. METHODOLOGY
TL age (TTL) is obtained from the equation:
TTL = ED/Dr, (3.1)
where equivalent dose (ED) is the laboratory dose which
produces TL corresponding with natural TL in a sample;
annual dose (Dr) is the effective dose received in a unit
of time.
Two methods were used for evaluation of the equiva-
lent dose (ED): regeneration (R) and total-bleach (TB)
techniques. All measurements were carried out on the 45-
63 µm polymineral grain size fraction sieved wet. Possi-
bility of use of similar size fraction was presented by
Wintle (1987) who wrote: „the grain size of loess usually
has a silt (2-63 µm) content of 50-80% and this has re-
sulted in the application of fine grain (4-11 micron) or
intermediate (e.g. 50-56 µm) grain size techniques.”
The obtained aliquots were pre-treated with 10% HCl and
30% H2O2 to remove carbonates and organic material.
Optical bleaching was performed using an UV-lamp
R U S S I A
A zov
a of
Se
Fig. 1. Location of the
Zahvizdja profile.
 J. Kusiak et al.

(Osram Ultra-Vitalux 300 Watt) for 16h (Frechen et al.,
1992). Laboratory irradiations were carried out at the
Institute of Nuclear Chemistry and Technology in War-
saw using a 60Co gamma source. The samples were irra-
diated with 9 additional gamma doses from 300 to 5000
Gy. Unstable thermoluminescence introduced into the ar-
tificially irradiated samples causes underestimation of the
obtained TL ages, so the irradiated samples must be
heated before readout of the TL glow curves (Berger et al.,
1992). Therefore, all aliquots were preheated at 160 oC
for 3 hours. All samples were left at room temperature
for 2 years after irradiation and for at least 3 days after
preheating. The TL glow curves were recorded with use
of the RA’94 TL reader-analyser with the EMI 9789 QA
photomultiplier. Aliquots were glowed out in an argon
atmosphere at a heating rate of 5 oC/sec up to 400 oC. The
optical filter BG-28 (380-500 mm) was used (Berger et al.,
1992). Dose response was calculated with the FIT-SIM
programme of Grün (1994) which is based on the simplex
fitting procedures and analytical error calculation by Brumby
(1992). Plateau test was carried out for each sample.
The annual dose (Dr) was calculated from the formula:
Dr = k a dα + dβ + dγ + dc, (3.2)
where:
dα , dβ , dγ and dc – doses coming from the α, β, γ and cos-
mic radiation, respectively; k = 0.14 – α-efficiency factor
for grains ≤ 10 µm in diameter; a = 0.5 – a correction resul-
ting from the fact that the 45-63 µm grain size fraction
was used.
The alpha particle efficiency can be measured for fine
grain samples using a laboratory alpha source, but the
contribution of alpha particles to grains over 10 µm in
diameter is more difficult to measure but may be esti-
mated – e.g. computer calculations predict that a 50 mm
quartz grain would experience only 50 % of the alpha dose
received within the same sediment by a grain of 10 µm or
less. The beta and gamma doses would be the same for
both grain sizes (Wintle, 1987).
Doses dα, dβ and dγ were calculated on the basis of con-
centration measurements of the natural radionuclides:
40
K, 226Ra, 228Th, with use of the three-channel γ spectro-
meter of MAZAR-95 type, assuming equilibrium in the
decay series. Radionuclide concentrations (in Bq/kg) were
converted to α, β and γ dose rates (in Gy/ka) on the basis
of data published by Aitken (1983). Cosmic dose rate was
determined on the basis of data published by Prescott
and Hutton (1988). Corrections for deposit moisture were
taken after Berger (1988). Average moisture of samples
in the studied profile was 15±5 %.
4. DATING RESULTS
Ten samples were taken from the studied profile for
TL dating: seven from the upper unit and three from the
middle unit. TL ages were obtained for nine samples; age
of a sample from the lowest paleosol was not determined.
The results of TL analysis are presented in Table 1.
The TL age of the first paleosol from the top of the pro-
file (sample Lub-3680 from a depth of 1.0 m) obtained by
the regeneration method (R) is 150±27 ka. It suggests
the Eemian age of this soil. The TL age obtained by using
the total-bleach method (TB) is 234±47 ka, and it indi-
cates that this paleosol was formed in the Lublinian
(= Rügen) Interglacial.
The TL age of Lub-3681 sample (from a depth of 6.0 m)
obtained by using the R procedure (268±42 ka) indicates
that this loess was accumulated during the Odranian (=
Drenthe) Glacial. The TL age obtained by using the TB
method is 532±101 ka, therefore the deposition period
of this loess can be correlated with the Sanian 2
(= Elsterian 2) Glacial. Next sample, Lub-3682, was taken
from a depth of 8.7 m, i.e. from the third paleosol from
the top of the profile. The TL age obtained by using the

Table 1. Results of TL dating.

No. Lab. Depth Annual dose Dr Method Plateau Equivalent dose ED TL age
[m] [Gy/ka] [°C] [Gy] [ka]
3680 1.00 3.660±0.40 R 250-310 550±77 150±27
TB 240-380 856±144 234±47
3681 6.00 3.448±0.26 R 250-300 925±130 268±42
TB 315-400 1831±327 532±101
3682 8.70 2.554±0.23 R 300-400 940±132 368±63
TB 295-370 1497±269 586±117
3683 9.30 3.166±0.41 R 250-400 980±108 310±53
TB 270-400 1969±479 622±174
3684 10.50 2,918±0,36 R 290-360 1051±158 360±68
TB 290-350 1762±460 604±174
3675 12.70 3.356±0.30 R 290-340 940±113 280±42
TB 280-370 2478±669 738±207
3676 13.70 3.376±0.24 R 300-350 1050±221 311±68
TB 310-380 2833±896 839±277
3677 15.30 2.917±0.35 R 300-360 950±105 326±52
TB 295-400 2577±1126 883±398
3678 18.30 3.166±0.38 R 290-350 970±204 306±73
TB 290-400 2386±916 754±301

29
 DIVERGENCE IN THE TL DATING RESULTING FROM DIFFERENT METHODS ...

regeneration technique is 368±63 ka and corresponds to

the Zbójnian (= Domnitz) Interglacial. The TL age ob-
tained by using the total bleach method (586±117 ka)
indicates the Ferdynandowian (= Voigtstedt) Interglacial.
Samples Lub-3683 and Lub-3684 were taken from the
depths of 9.30 and 10.50 m, i.e. from this part of the pro-
file, which occurs between the third and fourth paleosol
from the top. The results of the R method for Lub-3683
sample (310±53 ka) and for Lub-3684 sample (360±68
ka) indicate the Zbójnian (= Domnitz) Interglacial. The
TL ages of both samples obtained by using the TB method
(622±174 ka and 604±174 ka) can be correlated with the
Ferdynandowian (= Voigtstedt) Interglacial.
Samples: Lub-3675 and Lub-3676 were taken from
depths of 12.7 and 13.7 m, i.e. from silty loess-like deposit
2.50 m thick. The TL ages for Lub-3675 and Lub-3676
samples obtained by using the regeneration procedure
(280±42 ka and 311±68 ka) indicate that this deposit was
accumulated during the Odranian (= Drenthe) Glacial.
The TL age obtained by the total-bleach method for Lub-
3675 sample is 738±207 ka, and for Lub-3676 sample –
839±277 ka, so the deposits can be older than the Sanian
1 (= Elsterian 1) Glacial.
Two last samples – Lub-3677 and Lub-3678 – were
taken from the pedocomplex occurring at a depth of 14.5-
19.0 m. The results of the R procedures for Lub-3677 sample
(326±52 ka) and for Lub-3678 sample (306±73 ka)
correspond to the Zbójnian (= Domnitz) Interglacial. The
TL age obtained by the TB method for sample Lub-3677
is 883±398, and for sample Lub-3678 – 754±301 ka,
so the deposit can be correlated with warm periods pre-
ceding the Sanian 1 (= Elsterian 1) Glacial.

5. DISCUSSION

The presented results of TL analysis show how great

are the interpretation problems of the TL datings. Two
Fig. 2. Lithology, TL ages and stratigraphy of the deposits in the
groups of TL ages were obtained for each sample. Each
Zahvizdja profile.
group can be correlated with different glacial or intergla-
cial. For Lub-3680 sample the TL age obtained by the
regeneration procedure of equivalent dose determination
1000
corresponds to the Eemian interglacial. For the rest of
900
samples (from Lub-3681 to Lub-3684 and from Lub-3675
to Lub- 3678) all TL ages obtained by using the R tech- 800
nique are related to the period from the Lublinian 700
TL age (ka)

(= Rügen) Interglacial to the Zbójnian (= Dömnitz) 600

Interglacial. It is very important that despite the occur- 500
rence of eight paleosols of high stratigraphic rank, a dis- 400
tinct increase of TL age in the profile is observed only 300
to a depth of 6.0 m (Fig. 3). From 6.0 to 18.3 m the R 200
procedure gives chaotic results ranging from 268±42 to 100
368±63 ka. Lack of a systematic and distinct TL age
0
increase with depth arouses our great doubts about relia- 0 5 10 15 20
bility of the TL datings carried out using the discussed
TB R Depth (m)
procedure. The results of complex investigations of the
profile, and especially of the paleomagnetic analysis, con- Fig. 3. Comparison of obtained TL ages using different TL
firm these limitations. Therefore, the TL ages obtained techniques.
by using the regeneration method are accidental values,
which are not in agreement with geological age of depo-
sits studied (Fig. 2).

30

In order to explain divergences between the deposit
age estimated on the basis of paleomagnetic analyses, and
also geomorphological, paleogeographical and paleope-
dological criteria, and its TL age obtained by the rege-
neration method we should make a thorough analysis of
the equivalent dose determined for the particular samples.
The ED values, just as the TL ages, distinctly increase
with depth only to a depth of 6.0 m (Fig. 4). From 6.0 to
18.3 m the ED values obtained by the R procedure change
chaotically from from 925±130 to 1051±158 Gy. It may
suggest that the presented ED values correspond to the
luminescence saturation level of deposits in the studied
profile and demonstrate the apparent saturation age for
the applied regeneration method. Age underestimation
related to use of the regeneration method was noticed by
several authors, among others by Berger et al. (1992) who
found that the regeneration procedure gave age under-
estimation for samples older than 80 ka, with maximum
TL ages of about 150 ka for samples of 500 to 800 ka age.
Frechen et al. (1999) discovered that a systematic error in
ED determination using the regeneration method re-
sulted from a change in luminescence sensitivity of the
material which was exposed to artificial or natural light.
The upper limit of the ED value which can be obtained
by the regeneration method is estimated at 1000-1200 Gy,
so the corresponding TL age is 200-250 ka (Frechen
et al., 1997).
When estimating results obtained by the total-bleach
method, we have quite different situation to that dealing
with the regeneration technique. Lub-3680 sample was
taken from the paleosol undoubtedly older than the
Eemian Interglacial, as it is evidenced by geomorphologi-
cal situation and paleopedological criterion. Therefore,
the TL age obtained by the TB method (234±47 ka) can
be correlated with deposition time of the studied sediment
(Boguckyj et al., 2001). The result of the TB for Lub-3681
sample (532±101 ka) is in a good agreement with its
expected geological age corresponding to the Sanian 2
(= Elsterian 2) Glacial. Three samples – Lub-3682
(586±117 ka), Lub-3683 (622±174 ka) and Lub- 3684
(604±174 ka) – were collected from depths of 8.7, 9.3
and 10.5 m, respectively. They represent the pedocom-
plex of two forest soils occurring between 8.0 and 10.8 m.
3000
2500
2000
ED (Gy)
1500
1000
500
0 are conflicting. Some authors think that the reliable and
0 5 10 15
TB R Depth (m)
Fig.4. Comparison of obtained ED results using different TL
techniques.
J. Kusiak et al.
Lub-3682 sample was taken from the upper paleosol (third
from the top of the profile) developed on muds or sandy-
gravelly loams of a fluvial origin. Lub-3683 and Lub-3684
samples were taken from a muddy insert within deposits
occurring between the third and fourth paleosol. These
fluvial deposits are evidently a foreign component in the
loess-paleosol profile. Their spatial extent is limited, and
we can consider them as an infill of a small transversal
valley, which once has developed on a slope and it prob-
ably has filled with material denuded from a plateau-ridge
surface. The obtained TL ages are generally in a good
agreement with geological estimates for the discussed part
of the profile, i.e. they correspond to the Ferdynandowian
Interglacial. Lub-3675 and Lub-3676 samples were taken
from the lowest layer of the upper lithological unit, i.e.
from deposit which can be correlated with the Sanian 1
(= Elsterian 1) Glacial. Lub-3675 sample from a depth
of 12.7 m was dated at 738±207 ka, and Lub-3676 sample
from a depth of 13.7 m – at 839±277 ka. Two next samples
were taken from the middle lithological unit, i.e. the
pedocomplex of four paleosols occurring between 14.5
and 19.0 m. Lub-3677 sample from a depth of 15.3 m was
dated at 883±398 ka. The TL age obtained for Lub-3678
sample from a depth of 18.3 m is 744±301 ka. This sample
was collected from the third paleosol from the top of this
pedocomplex. Brunhes/Matuyama paleomagnetic bound-
ary dated at 783 ka (Nawrocki et al., in press) was found
within the illuvial horizon of this paleosol. Therefore, the
TL age of Lub-3678 sample obtained by the TB proce-
dure is in a very good agreement with the deposit age
determined by the paleomagnetic method. It indicates that
the TL ages of three samples (from Lub-3675 to Lub-
3677) are overestimated. It is possible to explain these
discordances by two reasons: (1) too weak bleaching of
mineral material resulting from short transport before
sedimentation; (2) too low doses used for irradiation of
samples. First reason may be connected with the fact that
the studied loess sediments can contain an admixture of
material coming from the underlying soils of the middle
unit; the first paleosol from the top of this unit is strongly
(in places even completely) denuded. Deflated or washed
soil material was probably incorporated into the discussed
part of the loess cover. Second reason may be connected
with ED values for Lub-3675, Lub-3676 and Lub-3677
samples which are the highest in the whole profile and
exceed 2500 Gy. Extremely low thermoluminescence
intensity in these samples, and too low additional doses
(up to 5000 Gy) caused relatively large errors in the ED
determination.
6. CONCLUSIONS
The reports on the range and reliability of the thermo-
luminescence dating method of the Quaternary deposits
20 reproducible TL ages can be obtained only for the last
100 ka (e.g. Frechen et al., 1997). Others are of opinion
that TL dating may give accurate ages in the range from
100 to 800 ka (e.g. Berger et al., 1992). These controver-
sies induced us to make a series of TL datings with use
31
 DIVERGENCE IN THE TL DATING RESULTING FROM DIFFERENT METHODS ...
of two procedures for the deposits of the Zahvizdja pro-
file, which were also dated by other methods. The total-
bleach method (TB) gave the results similar to the ex-
pected ones. With this method we were able to date
samples in the range from 200 to 900 ka. In spite of these
promising results, we should be prepared for difficulties
when estimating the ED values higher than 2000 Gy be-
cause luminescence may reach the saturation level. We
hope that further TL analyses planned to be carried out
for the Zahvizdja profile will allow us to specify the pre-
liminary results reported in this paper.
7. ACKNOWLEDGEMENTS
Investigations of the Zahvizdja profile are partially
supported by Grant 6 PO4E 031 15 (KBN) and are a part
of a planned series of monographic studies of key pro-
files of loesses of the Carpathian Foreland facies.
The authors are grateful to Dr Maria Wilgat who has
prepared the English version of this paper.
REFERENCES:
Aitken M.J., 1983: Radioactivity data using SI units. PACT 9: 69-71.
Berger G.W., 1988: Dating Quaternary events by luminescence.
Geological Society of America, Special Paper 227: 13-50.
Berger G.W., Pillans B.J. and Palmer A.S., 1992: Dating loess up to
800 ka by thermoluminescence. Geology 20: 403-406.
Boguckyj A.B., 1987: The main loess and palaeosol horizons of
periglacial Pleistocene loess-soil series in the southwestern part
of the Eastern European Platform (Osnovnye loessovye i pa-
leopochvennye gorizonty periglacialnoy loessovo-pochvennoy
seri pleystocena jugo-zapada Vostochnoevropeyskoy platfor-
my). In: Stratigraphy and correlation of maritime and continen-
tal Ukrainian sediments), 47-52. Naukova Dumka, Kiev.
Boguckyj A., Gozhik P., Lindner L., £anczont M. and Wojtanowicz
J., 2001 (in press): Main stratigraphic units of the Polish and
Ukrainian Quaternary (original). In: VIII Konferencja Straty-
grafia plejstocenu Polski „Serie rzeczne i lodowcowe po³udniowej
Opolszczyzny”, 2001, Jarno³tówek.
32
Boguckyj A., £anczont M. and Wojtanowicz J., 1999: Lower Ple-
istocene fossil soils in the loess cover of the Halicz Carpathian
Foreland (Dolnoplejstoceñskie gleby kopalne w pokrywie
lessowej Halickiego Podkarpacia). In: III Seminarium lessowe
„Geneza i wiek pokrywowych utworów pylastych po³udniowo-
zachodniej Polski”. Uniwersytet Wroc³awski, Wroc³aw-Bo¿ków (in
Polish).
Brumby S., 1992: Regression analysis of ESR/TL dose-response
data. Nuclear Trucks and Radiation Measurements 20: 595-599.
Frechen M., Brückner H. and Radtke U., 1992: A comparison of
different TL techniques on loess samples from Rheinahlen
(F.R.G.). Quaternary Science Reviews 11: 109-113.
Frechen M., Horváth E and Gábris G., 1997: Geochronology of
Middle and Upper Pleistocene loess section in Hungary.
Quaternary Research 48: 291-312.
Frechen M., Zander A., Clíek V. and Lo•ek V., 1999: Loess chrono-
logy of the Last Interglacjal/Glacial cycle in Bohemia and
Moravia, Czech Republic. Quaternary Science Reviews 18:
1467-1493.
Grün R., 1994: Fit-Sim. Computer program, QDRC, Canberra.
£anczont M., Boguckyj A., Wojtanowicz J., Racinowski R. and Seul
C.: Eopleistoceneand lower Mesopleistocene paleosols in the
Zahvizdja profile in the East Carpathian Foreland (W Ukra-
ine).. Quaternary International (in print).
Nawrocki J., Boguckyj A., £anczont M. and Nowaczyk N.R.: The
Matuyama-Brunhes boundary and the nature of magnetic
remanence acquisition in the loess-paleosol sequence from
western part of the East Europeanloess province. Palaeogeogra-
phy, Palaeoclimatology, Palaeoecology (in print).
Pillans B., Kohn B.P., Berger G., Froggatt P., Duller G., Alloway B.
and Hesse P., 1996: Multi-method dating comparison for Mid-
Pleistocene Rangitawa Tephra, New Zealand. Quaternary Geo-
chronology (Quaternary Science Reviews) 15: 641-653.
Prescott J.R. and Hutton J.T., 1988: Cosmic ray and gamma ray
dosimetry for TL and ESR. Nuclear Tracks 14: 223-227.
Wintle A.G., 1987: Themoluminescence dating of loess. Catena
Supplement 9: 103-115.
Wintle A.G. and Huntley D.J., 1980: Thermoluminescence dating
of ocean sediments. Canadian Journal of Earth Sciences 17:
348-360.
 GEOCHRONOMETRIA Vol. 21, pp 33-40, 2002 – Journal on Methods and Applications of Absolute Chronology

230
Th-EXCESS AND 14C DATING OF PELAGIC
SEDIMENTS FROM THE HYDROTHERMAL ZONE
OF THE NORTH ATLANTIC

V.YU. KUZNETSOV1, K.A. ARSLANOV1, V.V. SHILOV2, G.A. CHERKASHEV2

and S.B. CHERNOV1
1
Geographical Research Institute, St. Petersburg State University, Sredny Prospect 41, 199 004 Saint-Petersburg, Russia
2
Institute for Geology and Mineral Resources of the Ocean,
Angliysky Prospect 1, 190 121 Saint-Petersburg, Russia

Key words
words: Abstract: A comprehensive geochronological study of a pelagic sediment core altered by
230
Th-EXCESS DATING, hydrothermal processes from the Mid Atlantic Ridge (14.5°N) was carried out using both the
230
RADIOCARBON DATING, Thexcess and the radiocarbon methods. Complementary foraminiferal tests and oxygen-iso-
HYDROTHERMAL tope determinations were done. The main task was to check whether 230Thexcess dating of such
ACTIVITY, PELAGIC diagenetically changed sediments yields reliable absolute ages. For this purpose the vertical
SEDIMENT, distribution of the 238U, 234U, 232Th and 230Th activities along the core was measured. The re-
BIO-STRATIGRAPHY, sults proved that it was not disturbed during the aging of the sediment. The long-term hydro-
OXYGEN-ISOTOPE thermal influence had been constant during at least the last 300 ka and did not change the
STRATIGRAPHY, natural 230Thexcess distribution along the core. Hence, 230Thexcess dating yields reliable ages and
GEOCHRONOLOGY allows to calculate sedimentation rate. Between the uppermost and lowermost sublayers of
the core we obtained 1.35±0.15 cm/ka which agrees with 1.47±0.03 cm/ka derived from
conventional 14C ages. These numerical dates, the results of the foraminiferal tests and the
δ18O values place the studied sediments to the marine isotope stage 5 (MIS 5). These dates are
well correlated with the corresponding sedimentary records from pelagic sediments of the
North Atlantic Ocean.

1. INTRODUCTION Mid-Atlantic Ridge (MAR). We investigated: 1) the ver-

There is a growing interest to study different types of
pelagic sediments mixed with low and high temperature
hydrothermal components. High temperature hydrother-
mal fluids are discharged into the bottom ocean water
(Lisitsyn et al., 1990). Part of these hydrothermal matter
is deposited near the vents forming massive sulfides and
metalliferous sediments. These sediments are scattered
around large distances. Pelagic sediments are penetrated
by hydrothermal solutions in active hydrothermal zones
and chemical elements are deposited.
Many comprehensive chemical, mineralogical, geo-
logical, geophysical, biogeochemical and geochronological
studies have been carried out on hydrothermal sediments.
However, there are only few data on sedimentation rates
and absolute ages. In most cases the uranium-disequilib-
rium method was applied.
As there are usually no data on the biostratigraphy of
hydrothermal deposits numerical dating is essential to
classify such deposits. We undertook a comprehensive
biostratigraphic, isotopic and geochronological study of
a sediment core from the active hydrothermal zone of the
tical distribution of the uranium and thorium isotopes
(238U, 234U, 232Th and 230Th), 2) checked the possibility to
apply the 230Thexcess dating method to oceanic hydrother-
mal deposits, and 3) compared the results of our geochro-
nological, biostratigraphic and stable isotope study with
those of the North Atlantic Ocean.
2. LOCATION AND MATERIALS
The core KP-145 was taken on RV “Professor
Logachev” in 3105 m water depth at 14°45’44’’ N and
44°58’74’’ W in the Mid-Atlantic Ridge area in 1994. This
site is located about 300 m north of the hydrothermal field
“Logachev” which was discovered in 1993 (Krasnov et
al., 1995). The hydrothermal field is situated at the east-
ern slope of the rift valley about 35 miles far from the
fracture zone at 15°20’N (Fig. 1 and 2). Two layers are
distinguished in the core:
Layer 1 (0-18 cm): It consists of 90-95% grey-beige
biogenic calcium carbonate (coccolites and foraminifera)
with spotted ore-bearing silt. There are singular micro-
inclusions of black color (Fe-Mn oxides) and fragments
 230
Th-EXCESS AND 14C DATING OF PELAGIC SEDIMENTS FROM THE HYDROTHERMAL ZONE ...

of ultrabasic rocks. The spherical silt spots are beige-col-

ored, sometimes non-transparent and formed by
bioturbation. The upper sublayer (0-1 cm) is saturated
with seawater.
Layer 2 (19-115 cm): It mainly consists of calcium
carbonate (coccolites and foraminifera) which concentra-
tion gradually decreases downward from 78 to 72%. The
sublayer up to 60 cm contains hydrothermal material.
There is some beige-colored silt with singular black col-
ored (Fe-Mn oxides) micro-inclusions. The upper part of
the layer (19-25 cm) is affected by bioturbation with
numerous gray-beige dots and bands without sharp con-
tours.
Our sediment core KP-145 from the active hydrother-
mal MAR area contains complex genetic features which
could only be deciphered by a careful, comprehensive
geochronological and multidisciplinary study. The com-
mon pelagic sediment is depositionarily superimposed by
the penetration of hydrothermal fluids and associated and
geochemical processes. Parts of the sediments were mixed
by tectonics and bioturbation.

Fig. 2. Geological structure of axis region of Mid-Atlantic

Ridge in the zone of hydrothermal field 14o 45 N
(after Bogdanov et al., 1995).
A: 1 – rift valley; 2 – transform fault 15o 20 N; 3 – spreading
axis; 4 – normal fault scarps; 5 – vertical deep-seated fault;
6 – massif of serpentinous ultrabasites and gabbroides;
7 - active hydrothermal field.
B: Profile I-II: 1 – unconsolidated sediments; 2 – extrusive
basalts; 3 – serpentinous ultrabasites and gabbroides;
4 – vertical deep-seated fauls; 5 – active hydrothermal field.

Fig. 1. Location of “Logachev” hydrothermal field and station

KP 145. 1 – rift valley; 2 – “Logachev” hydrothermal field;
3 – isolines of floor relief; 4 – location of station KP 145.

34
 V.Yu. Kuznetsov et al.

3. ANALYTICAL METHODS

Uranium and thorium were radiochemically extracted

(Kuznetsov, 1993; Kuznetsov et al., 2000). The main steps
were:
l digestion and dissolution of 5-10 g of sediment by
concentrated HNO3, HF and HCl; removal of F- by
concentrated HClO4; addition of the double spike of
232
U and 234Th;
l adsorption of uranium and thorium isotopes on iron
hydrooxide in a carbonate-free ammonia solution at
pH 7 to 8;
l purification of the solution from all admixtures of in-
terfering alpha emitters; separation of the uranium and
thorium by anion exchange. Anionite AV-17 was used
to elute the Th fraction from the 7n HNO3 solution
and uranium from the 6n HCl/0.2n HNO3 solution;
l electrodeposition of uranium and thorium on platinum
discs from the ethyl alcohol solution (adding the 0.2 n
HNO3 solution) during 1.5 hours under current den-
sity of 60 ma/cm2 (Kim et al., 1966);
l alpha-spectrometric determination of the 238U, 234U,
232
Th and 230 Th activity using a semi-conductor
surface-barrier silicon detector (resolution: 30 KeV/ Fig. 3. Vertical distribution of 230Thexcess (A) and direct 230 Th
excess
channel) and the pulse analyzer AI-1024. dates (B) along the core KP-145
The chemical yield of uranium and thorium isotopes
were calculated from the activities of the 232U and 234Th
spikes. The results of a radiochemical analysis of the sedi-
ment core KP-145 are compiled in Table 1.
The organogenic fraction of the pelagic sediment was
transformed into benzene and 14C dated by liquid scintil-
Table 2. Absolute ages of sublayers of core KP-145.
lation counting (Arslanov, 1987). The 14C dates of the
No. Sublayer Conventional 14C Age 230Th/U age
various sublayers of the core are compiled in Table 2.
[cm] [BP] [years]*
1 0-1
4. RESULTS
2 5-6 4100 ± 400*

Radiometric measurements 3 13 - 15 10,800 ± 200 10,400 ±1100*

(11,170 BC-10,485 BC)
The manifold methods of uranium-series disequili-
4 30 - 31 20,800 ± 500 22,600 ± 2400*
brium dating are based on the offset of radioactive equi-
5 40 - 41 27,600 ± 600 30,000 ± 3200*
librium in oceanic sediments. One of these methods is
6 60 - 61 44,800 ± 4800*
the 230Thexcess method which uses the radioactive decay of
7 90 - 91 67,000 ± 7400*
the excess activity of 230Th over that of the parent uranium.
There are two prerequisites for the application of this 8 114 - 115 84,800 ± 9200
method: 1)230Th may not migrate in the sedimentary strata Comments:
The average sedimentation rate calculated by 230Th was 1.35±0.15 cm/ka; the standard
which has never been observed (Kuznetsov, 1976; deviation of the average sedimentation rate was calculated from that of the date of
Kuznetsov and Andreev, 1995; Huh and Ku, 1984; Lalou 84,800±9200 yr.
The average sedimentation rate calculated by 14C data was 1.47±0.03 cm/ka; the stan-
et al., 1988); 2)230Th is deposited with a constant deposi- dard deviation of the average sedimentation rate was calculated from that of the date of
tion rate. This prerequisite has to be checked for each 27,600±600 yr.
section with different genesis. *)=the age was calculated from the average sedimentation rate of 1.35±0.15 cm/ka.

Table 1. Results of a radiochemical analysis of the sediment core KP-145.

No. Layer 238U 234U 234U/238U 232Th 230Th*

[cm] [dpm/g] [dpm/g] [dpm/g] [dpm/g]

1 0-1 0.48 ± 0.02 0.51 ± 0.02 1.07 ± 0.06 0.90 ± 0.06 6.53 ± 0.37
2 5-6 0.51 ± 0.02 0.54 ± 0.02 1.06 ± 0.06 0.62 ± 0.04 5.51 ± 0.33
6 60 - 61 0.44 ± 0.02 0.48 ± 0.02 1.08 ± 0.06 0.55 ± 0.03 3.54 ± 0.22
7 90 - 91 0.14 ± 0.01 0.16 ± 0.01 1.11 ± 0.06 0.42 ± 0.03 3.38 ± 0.20
8 114 - 115 0.25 ± 0.01 0.25 ± 0.01 0.99 ± 0.06 0.55 ± 0.03 2.99 ± 0.19
230 234
*)=activity of Th, excessive over the equilibrium with parent U.

35
 230
Th-EXCESS AND 14C DATING OF PELAGIC SEDIMENTS FROM THE HYDROTHERMAL ZONE ...
The 234U/238U AR insignificantly vary within the core.
The 238U concentration ranges from 0.2 - 0.7 µg/g corre-
sponding to a specific activity of 0.14-0.51 dpm/g
(Table 1). The 232Th activity varies by a factor of two along
the core.
Foraminiferal tests, oxygen-isotope composition
and palaeotemperature
The composition of the well preserved and abundant
planktic foraminifera, the δ18O values and the ratio of
biogenic and terrigenous components in the sand sedi-
ment fraction were determined on 14 sublayers. The av-
erage annual paleotemperature was reconstructed from
the ratio of planktic foraminifera species Globigerina
Pachyderma (Fig. 4). The determination of the oxygen-
isotope analyses were done on the CaCO3 of all species
planktic foraminifera shells rather than an individual spe-
cies as relative large quantities of samples were required
for the mass-spectrometric measurement. Some of the
planktic foraminifera contained Fe-Mn oxides.
5. DISCUSSION
Radiometric measurements
The 234U/238U AR and 238U activities are in the range
of uranium in common pelagic and metal-bearing sedi-
ments (Kuznetsov, 1976; Lalou et al., 1988; Arslanov et
al., 1988). Hydrothermal fluid discharged from the ocean
floor is usually not enriched in uranium compared to sea-
water (Lisitsyn et al., 1990; Lisitsyn, 1970 and 1993; Arslanov
et al., 1988). Hence, the concentration and distribution
of uranium in the pelagic sediment may be primarily de-
termined by its terrigenous and hydrogenous origin and
by the supply of endogenous ore substance. This supply
decreases to some extent the uranium concentration in
the sediment. This concept is in agreement with the found
234
U/238U activity ratio which ranges from 1.0 (terrigenous
detritus) to 1.14 (near that of seawater; see Table 1). The
230
Thexcess activity in the core decreases gradually from the
surface downward as expected from radioactive decay
(Fig. 3). The direct absolute 230Thexcess dates calculated on
the basis of the 230Thexcess activity in the sublayers 1 and 2,
1 and 6, 1 and 7, 1 and 8 tend to increase along the core
(Fig. 3). These findings testify that any influx of endogenous
ore matter and from the hydrothermal plume was constant
and did not disturb the natural distribution (Table 1).
The maximum thorium concentration in sublayer 1
may reflect an insignificant supply of 232Th and 230Th dur-
ing the last several thousands of years.
Under the found conditions the 230Thexcess method was
used to determine the average sedimentation rate of the
core. On the basis of the 230Thexcess activity in the sublayers
1 and 8 we calculated the age of 84,800±9200 yr between
the sublayers 0-1 cm and 114-115 cm. The data allow to
calculate the average sedimentation rate of 1.35±0.15
cm/ka from which absolute ages were estimated for each
sublayer (Table 2). The latter and the corresponding 14C
dates agree well with each other. On the basis of the 14C
date of 27,600±600 (sublayer 40-41 cm) we calculated the
average sedimentation rate of 1.47±0.03 cm/ka.
36
Foraminiferal tests, oxygen-isotope compositions
and palaeotemperature
The elaborated reliable chronology of core KP-145
explains why these sediments were chosen for the com-
prehensive study including foraminiferal tests and comple-
mentary isotope-oxygen analysis. The results allowed
a stratigraphic and geochronological classification of the
core and its correlation with MIS (Shackleton and Opdyke
1973; Barash et al., 1983 and 1984; Barash, 1988; see Fig. 4).
The assemblage of planktic foraminifera in the sub-
samples 0-1 cm, 5-6 cm and 10-11 cm depth contains
mainly the species Globigerinoides sacculifer (Brady)
(Fig. 4), Gs. ruber d’Orbigny; Globorotalia menardii
(d’Orbigny), Sphaeroidinella dehiscens (Parker et Jones).
It corresponds to the tropical type of thanatocenosis of
the equatorial subtype. Due to the dominance of
Globorotalia menardii (d’Orbigny) these subsamples be-
long to the Zone Z defined by Eriksson et al. (1961 and
1963) which was deposited during the last 11,000 years.
The palaeotemperature was reconstructed according
to Barash et al. (1983 and 1988) and yielded an mean annu-
al temperature of the surface water of +25.0 to +26.5°C
(Fig. 4). The Holocene climatic optimum is reflected by
an insignificant temperature increase and a mould of the
isotope-oxygen curve at the layer between 5 and 6 cm
(Fig. 4). The 230Thexcess date of 4100±400 yr was determined
for this sublayer (Table 2). The conventional 14C and
230
Thexcess dates of the 13-15 cm are 10,800±200 yr BP
(the calibrated 14C date is 11,170 BC –10,485 BC, with
1σ confidence interval analysis) and 10,400±1100,
respectively (Table 2). The sedimentation rate for MIS 1
adopting the age of the boundary between MIS 1 and
MIS 2 of ~11 ka (Morley and Hays, 1981) is about
1.35 cm/ka (Table 3).
The dominant species of planktonic foraminifera of
Layer 2 (18-110 cm) were Globigerinoides ruber d’Orbigny,
Gs. sacculifer (Brady) (Fig. 4), Globorotalia truncatuli-
noides (d’Orbigny) with single individuals of Globorotalia
menardii flexuosa (Koch). This assemblage is characteris-
tic for Zone Y (Eriksson et al., 1961 and 1963) which lasted
from 75-11 ka.
The sublayers between 15-43 cm (15-16 cm, 20-21 cm,
30-31 cm and 40-41 cm) contained planktic foraminifera
of the tropical type of thanatocenosis tending to the equa-
torial subtype (Barash, 1988). The reconstructed
paleotemperature of the mean annual surface water was
closely to +25.0°C (Fig. 4). The δ 18O value and the
assemblage of planktic foraminifera as Globigerinoides
sacculifer (Fig. 4), Gs. ruber, Globorotalia truncatulinoides
are related to MIS 2 lasting from 27 to 11 ka. The con-
ventional 14C dates of the 30-31 cm and 40-41 cm are
20,800±500 and 27,600±600 BP, respectively (Table 2).
The 230Thexcess dates of 22,600±2400 and 30,000±3200 ka
were determined for these sublayers. The sedimentation
rate for MIS 2 adopting the age of the boundary between
MIS 2 and 3 of ~27 ka (Morley and Hays, 1981) is about
1.75 cm/ka (Table 3).
The sublayers between 43-85 cm (50-51 cm, 60- 61 cm,
70-71 cm and 80-81 cm) contained planktic foramini-
fera of the tropical type of thanatocenosis tending to the
 V.Yu. Kuznetsov et al.

equatorial subtype (Barash, 1988). The mean annual tem- the equatorial subtype without secondary changes
perature of the surface water was estimated to +26.0 (Barash, 1988). The estimated mean annual temperature
±0.5°C (Fig. 4). Both the isotope-oxygen curve and that of the surface water was close to +26°C (Fig. 4). The bio-
of the planktic foraminifera (Fig. 4) correspond to MIS 3 stratigraphic and isotopic results allowed a connection to
and the time range from 58 to 27 ka. The sample from MIS 5 (128 to 72 ka). The absolute 230Thexcess date of the
60-61 cm (230Thexcess) yielded 44,800±4800 yr (Table 2). sample from 115-114 cm is 84,800±9200 yr (Table 2).
The age of ~58 ka between MIS 3 and 4 (Morley and Zone X is represented by sediments below 110 cm.
Hays, 1981) yielded a sedimentation rate of about 1.35 It contained species of Globorotalia menardii: Globorotalia
cm/ka for MIS 3 (Table 3). menardii (d’Orbigny) and Globorotalia menardii flexuosa
The planktic foraminifera in the section of 85-105 cm (Koch) which were deposited between 128-75 ka.
(90-91 cm and 100-101 cm) belonged to the tropical type The good agreement between the results of the geo-
of thanatocenosis tending to the equatorial subtype chronological, biostratigraphic and isotopic analyses tes-
(Barash, 1988). The mean annual temperature of the sur- tifies the reliability of the derived climate-geochronologi-
face water was close to +25.0°C (Fig. 4). The assemblage cal course (Fig. 4).
of planktic foraminifera and the δ18O values allow a cor-
relation with MIS 4 (72-58 ka). The 230Thexcess date for 6. STRATIGRAPHICAL AND GEOCHRONOLOGICAL
the 90-91 cm sublayer is 67,000±7400 yr (Table 2). The COMPARISON OF THE CORES KP-145 AND L-66
age of ~72 ka between MIS 4 and 5 yielded a sedimenta-
tion rate of about 1.43 cm/ka for MIS 4 (Table 3). We compared our results from core KP-145 represent-
The sublayers between 105-115 cm (110-111 cm and ing the hydrothermal activity zone with the correspond-
114-115 cm) contained well-preserved planktonic forami- ing data of the sediment core L-66 from the pelagic zone
nifera of the tropical type of thanatocenosis tending to of the North Atlantic (Arslanov et al., 1988). By this the
geological section was correlated with the climate-strati-
graphic events for the Late Pleistocene-Holocene of the
Table 3. The sedimentation rates between the boundaries of MIS
in cores L-66 and KP-145. Central and North Atlantic Oceans.
Core L -66 was taken on the second cruise of RV
Marine isotope stage L-66 [cm/ka] KP-145 [cm/ka]
“Mikhail Lomonosov” (1958) in the European basin
MIS 7 1.6
(49°04´ N, 20°18´ W) in a water depth of 4000 m. The
MIS 6 0.4
core length is 298 cm. It contains alternating layers of
MIS 5e 1.2
white to light-gray silt (0-12, 134-149 and 168-255 cm).
MIS 5d - 5a 1.0
The terrigenous material of sandy silt with gravel, pebble
MIS 4 1.7 1.43 and detritus (12-134, 149-168 and 255-298 cm) domi-
MIS 3 0.5 1.35 nates over the biogenic, coccolite-foraminifera silt. In the
MIS 2 1.45 1.75 26-39 cm sublayer, volcanic ash is present. The terrigenous
MIS 1 1.2 1.35 sublayers, especially the thickest sublayer at 12-134 cm,

δ18O [‰]

Fig. 4. Results of geochronological study of cores KP-145 and L-66, their stratigraphical classification and correlation.
a) 1 – coccolith-foraminiferal ooze; 2 – terrigenous mud; 3 – volcanic ash; 4 – gravel, pebble, rock debris;
b) 1 – coccolith-foraminiferal ooze.

37
 230
Th-EXCESS AND 14C DATING OF PELAGIC SEDIMENTS FROM THE HYDROTHERMAL ZONE ...
are lithologically heterogeneous. They contain fine- to
coarse-grained interlayers with micro-laminated texture.
They are interpreted as reflection of significant changes
of the palaeo-oceanographic sedimentation.
From this core, 18 quantitative analyses of the com-
position of planktic foraminifera were done, the palaeo-
temperature and the ratio of biogenic to terrigenous com-
ponents in the sandy fraction of the sediment (>0.1 mm)
were calculated. In addition, 16 isotope-oxygen analyses
and 12 analyses of the carbonate concentration were
performed. Uranium, thorium and protactinium measure-
ments were carried out on eight sublayers between 0-6 cm
and 229-234 cm.
The sample from 150-154 cm yielded the 231Paexcess date
of 146,000±18,000 years representing the boundary of
MIS 5/MIS 6. The 230Thexcess date of 231,000±15,000 years
for the 229-234 cm sublayer corresponds to the early
climatic optimum of MIS 7 which is well correlated with
the course of the δ18O values (Morley and Hays, 1981;
see Fig. 4).
The stratigraphic classification of L-66 allows an esti-
mate of the absolute ages and the sedimentation rates
between the boundaries of MIS (Morley and Hays, 1981).
The sedimentation rate in core L-66 and KP-145 varied
noticeably (Table 3).
In agreement with other findings the sedimentation rate
of both cores KP-145 and L-66 is higher during the cold
periods (MIS 2 and 4) than during the warm periods (MIS
1 and 3) in the Central and North Atlantic. This is explained
by an increased supply of terrigenous material during the
cold epochs as plant cover fixes loose sediments.
The average sedimentation rate of 1.4 (230Thexcess, 14C)
and 1,0 ka/cm (230Thexcess, 231Paexcess) in the cores KP-145 and
L-66 for MIS 1-4 deviate slightly from each other. This
may indicate that the hydrothermal influence at the site
of KP-145 was insignificant and constant along the core.
7. CONCLUSIONS
The comprehensive geochronological study of the core
KP-145 proved that the 230Thexcess dating method yielded
reliable dates since the influx of hydrothermal matter was
constant or negligible and did not influence the vertical
distribution of uranium and thorium isotopes. The bios-
tratigraphic and oxygen-isotope results allowed a strati-
graphic and the 230Thexcess ages for chronological classifi-
cation of the sediment core from the MAR hydrothermal
zone and their correlation with MIS. The palaeotem-
perature for the Late Pleistocene-Holocene was recon-
structed for the surface water from the Central and North
Atlantic.
ACKNOWLEDGEMENTS
Thanks are due to anonymous reviewer for helpful
comments.
The financial support by the Russian Foundation of
Basic Studies for this study was highly appreciated
(projects No. 98-05-64764 and No. 01-05-64870).
38
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39
230
Th-EXCESS AND 14C DATING OF PELAGIC SEDIMENTS FROM THE HYDROTHERMAL ZONE ...

40
 GEOCHRONOMETRIA Vol. 21, pp 41-48, 2002 – Journal on Methods and Applications of Absolute Chronology

NEW AGE DATA OF BURIED PEAT DEPOSITS FROM THE

SITE “FILI PARK” (MOSCOW, RUSSIA) BY THE URANIUM-
THORIUM DATING AND PALYNOLOGICAL ANALYSIS
AND ITS STRATYGRAPHIC SIGNIFICANCE

V.YU. KUZNETSOV1, Kh.A. ARSLANOV1, M.N. ALEKSEEV2, V.V. PISAREVA2, S.B. CHERNOV1,
F.E. MAKSIMOV1 and N.G. BARANOVA1
1
Geographical Research Institute, Saint-Petersburg State University, , Sredny Prospect 41, 199 004 Saint-Petersburg, Russia
2
Geological Institute of the Russian Academy of Sciences, Pyzhevsky Str. 7, Moscow, Russia

Key words
words: Abstract: The chronostratygraphically important Quaternary buried peats from the site "Fili
URANIUM/THORIUM Park" (located on the territory of Moscow) on the Russian Plain were studied by the methods
DATING, of uranium-thorium dating (UTD) and palynological analysis. The deposits under study were
PALYNOLOGICAL the subject of intense debate: some number of the palynologists assigned ones to the Mikulino
ANALYSIS, (Eem) Interglacial, while the another investigators - to the Odintzovo Interglacial (Middle
GEOCHRONOLOGY, Pleistocene).
BURIED PEAT, Detailed palynological study gave the possibility to mark out the 3 palynozones (M2, M3 and
MIKULINO, M4) in section vertical profile and refer the deposits to the Mikulino (Eem) Interglacial. The
ODINTZOVO, uranium-thorium dating (by "leachate alone" method) was carried out in the middle layers,
INTERGLACIAL which would be expected to be a closed system in respect to uranium and thorium isotopes.
The direct uranium-thorium dating of inner layers showed the first UTD ages from 78.9 to
105.0 ka for deposits from the site "Fili Park". The corrected uranium-thorium age of buried
peat turned out to be younger than the currently adopted boundaries of the last Interglacial
(116-128 ka) and comprised 89±11 ka. There was probably an additional post-deposition
uranium uptake in the internal section layers that in general have led to an underestimated
age value. Nevertheless, we refered these questionable in chronostratigraphic respect depos-
its to the Mikulino Interlacial.
The geochronological data obtained were compared with the uranium-thorium dating results
(113±11 ka) for the closed geochemical samples from the Mikulino (Eem) Interglacial peats
of the stratotypical section "Mikulino" (Russian Plain). This comparison confirmed the reli-
ability of our conclusions.

1. INTRODUCTION series in buried peat or gyttja deposits. With time, from

Determination of the age of Quaternary continental
deposits is closely connected with application of adequate
methods for dating these formations. It is known that to
address the problems of chronostratigraphy of the Ho-
locene and Late Pleistocene sediments, a radiocarbon
method is widely used. It allows obtaining age data rang-
ing between several hundreds of years to 50-55 ka. At the
present time, for dating continental organogenous depos-
its (peat, gyttja), whose age is greater than the radiocar-
bon dating limits, one of the non-equilibrium geochronol-
ogy methods is applied, namely the uranium-thorium
method (UTD) with the age determination limit of up to
300-350 ka. This method is based on the established fact
of the disturbed radioactive equilibrium in the uranium
the parent uranium contained in the organic fraction of
the sample in significant quantities (up to 10 ppm and
more), a daughter 230Th isotope is accumulated while the
230
Th/234U ratio is a measure of the sample age.
The first results of using the uranium-thorium method
of dating buried peat were published in 1980 (Vogel and
Kronfeld, 1980). Then, a number of investigators con-
ducted studies of the geochemical behavior of uranium
and thorium isotopes in organogenous deposits, working
over the conditions for using UTD of these formations.
In combination with a palinological analysis, the chrono-
stratigraphy of buried peat deposits from the sections in
the West European territory was established (van der Wijk
et al., 1986 and 1988; van der Wijk, 1987; Hejnis et al., 1993;
Hejnis, 1995; Hejnis and van der Plicht, 1992).
 NEW AGE DATA OF BURIED PEAT DEPOSITS FROM THE SITE “FILI PARK” (MOSCOW , RUSSIA) ...
In recent years in Russia, we have began introducing
the uranium-thorium method for dating the Mikulino
(Eem) continental deposits in the Russian Plain territory
(Kuznetsov et al., 1998 and 2000a). A detailed study of
the geochemical behavior of uranium and thorium iso-
topes in the Mikulino (Eemian) Interglacial buried peats
in the Russian Plain allowed us to identify the layers of
these sediments suitable for dating and obtain the iso-
chron corrected age values of 113±11 ka for a stratotypical
“Mikulino” section from the Smolensk province (Kuzne-
tsov et al., in press).
This study aims to resolve a disputable issue of the age
of buried peat deposits from the “Fili Park” section
located in the Filevsky Park area in Moscow. Up to now,
there were two viewpoints of the chronostratography of
these sediments, namely whether they were the Late Pleis-
tocene deposits of Mikulino time (Mikulino, Eem Inter-
glacial) or belong to the Penultimate Interglacial (Odin-
tzovo Interglacial). Therefore, the main aim of the stu-
dies was to determine the age and chronostratigraphy of
buried peat deposits from the “Fili Park” section by the
methods of uranium-thorium dating and palynological
analyses.
2. SECTION DESCRIPTION
The “Fili Park” section in the Filevsky Park in Mos-
cow was carefully described in 1982 (Pisareva and
Lobachev, 1982). The outcrop is situated in the scarp of
the left slope of a deep gully in the upper portion of a
steep right bank slope of the Moskva River in the terri-
tory of the Filevesky Park in Moscow (Fig.1). The follow-
ing layers were outstripped in the outcrop (from top to
bottom; Pisareva and Lobachev, 1982):
Depth [m]
1. Yellow-brown sandy loam with plant remains passing
at a depth of 0.65 m to loam with rare gravel and pebble
............................................................................. 0,0-0,7
2. Yellow-brown close-grained sand with lenticular
“twisted” interlayers of dark-grey clay .......... 0,7-1,9
3. Light-grey fine-close-grained sand .................. 1,9-2,5
4. Loam with peat formation ............................... 2,5-2,7
Fig. 1. Location map of the sections “Fili Park” and “Mikulino”
42
5. Yellow-grey fine-grained sand with sandy clay interlayer,
horizontally-laminated towards the foot .......... 2,7-4,2
6. Clayey gyttja ....................................................... 4,2-4,3
7. Peat ..................................................................... 4,3-5,1
8. Platy gyttja .......................................................... 5,1-5,4
9. Gleying loam ...................................................... 5,4-5,6
10. Yellow close-grained sand with cryoturbations,
medium-grained from a depth of 6.75 m ........ 5,6-7,1
11. Brownish-brown light loam with inclusion of pebble
and debris of limestone, crystalline and effusive rocks
............................................................................. 7,1-7,9
12. Grey, fine-grained clayey thin-laminated sand
............................................................................. 7,9-8,5
13. Yellow close-grained sand, inequigranular from
a depth of 9.3 m .............................................. 8,5-10,4
14. Bluish-grey thin clay, brown from a depth of 11.3 m
with rare pebble of quartzite and silicon. Visible thick-
ness is 1.05 m ................................................ 10,4-11,45
In 1998 we collected samples from a buried peat layer
in 2 meters from the previous outcrop stripping in 1982.
The 1998 striping was made not in the central part of the
peat lens (there is now a landslide there), but closer to its
margin where the peat layer is undisturbed but has a
smaller thickness (55 cm against 80 cm in the central part
outstripped in 1982).
3. ANALYTICAL METHODS
The buried peat samples were collected every 5 cm
over the entire section depth (with a thickness of depos-
its of 55 cm). For radiochemical studies, dried peat
samples with a mass of 3-5 g were used. The determina-
tion of the levels of uranium and thorium isotopes was
made only in the organic fraction of specimens (using the
so-called „leachetes alone” method). Ashing of peat
samples was made at t =600°C for 24 hours. The residue
after calcination was leached by 7N HNO3. At this stage
of the analysis, the spikes of 232U and 234Th were injected.
After centrifuging (with mineral residue discarded), the
uranium and thorium isotopes were purified and sepa-
rated using chromatographic columns and then deposited
from alcohol solutions to the Pt-disks. The alpha-spec-
 V.Yu. Kuznetsov et al.
trometric measurements were made for several days
(Kuznetsov et al., 2000b). We used the 234Th (β-emitter,
T1/2=24.1 d) to determine thorium chemical yield. The
preparation of the spike is based on separation of the 234Th
from the parent 238U (Kuznetsov et al., 1963). The alpha-
spectrometric measurements and checking of β-decay
curve were used to control the 234Th radiochemical puri-
fication. The injection of the 234Th spike with activity of
2000-5000 pulse/minute enabled to determine the thorium
chemical yield quickly.
The preliminary treatment and preparation of peat
specimens for a pollen and spores analysis were under-
taken by standard methods (Arslanov et al., 1999). The
percentage of tree and herb pollen taxa are based on the
sum of terrestrial pollen; those of aquatic and unknown
taxa are based on the total pollen sum. Spores are calcu-
lated as percentages of the pollen and spores combined.
The Tilia and Tilia-Graph programs were used for draw-
ing of the diagram (Grimm, 1991).
4. RESULTS AND DISCUSSION
Palynological analysis of the buried peat bog samples
The results of previous palynological studies of peat
deposits carried out in 1982 (Pisareva and Lobachev,1982)
indicated the interglacial sedimentation conditions. Some
investigators refered the buried peat layer and underly-
ing gyttja to the Odintzovo Interglacial, while others to
the Mikulino time. The detection of single pollen of Picea
sec. Omorica, Pinus sec. Strobus, P. sec. Cembra, Larix sp.
and Abies sp. in the preparations, recorded during the
palynological analyses served as a basis for an older age.
In addition, a comparatively small content of hazel and
alder pollen was noted as well as the absence in the dia-
gram of pollen of broad-leaved species specific to the
Fig. 2. Pollen percentage diagram of the buried peat from the “Fili Park” section.
43
Mikulino Interglacial culmination. The latter fact is prob-
ably due to insufficiently good clearing of the outcrop.
The presence in the underlying layers the exotic conifers
pollen for this area can be attributed to redeposition. This
was confirmed by the fact that preparations contained
Tsuga sp., Pterocarya sp., as well as single Mesozoic and
Paleozoic spores evidently in the secondary bedding. In this
respect, specimens from the new 1998 clearing were more
promising to determine the age of deposits as they did not
actually contained the traces of redeposition (Fig. 2).
The palynological study of the samples (a total of 11
samples 5 cm thick each) has confirmed the interglacial
nature of the peat bog. As follows from the composition
of palynological spectra and plant remains, the peat bog
formed at the place of a mort lake and existed in the sur-
rounding of forest massifs. The species determinations
were difficult due to the absence of acetolysis treatment.
However, the floristic composition even at the generic
level and by the character of the change of the vegetation
cover is evidence of the Mikulino age of the buried peat
bog. The plant remains detected in the preparations al-
low us to refer peat deposits to a lowland type. Among
them, rootlets and epidermis of different sedges, epider-
mis of bur reed, buckbeen, more rarely of cat-tail and
other bog plants were found. Along with them, crust of
deciduous trees was detected at an almost complete ab-
sence of macro-remains of coniferous species. Pine, whose
pollen is abundant in all spectra, grew probably at the
slopes of the valley and water divides rather than in a bog.
Three palynological zones are identified in the diagram.
Based on the results of the palynological analysis,
a spore-pollen diagram was constructed (Fig. 2), where
in accordance with the adopted subdivision scheme of the
Mikulino Interglacial (Grichuk, 1961 and 1989), the fol-
lowing 3 palynological zones are delineated:
 NEW AGE DATA OF BURIED PEAT DEPOSITS FROM THE SITE “FILI PARK” (MOSCOW , RUSSIA) ...

l the first zone correlated with palynozone M2 of
Mikulino diagrams, refers to the lower peat layer, char-
acterized by the spectrum of sample 11. Pine domi-
nates here with the pollen of birch and alder present
in much smaller quantity. In single cases, the pollen
of willow and hazel was observed. The pollen of broad-
leaved species is absent. Among herbaceous and dwarf
shrub plants, Artemisia and Chenopodiaceae predomi-
nate, with sedge and grass being more rare. The com-
position of meadow herbage is relatively diverse, with
Ephedra noted. The data obtained indicate the devel-
opment of floristically poor monodominant pine and
birch forests (probably with small participation of
spruce). Such vegetation cover based on the published
data for the central areas of East Europe existed at
the beginning of the Mikulino Interglacial;
l the second zone, Μ3, according to Grichuk (1961 and
1989) reflects the appearance of pollen of broad-
leaved oak and elm species. Maple is sporadically
observed. Among herbs, the role of Poaceae and
Cyperaceae increases but Ephedra is still encountered;
l the third zone, M4, considered by Grichuk (1961 and
1989) as the initial zone of the climatic optimum
of the Mikulino Interglacial, corresponds to the time
of spreading of oligodominant broad-leaved forests of
oak and elm with hazel in the underbush and alder.
Thus, the first half of the Mikulino Interglacial is re-
flected in the diagram. A similar change of forest forma-
tions is traced in numerous paleobotanical materials pub-
lished for the central areas of the East European Plain
(“Moscow Ice Sheet of East Europe”, 1982).
The principal assumptions of using the uranium-thorium
method for dating buried peat
The UTD-method has two basic assumptions: 1) the
system to be dated should behave like a closed geochemi-
cal system with regard to U and Th; 2) there had to be no
Th at the initial moment of peat formation. However,
many of the peat sections studied earlier (Hejnis et al.,
1993; Heijnis, 1995) are contaminated with varying
amounts of detrital material. This contributes some 230Th,
234
U and 238U to the solution/leachate prepared during
chemical analysis. In such a case a mathematical correc-
tion should be done to determine the present-day
230
Th/234U ratio in fraction to be dated.
Several methods have been proposed to make a cor-
rection for detrital Th. The first one – the so-called
„leachate/residue” model for carbonate and peat samples
– was studied by Ku et al. (1979), Ku and Liang (1984)
and van der Wijk (1987). The second method is the
“leachate alone” model. It was proposed and studied in
detail by Schwarz and Latham (Schwarz and Latham,
1989). And the third method, the so-called „total sample
dissolution” model, was represented by Bischoff and
Fitzpatric (Bischoff and Fitzpatric, 1991). We use the
“leachate alone” method for our work.
Distribution of U and Th in vertical profile of the section
The results of radiochemical study of peat deposits
from the “Fili Park” section (Moscow) are given in Table 1
and Fig. 3. The vertical distribution of uranium, thorium
and the U/Th ratio in the organic fraction of samples and
the ash content can be compared with the distribution of

Table 1. Results of radiochemical analysis of peat samples from the section "Fili Park".
Sample Depth Ash U Th 238U/232Th Layers
[cm] [%] [ppm] [ppm]
LU-4343 0-5 17.52 10.39±0.38 2.40±0.20 4.33±0.39 A
LU-4331 5-10 10.40 6.03±0.21 1.02±0.06 5.91±0.35
LU-4342 10-15 9.18 5.14±0.24 0.73±0.04 7.04±0.50
LU-4327 15-20 11.27 6.54±0.19 0.69±0.04 9.48±0.62
LU-4341 20-25 10.78 7.94±0.21 0.45±0.02 17.64±0.91 B
LU-4329 25-30 9.68 3.71±0.13 0.53±0.02 7.00±0.35
LU-4340 30-35 10.82 4.44±0.21 0.41±0.02 10.83±0.68
LU-4330 35-40 10.61 6.24±0.10 0.45±0.02 13.87±0.72
LU-4344 40-45 10.62 11.90±0.39 0.57±0.04 20.78±1.52 C
LU-4328 45-50 18.99 30.53±0.58 3.17±0.12 9.63±0.41

Table 1 (continued)
Depth 238U 234U 230Th 232Th 234U/238U 230Th/234U 230Th/232Th Age Layers
[cm] [dpm/g] [dpm/g] [dpm/g] [dpm/g] [dpm/g] [dpm/g] [dpm/g] [yrs]
0-5 7.48±0.27 9.12±0.33 5.09±0.14 0.59±0.05 1.22±0.06 0.56±0.03 8.63±0.77 88700±6200 A
5-10 4.34±0.15 5.40±0.18 3.25±0.05 0.25±0.01 1.24±0.06 0.60±0.02 13.00±0.56 99700±6000
10-15 3.70±0.17 4.77±0.21 2.95±0.06 0.18±0.01 1.29±0.08 0.62±0.03 16.39±0.97 105000±8400
15-20 4.71±0.14 6.05±0.18 3.22±0.03 0.17±0.01 1.28±0.05 0.53±0.02 18.94±1.13 82500±3900
20-25 5.72±0.15 7.84±0.19 4.52±0.08 0.11±0.01 1.37±0.05 0.58±0.02 41.09±3.81 93300±4400 B
25-30 2.67±0.09 3.54±0.11 1.95±0.04 0.13±0.01 1.33±0.06 0.55±0.02 15.00±1.19 86400±5000
30-35 3.20±0.15 3.92±0.18 2.03±0.05 0.10±0.01 1.23±0.08 0.52±0.02 20.30±2.09 78900±6000
35-40 4.49±0.15 5.82±0.19 2.40±0.06 0.11±0.01 1.30±0.06 0.41±0.02 21.82±2.06 57600±3000
40-45 8.57±0.28 10.23±0.34 2.44±0.05 0.14±0.01 1.19±0.06 0.24±0.01 17.43±1.30 29500±1300 C
45-50 21.98±0.42 24.16±0.46 12.10±0.11 0.78±0.03 1.10±0.03 0.50±0.01 15.51±0.61 75300±2300

44
 V.Yu. Kuznetsov et al.

the same data by the depth of the earlier investigated
stratotypical section of the Mikulino Interglacial sedi-
ments in the territory of the Russian Plain (Mikulino vi-
llage, Smolensk province). As can be seen from the plots
in Fig. 3, the general tendency in the distribution of U,
Th, U/Th and ash contents is in general preserved for both
sections. Similar dynamics of changes of these values by
the “Mikulino” section depth, on the one hand, and the
constant and least values of U, Th, U/Th and ash content
in the central layer B, on the other hand, allowed a re-
liable identification of the inner “Mikulino” section
portion suitable for UTD. The corrected age of layer B,
calculated by the method of isochrones (Schwarz and
Latham, 1989; Heinis et al., 1993) comprised 113±11 ka
(Kuznetsov et al., in press). Good correlation is observed
in the “Fili Park” section in respect of the distribution of
uranium, thorium and ash content whereas the change of
U/Th values by the depth of deposits has a more compli-
cated character (Fig. 3). Based on the first three distribu-
tions, one can note that two upper and low layers are
enriched with uranium and thorium (at increased ash
content) compared to the internal layers. This can prob-
ably testify to a relative closeness of groundwater in whose
composition the dissolved uranium and the detrital forms
of uranium and thorium could be supplied to the buried
peat deposits. Then the upper and lower layers could be
considered as peculiar filters concentrating these radio-
nuclides of different genesis and preventing penetration

0-5
AA
5-10

10-15

15-20
Depth B
20-25
(cm)

25-30

30-35

35-40
C
40-45
Fig. 3a. Distribution of 238 U,
232 Th contents, 238 U/ 232 Th
45-50
ratios and ash values
0 10 20 30 0 1 2 3 4 0 10 20 30 0 10 20 30 40 of peat samples in the
vertical profile of the
U, ppm Th, ppm U/Th Ash (%) section "Fili Park".

5-10

A
30-35

45-50

60-65
B
Dept 70-75
h
(cm) 80-85

90-95

100-105 C

Fig. 3b. Distribution of 238 U,

110-115 232 Th contents, 238 U/ 232 Th

0 10 20 30 0 1 2 3 4 0 10 20 30 0 10 20 30 40 ratios and ash values of

peat samples in the vertical
U, ppm Th, ppm U/Th Ash (%) profile of the section
"Mikulino".

45
 NEW AGE DATA OF BURIED PEAT DEPOSITS FROM THE SITE “FILI PARK” (MOSCOW , RUSSIA) ...

of uranium and thorium inside the sedimentary strata. calculated. This age coincides with the 18O deep-sea stage
It follows from the description of the “Fili Park” outcrop 5b (Morley and Hays, 1981). However, the data of the
and spore-pollen diagram that the section investigated in spore-pollen analysis mentioned above testify that bur-
this work was washed out in its upper portion either quite ied peat from the section under study dates back to the
recently or at the glacial time. Due to this, the upper lay- first half of the Mikulino (Eem) Interglacial and corre-
ers of deposits (5-10 cm) accumulated the transported lates with the 18O deep-sea stage 5e. Probably, the cor-
uranium and thorium in smaller quantities than the low- rected uranium-thorium age obtained for the deposits is
est layers (40-50 cm). Hence, one can assume that the likely to be a little younger. It can be a result of the prob-
geochemical barrier thickness in respect of uranium and able post-depositional insignificant supply of uranium with
thorium should be greater in the lower section portion ground water into internal parts of the section (i.e., layer
than in the upper and comprise at least about 15 cm (in B cannot be considered as a completely-closed geochemi-
the interval of layers between 35 to 50 cm). In other words, cal system). In fact, the differences of uranium/thorium
all samples from peat layers A and C are suspected to be ratios along the length of the section (Fig. 3) might be
in the zone of open geochemical system in respect to U due to an additional uranium supply and correspondingly
and Th. Correlation of the uranium and thorium con- to a little younger age as a whole.
centrations with ash contents are remarkable in the inner
peat layer B. Besides, U, Th and ash contents are practi- 5. CONCLUSIONS
cally constant and least in the layer B. The data obtained
enabled to consider the inner part (layer B) of the peat as The internal part of the “Fili Park” section cannot be
a more or less closed system with regard to U and Th and considered as a completely-closed geochemical system
the uranium-thorium dating was applied. with regard to uranium. There was probably an additional
post-deposition uranium uptake in the internal section
Age results
The results of direct UTD measurements of all stud-
ied buried peat samples are summarised in Table 1. The
dating by the uranium/thorium method of the middle sec-
tion part (layer B) shows that individual uncorrected
sample ages are in the range of 78,9-105 ka. However,
the 230Th/ 232Th ratio indicates a presence of varying
amounts of thorium in the organogenic fractions, and
therefore a correction was applied. It is known that in the
process of peat dissolving, some quantities of 230Th, 232Th,
238
U and 234U can transfer from a clay component (detri-
tus) in a leachate/solution. This causes a distortion of the
230
Th/234U and 234U/238U ratio values in the sample organic
fraction dated. The fact of the detrital uranium and thorium
addition is established by the presence of 232Th in a sample
organic fraction because this long-lived isotope can be
present in peat sediments only in detritus. So, in order to
determine the „true” age of buried peat it is necessary to
know the value of 230Th/234U (for today) in the organic frac-
tion under dating. The mathematical correction of the
direct uranium-thorium dates is used with application of
the isochrones method. The essence of the method is that
when dissolving the coeval peat samples, the uranium and
thorium isotopes enter in a leachate/solution in the same
proportions (under the same conditions of an experi-
ment). In this case, the isotope ratio values obtained shape
a straight line on the 234U/232Th-238U/232Th and 230Th/232Th-
234
U/232Th graphs. The inclinations of the isochrones con-
structed in such a way correspond to the 234U/238U and
230
Th/234U ratios corrected to the detritus supply and are
used then when calculating the „true” absolute age of the
buried peat samples under study. Thus, using the „leach-
ing alone” method (Schwarz and Latham, 1989; Hejnis et
al., 1993), the results of the direct UTD measurements
were plotted on the isochrone plots. Five inner layers that
Fig. 4. Plots of 230Th/ 232Th vs 234U/232Th and 234U/232Th vs 238U/232Th
were interpreted to be in the more or less closed-system for leachates of the „Fili Park” samples; 230Th/234U and 234U/238U
were used to construct the isochron plots (Fig. 4). From as determinated from the slopes of the respective lines give an
the isochron plots, the corrected age of 89±11 ka was apparent age of 89±11 ka.

46
 V.Yu. Kuznetsov et al.
layers that in general have led to an underestimated age
value. Nevertheless, the corrected uranium-thorium date
of 89±11 ka of the buried peat was much of an age with
the currently adopted boundaries of the last Interglacial
(116-128 ka).
The results of palynological analysis were in accor-
dance with the adopted subdivision scheme of the
Mikulino (Eem) Interglacial.
The geochronological and palynological studies of the
buried peat layer from the “Fili Park” section located in
the Filevsky Park in Moscow allowed us to refer these
questionable in chronostratigraphic respect deposits to the
Mikulino (Eem) Interlacial.
The uranium-thorium dating of the closed geochemi-
cal samples from the inner part of the stratotypical
“Mikulino” section (Russian Plain) yielded the reliable
corrected age of 113±11 ka. This date corresponds to the
Mikulino (Eem) Interglacial and correlates with the 18O
deep-sea stage 5e.
ACKNOWLEDGEMENT
The work was supported by the Russian Foundation
of Basic Researches, grants No. 98-05-64764, No. 01-05-
64870.
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Bischoff J.L. and Fitzpatrick J.A., 1991: U-series dating of impure
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GrimmE., 1991: Tilia 1.12, Tilia-Graph 1.18. Illinois State Museum,
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Ku T.L. and Liang Z.C., 1984: The dating of impure carbonates with
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Kuznetsov V.Yu., Arslanov Kh.A., Cherkashev G.A., Shilov V.V. and
Maksimov F.E., 1998: New approach to geochronology of Mid
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(in Russian).
Kuznetsov V.Yu., Arslanov Kh. A., Chernov S.B., Maksimov F.E.,
Savelyeva L.A. and Kozlov V.B.: Uranium-thorium dating the
stratotypical section of the Late Quaternary Interglacial bur-
ied peat bog on the Russian Plain (in press).
Kuznetsov V.Yu., Arslanov Kh.A., Maksimov F.E., Savelieva L.A.
and Chernov S.B., 2000: Possibilities of uranium/thorium dat-
ing of Late Quaternary organogenic deposits from the Russian
Plain. Quaternary Environment of the Eurasian North (QUEEN).
Fourth QUEEN Workshop. Sweden: 27.
Kuznetsov V.Yu., Arslanov Kh.A., Shilov V.V., Cherkashev G.A. and
Maksimov F.E. 2000: Uranium and thorium distribution in
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North Atlantic. Radiochimija 6: 565-568 (in Russian).
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deep-sea chronology for the last 750,000 years. Earth and Plane-
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Pisareva V.V. and Lobachev I.N., 1982: Moscow glacial cover of the
Eastern Europe. Moscow, Nauka: 57-60 (in Russian).
Schwarcz H.G. and Latham A.G., 1989: Uranium series dating of
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van der Wijk A., El-Daoushy F., Arends A.R. and Mook W.G., 1986:
Dating peat withU/Th disequilibrium: some geochemical con-
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van der Wijk, A.r, 1987: Radiometric dating by Alpha spectrometry
on Uranium series nuclides. PhD thesis, University of Gronin-
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van der Wijk A., Ivanovich M. and Mook W.G., 1988: Correction
for environmental 230Th in U/Th disequilibrium dating peat.
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Vogel, J. and Kronfeld, J. 1980: A new method fer dating peat. South.
Africa Sci. 76: 557-558.
 GEOCHRONOMETRIA Vol. 21, pp 49-56, 2002 – Journal on Methods and Applications of Absolute Chronology

230
Th/U AND 14C DATING OF MOLLUSC SHELLS FROM
THE COASTS OF THE CASPIAN, BARENTS, WHITE
AND BLACK SEAS

Kh.A. ARSLANOV1, N.I. TERTYCHNY1, V.Yu. KUZNETSOV1, S.B. CHERNOV1, N.V. LOKSHIN1,
S.A. GERASIMOVA1, F.E. MAKSIMOV1 and A.E. DODONOV2
1
Geographical Research Institute, Saint-Petersburg State University, 199004, St.Petersburg, Sredny pr. 41, Russia
2
Geological Institute of the Russian Academy of Sciences, Moscow, Pyzhevsky Str. 7, Russia

Key words
words: Abstract: We dated Holocene and Late Pleistocene mollusc shells collected from coastal sedi-
URANIUM-THORIUM ments of the Caspian, Barents, White and Black Seas by means of both a modified 230Th/U
DATING, method and the radiocarbon method. Essence of the modification is the removal of the sur-
RADIOCARBON DATING, face (about 1/3 of the weight) of the mollusc shells by nitric acid as it may contain adsorbed
GEOCHRONOLOGY, detrital 232Th and 230Th. The 230Th/U dates of the inner part of the shells do not require detrital
TRANSGRESSION, correction with the 232Th activity and well agree with the corresponding reservoir-corrected
MOLLUSC SHELLS and calibrated 14C ages of mollusc shells with ages between 1300 and 13,500 BP.
We tested the modified 230Th/U method on thick-walled and well-preserved mollusc shells
from the transgression sediments of the Barentz, White and Black Seas derived during the
Mikulino Interglacial (MIS 5e) and the Early Valday Glaciation (MIS 5c). The 230Th/U ages of
the inner part of the shells from the Boreal (Eem) transgression sediments of the Barentz and
White Seas ranged from 86 to 114 ka and those from the Karangat (Eem) transgression in the
Black Sea (Maly Kut and Eltigen sections) from 95 to 115 ka. The new 230Th/U dates of the
shells from the section Eltigen ranged from 100 to 125 ka..

1. INTRODUCTION ously, comparison of the mollusc shell ages should be

230
Th/U dating of biogenic calcium carbonate (mollusc
shells, corals etc.) depends on three basic requirements: a)
uranium was incorporated into the biogenic calcium
carbonate during its formation and soon after the death
of the animal; b) the carbonate does not contain any no-
ticeable amounts of 232Th and detrital 230Th; c) the sample
behaved as closed system during aging in the sediments.
That means that neither loss nor accumulation of uranium
and thorium occurred.
Uranium is incorporated into corals during their for-
mation. Migration of uranium and thorium isotopes has
not been observed (Veeh, 1966; Kaufman et al., 1971).
However, uranium migration is recorded for fossil mol-
lusc shells subjected to groundwater action. Kaufman
et al. (1971) found that about 50% of 230Th/U dates from
60 mollusc shells deviate from the known Pliocene or
Pleistocene age. During geological time ranges (million
years) mineralogical, physical and chemical processes
might have accompanied by uranium migration. Obvi-
made within the age range of the method (300 ka).
Until now 230Th/U dating has been carried out on the
entire shells through radiocarbon dating of mollusc shell
demonstrated that the surface part of the shells behaves
as open system and often contains a secondary changed
14
C activity due to isotope exchange and diffusion pro-
cesses (Olsson and Blake, 1961/1962; Arslanov, 1987).
Similarly, the uranium isotope activity of the inner and
outer parts of shells may also be modified.
We analyzed the 238U, 234U, 232Th and 230Th specific acti-
vities of the surface, the outer layer and the inner part of
recent and fossil mollusc shells in order to study uranium
isotope migration within the shells. For this parallel radio-
carbon and uranium-thorium dating of the same samples
of mollusc shell with known ages within and just above
the dating range of the 230Th/U method were done. As first
test of the modified 230Th/U dating method of mollusc
shells collected from transgressive deposits of the White,
Barents and Black Seas were dated and correlated with
the Riss-Wrmian (Eem) transgression of the World Ocean.
 230
Th/U and 14C DATING OF MOLLUSC SHELLS FROM THE COASTS ...

2. METHODS 2. Passing of solution through the column filled with

Three of the authors (Kh.A.Arslanov, N.I.Tertychny
and N.V.Lokshin) collected recent mollusc shells from
many large rivers (Volga, Kama, Belaya, Zapadnaya
Dvina, Berezina and Dnieper) and from the coasts of the
Azov, White, Baltic and Caspian Seas in 1969 and 1970.
These authors together with many geologists and geogra-
phers selected fossil mollusc shells from reference sections
during 1969-1982. A.E.Dodonov submitted shells from the
reference profile Eltigen taken in 1998. Most of the geo-
chronological results were earlier published in Russian
Journals (Arslanov et al. 1977, 1978, 1981 and 1983).
The protocol of the radiochemical procedure to iso-
late uranium and thorium from mollusc shells was pub-
lished by Arslanov et al. (1976 and 1981). The following
steps were done:
1. Separation of the surface, the outer layer and inner
part of the mollusc shells by nitric acid after cleaning,
washing and drying (at 105 °C).
2. Admixture of known quantities of 234Th and 232U spikes
and Fe(NO3)3 (10 mg Fe) to the three sample fractions
in solution and co-precipitation of uranium and tho-
rium isotopes on Fe(OH)3 by passing carbon-free am-
monia through hot solution until pH=7-8 is attained.
3. Dissolution of the washed Fe(OH)3 residue in 4.5n HCl
and passing of obtained solution a column filled with
Teflon powder impregnated with di-2-ethylhexyl phos-
phoric acid in diethyl ether.
4. Successive extraction of uranium and thorium from
the column with 15 ml of concentrated HCl and with
20 ml of 0.5n oxalic acid solution, respectively.
5. Electrochemical deposition of uranium and thorium
on platinum disks from ethyl alcohol solution.
Recently, the stages 3-4 was altered (Kuznetsov et al.,
2000):
1. Dissolution of Fe(OH)3 with co-precipitated of ura-
nium and thorium in 7n HNO3 solution.
anion-exchange resin AV-17.
3. Successive extraction of thorium and uranium by 6n
HCl and 0.2n HNO3, respectively.
4. Electrochemical deposition of uranium and thorium
on platinum disks from ethyl alcohol solution.
The α-activity of 234U, 238U, 232U, 230Th and 232Th depo-
sited on platinum disks was measured with a silicon de-
tector of an area of 5 cm2 and the pulse analyzer AI-128
and AI-1024. Chemical yields of uranium were calculated
from the activities of the 232U and 234Th spikes. The count-
ing efficiency for uranium and thorium isotopes was
checked with a transuranium (239Pu and 241Am) standard
of known activity. Radiocarbon dating of mollusc shells
was done with benzene liquid scintillation counting
(Arslanov et al., 1993).
3. RESULTS
In order to study uranium transfer from groundwater
into recent mollusc shells, we determined the uranium
activity of 30 alive mollusc shells (Anadonta) from sev-
eral rivers of the European part of Russia and Belarus
(Volga, Kama, Oka, Belaya, Berezina, Zapadnaya Dvina
and Dnieper) and marine shells from the coasts of the Azov,
Black, Caspian and Baltic Seas. The uranium concentra-
tion of the river shells determined by luminescent tech-
nique ranged between 1.0-5.9·10-3 ppm and its distribution
through the shells was uniform (Arslanov et al., 1975).
The uranium concentration of marine mollusc shells
ranged from 2.5·10-3 to 0.65 ppm (Table 1).
Sea molluscs Mytilus edule contained 3.3·10-3 - 8.3·10-3
ppm uranium (Arslanov et al., 1975). Both the Mytilus
mollusc species and the fluvial Anadonta shells contained
high concentration of organic matter. The uranium con-
centration in the isolated organic matter of Mytilus edule
shell amounted to 0.5·10-3 ppm while the maximum value

Table 1. Uranium concentration in recent marine mollusc shells.

Seashore Mollusc species Uranium concentration [ppm]
Surface Outer layer Inner part
-3 -3 -3
Sea of Azov Mytilus edule, alive 5.8· 10 8.0· 10 8.3· 10
Caspian Sea Cardium edule 0.65 0.59 0.2
-3 -3
White Sea Mytilus edule, alive 4.5· 10 - 1.7· 10
-2
Baltic Sea, near Chione gallina, alive 5.0· 10 - -
-2 -2 -2
Klaipeda Chione gallina 4.7· 10 3.0· 10 2.1· 10
-2
Cardium edule 8.4· 10 - -
-3 -3 -3
Anadonta 3.9· 10 3.9· 10 3.3· 10
-2 -2
Dreiscenia 0.16 7.5· 10 4.5· 10
-2 -2 -2
Dreiscenia, alive 2.0· 10 1.8· 10 1.2· 10
-3 -3 -3
Black Sea, Mytulus edule, alive 2.5· 10 2.8· 10 3.8· 10
Taman peninsula Donox trinc, alive 0.13 0.09 0.09
Cardium edule, alive 0.17 0.10 0.075
-2 -2 -2
Clamus glabara 2· 10 2· 10 2.2· 10
-2 -2 -2
Chione gallina, alive 4.5· 10 1.75· 10 1.75· 10
Chione gallina 2.3 2.3 1.8
Cardium elule - 0.60 0.42
-2 -2 -2
Ostrea edulis 2.2· 10 2.0· 10 2.0· 10
-2 -2 -2
Gastropod, alive 1.1· 10 0.8· 10 0.9· 10

50
 Kh.A. Arslanov et al.

of 0.65 ppm was found in Cardium edule mollusc shells and fossil shells in river and marine young banks (Table 2).
from the Caspian Sea. Recent shells from the Baltic and In recent shells with lower organic matter (Dreissenia,
Black Seas had about 10-2 ppm. In general, the shells of Donox, Cardium edule and Chiohe gallina), highest ura-
alive molluscs contain less uranium (Table 1) than dead nium concentration is found in the surface layer. Gener-

230
Table 2. Uranium concentration and Th/U ages of fossil mollusc shells (A – outer layer, B – inner part).
Mollusc species and locality Lab. No Age Uranium
[BP] [ppm]
Cardium edule, Mamedkala 190A 2050±90 0.85±0.04
Settlement, Dagestan Republic 190B - 0.65±0.02
Same as above LU-191A 1570±100 1.50±0.05
LU-191B
1640±100 1.35±0.05
Cardium edule, Shirvan area, Azerbaijan LU-422A - 2.00±0.03
LU-422B 3400±90 -
Undetermined species, Dzhorat LU-421A - 2.40±0.03
settl., Apsheron peninsula, Azerbaijan LU-421B 5540±110 -
Didacna sp., Duvannye settlement Azerbaijan LU-192A 13,140±150 3.90±0.02
LU-192B
13,200±250 4.10±0.05
Didacna sp., Amia Cape, LU-193A - 1.20±0.06
Azerbaijan LU-193B 12,480±150 1.00±0.05
Didacna sp., Shirvan area, LU-423B 12,330±140 4.5±0.02
Azerbaijan
Didacna sp., near Maloye Turaly Lake, Dagestan Republic LU-424A 13,110±490 3.60±0.18
LU-424B
12,720±400 3.80±0.19
Didacna sp. Near Manas River mouth, Dagestan Republic LU-426A 12,700±450 6.00±0.30
LU-426B
12,500±300 5.40±0.27
Didacna sp. Shamkhal-Termen LU-432B 76,000±4000 7.30±0.30
Settl., Dagestan Republic
Same as above LU-400B 81,000±2000 2.50±0.40
Didacna sp. Shirvan, LU-430A 109,000±5000 5.50±0.20
Azerbaijain LU-430B
114,000±4000 5.70±0.20
Didacna sp, right bank of Achisu River, Dagestan Republic LU-401B ³300,000 2.5±0.04
Didacna sp, Apsheron peninsula, Azerbaijan LU-434A ³300,000 2.9±0.14
LU-434B
³300,000 3.20±0.16
Didacna, Aljatskaya Hill, Khanaly-Kyshlak settl., Azerbaijan LU-431A ³255,000 15.60±0.75
LU-431B
³300,000 14.80±0.74
Chione gallina, near Tuapse City LU-308B £2000 0.40±0.02
Dreissenia polymorpha, Pitsunda Cape, Abkhazia LU-413B
47,000±1700 1.00±0.02
Paphia senescens, Eltigen section, eastern coast of Kerch Strait LU-402A 96,000±2500 1.20±0.06
LU-402B
88,000±3000 0.95±0.03
Cardium edule, Malye Kut Section, Taman peninsula LU-403A 96,000±2500 2.60±0.10
LU-403B
85,000±3000 1.37±0.01
Chione gallina, Adler settl., near Sochi City LU-404A 76,000±3000 1.7±0.08
LU-404B
73,000±3000 2.20±0.11
Chione gallina, Tuzla Cape, Taman peninsula LU-410A 70,000±2500 4.60±0.18
LU-410B
65,000±3000 4.30±0.15
Chione gallina, Ashe River mouth, Krasnodar krai LU-409A 133,000±5000 1.61±0.08
LU-409B
139,000±12000 1.31±0.06
Cardium edule, west Manych River terrace LU-450A - 2.12±0.06
LU-450B 33,320±520 1.81±0.06
Cardium edule, Split Chyshka, Taman Peninsula LU-449B 40,700±1200 -
Chione gallina and Cardium edule, same as above LU-448A - 6.61±0.19
LU-448B 41,250±1340 1.00±0.02
Paphia senescens, Golubaya Dacha Settl., Krasnodar Krai LU-406A 124,000±3500 1.00±0.02
LU-406B - 1.07±0.03

51
 230
Th/U and 14C DATING OF MOLLUSC SHELLS FROM THE COASTS ...

ally, the initial organo-mineral complex of shells contains
only very little uranium.
Fossil mollusc shells have as high as two orders of
magnitude higher uranium concentration (Table 2) than
recent shells (Table 1). In most cases the uranium con-
centration was slightly lower in the inner part than in the
outer layer (Arslanov et al., 1975).
The 234U/238U activity ratio was higher than the ave-
rage value of seawater of 1.14±0.014 (Arslanov et al.,
1976). It is known that groundwater often has a higher
234
U/238U ratio (Cherdyntsev, 1969).
232
Th and 230Th activities were determined from the
surface of nine fossil mollusc shells (Table 3). All samples
contained adsorbed detrital thorium. Only two out of 33
mollusc shells contained 232Th in the outer layer. 232Th was
absent in the inner layer of all analyzed samples.
The reliability of the modified 230Th/U method was
checked by complementary radiocarbon dating of eight
stratigraphically well-dated Holocene and Late Glacial
mollusc shells (Table 4). In addition, fossil Pleistocene
mollusc shells from Lower Khazarian deposits of the
Caspian Sea with age ≥300 ka were dated. The 14C dates
were reservoir-corrected by subtracting of 384±59 years
for Caspian shells and calibrated using the Groningen
Radiocarbon Calibration Program Cal-25.
The modified 230Th/U dating method was applied to
transgressive sediments in the White, Barents and Black
Seas. The large Karangat transgression of the Black Sea
and the Boreal (Eemian) transgression and study of the
White and Barents Seas are correlated with Mikulino
Interglacial (MIS 5e) based on the results of microfau-
nal, diatom, pollen and lithostratigraphic investigations
of thermophile species of shells (Arslanov et al., 1981 and
1983). According to the chronology of MIS (oxygen-iso-
tope record from deep-sea cores; Martinson et al., 1987),
MIS 5e (Eemian, Sangamon – 125 to 115 ka) corresponds
to the Mikulino Interglacial. Hence, the mollusc shells
from the geochronostratigraphic reference sections for
the Karangat and Boreal transgressions are considered
as stratigraphically well-dated.
Thick-walled and well-preserved mollusc shells from
transgressive sediments of the Barents, White and Black
Seas were selected for dating. Most of the results are

Table 3. Specific activity of thorium isotopes of fossil mollusc shells (in dpm/g).
Sample No Surface Outer layer Inner part
232 230 232 230 232 230
Th Th Th Th Th Th
LU-424 0.036 0.283 ≤ 0.005 0.181 ≤ 0.005 0.200
LU-421 0.015 0.076 ≤ 0.005 0.060 ≤ 0.005 0.066
LU-420 0.012 0.031 ≤ 0.005 0.012 ≤ 0.005 0.016
LU-413 0.029 0.219 ≤ 0.005 0.150 ≤ 0.005 0.150
LU-430 0.140 1.712 ≤ 0.005 1.669 ≤ 0.005 1.662
LU-436 0.086 0.952 ≤ 0.005 0.752 ≤ 0.005 -
LU-414 0.079 0.136 ≤ 0.005 0.043 ≤ 0.005 0.043
LU-432 0.040 1.940 ≤ 0.005 1.916 ≤ 0.005 1.916
LU-428 0.050 1.079 ≤ 0.005 0.993 ≤ 0.005 0.993
LU-192 - - ≤ 0.005 0.428 ≤ 0.005 0.400
LU-424 - - ≤ 0.005 0.181 ≤ 0.005 0.200
LU-190 - - ≤ 0.005 0.010 ≤ 0.005 0.012
LU-191 - - ≤ 0.005 0.050 ≤ 0.005 0.040
LU-422 - - ≤ 0.005 - ≤ 0.005 0.040
LU-193 - - ≤ 0.005 0.143 ≤ 0.005 0.179
LU-423 - - ≤ 0.005 - ≤ 0.005 0.234
LU-400 - - ≤ 0.005 - ≤ 0.005 1.310
LU-429 - - ≤ 0.005 1.134 ≤ 0.005 -
LU-435 - - ≤ 0.005 - ≤ 0.005 2.266
LU-401 - - ≤ 0.005 - ≤ 0.005 1.735
LU-434 - - ≤ 0.005 1.362 ≤ 0.005 1.307
LU-431 - - ≤ 0.005 8.619 ≤ 0.005 8.595
LU-308 - - ≤ 0.005 - ≤ 0.005 0.007
LU-413 - - ≤ 0.005 - ≤ 0.005 0.150
LU-402 - - ≤ 0.005 0.229 ≤ 0.005 0.193
LU-403 - - ≤ 0.005 0.738 ≤ 0.005 0.679
LU-404 - - ≤ 0.005 0.400 ≤ 0.005 0.522
LU-410 - - ≤ 0.005 1.059 ≤ 0.005 0.926
LU-406 - - ≤ 0.005 0.415 ≤ 0.005 0.362
LU-450 - - ≤ 0.224 0.245 ≤ 0.005 0.243
LU-448 - - ≤ 0.166 1.053 ≤ 0.005 0.759
LU-449 - - ≤ 0.005 - ≤ 0.005 0.522

52
 Kh.A. Arslanov et al.

230
Table 4. Th/U and 14C ages of mollusc shells from the Caspian Sea. A=outer layer and B=inner part.
14 230
Mollusc species and location Lab. No C Age Age Th / U
[BP] [Cal BP] Age [BP]
Cardium edule, Zorat Settl., Azerbaijan LU-476B 1510±70 1511 – 1313 1330±300
Cardium edule, Mamedkala Settl., Dagestan Republic LU-190B 2050±90 2145 – 1897 ≤ 2450
Cardium edule, Shirvan area, Azerbaijan LU-422B 3400±90 3821 – 3481 4100±300
Dzhorat settl., Apsheron peningula, Azerbaijan LU-421B 5540±110 6445 – 6200 6400±300
Didacna paralella, near Manas River mouth, LU-426A 11,600±400 14,000 – 13,100 12,700±450
Dagestan Republic LU-426B - - 12,700±450
At 48-th km from Baku, between railway stations LU-479B 11,550±90 13,795 – 13,425 11,800±350
Nasosnaya and Jashma, Azerbaijan LU-479A 11,680±160 13,820 – 13,485 12,900±350
Didacna sp. Shirvan, Azerbaijan LU-423B 12,330±140 15,055 – 14,125 14,400±400
Didacna sp., near Maloye Turaly Lake, Dagestan Republic LU-424B 12,720±400 15,600 – 14,425 13,800±440

already published in Russian (Arslanov et al., 1981 and 4. DISCUSSION

1983). Only the samples LU-4202-4215 submitted by
A. Dodonov in 1998 were recently analyzed Table 5.
The inner part of the mollusc shells from Boreal trans-
gression deposits of the White and Barents Seas yielded
230
Th/U ages of 86-114 ka, whereas that of shells from the
Karangat transgression of the Black Sea (Maly Kut,
Eltigen sequences) ranged between 102 and 130 ka. Mol-
lusc shells found with paired valves under living condi-
tions from the estuary clay section of Cape Krotkov were
dated to 98-100 ka (Table 5). This clay sequence contained
93 – 98% pollen of wood species (pine pollen: 55-65%;
spruce pollen: 27-35%; birch pollen: 12%; Arslanov et al.,
1983). Single pollen of beech, elm and oak represent
broad-leaved species. This pollen assemblage essentially
corresponds to that of the taiga forest and, most likely,
correlates with the beginning of the Valdai (Weichselian)
Glaciation.
Shells of an age of 1.5-2.0 ka contained up to two
orders of magnitude more uranium than recent shells.
However, we did not found a strong correlation between
the uranium concentration and the 230Th/U age. Hence,
the incorporation of the major portion of uranium into
shells ceases after several thousands of years in agreement
with the findings by Broecker (1963). The decomposition
of the organic matter of the mollusc shells enables the in-
corporation of uranium into the porous structure. Ura-
nium is incorporated into mollusc shells as more or less
soluble salts (uranotallite, swartzite and andersonite) or
as complex uranium compounds with albumen present in
the conchiolin of the shells.
The 234U/238U activity ratio >1.15 gives evidence that
the major portion of uranium in shells stems from ground-
water and is postsedimentarily incorporated.

Table 5. 230Th /U Ages of marine mollusc shells from transgression sediments of the Barents, White and Black Seas.
A = outer layer and B = inner part.
Lab. No Age [BP] Mollusc species and location
LU-455B 97,000±4000 Cyprina islandica from the section base, Svjatonossky gulf, Kola peninsula
LU-452A 102,000±4000 Astarta borealis from the Malaja Kachovka exposure, Kola peninsula
LU-452B 114,000±4000
LU-464A 85,500±3200 Cyprina islandica from the exposure On Chapoma River, Kola peninsula
LU-464B 86,000±3900
LU-808A 129,400±4900 Cardium edule from the marine sediments of Maly Kut section, Taman peninsula
LU-808B 115,000±3100 Same as above
LU-805A 125,000±5000 Paphia senessens from the middle part of the marine sediments of Eltigen section, eastem coast of Kerch strait
LU-805B 102,290±3200 Paphia senessens from the middle part of the marine sediments of Eltigen section, eastem coast of Kerch strait
LU-802A 90,600±3100 Cardium tuberculatum from the same layer
LU-802B 107,400±3800 Cardium tuberculatum from the same layer
LU-804-1A 88,900±2200 Cardium edule from the Krotkov cape section, westem part of Taman peninsula
LU-804-1B 98,000±2400 Same as above
LU-804-2A 98,900±2200 Same as above
LU-804-2B 100,500±2100 Same as above
LU-4022B 127,000±8900 Thick-wall, good preserved shells from the marine sediments of Eltigen Sections,
eastern coast of Kerch strait depth 2.6 m a.s.l.
LU-4203 107,000±7700 Same as above, depth 8.0 m a.s.l.
LU-4214 127,000±7700 Same as above, depth 13.8 m a.s.l.
LU-4205 117,000±11000 Same as above, depth 14.3 m a.s.l.
LU-4215 122,000±9600 Same as above, depth 14.8 – 15,8 m a.s.l.

53
 230
Th/U and 14C DATING OF MOLLUSC SHELLS FROM THE COASTS ...
Recent mollusc shells do not contain noticeable spe-
cific activities of 232Th and 230Th while fossil mollusc shells
often do. Sometimes, the activity of 232Th even exceeds
that of 230Th (Blanchard et al., 1967).
At pH>5 soluble thorium compounds become hydro-
lyzed and dissolved as colloids in groundwater even if tho-
rium is present in micro quantities (Starik, 1959). Ge-
neration of colloids Th(OH)5 hydroxyd is possible due to
the product of solubility PS [Th(OH)5] =10-45. Colloids
are easily adsorbed on the surface of shells; diffusion does
not seem to play any role as reflected from comparison
of the 232Th and 230Th activity ratio for the surface, the
outer layer and the inner part of fossil mollusc shells
(Table 3).
This finding confirms that the main prerequisites of
the uranium-thorium method are fulfilled for the dating
of mollusc shells: 1) thorium migration in shells is strongly
limited to the surface; 2) removal of the surface and
the outer layer discards all detrital thorium and allows
230
Th/U dating of mollusc shells without the ambiguous
detrital correction with the 232Th.
The common 230Th/U and calibrated 14C dates of most
samples (LU-423, 424, 426 and 479; Table 4) agree within
their two-sigma confidence intervals. This gave evidence
that the basic assumption conditions of the 230Th/U
method were fulfilled: uranium became incorporated into
the mollusc shells soon after their deposition into sedi-
ments. The reliability of the concordant dates of the two
geochemically different elements uranium and carbon is
confirmed.
The 230Th/U age of ≥300 ka of the fossil mollusc shells
from the Lower Khazarian also confirm the fulfillment
of the principles this 230Th/U dating method: any uranium
and 230Th migration (diffusion) at a later time would have
resulted in a deviation of the 230Th/234U ratio from unity.
Based on our experience and described findings mol-
lusc shells to be used for 230Th/U dating should have the
following properties (Arslanov et al., 1976):
1) they should be at least 1 mm thick, not weathered
or calcified, non-layered and mechanically stable, not fer-
ruginous and consists of aragonite;
2) suitable mollusc species are: Cardium edule, Chio-
ne gallina, Paphia senescens, Cyprina islandica, Astarta
borealis and Caspian Didacna. Shells with flaky structure
such as Mytilus edule, Clamus glabra, Ostrea edulis were
often been poorly preserved and may give ambiguous
dates;
Table 6. Comparison of Russian terms for glacials, interglacials and marine transgressions with corresponding European terms and
global term MIS.
Russian term
Late Valdai
Middle Valdai
Early Valdai
Mikulino Interglacial
Boreal transgression
Karangat transgressiion (Eltigen, Maly Kut sections)
Late Khazar transgression
Lower Khazar transgression
3) mollusc shells should not contain 232Th in the dated
fraction or anomalous concentrations of uranium.
5. CONCLUSIONS
The major part of uranium is incorporated into mol-
lusc shells during no more than 1.5-2 ka after their depo-
sition into sediments. The inner part of recent and fossil
shells did never not contain 232Th and are suitable for
230
Th/U dating. 232Th became only adsorbed at the surface
of shells.
230
Th/U and calibrated 14C dates agree well for shells
with ages up to 15 ka. Similar agreement is found with
the stratigraphically dated mollusc shells of Middle Pleis-
tocene age.
The 230Th/U ages of the inner part of shells from Bo-
real (Eem) transgression sediments of both the Barents
and White Seas ranged from 86 to 114 ka while those from
the Black Sea Karangat transgression ranged from 102 to
130 ka. The lower limit of these dates may indicate a slight
uranium accumulation as the Mikulino (Eem) Intergla-
cial lasted from 116 to 128 ka (MIS 5e). In any case, the
modified 230Th/U method yields most reliable absolute
dates in the age of 0-350 ka.
REFERENCES
Arslanov Kh.A., 1987: Radiocarbon: Geochemistry and Geochrono-
logy. Leningrad University Publiching House. Leningrad: 300
pp. (in Russian).
Arslanov Kh.A., Evzerov V.Ja., Gerasimova S.A. and Lokshin N.V.,
1981: On the age of the Boreal transgression sedimeuts on the
Kola peninsula. Pleistocene Glaciation on the Eastern Europe-
an Plane. Moscow: 28 – 37 (in Russian).
Arslanov Kh.A., Gerasimova S.A., Leontyev O.K., Lokshin N.V.,
Mamedov A.V., Rychagov G.I., Tertychny N.I. and Shirinov
N.Sh. 1978: Age of Pleistocene and Holocene sediments of
Caspian Sea. Bulleten Komissii po Izucheniye Chetvertichuogo
Perioda 48: 39 – 48 (in Russian).
Arslanov Kh.A., Gey N.A., Ismailov Ja.A., Lokshin N.V., Gerasimova
S.A. and Tertychny N.I. 1983: The age and climatic conditions
of sediment formation on Late Pleistocene Sea terraces of the
Kerch strait coast. Vestnik Leningradskogo Universiteta 12: 69 –
80 (in Russian).
Arslanov Kh.A., Tertychnaya T.V. and Chernov S.B., 1993: Problems
and methods of dating low-activity samples by liquid scintilla-
tion method. Radiocarbon 35 (3): 393-398.
European term MIS
Late Weichselian 2
Middle Weichselian 3
Early Weichselian 4, 5a,b,c
Eemian 5e
Eemian, Boreal 5e
Eemian 5e
Late Weichselian 2
Holsteinian 9 and/or 11
54
 Kh.A. Arslanov et al.
Arslanov Kh.A., Tertychny N.I., Gerasimova S.A. and Lokshin N.V.,
1975: On the Pleistocene carbonate formation dating by ura-
nium-ionium method. In: Sostojanye metodicheskikh issledo-
vaniy v oblasti absolytnoye chronologi. Rublishing House “Na-
uka”, Moscow: 144 – 152 (in Russian).
Arslanov Kh.A., Tertychny N.I., Gerasimova S.A. and Lokshin N.V.
1976: On the marine mollusc shell dating by the ratio 230Th/234U.
Geochemistry 11: 1724 – 1733 (in Russian).
Arslanov Kh.A., Tertychny N.I., Ostrovsky A.B., Izmailov I.A.,
Sheglov A.P. and Gey N.A., 1977: New data on stratigraphy and
chronology of Pleistocene manine terraces of Caucasian Black
Sea coast and Kerch-Taman province: In: Paleogeography and
Pleistocene Sediments of South Seas. Publishnig House “Nauka”.
Moscow: 61 – 68 (in Russian).
Blanchard R.L., Chevg M.H. and Potratz H.A., 1967: Uranium and
Thorium Series Disequilibria in Recent and Fossil Marine
Molluscan Shells. Journal of Geophysical Research 72 (18):
4745-4757.
Broecker W.S., 1963: A preliminary Evaluation of Uranium Series
Inequilibrium as a Tool for Absolute Age Measurement on
Marine Carbonates. Journal of Geophysical Research 68 (9):
2817-2834.
55
Cherdyntsev V.V. 1969: The Uranium – 234. Moscow: 350 pp
(in Russian).
Kaufman A., Broecker W.S., Ku T.-L. and Thurber D.L., 1971: The
status of U-series methods of mollusc dating. Geochimica et
Cosmochimica Acta 35 (11): 1155-1183.
Kuznetsov V.Yu., Arslanov Kh.A., Shilov V.V., Cherkashov G.A. and
Maksimov F.E., 2000: Distribution of uranium and thorium in
metallogenic sediments from the hydrothermal zone of the
North Atlantic. Radiochemistry 6: 565 – 568 (in Russian).
Martinson D.G., Pisias N.G., Hays J.D. et al., 1987: Age dating and
the orbital theory of the ice ages: development of a high reso-
lution 0 to 300000 year chronostratigraphy. Quaternary Rese-
arch 27: 1-30.
Olsson I. U. and Blake W., 1961–1962: Problems of radiocarbon
dating of raised beaches, based on experience in Spitsbergen.
Norsk Geogr. Tidssk. 18 (1-2): 47-64.
Starik I.E. 1959: Basis of Radiochemistry. Publishing House of USSR
Academy of Sciences, Moskow-Leningrad: 400 pp (in Russan).
Veeh H.H. 1966: Th230/U238 and U234/U238 Ages of Pleistocene High
Sea Level Stand. Journal of Geophysical Research 71 (14):
3379-3386.
230
Th/U and 14C DATING OF MOLLUSC SHELLS FROM THE COASTS ...

56
 GEOCHRONOMETRIA Vol. 21, pp 57-64, 2002 – Journal on Methods and Applications of Absolute Chronology

ESR AGES OF THREE LITHUANIAN MID-LATE

PLEISTOCENE INTERGLACIALS METHODICAL
AND STRATIGRAPHICAL APPROACH

ALGIRDAS GAIGALAS1 and ANATOLY MOLODKOV2

1
Department of Geology and Mineralogy, Vilnius University, Èiurlionio 21/27, LT 2009 Vilnius, Lithuania
(e-mail: Algirdas.Gaigalas@gf.vu.lt)
2
Institute of Geology, Tallinn Technical University, 7, Estonia Blvd., 10413 Tallinn, Estonia (e-mail: Molodkov@gi.ee)

Key words
words: Abstract: The electron spin resonance (ESR) dating was used for freshwater mollusc fossils
MID-LATE taken from interglacial deposits at the Gailiûnai and Neravai sites (Butënai/Holsteinian In-
PLEISTOCENE, terglacial), Valakampiai site (Snaigupëlë/Drente-Warthe Interglacial), Jonionys and Netiesos
INTERGLACIALS, sites (Merkinë/Eemian Interglacial) in Lithuania. Freshwater mollusc samples from the
LITHUANIA, Butënai/Holsteinian and Merkinë/Eemian Interglacials estimated by ESR yielded different
ELECTRON SPIN ages: Butënai – 455.0 to 307.0 ka and Merkinë – 112.5 to 101.5 ka BP. Two ESR dates deter-
RESONANCE, mined for Snaigupëlë Interglacial deposits suggest an average age of about 113.0 ka. This is
MOLLUSC therefore younger than expected from the palynological data, and it places Snaigupëlë into
the interglacial stage, possibly assigned to the MIS 5d that can likely be correlated with the
Merkinë/Eemian Interglacial (s.l.). Thus, further studies of the deposits and additional ESR
dates are needed to make sure that the Snaigupëlë bed is really much younger than expected
(about 200 ka) in all recognized sites in different parts of Lithuania.

1. INTRODUCTION pollen spectrum of all other intermorainic layers can not

The dominant Quaternary deposits in Lithuania are
barren of datable organics. The occurrence of sediments
of all glaciations known in Eastern Europe is a character-
istic feature of Lithuania. Up to five interglacials and up
to nine independent till beds are distinguished here. There
are seven metachronous till formations in Pleistocene
cover of Lithuania, left behind by independent glaciations
or their major stages (Gaigalas, 1979). These tills are re-
lated to advances and degradations of the ice sheets of
Katlëriai, Dzûkija, Dainava, Þemaitija, Medininkai and
Nemunas glaciations, the latter being represented by two
stages: the Grûda and Baltija. The glacial sediments are
separated by deposits of normal aquatic (fluvial and lacus-
trine) sedimentation which originated during various
interglacials: Vindþiûnai, Turgeliai, Butënai, Snaigupëlë
and Merkinë, and interstadials of the Last Nemunas/
Weichselian Glaciation. Interglacial lacustrine, boggy and
alluvial sands, silts, gyttja, clay, sapropelite with rare mol-
lusc shells are spread.
The Merkinë/Eemian and Butënai/Holsteinian inter-
glacial deposits serve as key horizons for the purpose of
correlation. They are represented by interglacial organo-
genic deposits clearly characterized by palaeobotanical
data (Kondratienë, 1996). Unfortunately, the spore and
be yet unambiguously interpreted, to provide clear evi-
dence in terms of stratigraphy and chronology. The pres-
ence of the Snaigupëlë Interglacial has been discussed
by several authors. According to some of them Snaigupëlë
Interglacial deposits are pre-Butënai (pre-Holsteinian)
in age (Velichkevich, 1979; Vozniachukh, 1978). At the
same time, V. Vonsavièius and Baltrûnas (1974) attrib-
uted the Snaigupëlë deposits to the Upper Pleistocene.
According to pollen data of O. Kondratienë (1996), the
Snaigupëlë Interglacial is younger than the Butënai/
Holsteinian and older than the Merkinë/Eemian Inter-
glacial that allowed her to correlate it with penultimate
interglacial period of isotope stage 7.
2. RESEARCH METHODS
Apparently, the only real possibility to unequivocally
solve the problem of the Lithuanian interglacials is the
timing of lacustrine and bog deposit formations. For this
purpose, the electron spin resonance (ESR) analysis of
freshwater mollusc fauna included in Butënai, Snaigupëlë
and Merkinë Interglacial deposits was undertaken. It al-
lowed to determine the absolute age of shell remains and
hence, the age of the embedding interglacial deposits.
 ESR AGES OF THREE LITHUANIAN MID-LATE PLEISTOCENE ...
In the present study an advanced version of the ESR-
dating method (Molodkov, 1988, 1993 and 1996) was ap-
plied to date freshwater mollusc fauna taken from inter-
glacial gyttja at the Gailiûnai and Neravai sites (Butënai
Interglacial), Valakampiai site (Snaigupëlë Interglacial),
Jonionys and Netiesos sites (Merkinë Interglacial). The
location of sites see Fig. 1.
The ESR dating method is based on a direct measure-
ment of the amount of radiation-induced paramagnetic
centres (radiation damages), that have been created in
shell material due to natural radiation. At the time of for-
mation the lattice of shell biogenic carbonate has no ra-
diation-induced centres, but radiation from the shell
itself and the environment (embedding matrix and cos-
mic) causes their gradual accumulation. A shell sample
will therefore have paramagnetic centres, the amount of
which relates directly to the total radiation dose that the
shell has received. The presence of paramagnetic carbo-
nate centres in mollusc shell material can be detected by
ESR spectrometry. It produces a plot of the microwave
absorption spectra where each paramagnetic centre is
characterised by specific signals, the amplitude of which
is related to the accumulated palaeodose, and hence to
the age of the shells. Details of ESR dating of subfossil
shells used in the present study are described elsewhere
(e.g. Molodkov et al., 1998) Analytical procedure are given
below.
ESR-analysis
Shell samples were analysed with an ESR-221
spectrometer (X-band) at room temperature. All the
freshwater shells studied were composed of calcite, and
displayed typical ESR spectra with a characteristic hyper-
Šiauliai
Klaipëda
Nemunas
Kaunas
Netiesos
0 25 50 km
Gailiûnai Jonionys
fine sextet and the forbidden transition associated with
the Mn2+ in shell carbonate (Fig. 2). The phase sensitivity
detection (PSD) technique (Molodkov 1988 and 1993)
was used to enhance the analytical line at g=2.0012,
∆Bpp ≈ 0.22 mT and to suppress the manganese signals as
well as the interfering radiation-induced signals in the
region of g=2.00.
ESR spectra of the shell samples were recorded with
a sweep width of 2000 mT, a scan time of 1620 s in the
region of g=2.00, and time constant of 0.01 s. The micro-
wave power used for dosimetric reading was 2 mW with
100 kHz magnetic field modulation at 1 mT. Reported
results are the average of ten measurements of the 2.0012
signal for each aliquot. Palaeodose for each sample was
obtained by fitting with the reciprocal exponential func-
tion -ln(1-I/Imax), where I and Imax are an ESR signal in-
tensity and that of the level at saturation dose, respectively.
The accumulated palaeodose, Ps , was estimated by ex-
trapolation of the regression line to the zero ESR inten-
sity (Fig. 3). Saturation intensity was determined itera-
tively by optimising the correlation coefficient r. Long-
term fading of absorbed palaeodose (Molodkov, 1989)
was taken into account proceeding from the estimated
time-averaged terrestrial temperature (about 5° C) and
thermal stability of the 20012 centres in the shells studied
(τ ≈ 10 Ma at 5° C).
Dose rate measurements
The external beta and gamma contributions to the total
dose rate were estimated from the contents of natural
radioactive elements, 238U+235U, 232Th and 40K in the
surrounding sediments. For detecting and identifying
naturally occurring radioactive elements in the surround-
Panevëþys
Ne
ris
Valakampiai
VILNIUS
Merkys
Fig. 1. Location map of
investigated sections.
58
 A. Gaigalas and A. Molodkov
Fig. 2. Typical ESR-spectrum of calcite freshwater mollusc
shells from Butënai lacustrine deposits about 330 ka in age
(Neravai site). Radiation-induced signal (arrow) is super-impo-
sed by forbidden Mn+2 transition line (A). Analytical line at
g=2.0012 (B) is separated by phase sensitive detection (PSD)
technique.
ing matrix a multichannel gamma-ray spectrometer with
a 100 x 150 mm dia low background sodium iodide crys-
tal was used. For better statistical accuracy up to five
samples about 1 kg each were taken within the sphere with
R~30 cm for assessment of the gamma and beta contri-
bution to the external dose rate. Estimates of the cosmic
dose (Yokoyama et al., 1982) were based on the half of the
present depth of burial to take into account the increase
in thickness of the deposits during the controlled time
interval. The dose rate conversion factors of Adamiec and
Aitken (1998) were used. The percentage of the beta dose
was estimated according to the shell geometry and pro-
portions etched off. Water content in the sediments was
also taken into account. Internal dose rate was calculated
basing on the determination of U-concentration in the
shells by NAA taking into account the in-growth of 230Th
with daughters in the shell during its buried state (Ikeya,
1985; Molodkov, 1986). Alpha efficiency was assumed to
be 0.15. The shell material was distributed uniformly in
embedding matrix (gyttja). In terms of the natural radio-
nuclide content the latter was rather homogeneous.
The results of the radiometric and ESR analyses are
given in Table 1. At present the dating method applied in
this work usually provides overall analytical precision of
up to about 10 %, when taking into account the standard
errors assumed for every parameter used in the age cal-
culation.
59
Fig. 3. Dose responses of the paramagnetic centres at
g=2.0012 in freshwater mollusc shells from the Butënai
lacustrine deposits. The solid line show the best logarithmic
fit for experimental data poins (circles), obtained by phase
sensitive detection (PSD) technique; each point is the mean
of 10 read-out values.
3. DATED SAMPLES OF INVESTIGATED SECTIONS
AND DATING RESULTS
For numerical dating of the Butënai, Snaigupëlë and
Merkinë organogenous lacustrine and boggy deposits fif-
teen shell samples were taken. Three samples were col-
lected from the Gailiûnai section and three samples from
the Neravai section of Butënai Interglacial. Two samples
were taken from the Valakampiai section of Snaigupëlë
Interglacial, as well as two samples from the Jonionys
section and seven samples from the Netiesos section of
Merkinë Interglacial.
The shells were represented by freshwater Pelecypod
and Gastropod species. Valvata cristata Müller, Lymnaea
peregra Müller, Anisus leucostomus Millet, Valvata
piscinalis Müller, Pisidium nitidum Jenyns, Pisidium sp.,
Armiger crista L., Sphaerium corneum L., Pisidium
moitessierianum Paladilhe are the most common species
of Butënai (Holsteinian) Interglacial in the Neravai sec-
tion (Sanko, 1999). The shells of Merkinë (Eemian) In-
terglacial in the Netiesos section were represented by
Valvata piscinalis Müller, V. cristata Müller, Bithynia
tentaculata Linné, Radix limosa Linné, Radix auricularia
L., Lymnaea stagnalis L., Acroloxus lacustris L., Gyraulus
albus Müller, G. laevis Ald. and Sphaerium corneum Linné
species.
The mammalian fauna of the Butënai Interglacial from
the Neravai section is characterised by the occurrence of
Arvicola mosbachensis Schmid., Microtus sp., M. agrestis
L., Clethrionomys aff. Glarealus Schreber and other spe-
cies (Vozniachuk et al., 1984).
 ESR AGES OF THREE LITHUANIAN MID-LATE PLEISTOCENE ...

Table 1. ESR results and radioactivity data for shell samples from Lithuanian interglacial deposits
No. Lab No. Field No. Site Altitude Depth Uin U Th K Dc Dint Dsed DΣ Ps ESR-age, T
[m a.s.l.] [m] [ppm] [ppm] [ppm] [%] [µGy/a] [µGy/a] [µGy/a] [µGy/a] [Gy] [ka]

1 221-095 Sample 1 Netiesos 86.3 8.2 0.11 0.72 0.74 0.29 93 24.6 525.2 642.2 57.9 90.5 ± 8.8
2 225-095 Sample 2 Netiesos 8.2 0.24 0.55 1.12 0.3 89 58.8 520.7 668.8 75.5 112.5 ± 10.8
Mean age 101.5 ± 11.5

3 222-095 Sample 1 Netiesos 8 0.11 1.32 3.62 0.97 76 26.1 1550.5 1652.9 164.9 103.3 ± 9.8

4 197-083 Sample 1 Jonionys 76.5 6 0.5 0.7 1.79 0.88 100 83 1182 1365 140.8 101.0 ± 11.0
5 198-083 Sample 1a Jonionys 6 0.56 0.6 1.44 0.87 100 105 1112 1317 155.4 118.0 ± 12.0
Mean age 109.5 ± 8.5

6 220-095 Sample 2 Netiesos 12.2 0.24 0.55 1.12 0.3 89 58.8 521 668.8 75.5 112.5 ± 10.8

7 222-095 Sample 3 Netiesos 13 0.11 1.32 3.62 0.97 76 26.1 1550.5 1652.9 164.9 100.3 ± 9.8
8 223-095 Sample 4 Netiesos 13 0.34 1.31 2.7 1.1 76 75.1 1625.6 1777 155.7 88.0 ± 8.5
9 224-095 Sample 5 Netiesos 13 0.23 1.34 3.14 0.98 76 62.9 1543.3 1682.6 247.1 148.0 ± 14.4
Mean age 112.1 ± 25.9

10 259-100 Sample 1 Valakampiai 88.0 0.42 1.23 3.45 1.11 110 122.6 951.3 1183.5 129.7 110.0 ± 12.1
11 260-100 Sample 2 Valakampiai 0.21 1.23 3.45 1.11 110 65.7 784.1 959.3 110.9 116.0 ± 10.8
Mean age 113.0 ± 3.0

12 101-079 Sample 1 Gailiûnai 81.0 <0.1 0.76 1.76 0.25 90 10 546 646 95 118.0 ± 15.0

13 103-079 Sample 3 Gailiûnai 2.1 1.7 5.35 0.61 70 777 1289 2136 587.5 307.0 ± 32.0
14 206-083 Sample Neravai 83.2 5.2 0.04 0.39 0.46 0.16 120 11 244 375 110 298.0 ± 28.0
1/1a
15 207-083 Sample Neravai 5.2 0.06 0.38 0.73 0.17 120 17 324 461 152.5 336.0 ± 30.0
1b/2
16 208-083 Sample Neravai 5.2 0.05 0.38 0.73 0.17 120 14 324 458 160 356.0 ± 34.0
N1/N2 Mean age 330.0 ± 24.1

17 102-079 Sample 2 Gailiûnai 1.5 0.41 2.23 0.23 70 631 539 1240 565 455.0 ± 40.0
Notes:
U in is the uranium content in shells; U, Th and K are the uranium, thorium and potassium content in sediments; Dc is the cosmic dose rate, Dint – the time-averaged internal dose rate;
Dsed – the sediment dose rate; DΣ – the total dose rate; Ps – the palaeodose. Uncertainties: U, ± 2-3%; Th, ± 3-4%; K, ± 1-2%; U in the shells, ± 1-3%; gamma irradiation, ± 3-5%.

Butënai Interglacial. Gailiûnai and Neravai outcrops
near Druskininkai town (South Lithuania) are parastra-
totypes of the Butënai (Holsteinian) Interglacial. Inter-
glacial deposits are represented here by lacustrine, boggy
and alluvial sands, silts, clays, peat, sapropelite and gyttja
(Fig. 4). The Gailiûnai exposure opens the socle of the
first above-flood plain terrace of the Nemunas River
(Gaigalas and Molodkov, 1996).
The vegetation of the Butënai Interglacial is of forest
type. Taxus baccata L., Picea omorica L., Ilex aquifolium
L., Abies alba Mill., Brasenia holsatica Web., Najas
macrosperma Wielczk., Nymphaea cinerea Wieliczk.,
Azolla pseudopinnata Nikit., Osmunda claytoniana L. are
the most common species (Riðkienë, 1979; Kondratienë,
1965).
The total weight of the pelecypod shells from the Ne-
ravai section (sample Νο. 206-083) was 600 mg, and that
of the gastropod shells (No. 207-083) 250 mg. In the labo-
ratory, the mixture of broken shell fragments of uniden-
tified species with a total weight of 880 mg (208-083) was
separated from the sediments taken from the same layer
6 m apart. Available amount of the shell material from
the Gailiûnai section was 2700 to 1300 mg. The uranium
content in the Neravai shells proved to be low ranging
from 0.04 to 0.06 ppm. The relatively low U content in
the shells compared to the 0.1 to 0.5 ppm of living shells
indicates that little or no post-depositional U enrichment
has occurred in these shells. The content of natural iso-
topes in embedding matrix at the Neravai site was unusu-
ally low. As a result, the dose rate derived from radiation
measurements in the environment of the shells turned out
to be also rather low – about 300 µGy a–1, which is much
lower than in Gailiûnai sediments (539 to 1289 µGy a–1).
The internal time-averaged dose rate due to U and daugh-
ters ranged from 11 to 17 µGy a–1 in the Neravai and from
631 to 777 µGy a–1 in the Gailiûnai samples.
The high thermal stability of the 2.0012 centre in the
shell substance allows to date the lacustrine deposits up
to 1.5-2.0 Ma in age. In the range up to 0.5 Ma the dating
of the shells should present no difficulties in terms of ther-

60
 A. Gaigalas and A. Molodkov

mal behaviour of the signal. The datings obtained on both
sites show internal consistency in ESR age estimates and
small scattering of the results, although in most cases the
age determinations were performed on the mixture of
broken shell fragments of unidentified species separated
from the matrix material. The ESR analyses of the fresh-
water shells taken from the sections studied yield mutu-
ally consistent dates of 356.0±34.0, 336.0±30.0 and
298.0±28.0 ka (Neravai), 455.0±40.0 and 307.0±32.0 ka
(Gailiûnai) for the Butënai Interglacial that allowed us to
correlate this terrestrial climate change with the marine
oxygen isotopic stages 9 and 11.
The ESR age of 118.0±15.0 obtained for a sample No.
101-079 taken from a recently-fallen block of peaty sandy
loam in the vicinity of the studied bed of the Gailiûnai
section indicates that the dated sample evidently belongs
to the stage 5 complex and can confidently be correlated
with the rest of the Merkinë age deposits studied.
Snaigupëlë Interglacial. The freshwater mollusc fauna
of the Snaigupëlë Interglacial was taken from gyttja at the
Valakampiai site (Eastern Lithuania; Fig. 4). The outcrop
of interglacial deposits at Valakampiai is located in the
northern part of the town of Vilnius and was discovered
45 years ago. Interglacial deposits are represented by
1-m-thick gyttja. The interglacial layer occurs in the socle
of the first above-flood plain terrace of the Neris River.
The age of the enclosing sediments was determined on
two samples of shell material. The ESR analysis yielded
mutually consistent dates of 116.0±10.8 and 110.0±12.1
ka BP with an average age of about 113.0 ka BP. The nu-
merical data obtained allow to link the studied Snaigu-
pëlë interglacial layer with the Merkinë/Eemian Intergla-
cial that according to materials of complex palyno-
chronostratigraphic investigations (Molodkov and
Bolikhovskaya, 2001) can most likely be compared with
the time interval from approximately 145 to 70 ka com-
parable with the whole of MIS 5 rather than the period of
optimum conditions in oxygen isotope substage 5e
(Eemian, s. s.).
The development of flora at Snaigupëlë is most simi-
lar to that at Merkinë (Liivrand, 1991 and 1998). The
Snaigupëlë stratotypical section is subdivided into 9 pol-
len zones with characteristic plants: Caulinia lithuanica
Rišk., C. tenuissima D. Benn., C. goretskyi Dorof., Brasenia
cf. borysthenica Wieliczk. (Riðkienë, 1979; Velichkevich,
1979). The Snaigupëlë pollen diagram of the Valakampiai
section also displays some similarity to the Merkinë/
Eemian ones. Therefore, Snaigupëlë was initially assigned
to the last interglacial (Kondratienë, 1959). Later on,
according to new palynological data (Kondratienë, 1996),
the deposits at Valakampiai have been attributed to the
independent Snaigupëlë Interglacial, which is younger
than the Butënai/Holsteinian and older than the Merkinë/

Fig. 4. Dated sections of Butënai (Gailiûnai and Neravai), Snaigupëlë (Valakampiai)

and Merkinë (Jonionys and Netiesos) Interglacials. Litological legend: 1 – sand;
2 – sandy-gravel deposits; 3 – silt; 4 – sandy silt; 5 – boulders; 6 – gyttja with mollusc
shells; 7 – gyttja; 8 – peat; 9 – peat with mollusc shells; 10 – peat with wood remains;
11 – clay; 12 – sand with mollusc; 13 – silty sand with wood detritus; gIdn – till of the
Dainava glaciation; gIIžm – till of the Þemaitija glaciation; gIImd – till of the Medininkai
glaciation.

61
 ESR AGES OF THREE LITHUANIAN MID-LATE PLEISTOCENE ...
Eemian Interglacial. The presence of independent
Snaigupëlë Interglacial within the MIS 7 is also supported
by many other investigators in Lithuania. Nevertheless,
the results obtained in the present work indicate that the
problem of whether the independent Snaigupëlë Intergla-
cial really exists should still be open for debate.
Merkinë Interglacial. The Jonionys section is the
stratotype of Merkinë Interglacial. The exposure is located
on the left bank of the Nemunas River about 3 km west
from Merkinë. The Jonionys section reveals the socle of
the second above-flood plain terrace of the Nemunas
River (Fig.4). The stratigraphy from waterline of the
Nemunas river to the top of the terrace is divided into 20
units (Gaigalas and Hütt, 1995). The age of freshwater
mollusc shells from lake-and-bog deposits of the Merkinë
Interglacial parastratotype in the exposure of Netiesos on
the right bank of the Nemunas River, about 6 km down-
stream from the town of Merkinë, was determined as
112.1±25.9 and 101.5±11.5 ka (for samples from the
lower and upper units, respectively). The continental
Merkinë deposits are composed mostly of peat, gyttja and
sandy sediments with rare mollusc shells of lake origin
(Gaigalas and Hütt, 1997). Palynological analyses of peat
and gyttja samples from Netiesos were carried out by O.
Kondratienë (1996) and resulted in a diagram. She found
spore-and-pollen zones from M1 till M4. The zone M5 was
not studied, because this zone is absent in the upper part
of the outcrop described at Netiesos. Flora from Netiesos
in its renovated form is the richest among all flora of the
Merkinë Interglacial in Lithuania known at present and,
owing to the taxonomic revision, it may be considered as
a standard for the whole group of flora of this age.
Four samples of lake sand deposits which covered the
organogenic sediments of Merkinë Interglacial (pollen
zone M1-M4 in Netiesos outcrop) were OSL dated by
G. Hütt (Gaigalas and Hütt, 1997). Their deposition pro-
bably took place just before the last glaciation. The dates
of Merkinë Interglacial correlate well with our ESR re-
sults obtained on the Eemian deposits in the Meetkerke
section (Belgium) – 104.4±9.5 and 97.1±8.9 ka BP
(Gaigalas and Molodkov, 1997), as well as with the da-
ting result of 109.5±8.5 ka on the Merkinë Interglacial in
the Jonionys stratotypes section (South Lithuania). The
stratotype of Merkinë Interglacial is the Jonionys-
Maksimonys area 3 km downstream from Merkinë town
on the left (Jonionys) and right (Maksimonys) sides of the
Nemunas River. Characteristic for the Merkinë Intergla-
cial are Tilia tomentosa Moench., T. platyphyllos Scop.,
Acer campestra L., A. platanoides L., Carpinus betulus L.,
Lycopus intermedius Dorof., Trapa europae Fler., Salvinia
natans (L.) All., Osmunda cinnamonea L. (Riðkienë,
1979).
4. CONCLUSIONS
Freshwater mollusc samples from the Butënai/
Holsteinian and Merkinë/Eemian Interglacials estimated
by ESR yielded different ages: Butënai – 455.0 to 307.0
and Merkinë – 112.1 to 101.5 ka BP. The ESR age of
62
mollusc shells from Snaigupëlë Interglacial deposits
(about 113.0 ka BP) can most likely be correlated with
the Merkinë Interglacial. Nevertheless, further studies of
the deposits and additional ESR dates are needed to make
sure that the Snaigupëlë bed recognised in different parts
of Lithuania is really Merkinë in age, because the place
of penultimate interglaciation of isotope stage 7 remains
still vacant.
The data produced for the Neravai and Netiesos sec-
tions are internally consistent and in agreement with other
evidence, e.g. the age of the organeous horizon in the
Gailiûnai and Jonionys sections and independent
palaeontological and geological data from these sites.
A comparison of the results obtained on the upper part
of the Butënai Interglacial lacustrine deposits in the
Gailiûnai section (307 ky BP) and those of the Neravai
section (330 ky BP) shows a good agreement between age
estimates at two different sites. Dates from Netiesos cor-
relate with our ESR results obtained on Eemian deposits
in the Meetkerke section (Belgium) – 104.4±9.5 and
97.1±8.9 ka BP (Gaigalas et al., 1994), as well as with
the results on the Merkinë Interglacial in the Jonionys
stratotype section – 109.5±8.5 ka BP.
Our present and previous studies show that the
Neravai site is undoubtedly Butënai and Netiesos-Merkinë
Interglacial in age. This, in its turn, provides a basis for
the conclusion that, in all probability, the Butënai Inter-
glacial may be ascribed at least to Stage 9 of oxygen-iso-
tope scale and correlated with the upper part of
Holsteinian (s.l.) markerbed traced in NW and Central
Europe. On an Arctic island, marine deposits correlated
with the Holsteinian Interglaciation and Stage 9 were
dated by ESR to about 300 ka BP (Molodkov et al., 1992).
The deposits studied contain very warm for that region
spore-and-pollen complex and the boreal foraminifera
association of Miliolinella pyriformis zone similar to those
found in marine facies of the Holsteinian Interglacial in
Germany. The questions whether the Butënai Intergla-
cial is also equivalent to Stage 11 and whether it should
be therefore subdivided into two ice-free periods (or into
two independent interglacial as has been suggested in
studies elsewhere, e.g. Bolikhovskaya, 1995), separated
by a sharp climatic cooling, remains open yet because of
the lack of geochronological data on the oldest lacustrine
deposits in Lithuania.
The data obtained in Lithuania by the ESR method
on younger deposits have provided more certain numeri-
cal chronology for the Pleistocene interglacials. Combined
with the independent stratigraphic investigations, ESR
can be considered as a promising approach for the study
of climatic changes, sedimentary dynamics, palaeoenvi-
ronmental reconstructions and correlation of Quaternary
deposits over broad geographical areas.
ACKNOWLEDGMENTS
This research was partially funded by grant from the
Estonian Science Foundation (No. 3625).
 A. Gaigalas and A. Molodkov
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ESR AGES OF THREE LITHUANIAN MID-LATE PLEISTOCENE ...

64
 GEOCHRONOMETRIA Vol. 21, pp 65-72, 2002 – Journal on Methods and Applications of Absolute Chronology

PALAEOMAGNETISM OF LITHUANIAN
UPPER PLEISTOCENE SEDIMENTS

ALGIRDAS GAIGALAS1, NIELS ABRAHAMSEN2, VAIDOTAS KAZAKAUSKAS3,

and MONIKA MELEÐYTË1
Vilnius University, Èiurlionio 21/27, 2009 Vilnius, Lithuania (e-mail: Algirdas.Gaigalas@gf.vu.lt)
1

Department of Earth Sciences, Aarhus University, Finlandsgade 8, DK-8200 Aarhus N, Denmark

2

(e-mail: Abraham@geo.aau.dk)
3
Department of Quaternary Geology, Institute of Geology, T. Ševèenkos 13, LT 2600 Vilnius (e-mail: vaid.kaz@geologin.lt)

Key words
words: Abstract: In the Lithuania, a palaeomagnetic study of Upper Pleistocene and Late Glacial
PALAEOMAGNETISM, sediments at five sections has been carried out. The palaeomagnetic study of the varved clays
UPPER PLEISTOCNE, in the Maskauka, Didþiasalis and Girininkai sections cover the time interval since 18,000 to
LITHUANIA 14,000 BP and Manèiagirë section covers the time interval since 12,700 to 11,630 BP. The
palaeomagnetic research of the Merkinë (= Eemian) Interglacial sediments (Netiesos sec-
tion) cover the time interval since 112.0±25 to 101.5±11.5 ka BP. The declination (D), incli-
nation (I) and intensity (J) of the natural remanent magnetization of glaciolacustrine clays
(Maskauka, Didþiasalis and Girininkai sections), as well as Merkinë (=Eemian) Interglacial
deposits (Netiesos section) and interstadial sediments (Manèiagirë section) were measured.
The result of these studies is presented in diagrams. The study reveals that considerable
palaeomagnetic information can be obtained from the varved clays.

1. INTRODUCTION A palaeomagnetic study of varved clays of the Late

Application of palaeomagnetic methods has shown
that such investigations may be a valuable tool for
stratigraphical research of Pleistocene sediments in Lithu-
ania. Palaeomagnetic investigations of Late Pleistocene
sediments in Lithuania previously have been published
by M. Pevzner and A. Gaigalas (1976) and A. Gaigalas
et al. (1991).
Various anomalous and even negative inclinations are
found in some deposits of Late Pleistocene in Lithuania
(Gaigalas et al., 1991). Anomalous magnetization of
a transitional type from normal to reverse inclination was
noted in the Merkinë (=Eemian) Interglacial deposits
(Maksimonys and Jonionys section). Reverse magnetiza-
tion was noted in the Grûda (=Brandeburgian) till
(22,000-18,000 years ago) with an otherwise normal mag-
netization (Padubysis section). Anomalous magnetization,
transiting to negative, was noted in varved clays, dated to
about 13,500-13,000 years ago (the Kurðënai section).
Negative magnetization was also noted in lacustrine de-
posits, aged 11,600-12,700 years ago.
Glacial has been carried out at Karelia in the north of
Lake Ladoga and in the west and east of Lake Onega for
the time interval 16,000-10,200 BP (Ekman et al., 1987;
Batchmutor and Zagniy, 1990). The detailed curves of
declination and inclination can be used for regional
magnetostratigraphic studies and for correlation of sedi-
ments in adjacent regions of East European plain.
A palaeomagnetic study can be used not only in stratig-
raphy and correlation of Late Pleistocene sediments, but
in palaeogeographic reconstructions too. New informa-
tion on fine structure of palaeomagnetic field should be
analysed in a palaeoclimatic aspect. The task is to esta-
blish relationships between climatic variations and the
geomagnetic field in the Pleistocene.
In Lithuania glaciolacustrine deposits and varved clays
are distributed widely in surface formation. They have
been formed in dammed periglacial basins near the mar-
gin of the retreating ice sheet. The study of varved clays
can be used to obtain the secular variations and for the
construction of a detailed time-scale of the geomagnetic
field in the Late Pleistocene.
 PALAEOMAGNETISM OF LITHUANIAN UPPER PLEISTOCENE SEDIMENTS
2. RESEARCH METHODS
In the present study more than 400 samples from five
sections (Girininkai, Didžiasalis, Maskauka, Manèiagirë
and Netiesos) have been magnetically investigated (Fig. 1).
Declination (D), inclination (I) and intensity (J) of the
natural remanent magnetization (NRM) of glaciolacus-
trine clay (Girininkai, Didþiasalis and Maskauka sec-
tions), as well as Merkinë (=Eemian) interglacial depos-
its (Netiesos section) and interstadial sediments
(Manèiagirë section, Fig. 2) were measured by a spinner
magnetometer (Digico Ltd.). These sections are located
in different deglaciation zones of the Last Glaciation that
allow us to cover a wide time interval. Oriented, 1-inch
specimens were collected in vertically cleaned profiles,
using magnetic compass and a spirit level for the orien-
tation. After performing an initial pilot study, all speci-
mens were AF-demagnetized in small steps up to typical
50 or 60 mT, and re-measured on the spinner
after each step. By a PCA-analysis (principal component
analysis), using Linefind in the IAPD (Interactive analy-
sis of Palaeomagnetic Data) program (Torsvik, 1992), the
ChRM (characteristic remanent magnetization) of each
specimen was isolated. In some cases SIRM (saturation
isothermal magnetization) experiments were performed,
and also the frequency-dependant magnetic susceptibi-
lity was measured. Results are plotted in the diagrams
(Figs 3 and 4). The magnetic minerals vary between dif-
ferent environments, and hence they may hardly be stated
as a general conclusion. However, the main ferromagnetic
component carrying the NRM is usually fine grained
magnetite, although maghemite may sometimes be
present. In some cases, according to the magnetic satu-
Ðiauliai
Klaipëda Panevëþys
as
Nemun
Ne
Kaunas
ris
Girininkai
VILNIUS
ky
er Maskauka
M
Netiesos
0 25 50 km
Manèiagirë
66
ration experiments, the carrier of the magnetic remanence
appear to be hematite (or goethite?) rather than magne-
tite or maghemite.
The palaeomagnetic study of the varved clays
(Maskauka, Didþiasalis and Girininkai) covers the time
interval from 18,000 to 14,000 BP. The sediment age has
been defined by varvometric, palynological, optically
stimulated luminescence, electron spin resonance and
radiocarbon analyses as well as concluded from geologi-
cal and geomorphological data. Sedimentological and
palaeomagnetic studies were carried out for each section.
High sedimentation rates of varved clays allowed us to
collect oriented samples with high resolution over the time
interval and without problems of material limitation. The
bedding of sediments used for studying the geomagnetic
secular variation is in a horizontal or near horizontal po-
sition.
3. MASKAUKA SECTION
The section represents the Grûda (=Branderburgian)
and Þiogeliai (=Frankfurtian) glaciolacustrine varves.
Magnetic declination, inclination and intensity of the sedi-
ments of Maskauka profile have been combined in one
plot (Fig. 5). Both angles of magnetic declination and in-
clination appear to show systematic trends, but with high
scatter. On the diagram (Fig. 5), each dot indicates the
AF-cleaned ChRM (characteristic remanent magnetiza-
tion) of one oriented specimen.
The declination may show a systematic trend, but the
scatter is quite high (Fig. 5). The westerly values between
4.7 and 5.1 m above the river level are situated just above
the Grûda sediment (4.3 m to 4.65 m).
Didþiasalis
s
Fig. 1. Location of the
Maskauka, Didþiasalis,
Manèiagirë and Netiesos
sections of Late Pleistocene
deposits.
 Gaigalas et al.

Maskauka Didþiasalis Girininkai Manèiagirë Netiesos

(lower part)
16.0 0 0 3.0 7.8

Late Glacial (12,700 - 11,630 BP)

0.5
0.8 7.0
1.9

Merkinë (=Eemian) Interglacial (~125,000 - 105,000 BP)

1.5
1.6

Upper Pleistocene (~14,000 - 8,000 BP)

1.1
0.9
Upper Pleistocene (~18,000 - 16,500 years BP)

2.1 5.6
7.3
0.5

Upper Pleistocene (~15,000 - 14,000 BP)

2.6
0
m River level

5.9

4.7
2.6
7.1
4.3 7.1
4.0
1.8

0
m River level

1 2
11.2
11.6 4 5 6

7 8 9

0 12.7 10
m m
m River level

Fig. 2. Palaeomagneticaly investigated sections: Maskauka, Didþiasalis, Manèiagirë and Netiesos. 1 – sand, 2 – silt, 3 – varved clay,
4 – homogeneous clay, 5 – clay disturbed by cryogenic process, 6 – till, 7 – limnic tufa, 8 – sapropelite, 9 – gyttja, 10 – peat,
11 – deluvium.

67
 PALAEOMAGNETISM OF LITHUANIAN UPPER PLEISTOCENE SEDIMENTS
Þiogeliai (=Frankfurtian) varves cover the interval be-
tween 5.1 m and 7.4 m (sandy and silty lake sediments).
The top part between 7.45 m and 8 m consists of reddish
disturbed clay.
A certain pattern in the inclination may be present,
but the scatter is quite high (Fig. 5). Most values are more
shallow than the expected geocentrical axical dipole
(GAD) value of the site, Io=70.2°. The shallow inclina-
tion may indicate a sediment compaction. The low values
between 4.7 m and 5.1 m are situated just above the Grûda
sediment (4.3 m to 4.65 m). The top part between 7.45 and
8 m consists of reddish disturbed clay. The small maxi-
mum in the intensity between 4.7 m and 5.1 m is situated
just above the Grûda sediment (4.3 m to 4.65 m; Fig. 5).
Stereogram of the AF-cleaned direction of individual
specimens, with their individual α95 confidence circles is
given in Fig. 3. The mean direction of glaciolacustrine
varved clay, sand and silt of Grûda–Þiogeliai age is
(Dm,Im)=(7.0°W, 55.7°), N=52, α95 =8.1°.
M a sk a u k a
N o rth
N o rth
Fig. 3. Stereographic plot of AF-cleaned ChRM – directions of the Maskauka, Didþiasalis, Manèiagirë and Netiesos profiles.
68
4. DIDÞIASALIS SECTION
In the Didþiasalis section of varved clays both mag-
netic declination and inclination show a long-wave varia-
tion (Fig. 6), the declination with more westerly values
between 6 and 3.5 m depth, and a short-wave variation at
the top of the profile between 2.5 and 0 m. On the dia-
grams, each dot indicates the AF-cleaned ChRM of one
oriented specimen. The swings in declination between
3 and 2.5 m are likely to be due to some kind of sediment
disturbance, the intensity being quite high (Fig. 6).
Smoothed declination varies around 0° between ±30°
(Fig. 6). Except the top, the inclination is systematic low
as compared to the geocentrical axical dipole (GAD)
value of Io = 70.9°, which may indicate some compaction
of the sediment (Fig. 6). The variation as well as the local
scatter in the intensity values are likely to indicate
lithological variations in the clay and silt proportions of
the thin-laminated varved clays (Fig. 6).The mean direc-
tion of glaciolacustrine clay of Didþiasalis section is
(Dm,Im)=(6.5°E, 55.0°), N=58, α95 =5.7° (Fig. 3).
Didþiasalis
N o rth
N e tie so s
N o rth
 Gaigalas et al.

SA M PL E: G I 6
N

1 .0
90
A X IS = 5 m A /M L IN E S :

0 .0
0 20 40 60 80 1 00 m T

N 270, Up Gi 17

1 .0
360
A X IS = 1 0 m A /M L IN E S :

0 .0
0 20 40 60 80 1 00 m T

270, Up Gi 30

1 .0

A X IS = 1 0 m A /M L IN E S : 360

0 .0
0 20 40 60 80 1 00 m T

Fig. 4. Stereographic, intensity decay and orthogonal plots of AF-cleaned ChRM-directions of 3 pilot specimens (samples No. 6, 17
and 30) from the Girininkai profile.

69
 PALAEOMAGNETISM OF LITHUANIAN UPPER PLEISTOCENE SEDIMENTS

superposed upon a short-wave variation at the lower half

M a sk au k a of the profile. The general trend in declination is a change
M ag n e tic S e c u la r V a ria tio n from westerly declination at the lower part towards east-
D e c , In c & I n t (3 - p t m o v in g a v era g e )
erly declination at the top (Fig. 8). The swings in declina-
-1 2 0 -9 0 -6 0 -3 0 0 30 60 90 120 tion between 1.15 m and 1.35 m are likely to be due to
some kind of sediment disturbance, the intensity being
-8 quite high. The upper part of the profile may be disturbed
D ec In c due to roots and due to low intensity of more sandy sedi-
ment on the top.
In t
As mentioned above, systematic short wave pattern
appears between 0.4 m and 1.3 m in inclination from
around 70° at 0.8 m to around 80° at 2 m (Fig. 8). The GAD
value of the site is Io=70.1°. The NRM intensity of black
-7 gyttja is systematically higher than of the sandy intervals
H e ig ht a b ov e riv er (m )

at 1 m and above 2 m (Fig. 8). Mean direction of the

Manèiagirë profile (Alleröd) is (Dm, Im)=(30.0° W, 77.8°),
N=44, α95 =2.7 (Fig. 3).

-6
D id þia sa lis
M a g n e tic S ec u lar Va ria ti o n
D ec , In c & In t (3 -p t m o v in g av erag e )
-9 0 -6 0 -3 0 0 30 60 90 120
0
Int
-5 Dec Inc
1

Fig. 5. Magnetic inclination (Inc), declination (Dec) and intensity

D e p th b e lo w s o i l (m )

(Int) of deposits of Maskauka profile. Full lines are 3-point

moving averages.
3

5. GIRININKAI SECTION

Judging from 6 pilot specimens from the Girininkai 4

profile, the magnetic direction is fairly stable (Fig. 7).
However, magnetic declination is rather scatter, and is
hardly diagnostic for the geomagnetic secular variation,
5
expected variation of which would be close to true North,
i.e. 0°±20°. Inclination is also somewhat strange, being
rather shallow around 30°±30°, whereas the expected in-
clination for an average geomagnetic field in Lithuania 6
would be around 70°±10°. This shallow inclination may
indicate compaction of the sediment. The palaeomagnetic
investigation of the interstadial sediments covers the time
interval from 11,630±120 to 12,700±80 years ago in the 7
Manèiagirë section (Gaigalas, 1994).

6. MANÈIAGIRË SECTION
8
The Manèiagirë section spans the Alleröd interstadial
over the Ûla River. AF-cleaned declination and inclina- Fig. 6. Magnetic inclination (Inc), declination (Dec) and
tion both show a systematic trend with low values and low intensity (Int) of deposits of Didþiasalis profile. Full lines are
scatter between 0.4 m and 1.3 m above the river level, 3-point moving averages.

70

7. NETIESOS SECTION
The palaeomagnetic research of the Merkinë
(=Eemian) Interglacial sediments covers the time inter-
val since 112±25 ka to 101.5±11.5 ka years BP in the
Netiesos section. The Merkinë deposits are represented
by gyttja and peat with silt in the bottom part of the sec-
tion. The geomagnetic Blake event, some times recorded
in Eemian deposits (e.g. Abrahamsen, 1995), is not found
in the Netiesos profile (Fig. 9).
Declination (AF-cleaned) is mostly East of North, but
the scatter is quite high, due to sandy character of sedi-
ments (Fig. 9). In inclination, a certain pattern may be
seen in the 3-point moving average (full line), but the scat-
ter is rather high due to sandy character of sediments
(Fig. 9). There has been no compaction of the sediments,
as the average inclination is close to the GAD value of
the site, Io=70.2o. The NRM intensity of the profile
decreases upwards, the sediments becoming more sandy
G irin in k a i
M a g n e tic S e c u la r Va ria tio n
D e c , In c & In t
-9 0 -6 0 -3 0 0 30
0
D ec
1 M ag n etic S ec u la r V ar ia tio n
2 - 2 .2
3 - 2 .0
D e p th b e lo w s o il (m )
4
5
7
10
Fig. 7. Magnetic inclination (Inc), declination (Dec) and intensity
(Int) of deposits of Girininkai profile.
Gaigalas et al.
towards the top (Fig. 9). Stereogram of the AF-clean
direction of individual specimens. The mean direction is
(Dm,Im)=(19.4oE, 71.1o), N=66, α95 =3.2o, k=30.1 (Fig. 3).
8. CONCLUDING REMARKS
Our data appear to be too scattered to define any sig-
nificant excursion of the geomagnetic pole in the time in-
terval of 18,000-14,000 BP (Maskauka, Didþiasalis and
Girininkai) and in 11,600-12,700 BP (Manèiagirë inter-
stadial), as well as in the time of the Last interglacial
(112±25 ka to 101.5 ± 11.5 ka BP). However, some mag-
netic information can be obtained from the varved clays
of the Late Pleistocene time. The variation as well as the
local scatter in the intensity values are likely to indicate
lithological variations in the clay and silt proportions of
the thin laminated varved clays. The swings in declina-
tion are likely to be due to some kind of sediment distur-
bance (sediment compaction due to glacial activity), the
intensity being quite high.
We do not find the Gothenburg excursion in the time
interval of 18,000-11,000 BP. The VGP (Virtual geomag-
netic pole) do not fall below 60° N. The geomagnetic Blake
event, some times recorded in Eemian deposits is not
found in the Netiesos profile of the Merkinë Interglacial.
60 90
In c
M a n èia g ir ë
D e c , In c & In t (3 - p t m o v in g a v e ra g e)
In t
-1 5 0 -1 2 0 -9 0 -6 0 -3 0 0 30 60 90 120 150
Inc
Int
H e ig h t a b o v e riv er (m )
- 1 .5 Dec
- 1 .0
- 0 .5
Fig. 8. Magnetic inclination (Inc), declination (Dec) and intensity
(Int) of deposits of Manèiagirë profile. Full lines are 3-point
moving averages.
71
 PALAEOMAGNETISM OF LITHUANIAN UPPER PLEISTOCENE SEDIMENTS

ACKNOWLEGEDGEMENTS
N e tieso s (l o w er p a rt)
M ag n e tic S e c u la r Va ria tio n
D e c , In c & In t (3 - p t m o v i n g a v er ag e ) Financial support for the study was provided by the
Lithuanian State Science and Studies Foundation under
-6 0 -3 0 0 30 60 90
grant No. T-522 of 2001 year.
-7 In t
REFERENCES
D ec In c
Abrahamsen N., 1995: Palaeomagnetism of Quaternary sediments
from Anholt, Denmark. The onset of the Blake Event and Eem.
-6 Bull. Geol. Soc. Denmark 42: 96-104.
Bakhmutov V.G. and Zagniy G.F., 1990: Secular variation of the
geomagnetic field: data from the varved clays of Soviet Karelia.
In: Physics of the Earth and Planetary Interiors 63. Elsevier Sci-
ence Publishers B. V., Amsterdam: 121-134.
H e i g h t a b o v e ri v e r (m )

-5
Ekman I., Bakhmutov V. and Zagny G., 1987: Stratification and cor-
relation of varved clays in terms of the fine palaeostructures of
the Earth’s magnetic field. In: Methods for the investigation of
lake deposits: palaeoecological and palaeoclimatological aspects.
-4 Vilnius: 47-61.
Gaigalas A., 1994: On palaeogeography of Late Pleistocene in the
Lithuania. Acta Universitatis Nicolai Copernici. Geografia XXVI.
Nauki Matematyczno-Przyrodnicze – Zeszyt 92: 183-194.
Gaigalas A., Pevzner M. and Meleðytë M., 1991: Palaeomagne-
-3 tization of the Late Quaternary deposits of the South Baltic
region. In: Geochronological and isotope-geochemical research
into Quaternary Geology and Archaeology. Vilnius University
Press: 27-40 (in Russian).
Pevzner M. and Gaigalas A., 1976: Remanent Magnetization. In:
-2 The buried paleo-incisions of sub-quaternary rocks surface of the
South-East Baltic region. Mokslas Publishers, Vilnius: 65-74.
Torsvik T., 1992: IAPD – Interactive analysis of Palaeomagnetic
Fig. 9. Magnetic inclination (Inc), declination (Dec) and intensity Data. In: Manual. NGU, N-7002 Trondheim, Norway: 51.
(Int) of deposits of Netiesos profile. Full lines are 3-point
moving averages.

72
 GEOCHRONOMETRIA Vol. 21, pp xx-xx, 2002 – Journal on Methods and Applications of Absolute Chronology

210
Pb DATING OF YOUNG HOLOCENE SEDIMENTS IN
HIGH-MOUNTAINS LAKES OF THE TATRA MOUNTAINS

ADAM KOTARBA1, EDYTA £OKAS2 and PRZEMYS£AW WACHNIEW 3

1
Department of Geomorphology and Hydrology, Institute of Geography and Spatial
Organisation, Polish Academy of Sciences, Œw. Jana 22, 31-018 Cracow, Poland
2
The Henryk Niewodniczañski Institute of Nuclear Physics, Radzikowskiego 152, 31-342 Cracow, Poland
3
Faculty of Physics and Nuclear Techniques, University of Mining and Metallurgy, Mickiewicza 30, 30-059 Cracow, Poland
(e-mail: viw@ftj.agh.edu.pl)

Key words
words: Abstract: Topmost sediments in two oligotrophic lakes of the High Tatra Mountains were
210
Pb DATING, studied in terms of sedimentological characteristics and 210Pb dating. An alpine lake sediments
LACUSTRINE SEDIMENT, are important source of information on geomorphic process activity in glacial catchments.
SEDIMENTATION Two different sediment transfer models are represented. In Morskie Oko lake basin majority
RATE, HIGH TATRA of extreme, short lasting geomorphic events triggered on the surrounding slopes are registred
MOUNTAINS in lake sediments (minerogenic laminae), while in Zelene Pleso lake only an effect of pro-
longed flooding periods are to be seen. The sedimentation rates in both lakes are similar.

1. INTRODUCTION This paper attempts to calculate sedimentation rate

for two alpine catchments of the granodiorite High Tatra
Contemporary geomorphological evolution of moun- Mountains, which differ in size and geomorphological
tain landscape could be studied by use direct measure- units responsible for transfer of surficial material (Fig. 1).
ment of the effects of geomorphic processes on slopes and
in valley floors. Such studies are conducted by field ex-
periments, in which some fragments of landforms are
taken into monitoring of morphological changes after
certain periods. In this way one can collect quantitative
data on the rate and mode of transformation both by ero-
sion and accumulation processes. However, such data are
valuable for relatively small fragments of a given land-
scape, and cannot be used for evaluation of geomorpho-
logical changes within larger units, e.g. they are not suffi-
cient for estimates of sediment budget in alpine
catchments. Therefore, lacustrine sediment budgets are
commonly used as a measure of the operation of contem-
porary and paleogeomorphological processes in mountain
catchments (Wolman and Miller, 1960; Larsen and
Magnerud, 1981; Owens and Slaymaker, 1993). In such
studies, duration of the erosion period and the volume of
eroded bedrock, deposited in lake, is used as a measure
of erosion in glacial cirques since the ice withdrawal. It is
evidences by many authors that mountain cirque lakes
may trap a high portion of allochtonous minerogenic
material inflowing from the surrounding slopes. The sedi-
ments remain in the lake, and give records of environmen-
tal changes in the catchment, but not all material detached
from hillslopes reaches the lake basin. Thus, erosion rates
calculated according to sedimentation rates and total sedi-
ment volume may underestimate the true values. Fig.1. Location map for the Tatra Mountains.
 210
Pb DATING OF YOUNG HOLOCENE SEDIMENTS IN HIGH-MOUNTAINS LAKES...
2. METHODOLOGICAL BACKGROUND
AND STUDY AREA
An alpine sediment transfer model developed by
N. Caine (1974) consists seven possible internal transfers.
Complete set of slope and valley units contain all possible
geomorphological units within which transfer of surficial
material is going on. These fundamental units are used in
the examination of geomorphic process activity in a se-
quence of sediment transfers from interfluve to lake
basin. The final products of sediment transfers are stored
and registered in lake, and sedimentation rate in lake is
quantitative measure of alpine geomorphic activity. Pre-
cise dating of sediment units (members) provides an im-
portant tool in these studies. Thus, 210Pb dating seems to
be a useful method in studies of youngest Holocene sedi-
ments.
This study assesses dynamics and mode of two glacial
cirques in the High Tatra Mountains (Southern Poland
and Slovakia) during the last ca 150 years on the basis of
210
Pb dating of lacustrine sediments; in the Morskie Oko
Lake of Poland (MO) and the Zelene Pleso Lake of
Slovakia (ZP). These two oligotrophic lakes which a
straddle upper timberline-alpine ecotone are located on
the northern side of the mountains (Fig. 2). Two differ-
ent models are presented in the catchments taken into
consideration. The Morskie Oko model contains only
three internal transfers: free-face/rocky slope – talus – lake
basin. Zelene Pleso model contains five internal transfers:
free-face/rocky slope – talus – talus foot – valley floor –
lake basin. In hanging valley called “Medena Dolina” the
greatest Tatra glacierette exists. Hydraulic connection
exists periodically between glacierette and Zelene Pleso.
Morskie Oko Lake is located at 1395 m a.s.l., with a sur-
face area of 34.5 ha, and maximum depth of 51 m. The
basin is glacially scoured, with infill sediment thickness
5–6 m (Baumgart-Kotarba et al., 1993). The core was
extracted from the southern side of the basin at the depth
of 37 m. Zelene Pleso Lake located at 1542 m a.s.l.,
Fig.2. Location map for Morskie Oko (MO) and Zelene Pleso Lake (ZP).
74
is relativelly small (surface area of 1.77 ha) and shallow
(4 m). The core was extracted from a flat bed 4 m below
the water table.
Lake sediments were sampled with a 0.65 m Axelsson
corer. Cores were immediately stored vertically and trans-
ported to the Laboratory at the Department of Geomor-
phology and Hydrology, Polish Academy of Sciences in
Cracow together with the water rich uppermost unit.
Coring tubes filled with the sediment were X-rayed. On
extrusion the cores were sliced into subsamples, and taken
for absolute dating and grain-size distribution analyses.
The main reference for 210Pb dating of the Morskie Oko
sediments is Baumgart-Kotarba et al. (1993). The Zelene
Pleso core was extracted in 2000.
The Zelene Pleso core was sectioned at 2-3 mm in-
crements. The dry mass of sediment samples was 1-3 g.
210
Pb activities were determined via its granddaughter
210
Po. It was assumed that both isotopes were in radioac-
tive equilibrium. Polonium separation procedure followed
the method of Flynn (1968). The samples were treated
with a hot nitric acid and then H2O2 was added to them in
order to oxygenate organic matter. After mineralisation
the solution was evaporated to dryness. The dry residue
was dissolved in HCl and evaporated again. Nitric acid
was completely replaced with hydrochloric acid after dis-
solution and evaporation cycle was repeated three times.
Polonium was deposited on silver disc from the 0.5 M
solution of HCl at 930C. 0.4 g of hydrazine dichloride was
added in order to remove ions disturbing polonium depo-
sition. After 3 hours of deposition, the silver disc surface
was covered with white coating. Alpha activity was mea-
sured by Canberra Alpha Analyst spectrometer with
Si PIPS detector. Before the samples were treated with
the nitric acid 208Po was added to control efficiency of polo-
nium deposition and alpha detection. Counting time of
single sample was approximately 2 – 3 days. Errors of total
210
Pb specific activities depended on counting times and
sample 210Pb activities and varied in the range 0.002 – 0.016
Bq/g (1.6 – 8.8%).
 A. Kotarba et al.

3. RESULTS AND DISCUSSION 210

Pb [Bq/g]
0 0.5 1 1.5
Morskie Oko
0
Two distinct sediment types: gyttja and inorganic clas-
tic sediments dominates in the core. Inorganic individual 1983
1971
laminae or layers (silty and clayey material, with < 3% of

Depth [cm]
sand) are sharp and horizontally interbedded within gyttja
(Fig. 3; Kotarba, 1995). 2
1923
Fig. 4 summarises results of 210Pb dating obtained for
1918
the Morskie Oko sediments (Baumgart-Kotarba et al.,
1905
1993). Ages of 2-3 mm thick layers shown in the figure
1892
were calculated assuming the constant sedimentation rate 4
(0.37 mm/year) for the whole core. This sedimentation
Fig.4. Profile of specific activity of unsupported 210Pb and ages
rate was derived from the mean slope of 210Pb specific 2-3 mm thick layers of the Morskie Oko sediments (Baumgart-
activity plotted on a logarithmic scale (Robbins, 1978). Kotarba et al., 1993).
Ages of specific layers were determined by dividing their
depths by the sedimentation rate.
Total specific activity of 210Pb [Bq/g]
Zelene Pleso
0 0.1 0.2 0.3 0.4
Sediments of the Zelene Pleso Lake are different in
terms of lithological properties and sedimentation rate 0
1
values. Homogeneous, inorganic material is very fine-
2
grained, clayey-silty, grain size between 0.5 - 200 µm, and
Depth [cm]

3
median values (M50) between 20-50 µm. Organic matter
4
content is very low (2.15-6.23%) as well as organic car- 5
bon content (1.25-3.61%). 6
Fig. 5 shows total 210Pb activities in sediment core from 7
Zelene Pleso. It was assumed that 210Pb activities at depths 8
6.15 cm (0.064 Bq/g) and 7.05 cm (0.060 Bq/g) represent
supported 210Pb levels. Mass weighted average activity of Fig.5. Profile of total specific activity of 210
Pb in sediments
these two sediment layers (0.061 Bq/g) was subtracted of Zelene Pleso Lake.

Fig.3. X-radiograph, densitometric curve and dating of sediment core S3 from Morskie Oko Lake (according to Kotarba, 1995).

75
 210
Pb DATING OF YOUNG HOLOCENE SEDIMENTS IN HIGH-MOUNTAINS LAKES...

from total 210Pb activities in order to obtain unsupported
210
Pb levels. Unsupported 210Pb activity varied in the range
0.019 (4.95 cm) to 0.276 Bq/g (0.55 cm). The decline in
unsupported 210Pb activity with depth is nonmonotonous
with two distinct minima corresponding to depth ranges
2.0–3.0 cm and 4.8–5.0 cm (lowest activities in these ranges
are 0.090 and 0.080 Bq/g, respectively). Due to pro-
nounced non-monotonic change of the unsupported 210Pb
activity profile the CRS (constant rate of supply; Goldberg,
1963) model seems to be an appropriate mathematical
framework to evaluate ages and sedimentation rates for
the Zelene Pleso Lake sediments. The following formula
was used to determine ages of sediment layers:
t=(1/ λ)* ln (Ac(0)/Ac(x)),
where Ac(0) is cumulated specific activity of unsupported
210
Pb integrated over the whole profile, and Ac(x) repre-
sents cumulated activity integrated for the part of profile
below the depth x. Fig. 6 shows absolute ages calculated
for all sediment layers. Uncertainties (1σ) of age deter-
mination were lower than 4 years.
Ages of sediment layers were used to calculate appar-
ent sedimentation rates for each layer. It was assumed that
the calculated age corresponds to the centre of the layer.
Sedimentation rates presented in Fig. 7 were calculated
according to the following formula:
where rn is sedimentation rate for the interval between
centres of the n-1 and n-th layer, hn and tn are depth and
age of the n-th layer, h0 = 0, t0 = 0. General decrease of
the sedimentation rate down the profile reflects compac-
tion and/or diagenesis of the sediments. Superimposed on
this general trend are peaks of increased sedimentation
rates at depth ranges 4.8–5 cm and 2–3 cm. These ranges
correspond to periods 1905–1910 AD and 1970–1975 AD,
respectively. Average sedimentation rate calculated for
the whole profile is 0.044 cm/year.
Fig. 8 shows dry surface mass accumulation rates cal-
culated according to the CRS model:
r(x) = λ*Ac(x)/C(x), (3.3)
(3.1)
where r(x) is mass accumulation rate at depth x and C(x)
is unsupported 210Pb activity at depth x. Distinct maxima
of mass accumulation rate correspond to minima in 210Pb
specific activity (Fig. 5). According to the CRS model such
patterns reflect periods of accelerated sedimentation
when unsupported 210Pb bearing sediments were diluted
by material with lower 210Pb content.
The inventory of 210Pb in the sediment profile (Ac(0))
equalled 0.632 Bq/cm2. Provided that there is a steady state
between atmospheric supply and radioactive decay, the
flux of 210Pb from the atmosphere (Bq/cm2*year) was
obtained as:

rn = (hn - hn-1)/(tn – tn-1), (3.2) 210

Pb flux = λ*Ac(0), (3.4)

and equalled 0.020 Bq/cm2*year. This flux is less than twice

as much as atmospheric fluxes estimated for this part of
Age [years] Europe (Preiss et al., 1996) what advocates (Oldfield and
0 50 100 150 200 Appleby, 1984) use of the CRS model in this case.
0
4. CONCLUSIONS
1
Depth [cm]

2 Lake sediments in two glacial cirques of the High

3 Tatras differ in terms of sedimentological properties. This
4 is conditioned by various transfer of surficial material to
lake basins by contemporaneous geomorphic processes.
5
In the case of three internal transfers model of Morskie
6 Oko lake, lacustrine sediment contains relatively precise
record of all major geomorphic events which occurred on
Fig.6. Profile of ages of 2 mm thick layers of the Zelene Pleso
sediments. the slopes, first of all rapid mass wasting (debris flow).

Sedimentation rate [cm/year] Accumulation rate [g/cm2 year]

0.0 0.1 0.2 0.3 0.4
0 0.05 0.1 0.15 0.2
0
0
1 1
Depth [cm]

2
Depth [cm]

2
3 3
4 4
5
5
6
6

Fig.7. Profile of sedimentation rates for Zelene Pleso Lake. Fig.8. Profile of mass accumulation rates for Zelene Pleso Lake.

76
 A. Kotarba et al.
210
Pb dating of minerogenic laminae allow to distinguish
exact time of their trigger.
On contrary, within Zelene Pleso lake, where five in-
ternal transfers model is appropriate, the main source of
terrestrial sediment supply to lake basin is fluvial
(“glacifluvial”). The surrounding gullies and braided chan-
nels are seasonally active mainly during snowmelt peri-
ods. Thus, the sediments reaching the lake are fine grained
and monotonous. Distinct boundaries within these sedi-
ments mark only seasons of catchment flooding caused
by snowmelt waters supplemented with continuous
summer rains. Signals of debris flow activity do not exist.
Increased sedimentation rate at depth range 4.8–5.0 cm
and 2-3 cm, which corresponds to period 1905–1910 AD
and 1970–1975 AD could be interpreted as an effect of
specific weather conditions. Initial analysis made for
Zelene Pleso sediments showed that there exists signifi-
cant relation between precipitation regime and sedimen-
tation rate. Rainfalls of long duration (several days of
continuous rains) followed by intensive downpours, pro-
duced the great melt and high discharges in the High Tatra
Mountains and on the northern foreland. Substantial sum-
mer floods were recorded at that time span. Probably,
glacierette-generated runoff in hanging valley (the
Medena Dolina valley within catchment basin) was inten-
sified by summer rainfalls of 102.5 mm/day (Skalnate
Pleso station) and 300 mm/day (Hala G¹sienicowa sta-
tion) in 30 June 1973, and respectively 328–596.4mm in
June 1973. These circumstances explain maximum accu-
mulation rate at the depth of 2-3 cm. An important pe-
riod of slope alluviation, mainly by debris flows, identi-
fied by the use of lichenometry at the beginning of 20th
century, was also distinguished at Hala G¹sienicowa area
(Kotarba, 1997).
In spite of similar rate of sedimentation in both lakes
(MO–0.044 cm/year, ZP–0.037 cm/year), these indices are
not valuable as a measure of geomorphic process activity
on the surrounding slopes of alpine lake, because sediment
delivery to the lakes is a function of catchment size, topo-
graphy and first of all - surficial water circulation.
77
ACKNOWLEDGEMENTS
This paper is part of a programme founded by KBN
grant 6 P04E 037 19: The response of geomorphic pro-
cesses to climate change in the last 300 years in the High
Tatra Mountains awarded to Dr A. Kotarba. Lake sedi-
ment collection during winter fieldwork in Slovakia
(Zelene Pleso Lake) would have been impossible with-
out the energy and assistance of M.A. Maria Johansson
(Kiruna, Sweden) and M.A. Stanis³aw Kêdzia (Cracow,
Poland).
REFERENCES
Baumgart-Kotarba M., Kotarba A. and Wachniew P., 1993: Young
Holocene lacustrine sediments of the Morskie Oko Lake in the
High Tatra and their dating by use 210Pb and 14C radioisotopes.
Dokumentacja Geograficzna IG i PZ PAN, Z Badañ Fizyczno-
Geograficznych w Tatrach 4-5: 45-61 (in Polish).
Flynn W. W., 1968: The determination of low-levels of polonium-210
in environmental materials. Analytica Chemica Acta 43: 221-227.
Caine N., 1974: The geomorphic processes of the alpine environ-
ment. In: Arctic and Alpine Environments. London: 721- 741.
Goldberg E. D., 1963: Radioactive dating. IAEA Symp.: 121-131.
Kotarba A., 1995: Rapid mass wasting over the last 500 years in the
High Tatra Mountains. Questiones Geographicae, Special Issue
4: 177-183.
Larsen E., and Magnerud J., 1981: Erosion rate of a Younger
Dryas cirque glacier at Kråkenes, Western Norway. Annals of
Glaciology 2: 153-158.
Oldfield F. and Appleby P. G., 1984: Empirical testing of 210Pb
dating models for lake sediments. In: Haworth E. Y. and Lund
J. W. G., eds., Lake sediments and Environmental History. Leic.
Univ. Press, Leicester: 93-124.
Owens P. and Slaymaker O., 1993: Lacustrine Sediment Budget in
the Coast Mountains of British Columbia, Canada. In: McMa-
nus J. and Duck R..W.,eds., Geomorphology and Sedimentology
of Lakes and Reservoirs. J.Wiley & Sons Ltd: 105-123.
Preiss N., Melieres M. A. and Pourchet M., 1996: A compilation of
data on lead 210 concentration in surface air and fluxes at the
air-surface and water-sediment interfaces. Journal of Geophy-
sical Research 101: 28,874-28,862.
Wolman M. G. and Miller J. P., 1960: Magnitude and forces in geo-
morphic processes. Journal of Geology. 68: 54-74.
210
Pb DATING OF YOUNG HOLOCENE SEDIMENTS IN HIGH-MOUNTAINS LAKES...

78
 GEOCHRONOMETRIA Vol. 21, pp 79-84, 2002 – Journal on Methods and Applications of Absolute Chronology

A BETTER-DEVELOPED SOIL PROFILE DURING

BIBLICAL TIMES IN THE WESTERN GALILEE.
15
N EVIDENCE IN 14C - DATED GROUNDWATER
V. ROGOJIN1, J. KRONFELD1, ISRAEL CARMI2 and A.S. TALMA3
1
Department of Geophysics and Planetary Sciences, Tel-Aviv University, Tel-Aviv, Israel
2
Radiocarbon Laboratory, Weizmann Institute of Science, Rehovot, Israel
3
Quaternary Dating Research Unit, CSIR, Pretoria, South Africa

Key words
words: Abstract: Despite almost a hundred years of reforestation efforts, the recharge area of the
CARBON ISOTOPES, Judea Group aquifer in the hills of the western Galilee still shows the signs of the severe soil
NITROGEN ISOTOPES, erosion that transpired in previous centuries. At present the soil profile is thin and basement
SOIL, rock is often exposed. Historical and Biblical sources suggest that the hills in the past were
LANDSCAPE CHANGES, more forested. Therefore, the δ15N values of dissolved nitrate were measured in radiocarbon-
CLIMATE CHANGES dated groundwater to see if evidence for past soil conditions could be deduced. Nitrate mine-
ralization processes in soils lead to enrichment in 15N of the residual nitrate, which being
dissolved by rain enters into the groundwater without further isotopic fractionation. Previo-
us studies have shown that there is a trend of increasing δ15N in a soil profile from plant, to
litter, to the organic material in the soil. In addition, there is a tendency for higher δ15N values
to be observed in those samples that have been taken at greater depth in a soil profile due to
progressive mineralization and subsequent nitrification of soil organic material. As long as
the dissolved oxygen is not depleted, denitrification will not occur to alter the isotopic com-
position of the dissolved nitrate. The nitrate concentrations and δ15N values, water chemistry,
tritium and radiocarbon activities were measured from the phreatic outcrop recharge region,
and onwards into the confined portions of the Judea Group aquifer and its continuation into
the juxtaposed Kurdani and Pleistocene aquifers. The radiocarbon activity decreases
with flow. Tritium values of above 2 TU are restricted to the recharge region. Using an initial
14
C activity of 64 pMC the radiocarbon ages of the water are found to range from recent to
7800 BP. The δ15N values of the dissolved nitrate within the young water recharge area fall in
the range of +3.1 to +4.8‰ (Air), having a mean of +3.9‰ (n=5). In older water the nitrate
concentration increases slightly, while the δ15N ranges from +4.7 to +7.2‰ (Air), having
a mean of +6.4‰ (n=17). The increase in the δ15N values in the older water down-dip is not
due to denitrification processes; for, the waters are well oxygenated. These older waters infil-
trated at the same point of origin in the phreatic portions of the aquifer (non-contaminated)
as the recent water. As the earlier infiltrating water flowed down dip they retained the δ15N
values of the environment at that time. The δ15N values present evidence that, compared to the
present, the soil and plant cover was better developed in earlier times, including Biblical times.

1. INTRODUCTION
There are two dominant processes that cause changes
in the landscape. One is human activity and the other is
climate change. Beginning with our forebears who tra-
versed the Middle East about 100,00 years ago and spread
into Europe and Asia (Stringer and Mckie, 1997), the
Land of Israel has always been a zone in which people
have wandered back and forth (Fig. 1). To name a few,
we have the Egyptians, the Babylonians and the sons of
Israel who went to Egypt and came back (Genesis 47:1;
Exodus 15: 16-28). Likewise, in more recent times Napo-
leon and his forces, similar to other armies in the past,
marched up from Egypt and back again across the Land.
At other times, the Middle East corridor was accessed also
from the sea – in Biblical times, e.g. by the Philistines
(Amos, 9:7). In the middle Ages, waves of Crusaders came
to the land of Israel, by way of the land as well as by the
sea (Benvenisti, 1970). All these coming and going
through the Middle East left a mark on the landscape.
Trees were cut for firewood and for building. Space was
cleared for agriculture. The latest and most intensive as-
sault on the landscape was made by the Ottomans, who,
during the First World War, cut the forests of the country
 A BETTER-DEVELOPED SOIL PROFILE DURING BIBLICAL TIMES ...
at a rate of 10 tons/day, to feed their steam locomotives,
which traversed the country from the north down to Beer
Sheba (Sheffer, 1987). From the Bible, we know that dur-
ing the Iron Age, at the time of our Patriarchs, the land
was covered with extensive forests; although, the trees might
Fig. 1. The Land of Israel has served as a land corridor of the
Middle East, through which people have migrated and armies
have passed for millennia (Modified from Passover Hagada,
Koren Publishers; Jerusalem, 1979).
Fig. 2. Present day rainfall distribution map of Israel. There is
a steep north south gradient in the precipitation. The desert
boundary is located today in the vicinity of Beer Sheva. The
study area extends from the hills of western Galilee to Haifa Bay,
immediately north of Haifa.
80
not have been big (King Solomon had to import cedars
from Lebanon in order to build the temple (I Kings 5:6)).
Israel is not only a passage way but a transition zone
between temperate and desert climate regimes. The tran-
sition line between these two regimes has been delineated
by Goodfriend (1988) near the town of Beer Sheba (Fig. 2).
Clearly a northward shift of the desert would profoundly
affect the floral landscape. The possibility that the transi-
tion zone has not always been anchored near Beer Sheba
must be investigated before it can be excluded as having
been a cause of forest degradation to the north in the past.
In this paper we investigate the evidence, and evalu-
ate the causes for change in the landscape using climate
proxy data, preserved in the groundwater of an important
aquifer water in northern Israel, near Haifa (Fig. 2). The
aquifer (Fig. 3) is bounded by the hills of the lower Gali-
lee in the east and by the Coastal Plain, to the west (Mero,
1983). The direction of water flow is from the east, where
recharge takes place, westwards. The present-day top soil
is very thin and in many places the bed rock is exposed. It
had been eroded by rain flushing away the bare soil of
the denuded hills under the influence of the the steep
gradient of the terrain,which enabled the process to be
very efficient. In the cross section of the Judea Group
aquifer (Fig. 4) it is seen that the recharge in the east is
into a matrix of limestones and dolomites. Flowing down
dip from the phreatic recharge area, the water becomes
confined under an impermeable aquiclude. Further to-
wards the sea there are two small aquifers (Kurdani and
Pleistocene) overlain by a thick impermeable clay layer.
Faulting has juxtaposed portions of the permeable beds
of each aquifer against each other. Therefore, this has
enabled water from the Judea Group aquifer to drain into,
and recharge in turn, the carbonate Kurdani aquifer, and
then the sandy Pleistocene aquifer. A small outcrop of the
Kurdani aquifer supplies some water to the Pleistocene
aquifer as well. Other than this small recharge, no surface
water has entered these aquifers except that which has ori-
ginated the in hill region where the Judea Group outcrops.
Fig. 3. Geological map of the study area showing location of
the samples. The outcrop area of the Judea Group carbonate
aquifer is restricted to the hills in the east. It is overlain by
younger, impermeable strata westwards of the recharge. The
Kurdani aquifer, which receives drainage from the Judea Group,
has only two small surface exposures. The hydrologically
connected Pleistocene aquifer is only encountered in the
subsurface. The Pleistocene aquifer is not seen at the surface
because it is covered by recent dune aquifer.
 V. Rogojin et al.
Fig. 4. A schematic east-west hydrogeologic cross-section
is presented using representative wells from the recharge and
confined sections of the Judea Group aquifer. Sample 6 is
projected onto the section to show the hydrologic interconne-
ction between the Kurdani aquifer and the Judea Group, while
samples 4 and 33 are projected on this east-west cross section
to show interconnection between the Pleistocene aquifer and
the Kurdani aquifer.
2. METHODS
Water samples were collected from pumping wells that
exploit this multi-aquiferial system, with the purpose of
finding isotopic evidence for the timing and the causes of
changes in the landscape above the recharge area. More
specifically, evidence for the dilution or elimination of flora
and its subsequent effect on the topsoil was looked for.
In the water, two isotopic proxies were studied to dif-
ferentiate between the two possible scenarios outlined
above. One proxy is the ratio of the stable isotopes of
carbon. The composition of this isotopic ratio in aquifer
water is a result of the combination of inputs of carbon
from two end members: organic matter on the surface and
the matrix through which recharge water passes into the
aquifer (Mook et al., 1974). The source of organic matter
on the surface are plants that have grown there. In a tem-
perate climate these are predominantly C3 plants, with
δ13C values within the approximate range of –20 and –
32‰ (Clark and Fritz, 1997). When a temperate climate
gives way to desert conditions there is a corresponding
change in the flora. The land cover changes from C3 to
predominantly C4 plants. The latter are characterized by
δ13C values between –11 and –17‰ (Vogel et al., 1986).
As the other end member is a carbonate rock matrix, hav-
ing a δ13C of ~ 0‰ (Magaritz et al.,1983), then δ13C of
the dissolved bicarbonate in the water will be approxi-
mately half of the average soil gas value. Thus, if the aqui-
fer water were to exhibit a marked enrichment in13C, this
would be supportive of a climatic control; whereby, the
erosion would have resulted from a northward excursion
of the desert boundary from its present position.
The second proxy is the nitrogen isotope 15N. The ni-
trogen in water is also derived from organic matter in the
topsoil. The decomposition of this organic matter gener-
ates ammonium which can be partly volatilised as ammo-
nia gas (at high pH), and the remaining organic matter is
oxidized to nitrites and nitrates by bacterial nitrification.
When a light gas like ammonia is formed, it becomes rela-
tively depleted in 15N. The remaining nitrate becomes
enriched in 15N. The extent of the enrichment in 15N de-
pends on the intensity and duration of nitrification in the
81
top soil: when it is thick, more time is available for pro-
duction of ammonia and the 15N of nitrates becomes more
enriched. Previous studies have shown a trend of increas-
ing δ15N in a soil profile from plant, to litter, to the or-
ganic soil material. Moreover, there is a tendency for
higher δ15N values in samples that have been taken at
greater depth in a soil profile, due to progressive miner-
alization and subsequent nitrification of soil organic ma-
terial (Lajtha and Michener, 1994). By contrast, when the
topsoil is thin, the time of ammonia production is short
and the δ15N of the nitrate should be lower. Once in the
aquifer the isotopic signature of the dissolved nitrate will
not change unless either additional nitrate is added along
the water flow path, or if bacterial denitrification (which
occurs only under unaerobic conditions) of the dissolved
nitrate takes place. In the aquifer under consideration
both these effects can be excluded for: (1) no additional
inputs of nitrate, even if such sources were to have exis-
ted, could penetrate through the impermeable confining
aquicludes, and (2) the water of the Judea Group aquifer
is well oxygenated (8-9 mg/l in the recharge reigon and
4-7 mg/l in the confined region (Rogojin, 2000)). Thus,
anaerobic conditions never prevailed to allow for the al-
teration of the isotopic signature of the dissolved nitrate
by denitrification processes. Therefore, we feel confident
that the δ15N values of the groundwater at each sampling
site reliably reflect the isotopic signature of the dissolved
nitrate at the time of recharge. To use these proxies in
a historical context, we dated the aquifer water with 14C
and with tritium.
3. EXPERIMENT
The sampling was carried out in 1994-1996. Samples
for nitrogen analyses were collected in 1 liter plastic
bottles. The analyses were carried out at the Center for
Scientific and Industrial Research in Pretoria, South
Africa, using a SIRA 24 mass-spectrometer. The δ15N
values are reported relative to atmospheric air, with a pre-
cision of 0.15‰. Radiocarbon analyses required 50-liter
samples. The tritium and radiocarbon analyses were mea-
sured at the Radiocarbon Dating Laboratory at the
Weizmann Institute of Science in Rehovot, Israel. The
tritium was enriched by electrolysis, converted to ethane
and detected in proportional counters. Tritium concen-
trations are reported in tritium units (1 TU = 1 atom tri-
tium per 1018 atoms of hydrogen). The associated stan-
dard deviation is reported at the 1σ level of confidence.
The precision was better than 0.3 TU. Radiocarbon
measurements were carried out on the CO2 that was
precipitated as BaCO3 from 50 liters of water. It was con-
verted to ethane and 14C was detected in proportional
counters. The results are expressed in percent with respect
to “modern carbon” (pMC), with the associated statisti-
cal counting error at the 1σ level of confidence. The pre-
cision was better than 0.6 pMC. δ 13C was measured
using an Atlas MAT 250 mass spectrometer with a preci-
sion of 0.1‰.
 A BETTER-DEVELOPED SOIL PROFILE DURING BIBLICAL TIMES ...

4. RESULTS and 32.6 pMC; otherwise, it has a similar range nitrogen

Table 1 summarizes the data used in our interpreta-
tion. No NO2 was detected. The δ15N values of the dis-
solved nitrate within the recharge area fall in the narrow
range of +3.1 to +4.2‰. They gradually change to
higher values along the flow path, reaching +6 to + 7‰.
The nitrate values range from 12 to as high as 38 mg/L
nitrate but there is no consistent change in the nitrate con-
centrations with flow. The tritium values vary with geo-
graphical position. There are measurable amounts of tri-
tium in the phreatic recharge, and none in the confined
sections of the aquifer. The radiocarbon concentration
varies from 64-70 pMC in the phreatic region where tri-
tium is encountered, to 46 pMC in the well furthest the
down-dip (the Afeq-B well). The δ13C values vary from -
14.0 to -18.6‰ (PDB). In the Kurdani aquifer the δ13C
values vary from -12.3 to -15.2‰ (PDB), while the
radiocarbon activity is in the range of 50-55 pMC. The
nitrate values are similar to those most frequently encoun-
tered in the Judea Group water being in the range of ap-
proximately 12 to 23 mg/l, with a corresponding range in
δ15N values +5.6 to +7.0 ‰. The radiocarbon activity of
the water of the Pleistocene aquifer is much lower, 24.8
of isotopic values.
To convert the measured radiocarbon activity of the
water to an absolute age it is necessary to determine its
initial activity. According to the model of Ingerson and
Pearson (1964), the range of the initial activity of (pre-
thermonuclear) radiocarbon in the water is 64-66 pMC.
Kroitoru et al. (1989), using mass-balance considerations,
calculated the initial radiocarbon activity for recharge
water in the Judea Group aquifer to be 62±3 pMC. We
therefore use 64 pMC to calculate the ages of the water
in the aquifer (Table 1). Clearly, values above 64 pMC
have a component of thermonuclear radiocarbon and are
regarded modern. The oldest water in the main aquifer is
about 2800 years old. This defines the flow rate of this
aquifer to 5 m/yr, which is comparable with the rate of
flow of other carbonate aquifers in Israel (e.g. Kronfeld
et al., 1992). The waters in the Kurdani and Pleistocene
aquifers are significantly older, the oldest being about
7800 BP. Yet, they exhibit δ13C and δ15N values that are
similar to those from the confined portions of the main
aquifer. The hydraulic gradient near the coast is very
small, and this can explain the big difference in water ages
over small distance.

Table 1. Radiometric age data and nitrogen isotopic data in the multi-aquiferal system of the Western Galilee
Sample Wells Aquifer* Tritium δ 13C 14C Age NO3 δ 15N
Code # [TU] [‰, PDB] [pMC] [BP] [mg/l] [‰ Air]
Young samples from recharge region
41 Meged Kramim-1 J.G. 2.9±0.2 -15.1 64.0±0.6 Recent 14.6 3.7
42 Meged Kramim-2 J.G. 2.6±0.2 -14.6 70.1±0.4 Recent 15.5 4.0
43 Meged Kramim-3 J.G. 1.7±0.2 -14.9 66.1±0.5 Recent 12.4 3.1
44 Hazon-3 J.G. 5.6±0.2 -15.4 83.1±0.4 Recent 22.6 4.8
45 Hazon-4 J.G. 1.5±0.2 -15.5 76.4±0.4 Recent 20.4 4.2
Samples from confined section of the aquifer
38 Miar J.G. 0.5±0.3 -15.7 59.8±1.0 561±140 19.0 6.5
20 Akko-2 J.G. 1.9±0.2 -18.6 56.9±0.5 972± 73 23.5 6.8
40 Lokhamey K 2.0±0.2 -15.2 55.3±0.4 1208±60 22.6 6.9
HaGetto-Dror
39# Ahihud J.G. 0±0.2 -12.9 55.1±0.6 1238±90 12.4 4.7
6 Afeq-C K 0±0.2 -14.3 51.6±0.3 1780±49 12.0 5.6
16 Damun-5 J.G. 0.4±0.2 -14.0 50.5±0.4 1959±65 19.0 6.8
9 Kefar Masaryk-3 K 0.4±0.2 -12.3 50.0±0.7 2041±116 23.6 6.9
18 Akko-4 J.G. 1.1±0.2 -16.7 49.8±0.4 2074±66 14.6 5.1
13 Damun-3 J.G. 1.1±0.3 -14.5 48.3±0.4 2327±69 38.5 7.0
7 Afeq-B J.G. 0±0.2 -14.6 45.8±0.4 2766±73 17.3 6.6
4 Qiryat Khaim-24 P 0.2±0.2 -14.2 32.6±0.4 5577±102 10.2 6.1
33 Qiryat Khaim-22 P 0±0.2 -12.7 24.8±0.2 7838±67 11.5 7.2
Samples in confined section of the aquifer with measured δ15N but lacking concomitant radiocarbon ages
21 Birwa-3 J.G. n.d. n.d. n.d. - 13.7 5.9
19 Akko-3 J.G. n.d. n.d. n.d. - 16.4 7.0
15 Damun-4 J.G. n.d. n.d. n.d. - 25.7 6.8
14 Damun-1 J.G. n.d. n.d. n.d. - 31.9 6.4
10 Kefar Masaryk-2 K n.d. n.d. n.d. - 18.6 7.0
J.G. = Judea Group, K = Kurdani, P = Pleistocene,
# = a difference was noted, for this sample, between the nitrate concentration measured before the isotopic analysis and the yield of N that was produced in the laboratory- possibly
indicating that the isotopic analysis is suspect.

82

5. DISCUSSION
The 13C in the aquifer is quite depleted (Table 1) and
this suggests that the organic end-member of carbon in
the water, which came from the organic matter of the top-
soil, have always been C3 plants. For a contribution from
C4 plants we would expect values of δ13C around –7‰
and this is clearly not the case. We can thus conclude that
the change in the land cover was not due to the shift of
the desert line from Beer Sheba to the Lower Galilee.
Fig. 5. shows the δ15N data for water in the aquifer, as
a function of the age of the water, calculated from radio-
carbon. The broad picture is a practically stable value of
δ15N in the +6 to +7‰ range. This is in the range of δ15N
found in the literature for soil organic matter (Gormly
and Spalding, 1979; Heaton, 1984; Komor and Anderson,
1993). There are 5 additional measurements (Table 1) for
the confined portion of the aquifer that also fall within
this range; but, as we have no dates for them they are not
presented in Fig. 5. Though the aquifer contains one con-
tinuous water body, there is a sharp break in the nitrate
isotopic compositons that delineates the older from the
younger water groups, in which the δ15N of the dissolved
nitrate decreases to as low as +3.5‰. This change is taken
not as an isotopic evolution process that occurred within
the aquifer. No isotopic fractionation can be attributed
to bacterial denitrification within the downdip segment
of the aquifer to raise the δ15N; for denitrification requires
anoxic conditions and the waters are well oxygenated.
Indeed, no lowering of the nitrate concentration is noted.
Thus, the measured δ15N values have not been altered
within the aquifer. Therefore, these values reflect the
degree of isotopic fractionation of nitrogen within the soil
before the nitrate entered the aquifer. Thus it appears that
the groundwater preserves and records the changes in the
8
7 after the Arab conquest of the land, just before the Cru-
6 must remain speculative. It is clear, however, that a highly
5
d 1 5 N [‰]
?
4
3
2
1 responsible for the changes in the land cover of northern
0
0 11000
,0 0 0 22000
,0 0 0 33000
,0 0 0 44000
,0 0 0 55000
,0 0 0
R a dio ca rb on A g e [BP]
y e a rs B .P .
Fig. 5. The nitrogen isotopic composition of the groundwater
nitrate is plotted as a function of age. All of the groundwater
samples can be considered to have entered the aquifer in the
recharge area in the east before flowing to the point at which
they have been subsequently sampled in this study. The sample
#39 is denoted with a question mark; for, the isotopic analysis
may not be reliable (as discussed in Table 1).
V. Rogojin et al.
nitrogen isotopes of the dissolved nitrate, which in turn is
related to – and thus records – the thickness of the soil
and the extent of the overlying plant cover of the last few
centuries, when the region was ruled by the Ottoman
empire. This process, that led to erosion, could have be-
gun with uncontrolled grazing by goats, in conjunction
with the cutting of trees to avoid taxation and culminated
with the massive destruction of forests for use in the
Ottoman steam locomotives, at the beginning of the 20th
century. Whatever, the precise sequence of events, by the
end of the Ottoman rule, the landscape of the Galillee
was largely denuded of trees and soil. This necessitated
largescale reforestation projects that are still ongoing. The
nitrogen isotopic data supports the biblical description.
There are 3 data points in Fig. 5 with δ15N that fall
below the average for the older water. One of them (No. 6)
(Fig. 4) is also an outlier in the age gradient of the aqui-
fer. However, this well is very close to the small outcrop
of the Kurdani aquifer, which has a very thin soil cover
(Fig. 3). Therefore the water in this well could be a mix-
ture of the main aquifer water with young water, charac-
terized by higher 14C activity combined with lower δ15N.
If we take δ 15 N=+3.5‰ for the young water and
δ15N=+7.0‰ for the main aquifer, we find that this
sample from the Kurdani aquifer is composed of 40%
young water and 60% water from the main aquifer.
Assuming that the 14C content of the young water is 64 pMC,
we find the 14C content of the water from the main aqui-
fer to be 43.3 pMC with a corresponding age of 3130 BP.
This age is quite consistent with the gradient of ages along
the direction of flow in the main aquifer.
The other two points are well behaved hydrologically
and therefore they could be either an artifact or pertur-
bation of the grand trend, or they could represent actual
historical events. As historical events, they seem to sug-
gest reversible changes in the land cover: thinner topsoil,
or less organic matter in the top soil. The historical tim-
ing of these data points are Hellenistic, and some 300 years
saders. Until we have some more data, the interpretation
eroded soil profile produces much less isotopic fraction-
ation of 15N than a well developed soil profile, like the one
that covered the land when lions roamed the forests of
Judea (I Kings 13:24).
6. CONCLUSION
Our analysis shows that of the two potential culprits
Israel only one is to blame, namely, the changes brought
66000
,0 0 0 77000
,0 0 0 88000
,0 0 0
about by human hands. There is no evidence that the
desert line migrated this far north from its present posi-
tion during the last 8000 years. We think that it is of inter-
est to note that an aquifer can be an archive for the his-
tory of environmental processes.
83
 A BETTER-DEVELOPED SOIL PROFILE DURING BIBLICAL TIMES ...
REFERENCES
Benvenisti M., 1970: The Crusaders in the Holy Land. Israel Uni-
versities Press, Jerusalem: 408 pp.
Clark I. and Fritz P., 1997: Environmental Isotopes in Hydrology.
Lewis Publishers, New York: 328 pp.
Goodfriend G.A., 1988: Mid-Holocene rainfall in Negev Desert from
13
C of snail shell organic matter. Nature 333: 757-760.
Gormly J.R. and Spalding R.F., 1979: Sources and concentrations
of nitrate-nitrogen in groundwater of the Central Plate Region,
Nebraska. Ground Water 17: 291-301.
Heaton T.H.E., 1984: Sources of nitrate in groundwater in the
western Kalahari. Journal of Hydrology 67: 249-259.
Ingerson E. and Pearson F.J. Jr., 1964: Estimation of age and rate
of motion of groundwater by the 14C method. In: Recent re-
searches in the fields of atmosphere, hydrosphere and nuclear
geochemistry, Sugawara Festival Volume, Maruzen Co., Tokyo:
263-283.
Komor S.C. and Anderson H.W., Jr., 1993: Nitrogen isotopes as
indicators of nitrate sources in Minnesota sand-plain aquifers.
Ground Water 31: 260-270.
Kroitoru L., Carmi I. and Mazor E., 1989: Groundwater 14C acti-
vity as affected by initial water-rock interactions in the Judean
Mounains, Israel. Chemical Geology (Isotope Geoscience Sec-
tion) 79: 259-274.
84
Kronfeld J., Vogel J.C., and Rosenthal A., 1992: Natural isotopes
and water stratification in the Judea Group aquifer (Judea
Desert). Israel Journal of Earth Sciences 39: 71-77.
Lajtha K. and Michener R.H. (Eds.), 1994: Stable Isotopes in Eco-
logy and Environmental Science. Blackwell Science Publications,
Oxford: 316 pp.
Magaritz M., Issar A. and Azmon E., 1983: On the genesis of dis-
cordant dolostones bodies in the Northeastern Negev, Israel.
Chemical Geology 39: 93-114.
Mero D., 1983: Subsurface geology of Western Galilee and Zevulun
Plain. Tahal, Tel-Aviv, Internal Report No. 04/83/48: 36 pp.
Mook W.G., Bommerson J.C., and Staverman W.H., 1974: Carbon
isotope fractionation between dissolved bicarbonate and gaseous
dioxide. Earth and Planetary Science Letters 22: 169-176.
Rogojin V., 2000: The use of natural isotopes as an aid in studying the
geohydrological processes in the multi-aquiferal system of the Haifa
Bay region. Ph.D. Thesis, Tel-Aviv University: 71 pp.
Sheffer U., 1987: The cutting down of the oak forest on the Tiv’on
hills during World War I. Cathedra 44: 97-106 (in Hebrew).
Stringer Ch. and Mckie R., 1997: African Exodus. Henry Holt and
company, New York: 282 pp.
Vogel J.C., Fuls A. and Danin A., 1986: Geographical and environ-
mental distribution of C3 and C4 grasses in the Sinai, Negev and
Judea deserts. Oecologia 70: 258-265.
 GEOCHRONOMETRIA Vol. 21, pp 85-96, 2002 – Journal on Methods and Applications of Absolute Chronology

RADIOCARBON TIME SCALE FOR DEPOSITION

OF HOLOCENE CALCAREOUS TUFA FROM POLAND
AND INDIA (ORISSA)
ANNA PAZDUR1, RADOS£AW DOBROWOLSKI2, TOMASZ DURAKIEWICZ3, MANMOHAN
MOHANTI4, NATALIA PIOTROWSKA1 and SRIKANTA DAS4
1
Department of Radioisotopes, Institute of Physics, Silesian University of Technology,
Krzywoustego 2, 44-100 Gliwice, Poland
(e-mail: anna.pazdur@radiocarbon.gliwice.pl)
2
Department of Physical Geography and Palaeogeography, Maria Curie-Sk³odowska University,
Akademicka 19, 20-033 Lublin, Poland
3
Mass Spectrometry Laboratory, Maria Curie-Sk³odowska University,
Plac Marii Curie-Sk³odowskiej 1, 20-031 Lublin, Poland;
Los Alamos Laboratory, Condensed Matter and Thermal Physics Group, Los Alamos, Mailstop K764, NM 87545, USA
4
Department of Geology, Utkal University Bhubaneswar - 751004 (Orissa) India

Key words
words: Abstract: 14C concentration measurements together with carbon and oxygen stable isotope
14
C DATING, analysis in calcareous tufa give possibilities for reconstruction of time scale and palaeoclimatic
STABLE ISOTOPES, conditions of sedimentary processes. Results of isotope examinations of 2 profiles with
CALCAREOUS TUFA, organic and tufa sediments from Eastern Poland and 8 calcareous tufa sites from Eastern
HOLOCENE, India (Orissa) are given. A systematic error of 14C conventional age of carbonate fraction of
POLAND, INDIA tufa samples as reservoir age (TR) was estimated. The TR values of different type of tufa sedi-
ment are determined by stream water energy. On the basis of known experimental depen-
dence between TR and δ13C for tufas deposited in high, average and low energy water,
unknown values of TR and corrected 14C ages (TCCA) were calculated for samples from India
tufa sites. Continuous deposition of organic and carbonate sediments in Polish profiles give
the possibility to calculate the approximated TCCA ages on the basis of dependence between
TCCA and a sample depth in a profile, and time scale reconstruction of δ13C and δ18O changes
in carbonate fraction of tufa samples during the whole Holocene.

1. INTRODUCTION during sedimentation processes are concerned with pri-

Tufas are freshwater carbonate deposits, the deposi-
tion of which is affected by physico-chemical and/or bio-
chemical processes. Continental carbonate deposits like
tufa are now being used for radiocarbon dating (Geyh and
Schleicher, 1990; Pazdur, 1988; Pazdur et al., 1988a; Srdoc
et al., 1980, 1982 and 1983; Thorpe et al., 1980 and 1981).
These deposits are also considered as reliable recorders
of palaeoclimatic and environmental changes (Andrews
et al., 1994; Pazdur et al., 1988b and Turi et al., 1986).
Results of 14C measurements of tufa from several sites
in southern and eastern Poland indicated significant
variability of initial 14C activity and its dependence on sedi-
mentological and geochemical processes (Dobrowolski
et al., 1999; Pazdur, 1988 and Pazdur et al., 1988a).
A number of factors determine the reliability of 14C dates
of the tufaceous sediments. Carbon isotopic fractionation
mary factors, which determine the initial 14C concentra-
tion in carbonates. Isotopic studies of groundwater give
some information about this process. Radiocarbon stu-
dies of groundwater have resulted in formulation of di-
fferent models which estimate initial 14C activity of HCO3-
ions dissolved in water (Mook, 1976 and Pearson, 1992).
However, physicochemical processes involved in precipi-
tation of tufa are complex and numerous environmental
factors may influence them (Friedman, 1970; Usdowski
et al., 1979 and Pazdur et al., 1988a, b). Direct application
of such models in 14C dating of tufa has led to unsatisfac-
tory results.
All investigated calcareous tufa samples collected from
different regions and profiles indicate depletion in 14C
isotope in the moment of deposition. It causes a system-
atic error of conventional radiocarbon dates of carbon-
ate fractions, i.e., so called reservoir (or apparent) age.
 RADIOCARBON TIME SCALE FOR DEPOSITION OF HOLOCENE CALCAREOUS TUFA ...
Conventional 14C age of carbonate sample is “older” than
true radiocarbon age. The value of reservoir age has con-
nection with the environment of tufa deposition. In
streams with turbulent and fast flow, tufaceous sediments
show the highest values of reservoir age, even 4000 years.
Deposits of streams with moderate and variable flow show
the lowest values of the reservoir age (ca 2500-2100 years),
while the stagnant water deposits have the lowest values
(less than 1000 years).
According to Szulc (1983) and Pazdur and Szulc
(1988a) a slightly simplified classification of was done:
l Spring tufa: precipitated in turbulent, high energy
water flow (oncoids, stromatolites and moss
travertines).
l Tufas (oncoids and moss travertines) and peloidal cal-
careous muds: precipitated in streams with low or vari-
able water flow.
86
Fig. 1. Location of studied sites with tufa
deposits in Eastern India (Orissa State):
Phulbani, Boudh, Nayagarh, Keonjhar and
Mayurbhanj and in Eastern Poland (Lublin
Upland): Krzywice-1(K) and Rudka-2(R).
l Calcareous muds precipitated in shallow, stagnant-wa-
ter basins in conditions of semilimnic sedimentation.
In the Indian context, tufa deposits (see Figs 3, 4 and
5) are classified as follows (Das and Mohanti, 1997).
l Waterfall tufa (Fig. 3): precipitated from turbulent wa-
ter flow (high energy condition); include stromatolic
tufa, phytohermal (moss) tufa, phytoclastic tufa and
occasional pisoids.
l Slope tufa (Fig. 4): precipitated from moderately agi-
tated water flow conditions; include stromatolitic tufa,
phytotermal tufa and phytoclastic tufa.
l Low gradient stream /river channel margin tufa (Fig. 5):
precipitated from low or variable water flow; include
stromatolic tufa and coated pebbles.
None of the deposits indicate shallow or stagnant-
water basin conditions.
 A. Pazdur et al.
Redeposition and diagenetic modifications are con-
sidered as secondary factors influencing the 14C dates of
tufaceous sediments. Post-depositional changes include
dissolution and reprecipitation of CaCO3 within the sedi-
ment. Cementation of tufaceous sediments leads to con-
tamination of primary carbonates with 14C contained in
percolating water. Radiocarbon dating of redeposited and
diagenetically modified calcareous tufa yields erroneously
high values. Detailed examination of the profile during
sampling may help to overcome this type of error.
2. RESERVOIR EFFECT IN 14C DATING
OF TUFACEOUS SEDIMENTS
Radiocarbon activity of freshwater carbonate sediment
at the moment of precipitation (A0) is obviously influenced
by isotopic composition of carbon compounds dissolved
in water.
The conventional radiocarbon age (TC) of carbonate,
determined by the ratio of measured 14C activity (A) in
a sample to 14C activity of the contemporary biosphere
(AOX), defined as 95% of the activity of NBS oxalic acid
standard (Stuiver and Polach, 1977), i.e.,
æ A ö
TC = -8033 ´ lnç ÷
(2.1)
ç ÷
è AOX ø
is greater than the real age of sediments because of
depletion of initial 14C activity in precipitated carbonate
with respect to biosphere. Difference between TC and the
real age is characterised by so called “reservoir age” TR
(or apparent age TAPP; Pazdur, 1988). The value of TR is
related to initial 14C activity of carbonate (A0) and reser-
voir dilution factor (q) through the equation
æ A ö
ç ÷
TR = -8033 ´ lnç o ÷ = -8033 ´ ln q (2.2)
ç A ÷
è ox ø
The real conventional radiocarbon age TCCA is obvi-
ously described by
(2.3)
TCCA = TC - TR
The value of reservoir age TR observed for calcareous
tufa, lake marl, lacustrine gyttja and cements is charac-
teristic for depositional environment of carbonate, which
includes geographic locality of the karst area, type of veg-
etation, and type of bedrock as well as it contains infor-
mation on sources of carbon and its geochemical cycle in
environment. Observed TR values for these sediments
range from several hundred to several thousand years and
sometimes more (Pazdur, 1988 and 2000 and Pazdur et al.,
1995a, b). Speleothems have relatively constant reservoir
age determined by stable sedimentation conditions in
caves (Hercman, 2000; Holmgren et al., 1994 and Pazdur
et al., 1999).
The scattering of values of TR observed by various
authors could be explained by the dependence of TR on
the bedrock type (which is a source of 14C-free carbon)
87
and the type of sediment. The type of calcareous sedi-
ments depends strongly on hydrodynamic conditions of
water flow (Szulc, 1983).
Observed values of q in both recent and ancient tufas
range from 0.5 to 0.95 (Srdoc et al., 1983; Thorpe et al.,
1981; Pazdur 1988; Pazdur et al., 1988a and Pazdur and
Pazdur, 1990) and consequently the values of TR are in-
cluded in interval from 500 to 5500 yr. They can be of
extremely high value ca 11 kyr (Pazdur, 1988).
The factors determining the precipitation of freshwa-
ter carbonates should be reflected by isotopic composi-
tion of carbon (δ13C, A0) in carbonate samples and should
influence the TR value. The measured values are TC (see
Eq. (2.1)) and some dependence between δ13C and TC is
expected.
Radiocarbon dating of tufaceous sediments should be
associated with detailed sedimentologic studies and car-
bon stable isotope δ13C measurements (Pazdur, 1988).
Estimating true ages TCCA of individual tufa layers is rela-
tively easy even when few organic horizons can be found
in the investigated profile. In such case, measured values
of 14C ages of carbonate and organic fractions can be co-
rrelated with δ13C values of tufa carbonate. A constant
value of δ13C in the profile indicates a constant value of
apparent age, which can be determined independently
by comparing 14C ages of carbonate and associated organic
matter or detrital organic matter dispersed in the carbo-
nate, itself. Assuming that the age of organic remnants
reflects the actual age of carbonate precipitation, we can
define the reservoir age TR of carbonate
TR = TC - TORG (2.4)
This value determined for a tufa profile with known
values of δ13C across the profile, can be used for estima-
tion of the real age of tufa horizons on the basis of TC
measurements.
Profiles of tufaceous sediments that do not contain
organics, may be characterised by constant value of the
reservoir (apparent) age and can be dated with accept-
able accuracy. It was found, that constant TR value in a
profile reveals peloidal calcareous muds precipitated from
stagnant or low-energy water, and tufas precipitated from
turbulent water, which do not exhibit significant correla-
tion of δ13C and TC (Pazdur, 1988).
To estimate magnitude of the reservoir age the rela-
tion between TR and δ13C can be used in the shape of equa-
tion characteristic for spring tufa precipitated from higher
energy water
TR = (13.50±3.27) + (0.96±0.34) x δ13C [kyr] (2.5)
or characteristic for tufas precipitated from average
and lower energy water
TR = (4.41±0.98) + (0.25±0.11) x δ13C [kyr]. (2.6)
The TR values may be calculated on the basis of equa-
tions (2.5) or (2.6), and in consequence TCCA, using equa-
tion (2.3) for each measured pair TC and δ13C in tufa
samples, may be determined.
 RADIOCARBON TIME SCALE FOR DEPOSITION OF HOLOCENE CALCAREOUS TUFA ...
3. INVESTIGATED SITES AND SEDIMENTS
Lublin Upland, Eastern Poland
Calcareous tufas and travertines occurring in Poland
are formed by precipitation from groundwater circulat-
ing through/carbonate rocks of different lithology (lime-
stones, chalks, marls) and stratigraphic position (Devo-
nian, Lower Carboniferous, Jurassic, Cretaceous and
Tertiary). Their sites are found mainly in the Southern
Poland (Carpathians and Cracow-Wieluñ Upland; Szulc,
1983) and Eastern Poland (Lublin Upland; Dobrowolski
et al., 1999; see Fig. 1). Sites with tufaceous sediments from
the Eastern Poland are connected with soligenous mires:
carbonate deposition strongly depends on groundwater
circulation and structure of the Upper Cretaceous bed-
rock.
88
Krzywice-1 and Rudka-2
Carbonate sediments are presented by moss tufas de-
posited in well oxidised ascending springs, and by calcar-
eous muds formed in shallow, stagnant water basins in
conditions of semilimnic sedimentation (Dobrowolski et
al., 1999 and 2001; Fig. 2A). The thickness of tufa layers
in examined profiles varies from ca 0.5 to 40 cm. These
unconsolidated carbonate sediments, with no diagenetic
changes, were formed as incrustations of hygrophyte
plants (Cyperaceae, Phragmites, Calliergon giganteum and
Scorpidium scorpioides). Thickness of organic-carbonate
sequence in the Krzywice-1 profile is ca 6m and in the
Rudka-2 profile - ca 4m. Simplified lithology of sediments
from both profiles is given in Fig. 2.
Fig. 2. Sediment profiles with tufa deposits and results
o radiocarbon dating: part A - profiles from Poland with
TORG or TCCA ages (see Table 1) used for calculation of
curves described by Eqs (5.7) and (5.8); part B - profiles
from India with TCCA ages of samples (see Table 2).
 A. Pazdur et al.
Orissa, Eastern India
Several freshwater tufa deposits occur in the tropical
setting in Phulbani, Boudh, Nayagarh, Keonjhar and
Mayurbhanj districts of Orissa State (Fig. 1). The depos-
its occur as surficial deposits in hilly topography; at sites
of waterfalls, where streams have steeper gradients or
margins of small river where boulders or bedrock occur.
In Phulbani, Boudh and Nayagarh districts the rock types
are charnokites, khondalites and granite gneisses belong-
ing to the Easternghat Group. In Keonjhar district, the
deposit rests over quartzite, which is overlain by basic lava
and tuff of Simlipal Group and underlain by the
Singhbhum Granite. The deposits in Mayurbhanj district
have been formed at the contact of quartzites of Iron Ore
Group and younger dolerite intrusives. The quartzites
along with a thin band of ferruginous shale overlie the
Singhbhum Granite, which is invaded by numerous dol-
erite dykes.
The tufa deposits can be broadly classified as stroma-
tolitic tufa, phytohermal tufa and phytoclastic tufa. The
cross sections of these different sediments are shown in
89
Figs of 3 to 5. Phytohermal tufas are mostly calcified
mosses (Das and Mohanti, 1997). When the mosses are
less than 2 cm in size, these tufa are named as microhermal
tufa, in which case some pteridophytic plants and algae
may be associated. Occasionally, pisoids also occur along
with intraclastic deposits. Porous zones show thin inor-
ganic crusts called sinter. Larger cavernous zones show
speleothem-like deposits like stalactites and laminated
flowstone.
The deposits show variations in the thickness of dif-
ferent tufa facies. Tufa profiles were constructed from
quarry faces and stream-cut sections after careful exami-
nation of the sequence of tufa facies and associations (Figs
3, 4 and 5). Samples were collected from various layers
showing major sedimentary intervals (Fig. 2B). Profile
samples were collected from three localities (i.e.,
Mundapathar, Sulagan and Kudipasa). Some number of
tufa samples were found in five other localities
(Banigochha, Madhapur, Bhaliadal, Mitikoli and Takara;
see Fig. 1). Organic-rich soils occurring in small pockets
were collected from the profiles.
Fig. 3. Sequence of various tufa facies (encrousted boulders,
stromatolitic tufa, phytohermal tufa and phytoclasic tufa with
sinter) in slope deposits.
Fig. 4. Occurrence of stromatolitic tufa (showing varying
disposition), phytohermal (moss) tufa and speleothem-like
sediments in waterfall deposits.
 RADIOCARBON TIME SCALE FOR DEPOSITION OF HOLOCENE CALCAREOUS TUFA ...
Mundapathar
The deposit is characterized by dominantly stroma-
tolitic and phytohermal (moss) tufa (Fig. 3). Above the
level of 3.6 m from the bottom (MS-7, Table 2), a cavern-
ous zone occurs which shows speleothem-like deposits.
Pisoids occur along with intraclastic tufa at the depth 5.5
m (MS-10, Table 2) within disrupted crusts of stromatolitic
tufa.
Sulagan
The lower parts of the deposit show phytohermal
(moss) tufa alternating with thin layers of stromatolitic
tufa. At levels of 3.5 m (SS-4) and 5.2 m (SS-6, Table 2),
microhermal tufas form thick zones. A narrow cave oc-
curs above the level SS-3 showing botryoidal hangings and
thin inorganic crusts with ramifying projections. The up-
permost part of the deposit shows occurrence of stroma-
tolitic tufa which is partly covered by soil.
Kudipasa
At the lower level of the deposit tufa is found to en-
crust quartzite boulders. The boulder zone is overlain by
a thin layer of stromatolitic tufa, which is overlain by a
thick zone of phytohermal (moss) tufa. Microhermal tufa
shows pocket-like deposits on the level 1.8 m (KS-3, Table
2). In the whole cross section of outcrop the deposits are
dominated by very thick zones of phytoclastic deposits.
Sinter crusts show plate-like growths within the
phytoclastic deposits. The top portion of the deposit shows
laminated flowstone, which is covered by soil.
Regional samples
Some number of tufa samples were found in the five
localities (Banigochha, Madhapur, Bhaliadal, Mitikoli and
Takara; see Fig. 1) as single calcareous incrustations in
sediments. They are called “regional samples”.
The regional samples are stromatolitic tufa. The
samples MBS-5 is a modern crust collected from the
stream channel where active tufa deposition is observed.
90
Fig. 5. River channel margin tufa
deposits showing occurrence of tufa-
encrusted boulders, stromatolitic tufa
and coated pebbles.
4. RESULTS OF 14C DATING AND δ13C AND δ 18O
MEASUREMENTS
14
C dating
All analyzed samples were dated using CO2-filled pro-
portional counters (Pazdur et al., 2000). Radiocarbon ages
TC or TORG (Table 1 and 2) are the conventional 14C ages
of carbonate (TC) and organic matter (TORG) normalized
to δ13C=-25‰, according to recommendations of Stuiver
and Polach (1977). The analysis was carried out at the
Gliwice Radiocarbon Laboratory, Silesian University of
Technology, Poland.
δ 13C and δ 18O measurements
The measurements of relative stable isotope concen-
tration 13C and 18O in samples from Polish sites were car-
ried out at the Mass Spectrometry Laboratory, Maria
Curie-Sk³odowska University, Lublin, Poland. The same
analysis for samples from India sites was carried out at
the Department of Geology, University of California,
USA. Measurements were performed using standard mass
spectrometry techniques with gaseous CO2 obtained from
chemical reaction of carbonate fraction of tufa samples
with concentrated orthophosphoric acid (>103 %). The
δ13C and δ18O values were expressed relative to the PDB
standard (Tables 2 and 3).
5. CONVENTIONAL 14C CORRECTED AGE (TCCA)
OF TUFACEOUS SEDIMENTS
Krzywice-1 and Rudka-2 sites
Both tufa profiles contain organic matter mixed with
carbonate or occurring as separate layers. There are also
layers consisting only from carbonate fraction (see Table 1).
The determination of time scales for sedimentation of
carbonates, where possible, was based on 14C dating of
organic fraction (TORG). For layers with no organic frac-
tion, the reservoir age TR (estimated according to Eq.
(2.4)) was assumed the same as for younger (higher) level.
 A. Pazdur et al.

Table 1. Results of radiocarbon dating of carbonate (TC ) and organic fraction (TORG ), δ13C measurements and estimation of
reservoir effect (TR ) and corrected carbonate age (TCCA ) of organic sediments and tufa samples from Polish sites.
Sample Depth Lab.No. F T T C , T ORG ä 13C TR T CCA
[m] Gd- [BP] [‰, PDB] [years] [BP]
Krzywice-1
KRZ 1/94 5.37-5.50 10280 O H 11530 ± 100 11530 ± 100
KRZ 2/94 4.37-4.60 10070 O PT 10770 ± 140
KRZ 4/94 4.00-4.10 7516 C TF 10590 ± 80 -7.43 9970 ± 140
KRZ 4/94 4.00-4.10 10072 O PT 9970 ± 140
KRZ 5/94 2.80-2.95 9237 O PT 6670 ± 170
KRZ 5/94 2.80-2.95 7517 C TF 10620 ± 50 -7.32 6670 ± 170
KRZ 6/94 2.70-2.79 7518 C TF 10540 ± 70 -8.08 3950 ± 250 6590 ± 200
KRZ 7/94 2.42-2.55 10073 O PT 6120 ± 100
KRZ 8/94 2.31-2.43 7519 C TF 9670 ± 60 -6.71 3950 ± 250 5720 ± 200
KRZ 9/94 2.16-2.31 7522 C TF 9730 ± 70 -6.71 3950 ± 250 5780 ± 200
KRZ 10/94 2.00-2.15 10074 O PT 3620 ± 130
KRZ 11/94 1.00-1.12 10079 O PT 1530 ± 70
KRZ 12/94 0.79-0.92 7524 C TF 4340 ± 60 -8.17 3530 ± 60 810 ± 100
KRZ 13/94 0.56-0.66 7525 C TF 4200 ± 50 -9.04 3530 ± 60 670 ± 80
KRZ 14/94 0.56-0.43 7520 C TF 3530 ± 60 -8.28 3530 ± 60 0 ± 60
KRZ 14/94 0.56-0.43 9231 O PT MODERN
Rudka-2
R2 - 1 4.20-4.10 10655 O TF 8700 ± 180
R2 - 2 3.21-3.09 10642 C CM 7130 ± 190 -6.57 1360 ± 130 5770 ± 120
R2 - 3 3.09-3.01 10651 C CM 6980 ± 180 -6.57 1360 ± 130 5620 ± 160
R2 - 3 3.09-3.01 10649 O PT 5620 ± 160
R2 - 4 2.80-2.70 10645 C CM 7670 ± 150 -7.39 1780 ± 220 5890 ± 270
R2 - 4 2.80-2.70 9816 O PT 5890 ± 270
R2 - 5 0.92-0.87 10646 C CM 2720 ± 140 -7.74 500 ± 140 2220 ± 190
R2 - 5 0.92-0.87 9801 O PT 2220 ± 190
R2 - 6 0.87-0.82 10659 C CM 2870 ± 140 -7.74 (*)
R2 - 7 0.82-0.74 7980 C CM 3080 ± 70 -7.74 (*)
R2 - 8 0.74-0.71 9797 C CM 3530 ± 210 -7.25 1780 ± 150 1750 ± 180
R2 - 8 0.74-0.71 9807 O PT 1750 ± 180
R2 - 9 0.71-0.65 10663 C CM 2980 ± 140 -7.25 1780 ± 150 1200 ± 110
R2 - 10 0.48-0.37 7983 C CM 2190 ± 60 -8.27 1860 ± 120 330 ± 220
R2 - 10 0.48-0.37 9809 O PT 330 ± 220
F = fraction of the sample; C, O = carbonate and organic fraction; (*) = assumed δ13C values in carbonate fraction; in organic
fraction δ13C = -25‰ was assumed. Type of sediment: TF = tufa, PT = peat, H = humus/soil, CM = calcareous mu

Much more of small carbonate samples than for 14C
dating were collected for stable isotope 13C and 18O analy-
ses. Full time record of δ13C and δ18O needed separate
construction of time scale. For this experimental depen-
dence between known TCCA and depth d of samples in sedi-
ment profiles was used, for Krzywice-1 and Rudka-2 sepa-
rately. This dependence is shown in Fig. 6 and described
by the best fit of polynomial functions:
TCCA= -251.95 x d2 +3924 x d - 2082.9 [years BP]
for Krzywice-1 profile, with correlation coefficient
r2=0.9938, and
TCCA= 374.62 x d3-2748.1 x d2 +7670.5 x d - 2630.6 [years BP]
(5.8)
for Rudka-2 profile, with correlation coefficient r2=0.9937.
Results of TCCA calculations and δ13C and δ18O measure-
ments are listed in Table 3. The errors of estimation are
less than 100 years.
Sites from Orissa
(5.7) As we can study from the data sheet (see Table 2) all
organic fractions of tufa samples from all profiles are rela-
tively young. This may suggest that there is some input
from modern carbon sources. The tufas are generally
porous and permit movement of water, which might have

91
 RADIOCARBON TIME SCALE FOR DEPOSITION OF HOLOCENE CALCAREOUS TUFA ...

Table 2. Results of radiocarbon dating of carbonate (TC ) and organic fraction (TORG ), stable isotope
measurements (δ13C and δ18O) and estimation of reservoir effects (TR ) and corrected carbonate ages (TCCA )
of tufa samples for sites from India.
Sample Lab. F/T, WE T C, T ORG d13C d18O TR TR T CCA T CCA
No. [BP] [%
[‰]o, [%
[‰]o, [years] [years] [BP] [BP]
Gd- PDB] PDB] (5) (6) (5) (6)

Kudipasa
KS-1 12065 C/ST,M 15470 ± 120 -4.30 -3.83 9370 3340 6100 12130#
KS-1/S-1 C/H, M -4.30 -3.83
KS-1/S-1 9841 O/H, M 90 ± 180 -25 (*)
KS-2 12059 C/PHT, M 16570 ± 180 -4.46 -3.98 9220 3300 7350 13270#
KS-3 12070 C/PHT, M 16600 ± 180 -6.78 -4.74 7000 2720 9600# 13880
KS-3/S-2 C/H, M -6.78 -4.74
KS-3/S-2 9828 O/H, M 102.0 ± 2.7 -25 (*)
PM
KS-4 C/PCT, M -3.89 -4.21
KS-5 C/S, M -4.54 -4.30
KS-6 C/ST, M -4.26 -4.15
KS-7 C/PCT, M -5.35 -3.87
KS-8 12067 C/S, M 10970 ± 90 -7.80 -4.01 6000 2460 4970# 8510
Mundapathar
MS-1 12008 C/ST, H 7050 ± 80 -8.53 -5.60
MS-1/M-1 C/H, H -8.53 -5.60 5310 2280 1740 4770#
MS-1/M-1 9824 O/H, H 1120 ± 180 -25 (*)
MS-2 10678 C/PHT, H 8270 ± 210 -10.41 -6.01 3510 1810 4760 6460#
MS-3 C/ST, H -10.47 -5.98
MS-4 12007 C/ST, H 7620 ± 90 -9.26 -6.21 4610 2100 3010 5520#
(-9.28) (-6.27)
MS-5 C/H, H -11.27 -6.06
MS-5/M-2 12001 C/PHT, H 7660 ± 100 -11.27 -6.06 2680 1590 4980 6070#
MS-6 10674 C/ST, H 9070 ± 230 -10.60 -5.60 3320 1760 5750# 7310
MS-7 10677 C/S, H 6920 ± 190 -9.75 -6.54 4140 1970 2780 4950#
MS-8 12004 C/PHT, H 8310 ± 60 -11.92 -5.84 2060 1430 6150 6880
MS-9 10675 C/ST, H 5220 ± 180 -9.84 -6.02 4050 1950 1170 3270#
MS-10 10671 C/P, H 5220 ± 180 -10.40 -5.97 3520 1810 1700 3410#
MS-11 12000 C/ST, H 5770 ± 80 -10.92 -6.01 3020 1660 2750# 4110
MS-12 10679 C/PHT, H 4350 ± 180 -9.29 -5.83 4580 2090 MOD 2260#
Sulagan
SS-1 12072 C/ST, H 10280 ± 110 -9.20 -3.36 4670 2110 5610 8170#
SS-2 12069 C/PHT, H 11400 ± 120 -6.65 -3.72 7160 2750 4240 8650#
SS-2/R-1 9822 C/H, H 3700 ± 220 -6.65 -3.72 7160 2750 MOD 950#
SS-2/R-1 9831 O/H, H 110 ± 8 PM -25(*)
SS-3 C/ST, H -4.77 -6.04
SS-4 C/PHT, H -8.48 -3.49
(-8.48) (-3.44)
SS-5 C/ST, H -9.51 -4.09
SS-6 C/?, H -8.92 -4.27
SS-6/R-2 9818 C/PHT, H 8010 ± 300 -8.92 -4.27 4940 2180 3070 5830#
SS-6/R-2 10669 O/H, H 109.5 ± 1.4
PM
SS-7 12071 C/ST, H 8930 ± 110 -9.97 -4.63 3930 1920 5000# 7010
Regional samples
BA-1 C/ST, L -10.74 -5.02
(-10.95) (-5.05)
MA-1 12067 C/ST, M 10970 ± 90 -9.74 -4.23 4150 1980 6820 8990#
MB-4 12061 C/ST, M 19850 ± 290 -2.52 -3.39 11080 3780 8770# 16070
MB-5 12058 C/PHT, M 12780±140 ? ?
MBS-5 11385 C/ST, M 220 ± 90 -11.67 -6.82 2300 1490 MOD MOD
MI-1 11375 C/ST, M 10750 ± 210 -8.26 -3.79 5570 2350 5180 8400#
MUC-1 12068 C/ST, H 9370 ± 100 ? ?
TA-2 C/ST, L -7.81 -4.0
F = fraction of the sample; C, O = carbonate and organic fraction; MOD = modern; (*) = assumed δ13C values in organic
fraction; (5) and (6) indicate the number of equation in chapter 2, used for estimation of T R (and TCCA ); (#)= estimated ages
of tufa carbonate fraction giving the best stratigraphy of sediments. Type of tufa samples T: P = Pisoid, PCT = Phytoclastic
tufa, PHT = Phytohermal (moss) tufa, S = Sinter/flowstone, ST = Stromatolitic tufa, H = Humus/soil. Name of regional
samples: BA = Banigocha, MA = Madhapur, MB = Bhaliadal, Ml = Mitikoli, MUC = Mundapathar, TA = Takara.
Water energy WE: H = High, M = Moderate, L = Average and Low.

92
 A. Pazdur et al.
dissolved the modern carbon from the upstream area and
contributed to the organic deposits. Secondly, as the tu-
fas are dampened by water films, they support the growth
of modern/recent cyanobacterial/algal flora. These might
have possibly contributed some modern carbon to organic
samples. Because of this, the dates of organic fraction
associated with tufa carbonate are not real ages of tufa
samples. The 14C time scale for studied changes of sedi-
mentary conditions and δ18O in tufa carbonates from the
study area can be reconstructed on the base of relation
between the reservoir age TR and δ13C values (see Eqs (2.5)
and (2.6)).
The measured values are TC and δ13C; some depen-
dence between them is expected. Values of δ13C of car-
bonate are plotted in Figs. 7 and 8 against the carbonate
age TC of samples of all investigated profiles, each of the
separate profiles and regional samples. Smoothed depen-
dence of δ13C upon TC is shown by solid lines
δ13C = a0C + a1CTC (5.9)
obtained by least squares method. Parameters of least
squares line (a0C, a1C), the value of correlation coefficient
R, and number (n) of experimental points used in calcu-
lation for separate profiles are listed in Table 4. The de-
pendence of δ13C upon TC is insignificant for separate
profile and has relatively high confidence level for experi-
mental points from regional samples and all points
together. To estimate magnitude of the reservoir age, the
relation TR and δ13C can be used in the shape of equation
characteristic for spring tufa precipitated from high
energy water or characteristic for other tufas (Eqs (2.5)
and (2.6)).
93
The TR values and corrected carbonate ages for the
reservoir effect (TCCA) of tufa carbonate are listed in Table
2. The TR and TCCA values were determined on the basis
of both relation (5) and (6) for each measured pair TC
and δ13C in tufa samples. For reconstruction of the radio-
carbon time scale for sedimentary processes and
palaeoclimatic interpretation of stable isotope results
(Pazdur et al., 2002) we assume, that the best calculated
ages are ages which give corrected stratigraphy of inves-
tigated sediment layers in profiles. These results are indi-
cated in Table 2. It may be noted, that the best stratigra-
phy order of TCCA ages in profile is not in agreement with
information about relation of tufa type to water energy.
The relative errors of such estimated TCCA ages range
within 25-30 %. Inverses observed for samples in profiles;
Kudipasa (Gd-12001), Mundapathar (Gd-12008 and Gd-
10678, Gd-12007 and Gd-12001), Sulagan (Gd-9822 and
Gd-9818) can partly result from great estimation errors,
but the main determinant is the mechanism of sedimen-
tary and post-sedimentary processes and possibilities of
contamination of tufas by “younger” or “older” carbon.
It appears that the older deposits at the lower levels
of the tufa profiles have been partly affected by cementa-
tion in the vadose realm. The meteoric water might have
dissolved younger carbon from humus/ soil zone or mod-
ern tufas, and while moving through the porous older tu-
fas have probably contaminated the tufas. Contamination
by older carbon seems very unlikely. It is possible too, that
cementation processes provide discrepancy of calculated
TCCA ages and classification of type tufa sediments.
Fig. 6. Dependence of experimental values
of TCCA on the depth of a sample in the
Krzywice-1 and Rudka-2 profiles (Poland).
 RADIOCARBON TIME SCALE FOR DEPOSITION OF HOLOCENE CALCAREOUS TUFA ...

Age Tc [BP] Table 4. Parameters of the least squares lines described by

0. 4000 8000 12000 16000 20000 Eq. (5.9). a0C and a1C - least square estimates of the coefficients
of straight line (Figs 7 and 8); r - correlation coefficient;
-2.00
n - number of experimental points.
Y = 4.08*10-4 * X - 12.44 Profile a0C [‰] a1C [‰/kyr] r N
r = 0.58 (n = 24) Kudipasa 0.00043 -0.0123 0.45 4
-4.00 Mundapathar -0.00022 -0.0086 0.12 11
Sulagan -0.00015 -0.0070 0.08 5
Regional 0.00045 -0.0128 0.86 4
d 13C [‰ PDB]

-6.00 samples
All samples 0.00041 -0.0124 0.58 24

-8.00

-10.00

-12.00

Fig. 7. Dependence of δ13C upon TC for all investigated profiles

from the Eastern India (Orissa) sites. Straight line is described
by equation shown in Figure. n - number of experimental points,
r - correlation coefficient.

Fig. 8. Dependence δ13C upon TC for separate profiles

and for regional samples from the Eastern India
(Orissa) sites. Values of correlation coefficients are
given in Table 4.

94
 A. Pazdur et al.

Table 3. Values of unknown corrected radiocarbon ages TCCA of samples analysed on δ13C and δ18O from Krzywice and Rudka sites
(Poland), estimated on the basis of approximation of TCCA as function of depth, described by Eqs (5.7) and (5.8).
Krzywice 4,43 10336 -6,34 -10,61
Depth [m] TCCA [BP] δ 13C [‰, PDB] δ 18O [‰, PDB] 4,58 10583 -9,95 -11,72
0,6 180 -9,04 -7,95 4,7 10772 -3,67 -13,78
0,7 540 -8,68 -8,76 4,75 10849 -3,04 -13,1
0,8 894 -8,17 -8,22 4,95 11143 -0,77 -12,55
1,1 1927 -8,21 -8,27 5,4 11731 -7,03 -11,27
1,4 2915 -7,75 -8,29
1,55 3392 -7,52 -8,81 Rudka
1,6 3548 -7,33 -8,65 Depth [m] TCCA [BP] δ 13C [‰, PDB] δ 18O [‰, PDB]
2,05 4898 -9,35 -5,68 0,5 564 -7,52 -7,75
2,08 4985 -9,58 -5,4 0,65 1297 -7,25 -7,5
2,23 5410 -7,16 -7,88 0,85 2134 -7,74 -7,93
2,35 5742 -6,71 -8,18 1,05 2827 -7,64 -7,12
2,4 5878 -7,24 -8,34 1,1 2980 -7,25 -7,61
2,54 6252 -7,49 -7,95 1,15 3126 -8,44 -6,34
2,6 6410 -9,61 -3,18 1,2 3264 -7,99 -8,33
2,65 6539 -7,58 -8,6 1,25 3395 -6,96 -8,55
2,74 6770 -7,44 -8,23 1,35 3638 -7,06 -7,49
2,78 6871 -8,08 -9,98 1,45 3856 -6,96 -8,84
2,8 6921 -7,43 -8,63 1,55 4051 -6,43 -8,73
2,9 7169 -7,32 -8,63 1,65 4227 -7,46 -7,6
3,35 8224 -6,47 -8,7 1,75 4384 -7,15 -8,85
3,85 9275 -6,23 -8,83 1,85 4526 -6,87 -8,09
4,14 9827 -7,43 -9,8 2 4715 -6,46 -8,53
4,17 9882 -7,01 -9,84 2,15 4881 -6,66 -8,23
4,21 9954 -7,4 -9,65 2,4 5128 -7,12 -6,11
4,23 9990 -7,07 -9,93 2,55 5271 -6,1 -9,14
4,27 10061 -6,36 -9,75 2,65 5369 -7,41 -9,67
4,29 10096 -7,41 -10,06 2,7 5420 -7,39 -8,15
4,31 10131 -7,09 -10,4 2,8 5525 -7,4 -8,59
4,38 10252 -6,74 -9,88 2,9 5639 -6,6 -8,58
4,4 10286 -9,6 -10,21 3 5763 -7,29 -7,64
4,42 10319 -6,24 -11,53 3,1 5899 -7,13 -7,72

6. CONCLUSIONS ter in Orissa state, India, has been useful in calculating

To estimation of 14C ages of calcareous tufa, the res-
ervoir age TR, dependent on type of tufa sediments (wa-
ter energy conditions) should be known. Two indepen-
dent ways of TR determination were made.
The calcareous tufa of Krzywice-1 and Rudka-2 pro-
files in Lublin Upland, Poland represent calcareous muds
formed in shallow, stagnant water basins in conditions of
semilimnic sedimentation. Comparison of conventional
radiocarbon ages of carbonate and organic fraction of
several samples from each profile gave possibilities to
estimate reservoir age TR and use these values to deter-
mine corrected conventional 14C ages TCCA (corrected for
reservoir effect) of samples containing only carbonate
fraction. Non linear dependence between known TCCA and
depth of the carbonate samples in sediment profiles was
used for determination of unknown TCCA of samples des-
tined for δ13C and δ18O analysis.
The smoothed dependence between δ13C and TC for
calcareous tufa deposited in high and mean energy wa-
the best corrected ages (TCCA) of the dating samples. The
model used for calculation of reservoir age TR, on the basis
of observed relation, has empirical character and give only
approximated values. Some anomalies in 14C ages ob-
served in a few samples of the profiles are probably a func-
tion of post-depositional changes or contamination due
to excursion of modern carbon in the depositional system.
The δ13C values indicate greater input of biogenic
lighter carbon. The role of photosynthesis and evapora-
tion in the deposition of tufa is considered to be low due
to low residence time. The absence of any marine carbon-
ate source and high-energy conditions due to water tur-
bulence for Indian tufas, suggest partial disequilibrium
during isotopic fractionation.
ACKNOWLEDGEMENTS
We are filling grateful to Prof. Howard J. Spero for
the generous help he has rendered in the stable isotope
analyses of Indian tufa samples at the University of Cali-

95
 RADIOCARBON TIME SCALE FOR DEPOSITION OF HOLOCENE CALCAREOUS TUFA ...
fornia, Davis. He has critically read the manuscript on the
Indian part of tufa deposits and provided valuable com-
ments. We thank Justin Dailey for handling the isotope
analyses of the Indian samples. Prof. E. Usdowski kindly
carried out isotope analyses of some Indian samples at
the University of Göttingen, Germany - we are grateful.
We extend sincere thanks to Prof. Stephen Kempe, Ger-
many, for going through a previous draft manuscript on
Indian tufa deposits and giving valuable suggestions. The
research on tufa deposits of Orissa was carried out under
the Special Assistance Programme of the University
Grants Commission, India, operated in the Department
of Geology, Utkal University, Orissa, India.
Radiocarbon dating of Indian tufa samples was car-
ried out within BW projects sponsored by the Silesian
University of Technology and preparation of measure-
ments results and paper to print within grant No. 6 P04E
007 17 sponsored by the Scientific Research Committee,
Poland.
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Pazdur A. and Pazdur M. F., 1990: Further investigations on 14C
dating of calcareous tufa. Radiocarbon 32(1): 17-22.
Pazdur A., Pazdur M.F., Starkel L. and Szulc J., 1988b: Stable iso-
topes of the Holocene calcareous tufa in Southern Poland as
palaeoclimatic indicators. Quaternary Research 30: 177-189.
Pazdur A., Pazdur M.F. and Szulc J., 1988a: Radiocarbon dating of
Holocene calcareous tufa from Southern Poland. Radiocarbon
30(2): 133-146.
Pearson F.J., Jr, 1992: Effects of Parameter Uncertainty in Model-
ling 14C. In: Taylor R.E., Long A. and Kra R.S., eds, Radiocar-
bon After four Decades. An Interdisciplinary Perspective. Springer-
Verlag, New York: 262-275.
Srdoc D., Horvatincic N., Obelic B. and Sliepcevic A., 1982: Rudjer
Boskovic Institute radiocarbon measurements VII. Radiocar-
bon 24(3): 352-371.
Srdoc D., Horvatincic N., Obelic B. and Sliepcevic A., 1983: Radio-
carbon dating of tufa in palaeoclimatic studies. In: Stuiver M.
and Kra R.S., eds., International 14C Conference 11th, Proceed-
ings. Radiocarbon 25(2): 421-427.
Srdoc D., Obelic B., Horvatincic N. and Sliepcevic A., 1980: Radio-
carbon dating of calcareous tufa : How reliable results can we
expect? In: Stuiver M. and Kra R. S, eds, International 14C Con-
ference 10th, Proceedings. Radiocarbon 22(3): 858-862.
Stuiver M. and Polach H., 1977: Discussion: Reporting of 14C data.
Radiocarbon 19: 355-363.
Szulc J., 1983: Genesis and classification of travertine deposits.
Przegl¹d Geologiczny 31: 231-236.
Thorpe P.M., Holydak D.T., Preece R. C. and Willing M.J., 1981:
Validity of corrected 14C dates from calcareous tufa. In: For-
mations carbonates externes, tufas et travertines. Actes Colloques
AGF. Paris:151-156.
Thorpe P.M., Otlet R. L. and Sweeting M. M., 1980: Hydrological
implications from 14C profiling of UK tufa. In: Stuiver M. and
Kra R. S., eds, International 14C Conference, 10th, Proceedings.
Radiocarbon 22(3):897-908.
Turi B., 1986: Stable isotope geochemistry in travertines. In: Fritz
P. and Frontes J. S., eds, Handbook of Environmental Isotope
Geochemistry 2. Elsevier, Amsterdam: 207-235.
Usdowski E., Hoefs J. and Menschel G., 1979: Relationship between
13
C and 18O fractionation and changes in major elements com-
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cal variations with inorganic CaCO3 precipitation. Earth and
Planetary Science Letters 42: 267-276.
 GEOCHRONOMETRIA Vol. 21, pp 97-108, 2002 – Journal on Methods and Applications of Absolute Chronology

δ 13C and δ 18O TIME RECORD AND PALAEOCLIMATIC

IMPLICATIONS OF THE HOLOCENE CALCAREOUS TUFA
FROM SOUTH-EASTERN POLAND AND EASTERN
INDIA (ORISSA)

ANNA PAZDUR1, RADOS£AW DOBROWOLSKI2, TOMASZ DURAKIEWICZ3,

NATALIA PIOTROWSKA1, MANMOHAN MOHANTI4 and SRIKANTA DAS4
1
Department of Radioisotopes, Institute of Physics, Silesian University of Technology,
Krzywoustego 2, 44-100 Gliwice, Poland
(e-mail: anna.pazdur@radiocarbon.gliwice.pl)
2
Department of Physical Geography and Palaeogeography, Maria Curie-Sk³odowska University,
Akademicka 19, 20-033 Lublin, Poland
3
Mass Spectrometry Laboratory, Maria Curie-Sk³odowska University,
Plac Marii Curie-Sk³odowskiej 1, 20-031 Lublin, Poland;
Los Alamos Laboratory, Condensed Matter and Thermal Physics Group, Los Alamos, Mailstop K764, NM 87545, USA
4
Department of Geology, Utkal University Bhubaneswar - 751004 (Orissa) India

Key words
words: Abstract: Measurements of δ18O and δ13C in tufa samples dated by 14C method have been
CALCAREOUS TUFA, used to reconstruct climatic changes in Southern and Eastern Poland and in Eastern India
STABLE ISOTOPES, (Orissa) for the last ca 13,500 years. Stable isotope time record δ18O in calcareous tufa pro-
PALAEOCLIMATE, files can be interpreted as palaeoclimatic record if dependence between oxygen isotope com-
HOLOCENE, position and temperature for the specific climatic region is known. Estimated sedimentation
POLAND, INDIA temperatures of calcareous tufas from Polish sites indicate the mean year of air temperatures
during the last 12,000 years and mean winter and summer temperature for Orissa state, using
stable isotope analysis for calcareous tufa from Indian sites. The estimated temperatures have
real values, comparable with contemporaneous sedimentation temperature. The characteris-
tic trend of the temperature changes increasing for Poland and decreasing for Orissa, since
the beginning of the Holocene till today, can be observed with climatic optimum ca 5000-
6000 BP synchronous in both countries.

1. INTRODUCTION Precise dating of speleothems by 14C and other dating

Calcareous tufa and speleothems appear to be signifi-
cant indicators of palaeoenvironmental and palaeocli-
matic changes. These deposits reflect the combined
effects of karst processes, controlled to a great extent by
climatic factors, especially temperature and humidity.
Freshwater tufas in continental realm, deposited by physi-
cochemical and/or biochemical processes are also consid-
ered as reliable recorders of palaeoclimatic and environ-
mental change (Andrews et al., 1994 and Pazdur et al.,
1988b). Stable isotopes, like 18O and 13C, and chemical
analysis, frequency distribution of U/Th and 14C dates have
frequently been used as a tool for analysis of sedimento-
logical processes and reconstruction of palaeoclimatic
conditions, as well as for stratigraphic purposes. Measure-
ments of δ18O and δ13C in tufa samples dated by 14C
method have been used to reconstruct Holocene climatic
changes in southern and eastern Poland (Pazdur, 2000).
methods along with δ13C and δ18O measurements have
been used to interpret palaeoclimatic changes (Pazdur et
al., 1995). The frequency distribution of 14C and U/Th
dates has been successfully applied to palaeoclimatic stud-
ies using speleothems (Goslar et al., 2000; Hercman,
2000).
Interpretation of isotopic investigations in lacustrine
carbonates is much more sophisticated and difficult be-
cause of the complex nature of sedimentation, influenced
by a number of physicochemical and biological factors.
Palaeolake level changes of the Goœci¹¿ Lake (Central
Poland) have been studied from the lake and lake-mar-
gin sediments with help of deposits constituted of lami-
nated sediments, peat, lacustrine gyttja and beach sedi-
ments together with radiocarbon chronology and carbon
isotope content interpretation. The behaviour of this lake
during the last 12 ka reflects global climate change in the
temperate zone fairly well (Pazdur et al., 1994 and 1995b).
 δ13C and δ18O TIME RECORD AND PALAEOCLIMATIC IMPLICATIONS OF THE HOLOCENE CALCAREOUS TUFA ...
The significance of undisturbed lacustrine calcareous sedi-
ments as potential geochemical archives of isotopic
records of palaeoenvironmental changes has been recog-
nized. Isotopic studies of pedogenic carbonates (caliche,
concretions) and cements provide information related to
circulation of groundwater and precipitation, and, indi-
rectly, lead to palaeoclimatic conclusions (Pazdur et al.,
1995a).
Several authors dealing with freshwater carbonates
assumed that kinetic effects during isotopic fractionations
are small (except at spring heads) and used the isotopi-
cally derived temperature for studying local and regional
palaeoclimatic and palaeoenvironmental records
(Andrews et al. 1993 and 1994; Pazdur et al. 1988b).
Usdowski et al., (1979) and Dandurand et al., (1982), while
studying calcite precipitation at springs and streams, at-
tributed the variations in isotopic composition to disequi-
librium condition due to kinetic effects. Turi (1986) noted
that isotopic equilibrium is seldom attained in the depo-
sition of travertines mainly as a consequence of kinetic
effects. Recently, Chafetz and Lawrence (1994) demon-
strated that δ18O values of the precipitates can change
drastically within a travertine system and stressed that the
overall changes with water flow, microenvironmental con-
trols and disequilibrium precipitation determine the iso-
topic signatures of these freshwater deposits. It is, there-
fore, necessary to stress the depositional conditions be-
fore establishing the isotopic signatures and reconstruct-
ing the palaeoclimatic change.
Generally, tufa deposits, for example European tufas,
involve headwaters, which contain dissolved calcium car-
bonate derived from marine (isotopically heavy) carbon-
ates. In contrast to these deposits, tufas of Orissa State
98
Fig. 1. Map of Europe and Asia
where tufa samples have been
studied in Poland and India (Orissa).
are formed in a Precambrian terrain of crystalline and
metasedimentary rocks. Due to the absence of any ma-
rine limestone or dolomite, the tufa depositional system
forms an interesting geochemical system. Das and
Mohanti (1997) recently presented the fabrics of micro-
bial tufas and discussed depositional processes. In this
paper, we have attempted to date the tufa carbonates and
apply the stable isotopic signatures to understand the
implications of climatic changes in Orissa during the
Holocene.
For reconstruction of time record of palaeoenviron-
mental conditions of the sedimentary processes the time
scale of carbonate deposition should be reconstructed.
Radiocarbon, U/Th, TL and AAR dating methods may
be usually used.
The large number of dating results obtained by dif-
ferent methods enable interpretation of results with use
of probabilistic methods (Baker et al., 1993; Smart and
Richards, 1992; Srdoc et al., 1983; Hercman, 2000).
Frequency distributions of dates may be compared with
results obtained by other methods, like changes of
temperature and precipitation in the past, reconstructed
from pollen analyses of peat-bog profiles and lake sedi-
ments of non-glaciated areas, and with palaeoclimatic
records from deep sea cores (Guiot et al., 1989;
Schackleton, 1967).
2. INVESTIGATED SITES IN POLAND AND IN INDIA
The radiocarbon time scale record of δ13C and δ18O
from sites situated in the Cracow-Wieluñ Upland
(Rac³awka, Rzerzuœnia, Trzebienice; southern Poland)
and the Holy Cross Mountains (Sieradowice; south-
 A. Pazdur et al.
eastern Poland) and their palaeoclimatic interpretation was
given by Pazdur et al. (1988b). In this paper the results
are used for comparison of those from Krzywice-1 and
Rudka-2 (Lublin Upland, eastern Poland; Dobrowolski
et al., 1996) with Mundapathar, Kudipasa and Sulagan
(Orissa, eastern India). Dobrowolski et al. (1999 and
2002), presenting δ13C and δ18O record in time related to
Holocene stratigraphical division, but without detailed ra-
diocarbon time scale. Das and Mohanti (1997) and Pazdur
et al. (2002) described results of radiocarbon dating, δ13C
and δ18O measurements, and sedimentological descrip-
tion for sites in India.
Poland
Sedimentological and isotopic studies were made for
profiles from the following geographical regions:
l Cracow-Wieluñ Upland (southern Poland): 27 samples
of calcareous tufa of biogenic origin (autochthonous
calcareous muds, stromatolites, oncoids, and moss
travertines; Pazdur et al., 1988a) from three sites
(Rac³awka, Rzerzuœnia and Trzebienice). The sites
represent different hydrodynamic conditions of tufa
sedimentation. They are situated in small valleys en-
trenched in carbonate rocks of Lower Carboniferous
(Rac³awka), Jurassic and Cretaceous (Trzebienice and
Rzerzuœnia).
l Holy Cross Mountains (south-eastern Poland): 11
samples of fine-grained calcareous muds, rich in or-
ganic matter, precipitated in shallow stagnant water
basin (Pazdur et al., 1988a). The Sieradowice profile
is situated in a small valley cut in Devonian carbonate
rocks.
l Lublin Upland (eastern Poland): both sediment pro-
files, Krzywice-1 and Rudka-2, consist of calcareous
muds rich in organic matter precipitated, like tufa from
Sieradowice, in low-energy water conditions. They are
situated on Upper Cretaceous rocks (Dobrowolski et
al., 1999 and 2002).
99
Radiocarbon chronology of sedimentation was made
on the basis of 8 organic and the same number of carbon-
ate 14C dates for Krzywice-1, and 6 organic and 9 carbon-
ate 14C dates for Rudka-2 profiles (Dobrowolski et al.,
2002). Sixty three carbonate samples for stable isotope
13
C and 18O analyses were taken (37 from Krzywice-1 and
26 from Rudka-2 profile) and radiocarbon time scale for
δ13C and δ18O time record was reconstructed (Pazdur et
al., 2002). The construction of similar time scale for other
profiles from Poland and India was based on dependence
between reservoir age and δ13C values in tufa samples. The
methodology and details of the reconstruction are given
by Pazdur (1988) and Pazdur et al. (2002).
India (Orissa)
Detailed description of profiles and classification of
tufa samples is given by Pazdur et al. (2002). Sedimento-
logical and isotopic studies are based on:
l Mundapathar: 13 tufa samples from one profile, in-
cluding stromatolic tufa, moss (phytohermal) tufa,
phytoclastic tufa, pisoid and sinter. The deposit of
about 7 m in thickness is situated at a small waterfall
formed on charnockite under high-energy conditions.
l Kudipasa: 8 tufa samples from one profile, including
stromatolic tufa, moss tufa, phytoclastic tufa and sin-
ter. The deposit measuring about 6 m in vertical thick-
ness is located on a hill slope. Streams depositing the
tufa drain basic lava, tuff and quartzite under moder-
ate hydrodynamic conditions.
l Sulagan: 7 tufa samples including stromatolic tufa and
moss tufa. The deposit is about 6 m in vertical thick-
ness. It is located at a small waterfall formed on
charnockite under high-energy conditions.
l Single tufa samples from various sites (regional
samples). Miticoli and Mundapathar represent high-
energy conditions, Madhapur and Bhaliadal represent
moderate energy conditions, Takara and Banigochha
represent low hydrodynamic conditions.
Fig. 2. Stromatolitic crusts draping
over moss-rich pockets on the lower
part (close to the hammer). Upper
part shows stromatolitic crusts
alternating with phytohermal (moss-
rich) deposits. Central region of the
photograph shows speleothemic
crusts. Locality: Mundapathar.
 δ13C and δ18O TIME RECORD AND PALAEOCLIMATIC IMPLICATIONS OF THE HOLOCENE CALCAREOUS TUFA ...
Radiocarbon time scale of sedimentation of the tufa
profiles was made on the basis of 11 carbonate and 2
organic 14C dates for Mundapathar, 6 carbonate and 2
organic 14C dates for Kudipasa, and 4 carbonate and 2
organic 14C dates for Sulagan. Radiocarbon dating of the
regional samples was made for the carbonate fractions.
Thirty three carbonate samples were taken for stable 13C
and 18O analysis from all sites together (Pazdur et al.,
2002).
3. PRESENT CLIMATIC BACKGROUND
Sites from Poland
Sedimentation of biogenic calcareous tufa occurs
mostly during spring months. In the southern and south-
eastern Poland, the temperature of spring water at this
time is equal to mean annual air temperature; therefore,
100
Fig. 3. Phytohermal tufa (calcified
moss) showing several stages of
growth and high porosity.
The unidirectional orientation of the
moss indicate hydrodynamic control
on phytoherms. Sample from
Mundapathar. Each division of the
scale is 1 cm.
Fig. 4. Stromatolitic crusts showing
alternate dark and light laminae. The
darker laminae are thicker at the lower
parts and appear convex due to
growth over small bushy mosses.
Sample from Bhaliadal.
the mean annual temperature of meteoric water coincides
with temperature of tufa sedimentation. Climatic data
from the Cracow Upland show that the mean annual tem-
perature varies from 7 to 8oC and mean temperature of
springs from 7 to 9oC (after Pazdur et al., 1988b). The tem-
perature of streams fluctuates between 7 and 12oC.
Studied tufas from the Cracow Upland were sampled
with a thickness less than 5 cm. It means that each sample
covers 10- to 20-yr time interval according to determined
sedimentation rate (several mm/yr). This intervals are
insignificant when compared to errors of the age deter-
mination. Sampling of Krzywice-1 and Rudka-2 sites was
made across profiles, with small (ca 30 mg) amounts of
carbonate. The results of δ18O analysis present mean val-
ues in a shorter period of time than in the case of samples
from the Cracow Upland profiles, even though the sedi-
mentation rate is about several or more mm per year.
 A. Pazdur et al.
Sites from India (Orissa)
The warm and humid tropical climate of Orissa is
characterised by seasonal southwest monsoon rainfall.
The annual mean precipitation is ca 150-200 mm. Major
part of the rainfall is concentrated in the monsoon sea-
son (Mid-June to Mid-October, with an average of ca 200-
350 mm of rainfall).
The ranges of air temperature change are as follows:
in winter 8-12oC minimum and 25-28oC maximum and in
summer 25-28oC and 36-42oC, respectively. Water tem-
peratures when tufa precipitates are influenced by gen-
eral thermal conditions. Water temperatures are as fol-
lows: 19-20.5oC in winter (December-January) and 27.5-
29oC in summer (April-May).
The deposition of tufas takes place mostly during
spring (February-March) and summer (April-May) peri-
ods. Presently, summer deposition is negligible – possibly
due to the groundwater table fall and limited or missing
surface flow. The sparitic and micritic laminae in stroma-
tolitic tufa indicate seasonal deposition (spring-summer
and rainy-winter periods). Thickness of laminae couplets
suggests a depositional rate of 1 mm to a little more than
1 cm per year.
Stream waters depositing the tufa show a pH value of
8.0 to 8.6. Concentrations of Ca2+, Mg2+ and HCO-3 vary
within the range of 30-80 mg/l, 9-28 mg/l and 200-
310 mg/l respectively (Das and Mohanti, 2001).
4. TIME RECORD OF δ 13C
The enrichment of carbonate in heavy carbon isotope,
in comparison to water solution, may be induced by par-
tial disequilibrium between HCO-3 in water and atmo-
spheric CO2 during precipitation. This is attributed to
kinetic effects during CaCO3 precipitation from highly
supersaturated solution in which the rate of carbonate
precipitation is faster than equilibrium fractionation with
the respect to the stable isotopes (Usdowski et al., 1979;
Dandurand et al., 1982; Turi, 1986; Chafetz et al., 1991).
In natural environments, the exchange of CO2 can only
lead to equilibrium if sufficient residence time is avail-
able, which can be attained in standing water bodies like
lakes. The geomorphic setting of our tufa deposits indi-
cates a very low residence time and great water turbulence.
This situation favours the idea of partial disequilibrium
precipitation.
We believe that dominant part of the carbon has been
derived from biogenic sources and may be partly from the
atmosphere. The range of δ13C values indicates relative
enrichment of tufa in heavy isotopes. The enrichment in
heavy isotopes may be determined by photosynthesis of
plants, which preferentially use lighter carbon (12C) leav-
ing the remaining HCO-3 enriched in 13C (Pentecost and
Spiro, 1990; Merz, 1992; Casanova and Hillaire-Marcel,
1993; Guo et al., 1996). But the photosynthetical removal
of CO2 requires relatively longer residence time. Tufas in
the Orissa State originate in discharge basins with low
residence time of water. Even though profuse amount of
cyanobacteria, diatoms and mosses are involved, the rate
of photosynthetic removal of CO2 by these plants is small
101
in comparison to the rate of physical degasation due to
turbulence of water. Photosynthesis may be locally sig-
nificant, depending on the amount of biomass, especially
where cyanobacteria or algae and moss thrive together.
The range of δ13C of tufa from Poland sites is ca from
-10.5 ‰ to -6 ‰ for the last 10,600 years (Pazdur, 1988).
The significantly higher values are observed for the
Krzywice-1 site, with the longest time record, in the time
of 11,800-10,800 BP (Fig. 5). The δ13C values from the
Orissa sites receive ca -2.5 to -11.7 ‰ in the whole inves-
tigated period between 13,500 BP and the present time.
The range of δ13C values of tufa from the Polish and Orissa
sites is in accordance with a deposition from freshwater
and suggest the presence of isotopically lighter organic
carbon.
As there is no marine limestone and/or dolomite in
the studied area of Orissa, we believe that the carbonates
have originated mostly from organic matter. Ca++ ions are
derived from weathering of silicates, mostly plagioclase
and pyroxene. Kalsotra and Prasad (1979) and Pawar et
al. (1988) have reported tufa deposits from sandstones and
shales and basaltic areas in India. Augustithis (1982) also
noted the formation of carbonate nodules from disinte-
gration of olivine basalts in Duncan, south of Addis-
Ababa.
Tufas are depleted in heavy isotope 18O in all Polish
and Indian sites (see Fig. 7), when compared to δ18O val-
ues expected for equilibrium sedimentary processes. The
low and negative δ18O values suggest a low rate of evapo-
ration.
Individual δ13C values of tufa samples shown in Fig. 5
as time records reveal short-time fluctuations and in-
crease/decrease trends, different in detail from a profile
to profile. The co-variation of oxygen isotope data with
the carbon isotope ones (Fig. 6) indicate similar trend of
changes in disequilibrium condition for all the India sam-
ples; correlation coefficient is equal to r = 0.73 (22 pairs
of δ13C and δ18O). For all Polish samples, the dependence
between both delta values is positive (r = 0.20), if we re-
move 6 extreme points with δ13C > -4 ‰ and δ18O >-6 ‰
(Krzywice-1 profile) from period older than 10,000 BP.
It means high confidence level and confirm disequilibrium
sedimentary conditions and presence of isotopic kinetic
fractionation effect. The relations indicate, that organic
consumption of CO2 may be significant because of the
presence of chemo- and heterotrophic bacteria (Pazdur
et al., 1988b) observed for tufa sites in the southern
Poland. Enrichment of tufas in the heavier carbon isotope
(13C) during the warmer periods may be connected to
some extent with activation of plant consumption.
5. TIME RECORD OF δ18O AND TUFA SEDIMENTATION
TEMPERATURE
δ 18O of tufa in palaeoclimatic studies
Isotopic investigations of tufa from Poland deals with
sites of spring tufa deposition in variable conditions of
river water energy (southern Poland; Pazdur et al., 1988a)
and semi-limnic conditions (south-eastern Poland; Pazdur
et al., 1988a; Dobrowolski et al., 1999). The palaeotem-
 δ13C and δ18O TIME RECORD AND PALAEOCLIMATIC IMPLICATIONS OF THE HOLOCENE CALCAREOUS TUFA ...
perature curve was constructed (Pazdur et al., 1988b) on
the basis of the time scale reconstruction using radiocar-
bon dating and interpretation of stable isotope carbon and
oxygen composition in sedimentary processes. The curve
describes the annual mean temperature changes for the
southern Poland in the period of 2000-9600 BP, i.e., in
which sedimentation of tufa took place in Rac³awka,
Rzerzuœnia, Trzebienice and Sieradowice (see Figs 5
and 7). Thirty eight results of 14C dating and stable iso-
tope analysis were used for palaeoclimatic reconstruction.
Dobrowolski et al., (1999) carried out isotopic investiga-
tions on two eastern Polish sites, Krzywice-1 and Rudka-
2. Radiocarbon time scale of tufa sedimentation was con-
structed for those sites (Pazdur et al., 2002) and palaeo-
climatic interpretation of 61 new results of stable isotope
analyses can be done together with the previous results.
Time record of δ18O measurements in individual and all
tufa sites from Poland and India is shown in Fig. 7.
102
The variation in δ18O values indicates differences in
isotopic composition of tufa depositing waters controlled
by water temperature. The temperature of cold spring
waters in continental conditions is influenced by rainfall
and atmospheric temperature, i.e., climate controls the
tufa deposition.
Temperature precipitation of tufaceous sediments in
Poland and India
Despite difficulties caused by disequilibrium precipi-
tation of CaCO3, it may be expected that the isotopic com-
position of oxygen of Holocene tufa might be useful for
the reconstruction of the approximate thermal condition
of sedimentation, or strictly speaking, the temperature of
water, from which carbonate precipitated. Reconstruction
of palaeotemperature changes for a given geographical
region may be based on known seasonal dependence of
δ 18O in meteoric water upon temperature (Van der
Fig. 5. Time record of δ13C in
separate tufa sites of Poland and
all sites together from India.
 A. Pazdur et al.
Straaten and Mook, 1983). Any attempt to estimate tem-
peratures of sedimentation from measured values of δ18O
in calcareous tufa requires several simplifying assump-
tions, which are based on the results of investigation of
recent tufas (Pazdur et al., 1988b). One of this is that the
temperature gradient of δ18O is not changed in the pro-
cess of deposition, i.e., the temperature gradient of δ18O
in the sediment is the same as in precipitation and stream
water, and second – kinetic fractionation effect of oxygen
isotopes is independent on sedimentation temperature.
To reconstruct temperature record for the Late Glacial
and Holocene, the constant values of temperature oxy-
gen gradient and kinetic effect in the whole period must
be assumed (Pazdur et al., 1988b). It means that in this
whole time period the circulation of air mass was the same
(Ró¿añski, 1985). The temperature t of tufa sedimenta-
tion may be estimated on the basis of simple equation
(Pazdur et al., 1988b):
é d(d18 O) ù
(d18 O)C = ê ú ×t+ A+ D, (5.1)
ë dt û W
103
where A means extrapolated δ18O value of water in
0 C, equal to -13.0±0.4 ‰ (Pazdur et al., 1988b) and ∆
o
– the value of kinetic fractionation effect for oxygen iso-
topes in sedimentary processes of carbonates, i.e., the dif-
ference between the δ18O value in carbonate (vs. PDB)
and the same value in water solution, from which the sedi-
ment was deposited (vs. SMOW).
The global temperature gradient for coastal region in
meteoric water is equal to 0.72 (Van der Straaten and
Mook, 1983) and 0.37 ‰ /oC for continental climatic area
(Pazdur et al., 1988b). The estimation ∆ (Pazdur et al.,
1988b) receive values between -1.7 and -2.5 ‰ for recent
tufa from the southern England (Thorpe et al., 1980) and
change from +0.26 to -0.04 ‰ for Germany, Central
Europe (Usdowski et al., 1979).
To estimate the temperature time record in Poland,
the mean 500-year δ18O values were used for calculations
of t, on the basis of Eq. (5.1); the maximal and minimal
values of ∆ like for Germany were applied. Such values
of ∆ give correct value of present water spring tempera-
ture in the southern Poland (ca 8 oC) if the measured value
Fig. 6. Dependence between δ13C and δ18O
for all tufa profiles of India and Poland.
Correlation between both delta values is
negative for Polish samples and positive for
samples from India.
 δ13C and δ18O TIME RECORD AND PALAEOCLIMATIC IMPLICATIONS OF THE HOLOCENE CALCAREOUS TUFA ...
of δ18O in contemporaneous spring water (ca 10 ‰) is
taken into account. It confirms assumed way of tempera-
ture reconstruction in the past.
The estimation of temperature time record for India
is more problematic, as the dependence between δ18O and
temperature of precipitation and spring water is unknown.
If we assume the gradient temperature of δ18O the same
as in Poland and ∆ values characteristic for the southern
England (-1.7 and -2.5 ‰), the precipitation tempera-
ture at present, estimated on the basis of δ18O in modern
tufa sample, would be ca 22oC. This value is too low in
comparison with 28-29oC of water in streams, if deposi-
tion of tufa took place in summer time mainly, when bio-
genic processes are intensive. The other combinations of
model parameters (grad δ18O and ∆ values) give lower
temperature values in every case.
104
The reconstructed temperature curves in ca 500-12,000
for Poland and 0-13,400 BP for India are shown in Fig. 8.
The width of both curves is bordered by temperature val-
ues calculated for maximum and minimum ∆ values.
6. WARM/DRY AND WET/HUMID PHASES IN THE
HOLOCENE OF POLAND AND INDIA
The time records of δ18O and estimated temperature
cover 500-12,000 BP for Poland and 0-13,500 BP for
Orissa (India). Periods of carbonate sedimentation started
in different times in the southern and south-eastern
Poland, i.e. at 9600 BP in Cracow and at 11,800 BP in the
Lublin Upland. This difference is determined by environ-
ment of sedimentation, which determined the type of tu-
fas: high-energy water tufas in the Cracow Upland
Fig. 7. Time record of δ18O of
southern (Rac³awka, Rzerzuœnia,
Trzebienice and Sieradowice),
south-eastern Poland (Krzywice-1
and Rudka-2), all sites of Poland
together and all India sites.
Additionally, curve of mean values of
δ18O in 500-years intervals is given,
which was used for estimation of
temperature ranges shown in Fig. 8.
The numbers near points on the
Figure give the numbers of δ18O
results in 500-years intervals.
 A. Pazdur et al.
(Rac³awka, Rzerzuœnia and Trzebienice) and low-energy
water in the Lublin Upland (Krzywice-1, Rudka-2 and
Sieradowice). The longest time records of δ18O and δ13C
are observed for Krzywice-1 (Figs. 5 and 7) depending
also on possibility of more detailed sampling of semi-
limnic sediments. The processes of tufa deposition have
been still observed both in Poland and in Orissa, although
no isotope analysis of Polish sites for the last 500 years
has been made.
The changes of oxygen isotope composition as the
function of the age can be transformed on temperature
time record. The frequency distribution of tufa samples,
in division on time ranges, should be connected with in-
tense precipitation and, because of this, with humid cli-
matic phases. Warm and humid phases are especially
favourable environmental conditions for tufa deposition.
Both climatic curves for Poland and India (Figs 7 and
8) indicate trends of temperature changes. They are op-
posite – increasing for Poland and decreasing for India in
the whole period of 12,000 years. Numerous warmer and
cooler fluctuations are visible on curves. The confidence
level of fluctuations for Poland is higher owing to a greater
number of experimental points (99) than for India (24).
The shape of both temperature curves at their begin-
ning is completely different. The Holocene warming is
visible before 10,000 years BP on the Polish curve, im-
mediate decrease of temperature to this time is clear on
the Indian curve. The similar directions of changes of δ18O
(and temperature) for both curves are shown in time pe-
riods:
l Lower values, indicating cooler climatic conditions, are
observed at ca 9600-9400, 8000-7500, 5800-5200, 4500-
4200, and 2500-1800 BP;
l Higher values, dependant on warmer periods, are vis-
ible at ca 9200-8200, 6200-4500 (with several relatively
high fluctuations on both curves), and 1800-500 BP.
After ca 1000 BP until present, the temperature de-
creased to final 23 in India and 9oC in Poland.
105
It may be noticed that frequency of samples in warmer
periods are the highest, which means humid climatic con-
ditions. Because of difference in geographical position of
India and Poland, we can assume, that indicated warm and
cool periods have global character.
7. CONCLUSIONS
δ18O time records, based on the radiocarbon time scale,
in calcareous tufa provide information on temperature
changes during the last ca 12,000 years in the south-east-
ern Poland and 13,500 years in India (Orissa). Recon-
structed temperature values are realistic and reflect mean
annual temperature of air in Poland and mean annual
temperature of water in streams for Orissa. The mean
annual water temperature is several degrees lower than
the mean annual air temperature. The general trends of
temperature changes in both countries are opposite;
starting at ca 13,500 BP the mean annual temperature is
decreasing in Orissa until present. In the range of 12,000-
11,000 BP the temperature decreased, and after this time
increased again in Poland. Observed temperature fluctua-
tions, with different amplitudes, have been correlated in
time. Some warmer and cooler phases of the same age
ranges occurred in Poland and India, indicating their glo-
bal character.
ACKNOWLEDGEMENTS
The interpretation and preparation results of isotope
analyses to print has been made within the projects BW
and BK sponsored by Silesian University of Technology,
Poland, during the last 2 years and Scientific Research
Committee, Poland, within grant No. 6 P04E 007 17
Fig. 8. Temperature time record
for Poland and India estimated with
assumption of isotope kinetic
fractionation effect in sedimentary
processes of tufa. The ranges of
temperature were determined for
minimal and maximal values of ∆
according to (5.1) Equation.
 δ13C and δ18O TIME RECORD AND PALAEOCLIMATIC IMPLICATIONS OF THE HOLOCENE CALCAREOUS TUFA ...
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107
 GEOCHRONOMETRIA Vol. 21, pp 109-118, 2002 – Journal on Methods and Applications of Absolute Chronology

TIME RECORD OF PALAEOHYDROLOGIC CHANGES

IN THE DEVELOPMENT OF MIRES DURING THE LATE
GLACIAL AND HOLOCENE, NORTH PODLASIE LOWLAND
AND HOLY CROSS MTS

S£AWOMIR ¯UREK1, DANUTA J. MICHCZYÑSKA2 and ANNA PAZDUR2

1
Institute of Geography, Œwiêtokrzyski University,
Œwiêtokrzyska 15, PL-25-406 Kielce, Poland
(e-mail: slavomir.zurek@pu.kielce.pl)
2
Department of Radioisotopes, Institute of Physics, Silesian University of Technology,
Krzywoustego 2, PL-44-100 Gliwice, Poland
(e-mail: danuta.michczynska@radiocarbon.gliwice.pl)

Key words
words: Abstract: Radiocarbon dating of mire sediments is useful tool for reconstruction of time scale
RADIOCARBON, of wet and dry phases during the Late Glacial and Holocene. The method is applied here to
MIRES, LAKES, determine palaeohydrological conditions of some Polish regions. On the basis of 14C dating of
ENVIRONMENT, sediment profiles from North Podlasie Lowland and southern piedmont of Holy Cross Mts.,
PALAEOHYDROLOGY, duration of wet (1100-1400, 2100-2600, 4700-5000, 7300-7500, 8000-8400, 8800-9200 and
HOLOCENE 10,500-10,850 BP) and dry (1700-2200, 2600-2800, 3400-3700, ca 4000 and 4500, 5100-5700,
ca 6400, 6900-7100, 9200-9300, ca 10,100 and 10,900 BP) periods is suggested.

1. INTRODUCTION shorter flooding with longer ground water presence oc-

The mire is composed of four parts: vegetation, wa-
ter, acrotelm and peat deposit. Decomposition of plant
remains in mire differs in the relation to above and un-
derground parts of plants. In contrast to the complete
decomposition and mineralization of the aboveground
parts, resulting in the production of humus, decay pro-
cesses of underground, submerged plant remains produce
undecomposed peat fibre. Transformation of plant
matter into peat takes place in the acrotelm layer, where
aerobes, actinomycetales and fungi transform biomass
into humus in periodical aerate conditions. Structural
plant remains together with humus reach lower, highly hy-
drated deposit layer. Here, in anaerobic conditions, mi-
nor changes occur; peat is exposed to anaerobic bacteria
activity that leads only to weak mineralization process, not
to peat humification.
The ratio of undecomposed remains to humus in peat
depends on different water conditions. In wide valley
flooded by stagnating water for a long time medium and
highly decomposed, plastic, often silt-covered reed fen
peat is deposited. Under conditions of short-time flood-
ing and constant inflow of ground water medium decom-
posed, rather fibrous tall sedge peat is accumulated. When
cur, accumulation of highly decomposed, granulous-amor-
phous forest peat is observed as well. Regular and con-
stant ground-water inflow, often ascending, and absence
of flooding lead to accumulation of slightly decomposed
sedge-moss peat with fibrous-spongy structure. Gradual
reduction of ground-water flow creates transition bogs,
and, when supplied with rainfall, raised bogs. Whole year’s
superiority of rainfall over evaporation, and its corollary
- presence of ground water in the surface level of mires
leads to sedimentation of slightly decomposed sphagnum
peat, whereas its periodic subsidence results in accumu-
lation of medium and highly decomposed cotton-grass
peat material. Presence of wood and tree trunks in raised
bog peat testifies to the reduction of water level and mire
afforestation, what can result from climatical change (dry
phase) or other, local changes (e.g. erosion of the dome
and drainage of its slopes). As a consequence, cessation
or considerable reduction of the raised bog peat produc-
tion follows. When wetter period comes and ground-wa-
ter table rises slightly humified raised bog grass peat is
accumulated again. Persisting lowering of ground-water
table in fen bogs causes high peat humification and its
gradual mucking. Thus climate, through changes of hu-
midity and temperature, controls development of valley
 TIME RECORD OF PALAEOHYDROLOGIC CHANGES IN THE DEVELOPMENT OF MIRES DURING ...
fen bog, transition bog and raised bog in watershed zone.
The control is realised by supplying of concave landforms
i.e. various depressions and valleys, where the peat for-
mation process is located, with water.
Initial stage of mire formation in the territory of Po-
land is dated back to the late Vistulian (¯urek 1990, 1993).
During warm periods of the Late Glacial more than ten-
centimetre strata of the moss-fenn were deposited in shal-
low depressions. Melting of dead or ground ice resulted
in greater depth of hollows and in their flooding, what is
reflected by the presence of gyttja superimposed over the
peat. During the cold oscillations, dunes often encroached
onto wetlands, and so blown sands covered the peat.
The dominant feature of the early Holocene landscape
represented lakes, with moss fen mires on the shores. At
first deep, these concave landforms were subjected to
paludification because of the ground-water table was few
metres beneath its present state; bottom of the depres-
sions were often supplied by waters of head from deeper
water-bearing horizon. In isolated depressions, moss fenn
peat accumulated. Initial process of peat formation did
not cease generally but was rather reduced to peat pro-
duction in dry periods. While at the beginning of
Mezoholocene water level raised, during the second half
of the period it dropped. At that time a lot of shallower
lakes that were subjected to the process of peat accumu-
lation disappeared. On the other hand, rise of water level,
resulting from permanently increasing accumulation,
caused swamping of hitherto dry depressions and higher
altitude areas within the local relief. A variety of mires
characterised with a particular peat type appeared dur-
ing the period: apart from moss fen mire, forest fen, reed
fen and transitional bog are to be encountered. Further,
intensification of mire development occurred at the be-
ginning of Subboreal and Subatlantic periods. In valleys
dominated supreme mires supplied with surface and
ground water such as sedge fen and alder swamp; for
watershed area transition and raised bogs are to be men-
tioned.
Reflection of human activity can be traced in the Pol-
ish peat deposits through the past thousand years. Vari-
ous form and intensity of deforestation has contributed
to transformation of forest communities into open moss-
sedge mires and sedge fens, clearance of vegetation on
slopes in valleys and depressions has triggered process of
covering the valley mires by alluvial or deluvial silts. How-
ever, substantial cause of the mire development variations
is still the natural water regime. The evidence of environ-
mental humidity represent gyttja, chalk lake insertions in
peat, decrease of peat decomposition degree,
paludification of hitherto dry depressions, fen spring de-
velopment, forest and shrubs retreat for the benefit of
open associations like rushes, moss-sedge mires or rushes
entering into transitional or moss-sedge mires. Con-
versely, increase of peat decomposition degree, affores-
tation of mires, lake terrestrialization, appearance of open
communities with ferns, shrubs and sedge Carex paradoxa
testify to dry climatic phase, drainage and lowering of
ground-water level.
110
2. MATERIAL FOR 14C ANALYSIS
Profiles of sediments from North Podlasie Lowland
The Bia³ostocka Plateau that belongs to the North
Podlasie Lowland (Fig. 1) is apparently distinguished from
other early glacial marainic plateaux. Numerous outflow
depressions with fossil lakes, narrowing and widening river
valleys, lofty kame hills, morainic and outwash plains re-
semble the last glaciation landscape. It differs only in ab-
sence of lakes and outflowless depressions. Two of the
kettle holes, covered by forest vegetation and protected
within natural reservations “Stare Biele“ and “Jesionowe
Góry“ with mire Machnacz, have been meticulously ex-
plored from the point of genesis of the peat deposits
(¯urek, 1992, 1996a and 2000). Stare Biele mire is an out-
flow depression with numerous bays, of elliptic shape with
4 km and 1.5 km long axes. Position plan and cross sec-
tion of the mire can be found in the article of S. ¯urek
and A. Pazdur (1999). Marginal zone of this carr mire
includes fragments of transition and raised bogs. Sondage
that was to bring the evidence on strata succession in few
sections demonstrated that the thickness of peat, super-
imposed over thin gyttja layers, varied from 1.5 to 2 metres
for most of the sampled spots (Table 1). Sedge-moss
schwingmoore spread throughout the lakes, which, con-
sequently, suffered from rapid afforestation with alder
communities dominating for a long period. In places,
within the upper part of the strata succession, alder peat
is covered by sedge-moss fen peat. At the bottom of alder
peat, in depth of some 1-1.3 m, occurs dark, highly humi-
fied, clammy layer indicating the period of the deposit’s
drainage. This layer was sampled for dating at three dif-
ferent places within the mire. Far away from the centre,
in south-western bay, two highly humified layers were
found in the peat that overlies a fossil upper terrace. Drill-
ing (up to 10 m) in a deep kettle hole with a diameter little
more than 10 m situated in northern bay showed that peat
deposits, which are underlain with fine detrital gyttja (see
Table 1) reach depth of 4.25 m.
Profiles of sediments from Bia³e £ugi, Holy Cross Mts.
Mire Bia³e £ugi, (southern piedmont of Holy Cross
Mts., Fig. 1) occupies 1 km wide and few km long fossil
valley between Belnianka (Nida tributary) and Czarna
Staszowska (Vistula tributary). The valley is filled by raised
peat over transitional and fen peat. There is also carr peat
located on the both valley banks, where small rivers
Trupieñ and Czarna are being formed. In 1994-1998, ten
stratigraphical cross-sections of deposits were made and
a macro-remain analysis of 18 bores was carried out
(¯urek, 2001); the stratigraphical section and the geologi-
cal profiles can be found in ¯urek and Pazdur (1999). Roof
part of the succession (up to 0.8-1.0 m depth) is built by
slightly decomposed raised sphagnum peat over highly
decomposed cotton-grass raised peat. Beneath the latter
slightly and medium decomposed sedge-moss transition
peat is present, and in the bottom part of the profile sedge-
moss fen peat and brown-moss peat are encountered. In
the sediments of the Bia³e £ugi mire two 5-15 cm thick
strata of highly decomposed black peat were distin-
 S. Zurek et al.
guished. The upper one occurs at the depth of 0.8 to 1-
1.2 m, on the border between deposits of transition and
raised peat. Within the black peat stratum, under it or over
a dozen centimetres above fine 2-3 cm thick fire indicat-
ing layers of charcoal are incorporated. These represent
probably an evidence of dry stage, when large fire may
likely have occurred. The second, lower stratum of highly
humified deposit, richer in wood remains, is located at
the bottom part of the whole succession, on the border
between transition bog and fen peat.
3. METHODS AND RESULTS OF 14C DATING
Samples that were submitted for radiocarbon dating
consisted of solely organic sediments. According to low
portion of carbon in the samples, the pre-treatment of 4%
HCl washing was chosen. After pre-treatment and
carbonisation the samples were combusted, and CO2 was
purified by standard method used in Gliwice Radiocar-
bon Laboratory (Pazdur and Pazdur, 1986). Finally, 14C
activity measurements were carried out by gas propor-
tional counting techniques (Pazdur et al., 2000). Results
of 14C dating from Gliwice Radiocarbon Laboratory are
listed in Table 1, marked with laboratory code Gd. Apart
from these, determinations measured in other radiocar-
bon laboratories are to be found here, namely, dates with
lab codes SRR-NERC (Scotland), Hv (Hannover, Ger-
many), TA (Tartu, Estonia), Lod (£ódŸ, Poland) and those
from Leningrad, now Petersburg, laboratory (Russia).
Fig. 1. Localization of investigated mires. Linear scale is the same for both window.
111
The values of 14C age listed in Table 1 represent con-
ventional radiocarbon age determinations calculated ac-
cording to the procedure of Stuiver and Polach (1977).
4. 14C EVIDENCE OF PALAEOHYDROLOGIC EVENTS
Long-term hydrologic changes have specific conse-
quences for the environment of mires. Climate desicca-
tion causes lowering of ground-water table, what effect
changes of physical and chemical properties of upper peat
layer. At first, increase of the peat decomposition degree
should be mentioned. Highly humified peat layers of dark
colour (when fresh) thick from 5 up to 20-30 cm have been
identified in course of stratigraphic studies of various fen
and bog deposits (¯urek, 1995). Sometimes in higher
decomposed peat (carr, reed fen, high-sedge fen, cotton-
grass) black and clammy layers are observed. These tes-
tify to the dry period of longer duration, when peat pro-
duction was drastically limited or stopped. Instead of or-
ganic matter accumulation, decomposition process and
its mineralization began, proceeding from top towards the
bottom levels. Nowadays, in artificially drained peatlands,
this process, called mucking, leads to high decomposition
and further to granulization of upper peat layers
(Okruszko, 1960).
In the peat profiles from Biebrza basin or Bia³ostocka
Plateau, dated by 14C, drainage led only to the increase of
decomposition degree (to 60-80%) without indices of
muck granules. Clamminess of highly decomposed peat
 TIME RECORD OF PALAEOHYDROLOGIC CHANGES IN THE DEVELOPMENT OF MIRES DURING ...

Table 1. 14C dating results of peat samples from different sites of Poland. All dated samples came from NE Poland except Bia³e £ugi site
(Central Poland). The symbols and numbers after slash in the column “Name of samples” indicate profile. Roman numbers (I, II, III)for
Wizna mean different sites. Depth = conventional depth in profile.
14
No. Name of sample Depth Lab. no. C Age Material Altitude References
[cm] [BP] [m asl]
1 Bia³e £ugi 1/13 315-320 Gd-9498 10880±250 sedge-moss fen p. 256,3 ¯urek, Pazdur, 1999
2 Bia³e £ugi 2/21 95-100 Gd-11211 3480±80 cotton-grass p. 256,5 ¯urek 1996b
3 Bia³e £ugi 3/21 175-185 Gd-10320 10170±120 sedge-sphag. p. 256,5 ¯urek, Pazdur, 1999
4 Bia³e £ugi 4/14 405-408 Gd-9508 6940±750 humus with sand 256,3 ¯urek, Pazdur, 1999
5 Bia³e £ugi 13/21 100-105 Gd-15137 2630±90 Eriophorum p. 256 not published
6 Bia³e £ugi 14/21 110-115 Gd-12266 6470±80 Sphagnum-Carex p. 256 not published
7 Bia³e £ugi 15/21 180-185 Gd-15135 8890±140 Carex p. 256 not published
8 Bia³e £ugi 16/21 190-195 Gd-15131 8750±150 Carex p. 256 not published
9 Bia³e £ugi 17/14 90-95 Gd-15129 1830±100 Carex-Sphagnum p. 256 not published
10 Bia³e £ugi 18/14 100-105 Gd-15127 2450±90 Carex-Sphagnum p. 256 not published
5 Biebrza Dolna 1/ Stójka (£awki) 112-118 Gd-7825 2810±60 osier peat 104,1 ¯urek, Pazdur, 1999
6 Biebrza Dolna 2/ Stójka (£awki) 125-130 Gd-7826 5110±60 osier peat 104,1 ¯urek, Pazdur, 1999
7 Biebrza Dolna 3/ Stójka (£awki) 270-280 Gd-10491 8450±100 brown-moss peat 104,1 ¯urek, Pazdur, 1999
8 Gorbacz 1 254-267 Gd-4487 8000±170 detrital gyttja Wicik, 1989
9 Gorbacz 2 180-200 Gd-6172 1460±90 bog peat Wicik, 1989
10 Klimaszewnica /27 145-152 Gd-10492 7150±80 reed-sedge peat 107,0 ¯urek, Pazdur, 1999
11 Kuwasy 1/EO 95-100 Gd-7827 3650±50 alder peat 114,6 ¯urek, Pazdur, 1999
12 Kuwasy 2/EO 186-191 Gd-10497 10850±150 brown-moss peat 114,6 ¯urek, Pazdur, 1999
13 Laskowiec 18-23 Gd-2301 830±80 peaty formation 103,5 ¯urek1987
14 Machnacz 1/ 6 405-415 Gd-5683 > 40800 sedge-moss peat 152,0 ¯urek 1992
15 Machnacz 1/18 150-160 Gd-10494 7300±130 reed-sedge peat 150,5 ¯urek, Pazdur, 1999
16 Machnacz 2/ 6 425-435 Gd-5864 > 43500 sedge-moss peat 152,0 ¯urek 1992
17 Machnacz 2/18 372-382 Gd-10495 11690±150 brown-moss peat 150,5 ¯urek, Pazdur, 1999
18 Machnacz 3/14 368-375 Gd-10499 29470±180 detrital gyttja 151,1 ¯urek, Pazdur, 1999
19 Machnacz/ 14 138-148 SRR-3176 4040±50 cotton-grass p. 151,1 Haslam 1987
20 Machnacz/ 14 72-82 SRR-3175 1120±50 cotton-grass p. 151,1 Haslam 1987
21 Machnacz/ III 14 380-390 Gd-4959 11100±140 brown-moss peat 151,1 Kupryjan.1994
22 Machnacz/ III 14 330-340 Gd-6818 10370±100 detrital gyttja 151,1 Kupryjan.1994
23 Machnacz/ III 14 280-290 Gd-6819 8570±100 sedge-moss peat 151,1 Kupryjan.1994
24 Machnacz/ III 14 165-175 Gd-6824 7470±100 cotton-grass p. 151,1 Kupryjan.1994
25 Machnacz/ III 14 130-140 Gd-6820 3430±80 cotton-grass p. 151,1 Kupryjan.1994
26 Machnacz/ III 14 50-60 Gd-4966 1720±60 cotton-grass p. 151,1 Kupryjan.1994
27 Maliszewo I/Ia 477-481 Hv-5527 11460±210 peaty formation 104,1 ¯urek 1978
28 Maliszewo II/Ib 186-191 TA-1077 5170±100 detrital gyttja 104,1 ¯urek 1986
29 Maliszewo III/II 370-380 TA-1078 8940±120 sedge peat 104,5 ¯urek 1986
30 Maliszewo IV/II 125-135 TA-1076 2350±100 reed peat 104,5 ¯urek 1986
31 Maliszewo V/Ic 205-212 Gd-10490 5720±110 detrital gyttja 104,1 ¯urek, Pazdur, 1999
32 Mocarze Ia 27-32 Gd-2302 1460±100 mud 102,5 ¯urek1987
33 Narew/ Narew-Strabla 160-170 Leningrad 3800±70 wood of alder 121,5 Czeczuga1979
34 Narew/Narew-Strabla 50 Leningrad 1470±50 wood of oak 121,5 Czeczuga1979
35 Niewodowo 200-230 Lod-27 1420±130 oak trunk 98,0 Musia³, Strasz.,1988
36 Sienkiewicze 2 33-38 Gd-2306 940±100 muddy-alluvium f. 119,0 ¯urek1987
37 Sienkiewicze 3 13-18 Gd-2303 670±90 peaty-muddy f. 119,0 ¯urek1987
38 Stare Biele 1/I 115-120 Gd-9506 1700±210 alder swamp peat 143,0 ¯urek, Pazdur, 1999
39 Stare Biele 2/I 180-190 Gd-11212 2690±70 alder peat 143,0 ¯urek, Pazdur, 1999
40 Stare Biele 3/I 245-255 Gd-10321 4000±120 alder peat 143,0 ¯urek, Pazdur, 1999
41 Stare Biele 4/I 995-1005 Gd-9503 13900±310 fine-detrital gyttja 143,0 ¯urek, Pazdur, 1999
42 Stare Biele 5/II 94-100 Gd-9497 2190±130 alder peat 143,0 ¯urek 1996b
43 Stare Biele 6/VII 120-130 Gd-10337 5310±100 alder peat 143,0 ¯urek, Pazdur, 1999
44 Stare Biele 7/24 170-180 Gd-7748 6420±60 alder peat 146,0 ¯urek, Pazdur, 1999
45 Stare Biele 8/29 110-118 Gd-10388 4480±130 alder peat 143,0 ¯urek, Pazdur, 1999
46 Stare Biele 9/63 150-163 Gd-10493 9010±120 moss p. + wood 143,0 ¯urek, Pazdur, 1999
47 Wieczorki 20-25 Gd-1820 1520±70 peaty formation 105,0 ¯urek1987

112
 S. Zurek et al.

48 Wizna 1/I 525-535 Gd-2017 12610±190 sedge-moss peat 104,5 ¯urek 1986
49 Wizna 10/I 535-542 Gd-2084 12710±240 detr.-clayey g. 104,5 ¯urek 1986
50 Wizna 11/85/ Maliszewo I 467-473 Gd-2562 11730±450 peaty formation 104,1 Balw.¯ur.1989
51 Wizna 11/Góra Strêkowa 145-155 Gd-1726 2210±70 sedge peat 101,5 ¯urek1987
52 Wizna 12/Góra Strêkowa 110-120 Gd-1727 1430±60 sedge peat 101,5 ¯urek1987
53 Wizna 13/85/ Maliszewo I 362-367 Gd-2563 9400±500 calcareous gyttja 104,1 Balw.¯ur.1989
54 Wizna 14/ Maliszewo I 240-245 Gd-2504 7960±180 calc. gyttja, wood. 104,1 Balw.¯ur.1989
55 Wizna 15/ Maliszewo I 165-170 Gd-4020 3340±120 detrital g. + peat 104,1 Balw.¯ur.1987
56 Wizna 16/ Maliszewo I 47-52 Gd-4021 1600±100 detr.-calc. gyttja 104,1 Balw.¯ur.1989
57 Wizna 18/ Maliszewo I 140-145 Gd-4334 4820±100 detrital gyttja 104,1 Balwierz1986
58 Wizna 19/ Maliszewo I 70-78 Gd-4299 2770±90 calcareous gyttja 104,1 Balwierz1986
59 Wizna 2/I 425-435 Gd-2010 9270±120 sedge peat 104,5 ¯urek 1986
60 Wizna 20/ Maliszewo I 35-40 Gd-2869 1770±100 detrital gyttja 104,1 Balwierz1986
61 Wizna 4/II 310-320 Gd-1530 9450±90 osier peat 106,0 ¯urek 1986
62 Wizna 5/III 130-142 Gd-1534 4270±70 sedge peat 102,0 ¯urek 1986
63 Wizna 6/II 65-75 Gd-1595 2050±40 alder-swamp peat 106,0 ¯urek 1986
64 Wizna 7/III 50-60 Gd-1596 1150±40 reed-sedge peat 102,0 ¯urek 1986
65 Wizna 8/ Maliszewo II 200-210 Gd-2086 7440±150 sedge peat 104,5 ¯urek 1986
66 Wizna 9/I 518-525 Gd-2085 12430±170 sedge-moss peat 104,5 ¯urek 1986

did not resulted from silting but from partly mineraliza-
tion of organic matter, since the ash content in the dis-
cussed layers is little higher than in underlying and over-
lying strata. Hard granules found now and then are small
fragments of charcoal coming from thin, black, fire-indi-
cating layers. Highly decomposed layers (ca. 40-50 %)
occur also within slightly humified sedge-moss fen peat.
Besides sedge and brown-moss, remains of shrubs, ferns
and some tall-sedge growing in mires with lowered water
e.g. Carex paradoxa appear here as well.
Beginnings of biogenic accumulation
Postglacial accumulation of biogenic formation was
initiated by climatic change. In warmer Lateglacial peri-
ods brown-moss peat or peaty formation were deposited,
representing thus first stage of periglacial tundra
paludification. Covering of biogenic deposits by gyttja
testifies to the beginning of thermokarst process, which
in Maliszewskie Lake (Fig. 1), as results of peaty forma-
tions dating (Gd-2562: 11,730±450 BP, Hv-5527:
11,460±210 BP) manifest it, took place during Alleröd
(¯urek, 1978; Balwierz and ¯urek, 1987 and 1989).
Melting of permafrost in the Machnacz mire (Bia³ostocka
Plateau) began probably earlier, in Bölling (Kupryja-
nowicz, 1991) and was intensified in Alleröd, as backed
by one date for brown-moss peat (Gd-10495: 11,690±150
BP). However, the opinion based on palynological analy-
sis of brown-moss peat at the bottom of the Machnacz
I profile about its Bölling origins has not found support
in the radiocarbon dates. First result for the brown-moss
peat brought value 11,100±170 BP (Gd-4959), second de-
termination for sample from the bottom part of gyttja was
as early as 29,470±170 BP (Gd-10499). The beginning of
under-gyttja peat accumulation in mire Kuwasy was pa-
lynologically dated to the second part of Alleröd (¯urek,
1970), in Lower Biebrza basin (Stójka) to the Late Gla-
cial (Oœwit, 1973). These results are supplied with the ra-
diocarbon dates from the Biebrza basin area, where was
sampled a bottom of brown-moss peat, which developed
in isolated depressions and was not covered by gyttja. The
dates for the bottom layers of brown-moss peat in Kuwasy
and Lower Biebrza are 10,850±150 BP (Gd-10497) and
8450±150 BP (Gd-10491), respectively; localisation of
Kuwasy profile EO and the section was published by
¯urek and Dziêczkowski (1971). It cannot be excluded
that the beginning of peat accumulation in Lower Biebrza
is not connected with ground ice melting in substratum
but with rise of ground-water table or lake-water level in
the neighbourhood, since in the nearby situated profile
Stójka 14a (Oœwit, 1973) Late Glacial brown-moss peat
is covered by gyttja. Gyttja from the deep thermokarst
depression of Stare Biele, dated to 13,900±310 BP (Gd-
9503), is probably of later origin, since the pollen analysis
(Kupryjanowicz 1998 and 2000) point to the Older Dryas
period. Accordingly, the beginnings of mire formation in
the North-East of Poland varied, and ranged from Bölling
to Alleröd. It cannot be determined whether this initial
stage of peat formation is connected only with the melt-
ing processes and when it came to an end. Current state
of knowledge does not allow to choose any of alternatives
(Nowaczyk, 1994) represented by the Late Glacial
(Kozarski, 1963) and early Holocene periods (Stasiak,
1971; Seibutis, 1963).
Dry phases in mires
Approaching from the point of stratigraphy and
changes of peat decomposition degree, humidity changes
in Polish mires have not been dated in detail. Two recur-
rent surfaces in raised bog Bór nad Czerwonym (Podhale
Basin) were observed in Subboreal Period (Obidowicz,
1978). One highly decomposed layer connected with
Subboreal period was also found in a fen in the Biebrza
basin (Oœwit, 1973; ¯urek, 1970). Recently, 2-3 highly
decomposed layers situated one above the other have
been identified in the mires Stare Biele (Knyszyñska
Wilderness: ¯urek, 1996a) and Bia³e £ugi in southern

113
 TIME RECORD OF PALAEOHYDROLOGIC CHANGES IN THE DEVELOPMENT OF MIRES DURING ...
piedmont of the Holy Cross Mts (¯urek, 1996b). These
enable to undertake a test dating of dry periods and
humidity fluctuations recorded in peat.
In the shallow profile 21 in Bia³e £ugi mire (see
Table 1) both of two highly decomposed layers were dated,
resulting in the determinations 3480±80 BP (Gd-11211)
for the upper (in the depth of 95-100 cm) and 10,170±120
BP (Gd-10320) for the lower (depth 175-185cm) one.
In the profile 13, located some 100 m away from the
former one, the bottom layer in the depth of 315-320 cm
was dated to 10,880±250 BP (Gd-9498). Considering the
situation in the profile 14, initially, the age of the lower-
most part of the 4m deep succession could not be deter-
mined by the 14C. The dating of organic layers (humus with
sand) under the peat gave result 6940±750 BP (Gd-9508)
and surprisingly, the age of the bottom part of peat over
humus has been stated as 12,900±360 BP (Gd-14015).
In the profile 6A (¯urek, 2001a, not included in Table 1)
of this mire 2 cm thick organic layer from the depth of
212-214 cm, under the peat, was dated to 18,300±600 BP
(Gd-14020). Hypsometric differences between position of
bottom highly humified layers in the profiles 21 and 13
(ca. 1.5 m, Table 1) can be viewed as indicating subsid-
ence of the central part of the deposit in a Younger Dryas
as a consequence of the permafrost extinction.
The date 13,900±310 BP (Gd-9503, see Table 1) for
the bottom sample of detrital gyttja from the kettle hole
in northern bay of Stare Biele mire seems to be too early
when compared to the palynological investigations setting
the sample towards the end of Older Dryas (Kupry-
janowicz, 2000). In the 4m deep succession of forest and
sedge-moss peat deposit, three strata of highly humified
peat (with the decomposition degree of 60-70%) were
observed, the dating of which brought following results.
The lower layer of highly humified dark forest peat from
the depth of 170-180 cm located in north-western bay,
representing the earliest Atlantic drainage period, was
dated to 6420±60 BP (Gd-7748). The second drainage
period, reflected by highly humified clammy alder peat
in the central part of the mire (profile 7, Table 1), depos-
ited 120-130 cm under present surface, is set to 5310±100
BP (Gd-10377); it is the period, when terrrestrialization
of lakes and afforestation of the central part of the mire
took place. Profile 29 situated in western bay brought the
evidence of highly humified layer in the depth of 1.1-1.18
m, which was dated to 4480±130 BP (Gd-10388). In north-
western bay, within a small area of transition bog (sedge
moss coniferous forest Carici chordorrhizae – Pinetum)
10 m deep kettle hole was discovered. Here, where the
accumulation rate was three times higher in comparison
to alder swamp peat in the rest of the mire, three highly
humified forest peat layers originated in Neoholocene
were identified at 1.15-1.20, 1.8-1,9 and 2.45-2.55 m
below present surface. According to 14C dating, two ear-
lier dry stages took place around 4000±120 BP (Gd-
10321) and 2690±70 BP (Gd-11212), respectively; the
latest is dated back to 1700±210 BP (Gd-9506). Regard-
ing the palynological evidence, the earliest layer suffered
from the lack of material and therefore it can be only
stated that it is situated over Early Subboreal phase of
114
Pinus-Quercus (Kupryjanowicz, 2000), the second dry
period corresponds to Pinus-Carpinus-Betula phase; the
BP date of the latest dry phase seems to be a bit younger
than palynology would suggest. With the latest dry phase
corresponds value Gd-9497: 2190±130 BP, measured on
sample of highly decomposed deposit located in the depth
of 0.94-1.00 m within the profile 2, situated in the distance
of 130m from the kettle hole. Subatlantic period recorded
within the mighty succession of the kettle hole probably
began with moisten, sedge-moss fen associations sup-
planted alder carr. Dry conditions of the latest period
opened the area for alder-birch forest.
In the cotton-grass bog peat of mire Machnacz an evi-
dence of distinct dry period is represented by layer in the
depth of 138-148 cm, dated to 4040±50 BP (SRR-3176,
Table 1); in the layer hummock sphagnum and pine
needles dominate (Haslam, 1987). Given the higher de-
composition of peat and distinct increase of the humus
content observed, Haslam showed that dry phases occur
also at the levels of 136 cm, 107 cm and 96 cm under
present surface.
In Biebrza basin, highly humified layers were dated at
three sites. Profile Stójka 14a in the East of lower Biebrza
Basin (not included in Table 1) incorporated, at the depth
of 95-105 cm, a layer of osier peat that was connected with
Subboreal period in the early seventies (Oœwit, 1973). In
the vicinity a profile with rather mighty, highly humified
layer situated a little deeper (112-130 cm) has been
sampled. Two radiocarbon dates, Gd-7826: 5110±60 BP
and Gd-7825: 2810±60 BP, obtained for the bottom and
the top of this layer show that in Subboreal period peat
accumulation process was interrupted or was very slow
indeed, and later, for the final phase of Subboreal, just
decomposition is indicated.
Another evidence of dry phase represents highly hu-
mified dark layer, found in the depth of 150-160 cm, in
deep sedge-moss fen peat of Klimaszewica. Entering of
hummock sedge Carex paradoxa and reed communities
to Caricetum diandre community attest to drainage. The
dating of decomposed peat at 145-152 cm giving the re-
sult of 7150±80 BP (Gd-10492) brought evidence of the
earliest Atlantic dry phase in this region.
Regarding situation of highly decomposed layer and
its thickness, the Kuwasy profile is essentially the same as
the profile 21 from Bia³e £ugi, what is shown also by date
Gd-7827: 3650±50 BP, measured on sample coming from
the bottom of forest peat at the level of 95-100 cm. While
drainage in the Biebrza area caused afforestation with
alder, in Bia³e £ugi it was cotton-grass raised bog com-
munity that entered into moss-sedge association of the
transition bog.
As for the sample collection is concerned it should be
stated that, unless highly decomposed layer was not thick
some 5-10 cm, it was sampled as a whole and in this case
an average age was received, without an opportunity of
determining the length of period when peat formation was
hibernated. Exceptionally, the discussed type of layer was
outstandingly mighty, namely in sediments of Lower
Biebrza mire, where 18 cm thick, highly humified stratum
enabled to take samples from its top and the bottom;
 S. Zurek et al.
radiocarbon dating of these samples showed that there
had been a large hiatus of some 2300 years in the local
peat accumulation. Furthermore, more detailed informa-
tion on rate of peat accumulation processes were received
when dates for peat under and over highly decomposed
layer were determined. In the vicinity of the profile 21 in
Bia³e £ugi mire, highly decomposed layers of which were
dated to 3480±80 and 10,170±120 BP (see Table 1), re-
spectively, almost no interruption occurred (8890±140
and 8750±150 BP), or, during later development, its du-
ration could have been as long as 3840 years, from
6470±80 to 2630±90 BP. In the profile 14 representing
the deepest spot of this mire, indices for some 620
BP-years long interruption were gathered (2450±90,
1830±100 BP). So long stagnation in the accumulation
of peat as shown by dates for the profile 21 (approx. 6000
years) from the shore part of Bia³e £ugi mire is even more
difficult to explain, when we consider that some 300 m
away it lasted only some 600 years. It is possible, that
Subboreal peat layer was burnt as a consequence of mire’s
fire.
Peat formation of Maliszewskie Lake
From the shore of Maliszewskie Lake (Wizna mire,
see Fig. 1), a sample of detrital gyttja indicating a drain-
age phase and lowering of the water table (connected with
the local peat formation; ¯urek, 1978 and 1986) was sub-
mitted for dating. The first result of the gyttja dating (Gd-
4020: 3340±120 BP) from this reference site of north-
eastern Poland is questionable, because of probable con-
tamination and rejuvenation of the deposit (Balwierz and
¯urek, 1987). In the synthetic study on the palaeo-
hydrology of Polish lakes and mires (Ralska-Jasiewiczowa
and Lata³owa, 1996) a hiatus spanned between 3500 and
7000 years BP was suggested for this profile. Dating of
dark, detrital gyttja, located approximately 10 cm lower
than in other profiles (205-212 cm), gave result 5720±110
BP (Gd-10490) connecting thus the local drainage period
towards the end of Atlantic period, what has already been
shown by measurement TA-10077: 5170±100 BP (¯urek,
1986). It seems that hiatus in so long period of time is
absent - derital-calcareous gyttja from level 140-145 cm
was dated to 4820±100 BP (Gd-4334). Temporary results
of pollen analysis of the detrital gyttja sediment (205-
212 cm) also point to the boundary of Atlantis and Subbo-
real periods (Balwierz, personal communication).
Wet phases in mires
Principal indicators of rise of the ground-water table
are decrease of peat decomposition degree, retreat of
trees and shrubs, increase of reeds and sedges populations,
and finally, submerging of the peat deposit.
The latest phase of increase of moisture appeared in
the vicinity of Góra Strêkowa. Peat from the old riverbed
exposed by lateral erosion of the channel was covered by
sandy alluvial loam dated to 1430±60 BP (Gd-1727;
¯urek, 1987). Climatic change leading to more humid con-
ditions caused avulsion of the river channel. Oaks found
in the river deposit of upper Narwia at Strabla (Czeczuga,
1969) and at Niewodów near £om¿a (Musia³ and
115
Straszewska, 1988) were felled at this time (1470±50 and
1420±130 BP). In the channel zone of Moczarze area
(Lower Biebrza basin), erosions and flows caused that
around 1460±100 BP (Gd-2302) mud formations started
to accumulate over sand-muddy sediments. Wet phase
began little earlier, because from around 1520±70 BP
(Gd-1820) peaty accumulations were formed in the shore
zone of shallow raised bog in the environs of Wieczorki
village (neighbourhood area of Maliszewskie Lake). Wet
phase marked by increase of hollow sphagnums (Sphag-
num cuspidatum, Sphagnum recurvum) at raised bog in
Machnacz was dated to 1120±50 BP (SRR-3175; Haslam,
1987). Haslam‘s study (1987) that dealt with 18 sites of
mires from western Ireland to north-eastern Poland al-
lowed to establish the pattern of climatic change during
Subboreal and Atlantic periods (Barber, 1993). From
works on wet phases recorded abroad we would like to
mention here article of Blackford and Chambers (1991)
pointing to distinct decrease of peat decomposition de-
gree in the blanket mires of Ireland and Great Britain
in1400-1300 BP.
After 2810±60 BP (Gd-7825) the evidence of profile
Stójka in Lower Biebrza region shows increasing amount
of reed contemporarily with the birch decrease down to
25%, and peat decomposition degree going almost up to
50%. Similar situation was noted in the profile Stare Biele
1 (¯urek, 2000). Here, after 2690±70 BP alder forest re-
treated and bryales appeared, with birch and reed remains,
i.e. sedge-moss shrub fen with constant and abundant
water supply developed.
In the shore profile of Maliszewskie Lake, over dark
detrital gyttja dated to 5170±110 BP (TA-1077; ¯urek,
1986) grey-brown detrital-calcareous gyttja was accumu-
lated, and in the upper whitish calcareous gyttja, indicat-
ing rapid rise of the lake water table, was present. Detri-
tal-calcareous gyttja from the depth of 140-145 cm was
dated to 4820±100 BP (Gd-4334), so wet phase began
around 5000 BP and could have lasted until around 4700-
4500 BP when in the profiles 1 and 29 of Stare Biele (see
Table 1) dry phases occurred. Similarly to Stare Biele, in
the kettle hole at Machnacz mire (Bia³ostocka Plateau)
after phase of moss-fen mire, with moss and low sedge,
supplied with constant, moderate ground-water inflow,
tall-sedge fen phase with dominating reed and tall sedge
began to develop (¯urek, 1992). Surface water, connected
with increased precipitation, and water inflow from little
catchments supplied the mire. This moist phase lasted
around 7300±130 BP (Gd-10494), what is in agreement
with gyttja of Maliszewskie Lake, appearing over the
sedge-moss fen peat dated to 7440±150 BP (Gd-2086).
The earlier wet period is related to the beginnings of
Boreal period (¯urek, 1986). Planting mires of central
Wizna with shrubs and lowering of water level were dated
to 9270±120 BP (Gd-2100). Later rise of water level,
decrease of peat decomposition degree and spread of low
sedge Carex lasiocarpa resulted from abundant ground-
water inflow. In the profile 9 of Stare Biele, the layer of
gyttja covering the sedge-moss fen peat dated to
9010±120 BP (Gd-10493) testifies to increasing of water
level as well. Uplift of water level during the initial
 TIME RECORD OF PALAEOHYDROLOGIC CHANGES IN THE DEVELOPMENT OF MIRES DURING ...

Younger Dryas can be reflected by presence of peat with
gyttja over highly decomposed layer dated to 10,880±250
BP (Gd-9498) in the profile 13 of Bia³e £ugi mire and by
accumulation of brown-moss peat in Kuwasy profile,
which began around 10,850±250 BP (Gd-10497). It is to
be added that the presence of peat with gyttja was stated
only according to macroscopically observations and
should be confirmed by the pollen analysis.
5. PALAEOHYDROLOGIC CHANGES IN NORTH
PODLASIE LOWLAND AND THE HOLY CROSS
MOUNTAINS IN LATE GLACIAL AND HOLOCENE
It seems that certain phenomena observed in the
stratigraphy of mires, particularly changes of peat decom-
position degree and botanical taxa spectrum, can be used
to determine hydrologic conditions in the past and to re-
construct succession of dry and wet phases. As for chro-
nology, radiocarbon dating of peat layers should be con-
firmed by pollen analysis. It may happen, however, that
14
C dates are in a strong disagreement with results of pa-
lynological investigation, being earlier or later than dat-
ing suggested by pollen spectra. Such case of major dif-
ference represent set of radiocarbon determinations for
samples from profile Machnacz III (Kupryjanowicz, 1994).
M. Kupryjanowicz suggested that the situation could be
explained by contamination caused by using a small-di-
ameter corer. According to him, sampling with a help of
corer with bigger diameter decrease probability of con-
tamination during sampling distinctively.
The radiocarbon dating of highly decomposed peat
layers has enabled to state approximate duration of dry
phases (Fig. 2A, after ¯urek and Pazdur, 1999, changed),
namely: in Subatlantic period 1700-2200 BP; in Subboreal

WET AND DRY PHASES IN MIRES OF EASTERN POLAND

A (¯urek, Pazdur, 1999, changed)

wet

dry

Lake-levels in Northern Poland

B (Ralska-Jasiewiczowa,1989; after Wojciechowski, 1999)

high

low

Wet and dry phases in raised bog Pesansuo in South-Western Finland

C (Ikonen, 1993)

wet

dry

H/Ho
1.2 Changes of relative depth of the Lake Goœci¹¿
D (Pazdur et al., 1995)
0.9

0.6

0.3

Lake levels in the Jura lakes

E (Magny, Ruffaldi, 1995; after Wojciechowski, 1999)
ONOZ 3
PETIT PETIT GRAND
CLAIRVAUX BOURGET PLUVIS CHALAIN MACLU CERIN JOUX REMORAY ONOZ 2
MACLU

Fig. 2. Correlation between

wet and dry phases in mires
of Eastern Poland and other
changes of climatic features
during Late Glacial and
0 1000 2000 3000 4000 5000 6000 7000 8000 9000 10000 11000 Holocene in Poland, Finland
Conv. Age [BP] and France.

116
 S. Zurek et al.
period 2600-2800 BP, 3400-3700 BP, ca. 4000 BP and
4500 BP, in Atlantic period 5100-5700 BP, ca. 6400 BP and
6900-7100 BP; at the end of Preboreal 9200-9300 BP; at
the beginning and at the end of Younger Dryas ca. 10,100
and 10,900 BP. On the other hand, wet phases can be ap-
proximately marked, according to the presented evidence,
as follows: the middle (1100-1400 BP) and the beginning
(2100-2600 BP) of Subatlantic period, the beginning
of Subboreal period (4700-5000 BP), in Atlantic period
7300-7500 BP, the end (8000-8400 BP) and the beginning
of Boreal period (8800-9200 BP). In Younger Dryas
water table was raised during its earlier stage (10,500-
10,850 BP).
Moisture changes plot for north-eastern Poland is in
good agreement with the results for lakes and mires in
Poland plotted in Figure 2B, elaborated by Ralska-
Jasiewiczowa (1989; Starkel, 1990; Ralska-Jasiewiczowa
and Lata³owa, 1996).
Good agreement is apparent also for the moist phases
up to 3 ka BP as recorded in the sites of north-eastern
Poland and raised bog Pasänsuo (Fig. 2C) in south-west-
ern Finland (Ikonen, 1993). Dry and wet phases were dis-
tinguished here according to presence of rhizopod
Amphitrema flavium, and 6 m long profile was dated by
means of radiocarbon in the way that every 5 cm of suc-
cession was sampled (120 dates). The divergence refers
periods 3400-3700 BP, 4700-5000 BP and 5200-5700 BP.
Similar agreement refers to high and low water level
noted in Goœci¹¿ Lake (Fig. 2D; Pazdur et al., 1994; Pazdur
et al., 1995), Biskupiñskie Lake (Niewiarowski, 1995;
Starkel et al., 1996) and Kórnik-Zaniemyœl Lakes
(Wojciechowski, 1999) sediments. High water levels in
both regions are connected with the beginning of
Subboreal and beginning of Subatlantic periods. Low
water levels occurred at the end of Preboreal period, in
the beginning and at the end of Atlantic period and in
Subboreal period. Relatively good coincidence of high and
low water-level stands with Polish and French Jura lakes
(Fig. 2E; Magny and Ruffaldi, 1995) was shown in Fig. 2.
CONCLUSIONS
It should be noted that changes stated in mires sedi-
ments, especially changes in peat decomposition degree
and botanical composition exploited to determine hydro-
logic changes in the past, especially to reconstruct of dry
and moist phases in the Late Glacial and Holocene. Com-
parison of wet and dry phases reconstructed on basis of
mires sediments from Eastern Poland are generally in
good agreement with periods of high and low water level
stands observed for Polish lakes, especially Goœci¹¿ Lake
and lakes from Northern Poland. The disagreement be-
tween wet and dry periods pattern recorded in the Polish
mires and the one reflected by the sediments of raised bog
Pesänsuo in Finnland is observed for the time horizon
prior 3 ka BP.
To conclude, authors‘ forthcoming research in the field
of reconstruction of time scale for wet and dry periods
pattern during the Holocene on the basis of radiocarbon
dating is to be focused on exploiting of statistical
117
methods for analysis of large sets of 14C dates for peat and
gyttja from various geographical regions.
ACKNOWLEDGEMENTS
The interpretation of radiocarbon results for sedi-
ments of Polish mires have been sponsored by the grant
from Scientific Research Committee No 6 P04E 007 17
and is continuation of earlier formulated problem in the
frame grant No 6 P04E 026 10.
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 GEOCHRONOMETRIA Vol. 21, pp 119-128, 2002 – Journal on Methods and Applications of Absolute Chronology

CHRONOSTRATIGRAPHY OF LATE PLEISTOCENE

FLUVIAL DEPOSITS IN THE WIS£OK RIVER VALLEY
BETWEEN RZESZÓW AND £AÑCUT,
SOUTH POLAND

PIOTR GÊBICA1, ANDRZEJ BLUSZCZ2, ANNA PAZDUR2 and KAZIMIERZ SZCZEPANEK3

1
Institute of Geography and Spatial Organisation, Polish Academy of Sciences,
Œw. Jana 22, 31-018 Cracow, Poland
2
Silesian University of Technology, Institute of Physics, Department of Radioisotopes,
Krzywoustego 2, 44-100 Gliwice, Poland (e-mail: pazdur@zeus.polsl.gliwice.pl)
3
Institute of Botany, Jagiellonian University, Lubicz 46, 31-512 Cracow, Poland

Key words
words: Abstract: This paper presents results of absolute dating of alluvial sedimentary series form-
ALLUVIAL SEDIMENTS, ing a rendzina terrace (higher floodplain) 7-8 m high above the Wis³ok River channel and
WIS£OK RIVER VALLEY, a sandy terrace 8-10 m high in the Subcarpathian Pradolina section of the Wis³ok River valley.
RADIOCARBON DATING, The organic mud infilling fossil depressions (palaeochannels?) in the lower part of the rendzina
LUMINESCENCE terrace have been dated by the radiocarbon method to more than 38,500 BP. The organic
DATING, series occurring within the sandy terrace yielded three ages >36,000 BP. Results of palyno-
QUATERNARY logical analyses carried out on both sites indicate tundra or forest-tundra environments with
water-filled depressions at the time of organic sediments deposition. The top of the 8-10 m
high sandy terrace is built of fluvial sands and eolian cover sands with dunes in the upper-
most part. Their age has been established by means of the OSL method to 11.2±0.9 ka BP.
The younger alluvial inset fill is formed of sands and silts with involutions occurring under
Holocene muds. They were deposited by a braided river during the Upper Plenivistulian as
indicated by two other OSL dates of 22.2±2.2 ka BP and 14.0±1.5 ka BP. Within the rendzina
terrace the youngest series of Vistulian age is built with peats and silts, infilling the wide
depression at the foots of sandy hillocks, dated to about 11,800 BP.

1. INTRODUCTION
The geological survey of the Wis³ok River valley
started at the beginning of the 20th century when
Friedberg (1903) elaborated Rzeszów and £añcut sheets
of the Geological Atlas of the former Austrian Galicia.
Friedberg (1903) described grey-blue clays underlying
glacial gravels in the lower part of rendzina terrace in
Terliczka and £ukawiec. He assigned them to the Young
Pleistocene or early Holocene period. Klimaszewski
assigned the middle terrace (up to 20 meters above the
river bed) loess-covered to the Middle Polish (Saalian)
Glaciation, and the lower-lying terrace (up to 10 meters)
with overbank loams in the top to the Last Glaciation. The
structure and age of the Wis³ok terraces in Rzeszów were
studied by Jahn (1957), Laskowska-Wysoczañska (1971)
and Starkel (1972 and 1980) who dated the higher terrace
sediments bearing a cover of loess or dunes to the North
Polish (Vistulian) Glaciation. According to Jahn (1957)
and Starkel (1960) the 6-8 m high rendzina terrace is ap-
parently inserted in the loess-covered terrace. Starkel
(1960) provided evidence for the Holocene age of the
rendzina terrace in Rzeszów, which comprise alluvial in-
set fills of different age. It also hides remnants of older
alluvia as, for example, documented by the profile in
BrzeŸnica in the neighbouring Wis³oka River valley, where
paleochannel deposits have been dated to between 46 and
36 ky BP (Mamakowa and Starkel, 1974). Starkel (1980)
cited a date of 43.9±2.1 ky for peat sample taken by him-
self in £ukawiec and obtained by M. Geyh in 1975.
Several years ago, in the frame of the Detailed Geologic
Map of Poland 1:50,000 project, geological mapping of
the Rzeszów, £añcut and Jaros³aw sheets has been un-
dertaken. Results of geological mapping have been pub-
lished in the form of several notes and presented during
the VI Conference on Stratigraphy of Pleistocene in
Poland, Czudec 1999 (Wójcik et al., 1999; Zimnal, 1999).
 CHRONOSTRATIGRAPHY OF LATE PLEISTOCENE FLUVIAL DEPOSITS...

During spring freshets of the year 2000, with the high-
est water level reaching 5 m above the river bed, Wis³ok
River made numerous undercuts in banks in the section
behind £¹ka where the river runs within the Subcar-
pathian Pradolina. When floodwaters subsided, P. Gêbica
found in several new exposures in the lower part of the
rendzina terrace a cohesive layer of silty clay and organic
mud, truncated in the upper part and covered with
younger alluvial series. A similar organic series and silts
were found nearby in Czarna-Podbór, in the open sand
pit located on the higher 8-10 m terrace.
Undertaken researches aimed at finding an age of dif-
ferent sequences of Vistulian fluvial sediments. Geomor-
phological mapping of the Wis³ok River valley bottom
between Rzeszów and £añcut was performed by P. Gêbica.
On the same occasion a number of accessible exposures,
presenting different stratigraphical units was profiled.
Information related to the range and thickness of terrace
sequences have been supplemented with data obtained
through geological drillings and taken from rich archive
documentation on earlier boring projects. The fieldwork
was also an occasion for taking samples for palynological
and granulometric analyses, and for radiometric dating.
Radiocarbon dating was performed on samples of peat
and organic silt sediments while OSL (optically stimulated
luminescence) dating was made on samples of mineral
sediments.
2. GEOMORPHOLOGICAL
AND GEOLOGICAL SETTING
The Wis³ok River beyond Rzeszów flows within an
erosional depression of the Subcarpathian Pradolina. The
pradolina is distinctively bordered from the south and the
north (Fig. 1). To the south an edge of the Kañczucka
Plateau (220-280 m a.s.l.) rises, which is covered with a
sequence of alluvial and glacial sediments, frequently
overlain by loess, deposited on a Miocene clays
(Laskowska-Wysoczañska, 1971; Zimnal, 1999). The edge
of the Kolbuszowski Plateau constitutes the north border.
It is built with Miocene clays, covered with preglacial
alluvial sediments, fluvioglacial sands, and glacial till from
the Sanian 2 (Elsterian) Glaciation. In the Subcarpathian
Pradolina near Jasionka at the elevation of 210-213 m a.s.l.
fluvioglacial deposits and washed glacial till cover an in-
terstadial organic series from the Sanian 2 Glaciation
(Laskowska-Wysoczañska, 1971). The bottom of the
Wis³ok River valley is terraced and filled with alluvia of
the thickness up to 20 m. Between Rzeszów and
Trzebownisko, a slightly inclined terrace plain ranges at

Fig. 1. Geomorphological map of the Wis³ok River valley between Rzeszów and £añcut:
1 – PeriCarpathian Loess Plateau, 2 –- Kolbuszowski Plateau, 3 – fluvioglacial level from the Sanian 2 Glaciation, 4 – alluvial terrace
from the Middle Polish Glaciation?, 5 – loess-covered terrace plain from the Vistulian Glaciation, 6 – sandy terrace 8-10 m high, 7 –
alluvial fan of the Vistulian age, 8 – dune ridges, 9 – higher floodplain (rendzina terrace) 7-10 m high, 10 – flatbottomed depressions
(floodbasins), 11 – lower floodplain 3-5 m high, 12 – alluvial fan of Holocene age, 13 –- paleochannel system, 14 – traces of braided
river (Late Vistulian age), 15 – peatbogs, 16 – erosional edges below 10 m, 17 – erosional edges above 10 m, 18 – geological transect
with borehole numbers, 19 – excavations, 20 – roads, 21 – railway.

120
 P. Gêbica et al.
the elevation about 20 m above the Wis³ok River level.
Its upper part consists of dozen-metre-thick loess, and its
lower part contains alluvial sands with organic mud in-
sets and gravels lying on the Miocene clays. These depos-
its are 20 m thick and they date to the Vistulian Glacia-
tion (Jahn, 1957). Along the left border of the valley, at
the height of 8-13 m above the Wis³ok River channel,
a sandy terrace stretches, 0.5 to 1.5 km wide, with a wind-
blown sands on the top. In places, undercut by
paleomeanders, it is separated from the rendzina terrace
by a 1-2 m high edge. Circular, wet depressions
(thermokarstic?) and natural levees with wind-blown
sands on the top have been profiled on the terrace sur-
face. The contemporary bottom of the Wis³ok River val-
ley, 4-6 km wide, is occupied by a Holocene rendzina ter-
race, which is cut 10 m deep in the vicinity of Rzeszów
and 7-8 m deep near £añcut (Fig. 1). It forms a higher
level of a floodplain that currently is not flooded even
during the highest freshets. It forms an alluvial fan be-
yond Rzeszów, with several abandoned (due to avulsion
processes) palaeomeander systems of the Wis³ok River
and its tributary Czarna River. The best known is a nar-
row and sinuous paleochannel system called Stary Wis³ok
abandoned after one of catastrophic floods in the half of
the 18th century (Strzelecka, 1958). The rendzina terrace
is built of gravels with sands in the lower part, and sands
with alluvial loams and 2-4 m thick clays in the upper part.
In the £¹ka locality a Pleistocene sandy terrace occurs in
isolated patches and it rises 1-3 meters above the flood-
plain (Fig. 1). This is probably a fragment of an alluvial
fan formed by the Wis³ok River during the Vistulian time,
which is indicated by an archaeological findings of
Mesolithic settlements (Czopek and Podgórska-Czopek,
1995). The lower level of the floodplain makes narrow
bench of swampy meadow terrace at the elevation of
3-5 meters above the river channel, being several tens to
500 m wide. It is covered with meadows and brush and it
is flooded almost every year during higher freshets. It is
mainly built of sandy loams overlying sands with gravel.
It has probably been formed during the last 150-200 years,
similarly like the swampy meadow terrace of the San River
(Szumañski, 1986). The channel of the Wis³ok River un-
derwent partial regulation in the beginning of the 20th
century, but it is not embanked. The present width of the
river is about 25-35 m.
3. SITE DESCRIPTIONS
£ukawiec-1
A very interesting profile, exposing two series of allu-
vial deposits (Figs 1 and 2), was found during the geomor-
phological mapping of the 7 m high terrace on the right
bank of the Wis³ok river. The lower series consisted of
fine sands covered with alternately stratified silt and yel-
low-olive sand. In the upper part of the sequence sand
distinctively graded into blue silty clays which in turn
gradually graded into organic silts and peaty mud of 0.6
metre thickness. At the contact between the organogenic
layer and the underlying silts and sands numerous sedi-
mentary involutions and cryogenic fissure structure filled
121
with organic material, had developed. The top of orga-
nogenic series has been truncated and covered with the
younger series of alluvial sediments of 5 m thickness. This
younger series consists mainly of sands with coarse gravel
(channel deposits) and sets of cross-bedded sands with
sandy silt insets (meander point bar deposits) and of over-
bank alluvial loams in the top. The peaty mud sample taken
at the elevation of 2 m above the present water level in the
river channel yielded the radiocarbon age >38,500 BP
(Gd-15157). Pollen analyses made on eight samples taken
from peaty mud organic silts in the profile £ukawiec-1
(Fig. 3) revealed large amounts of herbaceous plants
(NAP), particularly Cyperaceae and grasses (Poaceae).
Tree pollen percentage reaches almost 25% of the total
pollen count only in the top sample; in other samples it
varies between 9.8% and 20.2%. The taxonomic compo-
sition of samples is not much diversified. Among the trees
only pollen of common pine (Pinus silvestris) and of stone
pine (Pinus cembra) are abundant in all samples. Among
the bushes relatively high scores have been recorded for
dwarf birch (Betula nana). A few pollen grains of willow
(Salix), sporadic pollen grains of alder (Alnus viridis) and
abundant colonies of Pediastrum algae have been found.
They indicate the presence of shallow water depressions,
at least periodic. The results enable stating that the most
characteristic feature of the landscape of the area sur-
rounding this site was a prevailing number of open com-
munities of herbaceous plants. Most of all they were com-
munities of wet and waterlogged habitats. There were
probably some other types of plant communities, besides
grass-sedge ones, where dwarf birch shrubberies, alder,
willow and brown moss grew together with other plants
of dry non-forest steppe-tundra sites (Artemisia, Chenopo-
diaceae and Helianthemum). Trees could by found, if any,
sparsely in small assemblages or in the Wis³ok River val-
ley. Palynological data and results of radiocarbon dating
suggest that sediments were deposited in cool climatic
conditions during the older part of Pleniglacial of the
Vistulian glaciation. £ukawiec yielded yet another radio-
carbon date made on peat sampled by L. Starkel from the
layer forming rapids in the Wis³ok River bed, exposed on
the right edge of the terrace (Starkel, 1980). It is difficult
now to point the place from which the dated sample de-
rived. The age of peat, as obtained in 1975 by M. Geyh
and equal to 43.9±2.1 ky BP (Hv-6388), is indicative of
the interstadial series (interpleniglacial) of the last gla-
ciation (Gradowski and Nalepka, 1985; Starkel, 1980).
Czarna-Podbór
At the distance of some 0.5 km NNE of £ukawiec pro-
file, at the border of Czarna-Podbór hamlet, there are
several open sand pits. Sand pits are located on the ter-
race plain elevated about 8-9 m above the river bed and
up to 1.5 km wide. It is bordered on the floodplain by
a distinct edge of the old paleochannel up to 2 m high (Figs
1 and 2A). The terrace surface is slightly undulated with
flat swellings and depressions not higher, or deeper, than
2 m. Dune ridges, 5-10 m high, occur at higher elevations
and low levees occur in places closer to the edge of the
terrace. To the west of the biggest sand pit the terrace is
 CHRONOSTRATIGRAPHY OF LATE PLEISTOCENE FLUVIAL DEPOSITS...

11.2±0,9 ka BP

Fig. 2. Radiocarbon dating results and the cross-section through the sandy terrace (8-10 m) in Czarna-Podbór and the right bank
terrace (7 m) in £ukawiec site:
1 – Miocene, 2 – sand with gravel, 3 – sands, 4 – stratified sands with fine gravels (eolian cover sands), 5 – sandy silts, 6 – muds
and clays, 7 – stratified muds and sands disturbed by periglacial structures, 8 – peaty muds, 9 – organic silts, 10 – alluvial loams,
11 – fossil soil, 12 – Holocene soil 13 – involutions (drop soils) and frost wedges.

cut down by a valley of a small stream, the bottom of which
is covered with flood muds. In the biggest sand pit belong-
ing to Mr. Kazimierz Jeziorek from Medynia £añcucka
the layer of silt with organic matter was found at the depth
of 5 m below the terrace surface. The structure of the ter-
race was documented by 23 archival drillings made on the
sand pit area of 0.25 km2 . Sampling was made by three
additional geological drillings using “Geomeres” derrick
and samples for palynological and radiocarbon analyses
were taken.
Four basic members of deposits have been recognised
in the terrace structure (Fig. 2A). At the depth of 10-13 m
a sandy gravel cover, 2-5 m thick, lies on Miocene clays.
Above that there is a member of silty and sandy clays
bedded with organic silts and peaty mud, 1.5 to 2 m thick,
filling fossil depressions (paleochannels?) cut in the chan-
nel alluvia. The top of the terrace consists of dusty sands
truncated by coarse sands with an admixture of gravel,
1-3 cm size, with a pavement in the bottom. The thickness
of the upper members of the deposits is 3-4.5 m. Samples
for dating have been taken from two selected drilling sites.
A drilling core sample coming from an upper layer of
peaty mud lying at the height of 4 m above the river bed
in the Czarna-Podbór 3 profile, yielded an indefinite age
>36.6 ka BP (Gd-15148), and the second sample of peaty
mud from a layer lying 1 m below gave also an indefinite
age >36.2 ky BP (Gd-15155). Another peaty mud sample
taken from the Czarna-Podbór 1 drill core, 3.7-3.9 m
above the Wis³ok river bed was dated to >36.4 ka BP
(Gd-15154). The age of the sampled deposits corresponds,
probably, to the older part of the Middle Plenivistulian,
similarly to the profile in BrzeŸnica upon Wis³oka River
(Mamakowa and Starkel, 1974; Mamakowa et al., 1997)
or is much older.
Wola Ma³a
The site Wola Ma³a near £añcut, on the right bank of
a big southward bent meander of the Wis³ok River, re-
veals an interesting sequence of sediments (Figs 1 and 2B).
Below the overbank alluvial loams of Holocene age, sand
and silt layers are exposed, part of it being disturbed.
Holocene overbank deposits are represented by massive
clays interbedded with silts of the total thickness of 3.5 m.
A vertical profile exposes two sequences of deposits
below the alluvial loams. The lowermost part of the pro-
file, shows mixed sands with single gravels and silty sands
with involutions (overbank deposits). The top of these
sediments is cut and covered with another layer of cross-

122
 P. Gêbica et al.

Fig. 3. Pollen diagram from the £ukawiec-1 profile.

11.2±0,9 ka BP

Fig. 4. Schematic cross-section of the northern margin of the Wis³ok River valley floor near Czarna and £ukawiec:
1 – sands with gravels, 2 – fluvial sands, 3 – stratified fluvial sands with eolian cover sands in the top of the terrace, 4 – silty sands
5 – unstratified eolian sands, 6 – stratified sands and silts disturbed by involutions, 7 – laminated muds and sands, 8 – clays and
muds, 9 – alluvial loams, 10 – peaty muds, 11 – organic silts, 12 – involutions and frost figures.

123
 CHRONOSTRATIGRAPHY OF LATE PLEISTOCENE FLUVIAL DEPOSITS...
bedded sands with fine gravels and laminated silts (flood-
plain deposits). Layers of sands and silts in the top part
are inclined and subjected to sliding.
Single sand wedge being up to 0.5 m long and trun-
cated at the top, frost fissure and small faults caused prob-
ably by ground subsiding, were observed in the dusty
sands. Abundant involutions, described as drop soils were
found at the border between silts and sands. This type of
structures usually develops as a result of differences in
sediment density and processes of gravitational liquida-
tion of plastic masses of water-saturated sediment and
probably takes place during permafrost degradation
(French, 1996; Eissmann, 1997). Two samples taken from
this profile have been dated by the single aliquot optical
dating (SAR OSL) method. The sample WM-1 taken
from an undisturbed sands lying at the height of 2 m above
the water level in the Wis³ok River channel, and below
the previously described involution structures, gave an age
of 22.2±2.1 ka BP (GdTL -627). The second sample
WM-2, taken from laminated silt lying directly below
Holocene alluvial loams, 4 m above the river water level,
was dated to 14.0±1.5 ka BP (GdTL-628). Thus, the dated
alluvial series corresponds to the Upper Plenivistulian
and it is younger than sediments described in £ukawiec
and Czarna localities.
D¹brówki
On the left bank of the Wis³ok River, in the village of
D¹brówki, there is a small, sandy hillock developed on
a sandy plain. Its relative height is 3.5-4 metres and 13.5
meters above the Wis³ok River bed (Fig. 1). To the north
of this hillock, and slightly higher, there are dune ridges
up to 20 meters high. Due to exploitation of sands, the
western part of the hillock and the top part of the terrace
plain have been exposed, enabling insight into the struc-
ture of both forms down to the depth of 7 m (Fig. 2B).
The lower part of the terrace is built of sands, gravels and
silts, while the upper one consists mainly horizontally lami-
nated silty sands. The hillock consists mostly of somewhat
coarser material, mainly fine- and medium-grained sands,
alternately laminated with thin layers of coarse-grained
sand and gravel up to 0.5 cm diameter. The lamination
ceases towards the top of the hillock and sands become
better sorted, with a Holocene soil developed in the top.
The small size of the hillock and alternating layers of sand
grains makes it similar to hillocks made of eolian cover
sands found on the Polish Lowlands (Nowaczyk, 1976).
Structures described above have been recorded in eolian
sands of contemporaneously developing dunes (Fryberger
et al., 1992) as well as in Pleistocene cover sands (Schwan,
1986; GoŸdzik, 1998). The sample of sand taken from the
bottom layer of the hillock, about 10 m above the Wis³ok
River level, has been dated by SAR OSL method to
11.2±0.9 ka BP (GdTL-626). This result points the Late
Vistulian (Younger Dryas ?) when eolian processes inten-
sified and sand was reworked by strong winds. These date
correlates well with numerous eolian series of dune and
cover sands dated in Poland (Nowaczyk, 1986).
124
£¹ka
On the rendzina terrace, to the south of the present
Wis³ok River bed, several boreholes gave insight into the
structure of the flat-bottomed depression surrounding the
sandy patches of Pleistocene terrace near £¹ka (Figs 1
and 2B). The structure of the wide depression consists of
peat, lying on sands with silts, clays, and alluvial loams in
the top. The radiocarbon dating of a sample from the
£¹ka-4 borehole (sample from the bottom of the peat
layer at the depth 3.25-3.30 m) gave the result
11,820±250 BP (Gd-15146). This means that the infilling
of the depression started in Alleröd, and peat, probably,
covers a fragment of a Late Vistulian alluvial plain of a
braiding river.
4. DISCUSSION OF 14C DATING RESULTS
The measurements of 14C concentration have been
performed in the Gliwice Radiocarbon Laboratory by the
gas proportional counting method (except for the Hv-6388
result which was obtained in the Hannover Radiocarbon
Laboratory). Conventional radiocarbon age of each sample
has been normalised to δ13C = -25‰, following the
Stuiver and Polach’s procedure (1977). One definite 14C
date (sample £¹ka-4, Gd-15146) was calibrated using the
Gliwice Calibration Program GdCALIB (Pazdur and
Michczyñska, 1989) and the calibration curve of Stuiver
at al. (1998). Table 1 contains the results of radiocarbon
dating as conventional radiocarbon ages (14C Age, BP)
and results of the calibration procedure in the form of the
narrowest 68% confidence intervals (Cal. Age, BP).
The results of radiocarbon dating fell at or behind
the limit of the applied method, except for £¹ka-4 sample,
which yielded a definite age. Considering the stratigra-
phical division of the Vistulian glaciation (Kozarski, 1991),
radiocarbon dates obtained for £ukawiec and Czarna-
Podbór profiles (older than 38.5 ka BP and older than
36.0 ka BP, respectively) mean that the respective organic
sediments from the two sites were deposited during the
older part of the Middle Plenivistulian (interpleniglacial).
The probable candidate is the Hengelo interstadial
(warm) period and an immediately earlier stadial period.
Palynological data suggest that studied sediments were
deposited under relatively stable conditions, during
a period without significant climate fluctuations. The low
percentage of tree pollen, reaching 25% at the best, to-
gether with the domination of open sets of herbaceous
plants may be interpreted as a result of relatively stable
climatic conditions of the colder period (stadial) imme-
diately preceding the Hengelo interstadial. Numerous
involutions and small frost wedges found at the contact
between organic deposits and underlying layers developed
under periglacial conditions are the other proofs support-
ing this hypothesis. It is also congruent with results of other
studies of Middle Plenivistulian fluvial series in the south-
ern part of Poland (Jersak and Sendobry, 1991; Superson,
1996) and in eastern part of Germany (Eissman, 1997;
Mol, 1997).
 P. Gêbica et al.

Table 1. Description of the samples and their radiocarbon and luminescence ages. Calibrated age range (Gd-15146) has been
determined at 68% confidence level using GdCALIB program.
14
Sample name C Age [BP] OSL Age
type of sediment Stratigraphy Lab. No. Cal. Age [BP] [BP]
£ukawiec-1 top layer of peaty mud,
peaty mud 2 m above channel water level Gd-15157 > 38,500
£ukawiec Peat from a bank +2100
43,900 –1650
peaty mud forming a riverbed bar Hv-6388
Czarna Podbór-3 top layer of peaty mud,
peaty mud 5 m above channel water level Gd-15148 > 36,600
Czarna Podbór-3 Layer lying 4 m
peaty mud above channel water level Gd-15155 > 36,200
Czarna Podbór-1 Layer lying 4 m
peaty mud above channel water level Gd-15154 > 36,400
Wola Ma³a WM-1 Layer lying 2 m
sand above channel water level GdTL-627 22,200 ± 2100
Wola Ma³a WM-2 Layer lying 4 m
laminated mud above channel water level GdTL-628 14,000 ± 1500
D¹brówka Layer lying 10 m
sand above channel water level GdTL-626 11,200 ± 900
£¹ka-4/3.25-3.30 m 11,820 ± 250
peat lower layer of peat Gd-15146 [14,050 ÷ 13,530]

5. DISCUSSION OF RESULTS OF OSL DATING l aliquot mass: ca 3 mg;

l test dose: 1.9 Gy;
Luminescence dating of three sediment samples has l preheat after test dose: 0 s at 160° C;

been made in the Luminescence Dating Unit of the De- l regenerative doses: 9.6, 19.1, 38.3 Gy;
partment of Radioisotopes, Institute of Physics, Silesian l Preheat after regenerative dose: 10 s at 220° C;

University of Technology, Gliwice, Poland. The OSL l OSL taken at 125° C during 1 s of green light

measurements have been done on coarse quartz extracts
(125-200 µ) applying a single aliquot regenerative dose
protocol (SAR) to obtain values of paleodoses absorbed
by grains. The respective dose-rate values have been cal-
culated from radioactivity of the sediment samples mea-
sured by means of high-resolution gamma spectrometry,
making appropriate corrections for sediment water con-
tents, etching of quartz grains in concentrated hydrofluo-
ric acid, and taking into account the cosmic dose-rate.
OSL of quartz aliquots have been measured with Day-
break 1150 automated reader equipped with a green light
source (halogen lamp based) and a beta source for “in-
place” irradiations. Irradiations, preheating and OSL
measurements were executed automatically in a one con-
tinuous run. A typical SAR measurement protocol was
employed with the following parameters:
(514±17 nm wavelength) excitation followed by 58 s long
bleaching and then 1 s excitation for recording a back-
ground signal (a total of 60 s of green light exposure)
Equivalent dose (ED) values have been calculated by
interpolation of the non-linear saturated exponential fit
to the laboratory growth points. Results of the laboratory
measurements and OSL dating are presented in Tables 2
and 3.
The single aliquot method is usually applied to a num-
ber of aliquots making it possible to investigate the dis-
tribution of luminescence ages of quartz grains within the
sediment. In this case aliquots consisted of many indi-
vidual grains so the interpretation of the distribution is
less straightforward. Nevertheless, it was shown that only
a few grains give actually rise to luminescence observed
from an aliquot, so the distribution should have similar

Table 2. Depth, water content, radioactivity and effective dose-rate for three samples.
Sample Depth Water content Activity [Bq/kg] Dose rate
[cm] (assumed) [%] 238
U 232
Th 40
K [Gy/ka]
Wola Ma³a WM-1 600 12±3 5.18±0.86 3.76±0.29 249.2±4.3 0.99 ± 0.08
Wola Ma³a WM-2 400 12±3 18.12±1.48 15.10±0.58 420.9±7.4 1.93 ± 0.14
D¹brówki D-1 400 12±3 5.38±0.77 3.32±0.26 182.1±4.1 0.90 ± 0.03

Table 3. Equivalent dose (ED) and OSL age values obtained for the dated samples.
Sample Number of aliquots EDOSL OSL Age
[Gy] [ka]
Wola Ma³a WM-1 10 22 ± 1 22.2 ± 2.2
Wola Ma³a WM-2 10 27 ± 2 14.0 ± 1.5
D¹brówki D-1 40 10.1 ± 0.7 11.2 ± 0.9

125
 CHRONOSTRATIGRAPHY OF LATE PLEISTOCENE FLUVIAL DEPOSITS...

features as the individual grain distribution but broader
and with larger “background”. Figs 5 to 7 show the re-
sults for individual aliquots transformed in such a way that
each point represents a single date. The abscissa of
a point is inversely proportional to the dating error ∆Ti
and its ordinate is proportional to the age value Ti less an
arbitrary value (usually chosen to be an average of ob-
tained ages) and inversely proportional to dating error.
This transformation leads to that points representing same
0 stated for this sample cannot be interpreted as the age of
-10
age lie on a straight line going through the point of origin
(0, 0) and the larger the distance from the origin, the more
accurate the date is. This type of plot helps better judg-
ment of dominant features of the age distribution and its
interpretation.
Samples WM-1 and WM-2 have relatively simple
distributions meaning that deposition of the sediment took
place after a moderately long exposure to light. The
sample D-1, on the contrary, shows a quite complex
distribution (being the reason why we decided to repeat
dating for 40 aliquots). The most probable reason for this
is that in the history of this sediment several episodes of
reworking and re-deposition occurred. The OSL date
the whole form. It is rather the last episode of more
intense reworking. This site will be a subject of further
investigations, including OSL dating of more samples with
an aim to shed more light on the origin and age of the
form.

6. CONCLUSIONS
22.2
Radiocarbon and luminescence dating (OSL) confirm
complexity of alluvial series of deposits of Middle to
-20 Upper Plenivistulian age, occurring in the Subcarpathian
pradolina section of the Wis³ok River valley bottom
between £¹ka and £añcut. A schematic section shows
locations of dated alluvial series and their probable spa-
0.0 1.0 2.0 3.0 4.0 5.0 tial extension along the bottom of the valley (Fig. 4). The
distinguished Vistulian series of sediments occupies
Fig. 5. Results of the SAR method dating of the sample WM-1. mainly the northern zone of the Wis³ok River valley. The
The plot presenting single dates is constructed in such way that contemporary channel of the Wis³ok River cuts into this
“equal age” points lie on the ray coming out of the point (0, 0).
1 series.
The distance along the horizontal axis is equal to while the The thick series of InterpleniVistulian sediments form-
Ti - T DTi
distance along the vertical axis is . The ray shows an age ing a sandy terrace, 8-10 m high, has been dated to be older
DTi
of 22.2 ka.

8
20
29

4 10

0 0

18

-4 14 -10

11.2

-8 -20
0.0 0.2 0.4 0.6 0.8 0.0 1.0 2.0 3.0
Fig. 6. Results of the SAR method dating of the sample WM-2. Fig. 7. Results of the SAR method dating of the sample D-1. The
The ray shows an age of 14 ka. three rays show ages of 11.2 ka, 18 ka and 29 ka.

126
 P. Gêbica et al.
than 36 ka BP. The oldest links of this series occurring in
the floor of the 7 m terrace have been dated to be older
than 38 ka BP. The problem that needs further research
are the genesis and age of the sandy formations covering
the InterpleniVistulian series. Undoubtedly, a part of the
uppermost formations of the sandy terrace is of eolian
origin; besides dunes, low hillocks are found, that are built
of eolian cover sands. A single OSL date obtained for
these sands points to the end of the Late Vistulian.
The alluvial series, built of sediments dated back to
22-14 ka BP is covered with Holocene alluvial loams.
Further to the south of the contemporary Wis³ok River
bed fragments of the Late Vistulian alluvial plain are
found side by side with younger alluvial fills of fluvial sedi-
ments connected with abandoned paleochannel system of
the Wis³ok River. This feature may be related to migra-
tion of the river bed towards the left edge of the valley
bottom.
ACKNOWLEDGEMENTS
One of the authors (P. Gêbica) wishes to thank Mr.
Kazimierz Jeziorek from Medynia £añcucka for allowing
surveying his sand pit and making boreholes, and Prof.
Leszek Starkel for discussions during the fieldwork on
sites within the Wis³ok river valley and during writing this
paper, and Mrs. Maria Klimek, M.Sc., for drawing the
Figures.
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 GEOCHRONOMETRIA Vol. 21, pp 129-136, 2002 – Journal on Methods and Applications of Absolute Chronology

RADIOCARBON DATED WOOD DEBRIS

IN FLOODPLAIN DEPOSITS OF THE SAN RIVER
IN THE BIESZCZADY MOUNTAINS

JÓZEF KUKULAK1, ANNA PAZDUR² and TADEUSZ KUC3

1
Department of Geography, Pedagogical University, Podchor¹¿ych 2,
30-084 Cracow, Poland (e-mail: jkukulak@wsp.krakow.pl)
²Department of Radioisotopes, Institute of Physics, Silesian University of Technology,
Krzywoustego 2, 44-100 Gliwice, Poland (e-mail: pazdur@polsl.gliwice.pl)
3
Department of Physics and Nuclear Techniques, University of Mining and Metallurgy,
Al. Mickiewicza 30, 30-059 Cracow, Poland (e-mail: kuc@novell.ftj.agh.edu.pl)

Key words
words: Abstract: Tree logs and smaller fragments of wood debris occur in floodplain alluvium
WOOD DEBRIS, (1-3 m above the river level) of the San river in the Bieszczady Mountains (Polish East
ALLUVIUM, Carpathians). The greatest accumulations of wood debris occur in the lower part of the allu-
RADIOCARBON vium, beneath a layer of sandy muds. The wood debris in these accumulations was dated by
DATING, HOLOCENE, radiocarbon method. The dates fall within the time interval 3270±70 BP to 103.7±1.1 pMC,
CARPATHIANS but most of them are from 17th to 19th century. The abundance of the wood debris in the allu-
vium is the result of its intense supply to the river channel, caused by deforestation and large
floods. The age of the wood accumulations corresponds to the phase of settlement in the upper
San valley in the 16th to 17th centuries. The older wood debris could be redeposited to the
young alluvium from older alluvial terraces.

1. INTRODUCTION of fluvial channels (Œrodoñ, 1952; Alexandrowicz et al.,

Wood debris is usually a subordinate component in
alluvial sediments and it usually widely varies in size. Large
buried logs and other coarse wood fragments (branches,
roots) usually focus the attention of researchers. Less vi-
sible is fine debris (leaves, bark, fruits and seeds) and this
is usually omitted in descriptions of alluvial sediments.
Dating of wood debris of all size provides an important
insight into the age of alluvium and the evolution of river
terraces. The most common methods used to date wood
debris are radiocarbon (14C ) dating and dendrochro-
nology.
Wood debris in alluvium of the Carpathian rivers
occurs mainly in depositional covers of Holocene terraces.
These are better preserved in foothill sections of valleys,
not so common in the mountain zone. They are most com-
mon immediately below the outlets of the valleys from
the Carpathians, e.g. in the valleys of the Wis³oka, Wis³ok
and San rivers ( Starkel, 1960 and 1996; Klimek, 1974;
Kalicki and Kr¹piec, 1991; Kr¹piec, 1992; Kalicki, 1997;
Nogaj-Chachaj et al., 1999). Their presence is commonly
considered as indication of climate fluctuations and oc-
currence of floods in the Carpathians or lateral migration
1981; Starkel, 1996 and 1999; Kalicki and Kr¹piec 1991;
Kalicki, 1991).
Geological studies in the Bieszczady Wysokie Moun-
tains (Polish East Carpathians) have revealed the presence
of abundant wood debris also in the mountane section of
the San river (Haczewski et al., 1998 and 2001). This is
accumulated only in floodplain sediments of the San river
and its tributaries, far upstream from the margin of the
Carpathians. They form a continuous horizon in flood-
plain sediments, on the top of older gravels and at the base
of the younger sandy mud (Kukulak, 2000). The accumu-
lation of this wood debris seems to be not exclusively
caused by a climatic factor.
This paper presents a description of wood debris in
Upper San river floodplain alluvium and presents the
results of its dating by the 14C method. An attempt at
explaining the causes of rich supply of wood debris to the
river channel is also presented. The dated wood was col-
lected from its rich accumulations in the alluvium in the
headwater section (about 20 km long) of the San river,
between its source at the Uzhok Pass (863 m a.s.l.) and
the junction with the Muczny Stream (upstream from the
Kiczera Dydiowska).
 RADIOCARBON DATED WOOD DEBRIS IN FLOODPLAIN DEPOSITS OF...

2. CHARACTERISTICS OF THE STUDY AREA
This part of the San river watershed has mountane
relief near the water divide (long and steep slopes of the
Pasmo Po³onin Range) and foothill relief in the valley part
(low altitude differences and gentle gradients). Most of
the watershed is wooded (ca. 85%), only the highest parts
of the Pasmo Po³onin Range and the bottom of the San
river valley (especially the DŸwiniacz Depression) are not
forested. The dominant species of trees are beech (ca 46%
in the Tarnawa forestry area), less abundant are spruce
(ca 27%) and fir (ca 20%; Krygowski, 1975). The high
percentage of forests in the slope areas retards the sur-
face runoff from the abundant precipitation (ca 1100 mm
per year) and reduces flood waves in the streams. The sedi-
ment load in the streams is now small during high water

Fig. 1. Extent of the lower fluvial terrace along the San river and its tributaries.

130
 J. Kukulak et al.
states, as intense farming has ceased in the Polish part
of the San river watershed (ca 80% of the total) half
a century ago.
The floodplain is the lowermost level of alluvial depo-
sition in a valley, older terraces lie higher and are arranged
in steps. The height of the floodplain above the river level
gradually increases downstream, from 0.5 m to 2 m,
locally even to 3 m. At places it consists of two horizons
(1.5-3 m, 0.5-1.5 m). The width of the terrace is greatest
(50 m) in the DŸwiniacz Depression, where the vertical
gradient of the river is lower than 0.5 % and the channel
is meandering. The floodplain extends along the San river
from its very source, and penetrates into valleys of bigger
tributaries (NiedŸwiedŸ, Sych³owaty, Halicz, Litmirz and
Muczny streams). The sedimentary cover of the terrace
differs from the older covers in its finer-grained sediments
and a large content of wood debris. Fossil wood is only
sporadically found in the sediments of the older terraces.
The main horizon with wood debris has a constant strati-
graphic position in the floodplain sections. It extends in
the lower part of the alluvial cover, at the boundary be-
tween the lower gravels and the overlying sandy muds. The
wood debris lies in layers or lenses of a few centimetres
to 0.5 m thick. Meso-scale fragments of wood debris usu-
ally form one thick layer; the finer debris lies in two to
five thin, laterally extensive layers. The higher, fine-
grained part of the alluvial cover contains much less and
finer wood debris. Only locally it fills erosional channels
at different levels in the vertical sections or is dispersed
in mineral deposits.
3. MATERIAL AND METHODS
Accumulation of plant debris in exposures of flood-
plain deposits have been studied and documented in years
1996-2000. Determined were forms of the accumulations,
their state of preservation; the remains have been identi-
fied in selected sections of the terrace (Haczewski et al.,
1998). Wood from several debris accumulations was col-
lected for radiocarbon dating (Sianki, Beniowa, Bukowiec,
Tarnawa Ni¿na, £okieæ and Dydiowa). One or two samples
were taken from each of the selected accumulations, all
from the lower part of the vertical sequence (boundary
between gravel and sandy mud).
All datings were done in years 1997-2000; most of them
in the Gliwice (A. Pazdur), a part in the Cracow Radio-
carbon Laboratories (T. Kuc). 14C concentration in the
samples was measured in the Gliwice Radiocarbon Labo-
ratory by gas proportional counting and in the Cracow
Radiocarbon Laboratory by liquid scintillation counting.
δ13C was determined in mass spectrometer, thus conven-
tional radiocarbon age was normalised to δ13C = -25‰,
according to the Stuiver and Polach’s procedure (1977).
14
C dates were calibrated by use of the Gliwice calibra-
tion Program GdCALIB (Pazdur and Michczyñska, 1989),
except for some dates of radiocarbon age less than 300 BP,
which were calibrated by OxCAL (Ramsey, 1995). In both
cases the calibration curve of Stuiver et al. (1998) was used.
Table 1 shows the results of radiocarbon dating as
conventional radiocarbon ages (14C Age, BP) and after
131
calibration procedure, as the intervals of the highest prob-
ability at confidence level 68% (Cal. Age, AD/BC).
Geological, archaeological and historical data have
been compiled for the period indicated by the radiocar-
bon dates, including results of palaeobotanical analyses
of local peat-bogs (Pa³czyñski, 1962; Marek and Pa³czyñski
1962; Zarzycki, 1963; Ralska-Jasiewiczowa, 1969, 1980
and 1989). These mainly record changes in a vegetation
cover of the Bieszczady Mountains during the Holocene,
thus indirectly they reflect the phase of a climatic change
and early human activity. Archaeological findings are few
in the studied area and they suggest rather migrations
than settlement in pre-historic times (Reyman, 1958;
Parczewski, 1991). Historical data on the San river valley
have been collected from archival maps, cadasters,
chronicles and published studies (Kummerer, 1855; Akta,
1868; Stadnicki, 1848; Fastnacht, 1962). History of forests
and their management during the last five centuries are
well documented in the above sources.
4. RESULTS
Meso-scale components of fossil wood in the flood-
plain sediments are logs and their fragments, branches,
roots and sporadic polypores. The accumulation of fine
debris consist mainly of leaves, bark, fruits and seeds.
Noteworthy is the large proportion of bark, branches and
tree tops. The wood debris is accompanied by fragments
of peat, herbaceous plants and their fruits and seeds, fun-
gal sclerotia and insect remains. Microscope studies of the
fine alluvium reveal a significant admixture of microscopic
plant detritus in all size fractions. Coarse logs are usually
found in shallow erosional troughs dissecting gravels
(Beniowa) or in channel sediments at palaeochannel
bends (Tarnawa Ni¿na). They are buried in sand and fine
gravel, some logs are completely buried in gravel
(Bukowiec and Tarnawa Ni¿na). The finer wood debris
occurs only in the sandy mud, in sections of flat ancient
river bottom.
Most logs are well preserved. They lack large frag-
ments of bark, but all have cambium preserved. Stumps
complete with roots and branches are rare. Locally rot-
ten logs with still visible internal structure also occur.
A few logs at Beniowa and Bukowiec bear traces of work-
ing with tools (wedge-shaped axe-made incisions and saw-
made cuts). A wooden board, symmetrically cut on both
sides and perforated, apparently a household object, is
exposed at the bottom of the mud layer at Sianki. Many
finer wood fragments at Sianki and Tarnawa Ni¿na are
partly impregnated or coated with iron oxides, which
makes them more resistant to decay. Some of the wood
fragments are charred or scorched (Kukulak, 2000).
Each of the wood debris accumulations is a separate
assemblage of size classes, usually composed of several
similar classes. The accumulations of coarse wood debris
usually lack finer detritus or have only a small proportion
of it. The areally more extensive wood debris accumula-
tions display a lateral trend in grain size, depending on
the form of accumulation. Besides size sorting (layers of
leaves or branches), weight sorting also occurs (e.g. fruits,
 RADIOCARBON DATED WOOD DEBRIS IN FLOODPLAIN DEPOSITS OF...
bark). These features are better visible in the accumula-
tions of plant detritus in low-gradient segments of the
valleys (Beniowa and £okieæ). Wood in each of the eight
radiocarbon-dated samples, has a different conventional
radiocarbon age (Table 1). The obtained dates cover
a wide time interval: from 3270±70 BP (Tarnawa Ni¿na I)
to modern - 103.7±1.1 pMC (Sianki). Half of the dated sam-
ples represent wood that died at modern times (18th-19th
centuries). The dates of wood from Beniowa (122±60 BP),
wattle made from thin stems and twigs at £okieæ (150 ±60
BP) and a layer of beech leaves at Dydiowa (140±60 BP)
fall within a very narrow time interval. The other half of
the samples consisted of much older wood, and the diffe-
rences in their ages attain 500-700 years. Only at Tarnawa
Ni¿na, wood from a thick log (I) and fir cones (II) buried
in the same horizon, have similar ages (terminal part of
the Subboreal Epoch of the Holocene).
Dating of the studied wood debris indicate that wood
debris of various age has been buried in the floodplain
alluvium. Very young is the debris that fills an erosional
channel at Sianki, older are artificial wattle reinforce-
ments at £okieæ. The logs buried in the basal gravels at
Bukowiec are from the beginning of the Common Era,
and those at Tarnawa Ni¿na are as old as Subboreal. The
presence and predominance in the alluvium of wood de-
bris dated at the last three centuries, proves that most of
the debris was accumulated at times close to, or only
slightly later than, its radiocarbon dates. It could occur in
the 18th or 19th century. The dates of these samples do not
determine the age of the main wood debris horizon over
the whole length of the San valley. Also the presence of
the oldest wood in this horizon (Tarnawa Ni¿na) may be
the result of its redeposition from older terraces.
Table 1. Description (name, depth, material) and conventional and calibrated ages of the samples. Calibrated age range has been
determined with confidence level 68% using the GdCALIB programme, developed in the Gliwice Radiocarbon Laboratory and Oxford
programme OxCal for very young samples.
Sample name/depth Lab. No.
Dating material
Sianki/0.95-1.05 m
Twigs, cones Gd-15166
Beniowa I/0.7 m
Charcoal KR-168
Beniowa II/1.45-1.55 m
Leafs, twigs, bark Gd-11555
Bukowiec/2.6-2.8 m
Wood Gd-7860
Tarnawa Ni¿na I/1.1-1.2 m
Wood Gd-12136
Tarnawa Ni¿na II/1.60-1.65 m
Twigs, cones Gd- 15194
£okieæ/2.5 m
Wood KR-167
Dydiowa/0.7 m
Leaves, twigs KR-172
Cal. Age = calibrated age, Lab. No.= laboratory number, Gd- = Lab. No. of C dates from Gliwice Radiocarbon Laboratory, KR- = Lab. No. of 14C dates from
14
Laboratory of the University of Mining and Metallurgy, Cracow , (*) = pMC-percent of modern carbon.
132
5. DISCUSSION AND CONCLUSIONS
The times of plant death indicated by the radiocarbon
dates of wood are related to events of both climatic (the
older dates) and anthropogenic (the younger dates) na-
ture in the natural environment of the Bieszczady Moun-
tains. The age of the buried logs at Tarnawa Ni¿na corre-
sponds to the phase of frequent floods in the watershed
of the upper Vistula River towards the end of the
Subboreal time (Starkel, 1977 and 1994). Also the age of
the logs at Bukowiec is isochronous with floods in the
Carpathian rivers in Roman times, and the fragments from
Beniowa – with floods in early Mediaeval times (Fig. 2).
The flood sediments of the upper Vistula river laid down
at those periods include numerous buried logs (Awsiuk
et al., 1980; Kalicki and Kr¹piec, 1991 and 1996; Kr¹piec,
1992). The older dates from the studied wood debris fit
well within the phases of the San river floods and may be
related to climatic conditions. The number of older dates
is, however, too small to exclude that the coincidence is
only accidental.
The accumulations of the younger wood debris have
been also laid down during floods, but the cause of their
deposition seems to be mainly anthropogenic. It is related
to the phase of settlement and onset of farming in the part
of the Bieszczady Mountains during late Mediaeval and
early Modern times. Many permanent settlements of
farmers and wood workers have been founded here on
inhabited grounds during the second half of the 16th and
at the beginning of 17th century. These have evolved later
into agricultural villages (Fastnacht, 1962). The settle-
ments were located in areas that were already partly
deforested as pasture grounds at valley bottoms (Ternowe
14
C Age [BP] Range of Cal. Age
[AD/BC]
103.7±1.1pMC (*) MODERN
122±60 [1800, 1950] AD
1380±50 [636, 686] AD
1940±50 [21, 91] AD
3270±70 [1621, 1491] BC
2680±70 [1002, 762] BC
150±60 [1720, 1820] AD
140±60 [1800, 1890] AD
 J. Kukulak et al.
Pole, Beniowe Pole and Pole Bukowiec). The glades were
mainly the work of the Valachian herders who were com-
ing here seasonally from the 14th to 16th century, with their
herds of cattle and sheep (Kubijowicz, 1926; Parczewski,
1991).
The first villages were located in the DŸwiniacz Depre-
ssion: DŸwiniacz Górny (before 1529), Tarnawa Ni¿na and
Tarnawa Wy¿na (1537). The expansion of settlements
reached the Uzhok Pass in the end of the 16th century:
Bukowiec (1580), Beniowa (1580) and Sianki (1580). The
economy of these villages was based on cattle herding and
grain growing, activities that required wide expansion of
farmland. Clear cutting of forests began on great scale,
providing areas for arable fields and meadows. The clear-
cuts were not limited to the areas around villages but also
included widening of natural mountain meadows on the
mountain crests (so called poloninas). Tax registers from
the 16th and 17th centuries (Spisy, 1787), land cadasters
from the 18th. (Akta, 1868) and old maps from the 18th-19th
centuries (Liesganig, 1824; Kummerer, 1855) prove a
nearly complete deforestation of the valley bottom, a large
reduction in the forest area on slopes and lowered tim-
berline around the poloninas.
The clearing of forest was done mainly by fire clear-
ance. Initially, this was the easiest way to gain farmland,
133
Fig. 2. Corelation of phases of
settlement in the Bieszczady
Mountains with the age of wood
debris in the lowest (1-3 m) terrace.
A – period of permanent settlement
and farming in the Bieszczady
Mountains; B – record of human
influence on environment in pollen
diagrams of peat-bogs
(after Ralska-Jasiewiczowa, 1989);
C – radiocarbon dates; D – dated
wood fragments at the bottom of the
fine-grained; E – dated wood
fragments from the fillings of
erosional thoughs in the alluvial
terrace. Archaeologic periods:
I – Hallstatt, II - La Tène, III – Roman,
IV – Migration, V – Medieval,
VI – Modern times. Underlined are
dates from San tributary situated off
the west margin of Fig. 1.
then also to fertilise it (Kubijowicz, 1926; Broda, 1952;
Pa³czyñski, 1962). The settlers usually did not perform
complete clearcutting and did not clear the area of
branches, tree tops and bark. This wood debris was burnt
in place or thrown away to stream channels (Szwab, 1956).
The rapid re-growing of woods in non-cultivated ground
and repeated cutting in the same places favoured accu-
mulation of large amounts of wood debris in nearby
stream channels. The initial phase of settlement in the San
river valley had to be the most productive in wood litter.
The increased runoff due to deforestation of slopes
resulted in more violent flooding of the streams and en-
abled transport of the wood debris to the San river chan-
nel. This supply had to be rich, as the debris formed thick
accumulations in the channel sediments and erosional
troughs on terraces. The deposition of wood debris was
accompanied by increased load of slope-derived sedi-
ments in flood waters. This increased supply of clay from
arable fields resulted in a tendency to alluvial aggrada-
tion in the San river channel. The alluvial aggradation
was the fastest along reaches with low vertical gradient
(below 0.5%). It was also at those places where the great-
est amount of wood debris was laid down. The burnt and
charred wood found in this debris may be the product of
fire clearance. The radiocarbon dates from the burnt wood
 RADIOCARBON DATED WOOD DEBRIS IN FLOODPLAIN DEPOSITS OF...
at Beniowa correspond to the period of the greatest ac-
tivity of local wood-burning industries (potash-making
facilities, blacksmithery and steam-powered sawmills).
A large part of the buried logs may have come from un-
dercutting of river banks, as conditions for lateral chan-
nel migration existed during the greater floods.
All the wood debris, dated at various periods of the
late Holocene, is now buried in the alluvial cover of the
same terrace. The interpretation of time of their deposi-
tion in the alluvium is thus not unequivocal. One may
assume that the floodplain consists of fragments of dif-
ferent age, so that older wood is buried in the older frag-
ments, and younger wood in the younger ones. The divi-
sion of the terrace into fragments of different age is,
however, expressed in its stratification (gravels at bottom,
mud above) rather than in the presence of laterally adja-
cent segments of different age (due to lateral aggrada-
tion). Only a part of the fine-grained alluvium (the upper
part of the cover) includes fills of linear erosional troughs.
The main horizon of wood debris forms a layer in the ter-
race and it seems to be isochronous. It is thus more likely
that the older wood debris was redeposited to the young
alluvium from the older terraces of the San.
6. ACKNOWLEDGEMENTS
The paper is based on data obtained during geologi-
cal mapping in the Bieszczady Mountains. The mapping
project was led by Professor Grzegorz Haczewski who
provided assistance in the fieldwork, in the discusion of
the results and translated the text to English. Professor
Micha³ Parczewski of Jagiellonian University has intro-
duced J.Kukulak into the recent results of archaeological
research in the Bieszczady.
7. REFERENCES:
Akta Grodzkie i Ziemskie z Archiwum tzw. Bernardyñskiego we
Lwowie (Town and Land Acts from the so called Bernardine
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Alexandrowicz S.W., Klimek K., Kowalkowski A., Mamakowa K.,
Niedzia³kowska E., Pazdur M. and Starkel L., 1981: The evo-
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Glacial and Holocene. Folia Quaternaria. 53: 91 pp.
Awsiuk R., Niedzia³kowska E., Pazdur A., Pazdur M.F., Starkel L.
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of the Holocene alluvia at the left bank of the Wis³oka river
near Dêbica. Studia Geomorphologica Carpatho-Balcanica 14:
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Broda J., 1952: Gospodarka zrêbowo-wypaleniskowa w Beskidzie
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 GEOCHRONOMETRIA Vol. 21, pp 137-142, 2002 – Journal on Methods and Applications of Absolute Chronology

CHRONOLOGY OF THE VISTULIAN (WEICHSELIAN)

GLACIAL EVENTS IN THE LOWER VISTULA REGION,
MIDDLE-NORTH POLAND

WOJCIECH WYSOTA1, KRZYSZTOF R. LANKAUF2, JACEK SZMAÑDA2, ALICJA

CHRUŒCIÑSKA3, HUBERT L. OCZKOWSKI3 and KRZYSZTOF R. PRZEGIÊTKA3
1
Department of Geology and Hydrogeology, Institute of Geography, Nicholas Copernicus University,
Sienkiewicza 4, 87-100 Toruñ, Poland (e-mail: wysota@cc.uni.torun.pl)
2
Laboratory of Sedimentology and TL Dating, Institute of Geography, Nicholas Copernicus University,
Fredry 6/8, 87-100 Toruñ, Poland (e-mail: szmanda@geo.uni.torun.pl)
3
Thermoluminescence and Dating Laboratory, Institute of Physics, Nicholas Copernicus University,
Grudzi¹dzka 5/7, 87-100 Toruñ, Poland (email: przeciu@phys.uni.torun.pl)

Key words
words: Abstract: Stratigraphy of the Vistulian glacial events in the southern part of the Lower Vistula
NORTH POLAND, region in the north Poland is presented. Lithostratigraphic units and TL dating of Vistulian
VISTULIAN deposits exposing along the Vistula valley between Toruñ and the Che³mno Lakeland are
GLACIATION, described in detail. The obtained results indicate that the Vistulian sequences in the Lower
TL DATING Vistula region were deposited during five palaeogeographical episodes. Three glacial events
were distinguished: the first at the beginning of the Middle Vistulian (~65–70 ka) and two
younger ones during the Late Vistulian. The Middle and Late Vistulian glacial events were
separated by a long ice-free period, between 65 and 30 ka.

1. INTRODUCTION The paper presents the synthesis of the Vistulian Gla-

The studies of the Vistulian Glaciation stratigraphy
in the southern part of the Lower Vistula (Fig. 1) region
have been carried out for several recent years (Wysota,
2002; Wysota et al., 1996 and 2000). Thick and not de-
formed Vistulian stratigraphic sequences exposed along
the scarp of the Vistula Valley between Toruñ and
Che³mno have been the subject of detailed examinations.
Lithostratigraphical and sedimentological researches
have been carried out at seven key sites: Rzêczkowo,
£¹¿yn, Unis³aw, Kie³p, Starogród 1, Starogród 2 and
Che³mno (Fig. 1). They included: (1) identification and
lithofacial analysis of sedimentary units, (2) analysis of
directional elements (palaeocurrents, till fabric and ki-
nematic indicators), (3) lithologic and petrographic in-
vestigations (grain size composition, carbonate content,
quartz grain roundness, pethrographic composition of
gravels and heavy mineral composition), (4) TL dating
of deposits, and (5) spatial analysis of stratigraphic units.
Some results of the studies conducted at Rzêczkowo and
£¹¿yn sites have already been published (Wysota et al.,
1996 and 2000).
ciation stratigraphy in the southern part of the Lower
Vistula region. The new ideas of chronology and
palaeogeography of the Vistulian glacial events have been
also put forward.
2. STRATIGRAPHIC UNITS
The lower limit of Vistulian deposits has not been sat-
isfactorily recognized yet. It is supposed that upper flu-
vial series of the Lower Vistula formation, which so far
has been connected entirely with the Eemian (Makowska,
1979 and 1980), represents preglacial period of the Early
Vistulian (Fig. 2).
The sequence of Middle and Late Vistulian deposits,
that overlies the Early Vistulian fluvial sediments, has the
thickness of 25–70 m here. Three main stratigraphic units
have been distinguished: Che³mno clays formation,
Rzêczkowo formation and Starogród formation (Fig. 2).
Che³mno clays occur at the bottom of the Middle
Vistulian succession. They comprise varved clays and silts
up to 20m in thickness, which fill the upper part of the
Eemian/Early Vistulian palaeovalley. Overlying it,
 CHRONOLOGY OF THE VISTULIAN (WEICHSELIAN) GLACIAL EVENTS ...
Rzêczkowo formation is 15–25 m thick, and composed
mostly of fluvial sands. Lithofacies of planar cross-bed-
ded sands, parallel laminated sands and ripple-laminated
sands are predominant.
Starogród formation occurs at the top of the Vistulian
sequences. Two separate till units have been distinguished:
the lower till member – £¹¿yn till and the upper till mem-
ber – Starogród Zamek till. £¹¿yn till is 1.5–10m thick
and combines sandy and clay-rich massive and stratified
diamictons. It comprises three genetic types of subglacial
facies: deformation till, melt-out and decoupling till and
melt-out till. Till fabric shows NE and NNE ice movement
directions. Unis³aw clays, 2–6 m thick, of glaciolacustrine
origin and lying underneath £¹¿yn till can be found in
places. Glaciolacustrine sediments of up to 18-m thick-
ness (Kie³p clays) overlie the lower till member. Glacio-
fluvial series occur below and above them locally.
Starogród Zamek till constitutes the highest unit of
Starogród formation. It consists of massive brownish clay-
rich diamicton up to 8–10m thick. The diamicton usually
comprises two facies: lodgement till and melt-out till. Till
fabric shows N and NNE ice movement directions.
3. RESULTS OF TL DATING
Two sets of samples were dated by TL method. The
first one consisted of four samples related to Kie³p clays:
R-4, R-5, St1-1 and St1-2. The other seven samples: K-2,
K-3, Ch-1, Ch-2, R-6, Sa2-1 and Sa2-2 were related to
Rzêczkowo formation.
The material taken for TL analysis was cleaned and
afterwards the quartz grains of specified size were sepa-
rated and then etched, appropriate to the procedure de-
scribed earlier (Przegiêtka, 1999; Oczkowski et al., 2000a).
The bleaching of natural TL signal was performed in a
138
Fig. 1. Study area against the
ice sheet margins of the
Vistulian Glaciation in the mid-
western Poland.
L – Leszno phase, Pz – Poznañ
phase, Ch, Do – Chodzie¿,
Dobrzyñ readvance, Kr –Krajna
subphase, Pm – Pomeranian
phase, and Ga – Gardno phase.
specially designed chamber with sunlight simulator
(Oczkowski and Przegiêtka, 1998a). The bleached samples
were used for equivalent dose estimation by the regen-
erative method. The plateau test was applied to choose
the best temperature region. The additive method was
also applied for the majority of the samples. The Risø
System comprising the calibrated 90Sr source (Oczkowski
and Przegiêtka, 2000) was used for beta dose irradiation
and TL measurements. Details of equivalent dose deter-
mination procedures were presented earlier (Oczkowski
and Przegiêtka, 1998a; Przegiêtka, 1999; Wysota et al.,
2000). The annual dose rates were determined on the basis
of high-resolution gamma spectrum measured with HP
germanium detector and Canberra MCA-100 analyser.
Details of measurement and computational procedures
were published previously (Oczkowski and Przegiêtka,
1998b; Oczkowski et al., 2000b). Results are presented in
the Table 1.
Previously four samples related to Rzêczkowo forma-
tion were dated (Wysota et al., 2000). Those dates were
analysed together with seven new ones. The mean age
value T= 42.9 ka with standard uncertainty σ = ±1.7 ka
were obtained by the weighted averaging method. The
histogram showing the distribution of the eleven TL dates
is presented in Fig. 3.
Apparently these dates represent rather a continuous
process stretched over a certain period of time than a
single event (Fig. 4). Hence the mean age value is not suit-
able parameter for describing such a process. We assumed
that the set of eleven investigated samples was good
enough for the representation of Rzêczkowo formation.
The shape of the histogram (Fig. 4) may suggest that the
deposition lasted for the period of ca. 35 ky. Hence, we
concluded that sedimentation of Rzêczkowo formation
deposits started ca. 65 and ended about 30 ka ago.
 W. Wysota et al.

Table 1. TL dates of deposits from southern part of the Lower Vistula region.
No Section Stratratigraphic Sample Lab. No. Material Age Equivalent Dose Rate
Unit Name [ka] Dose [Gy] [Gy/ka]
1. Rzêczkowo Kie³p clays R-4 TOR-35 Glaciolacustrine silts 19 ± 3 35 ± 6 1.863
Kie³p clays R-5 TOR-36 Glaciolacustrine silts 20 ± 2 36 ± 4 1.805
Rzêczkowo Fm. R-6 TOR-37 Fluvial sands 33 ± 3 34 ± 3 1.023
Rzêczkowo Fm. R-2* TOR-25 Fluvial sands 49 ± 6 51 ± 6 1.045
2. £¹¿yn Rzêczkowo Fm. L-3* TOR-28 Fluvial silts 50 ± 8 104 ± 17 2.078
Rzêczkowo Fm. L-2* TOR-27 Fluvial sands 63 ± 20 126 ± 40 2.000
Rzêczkowo Fm. L-1* TOR-29 Fluvial sands 65 ± 20 130 ± 40 2.000
3. Kie³p Rzêczkowo Fm. K-2 TOR-31 Fluvial sands 39 ± 6 61 ± 9 1.564
Rzêczkowo Fm. K-3 TOR-32 Fluvial sands 57 ± 7 57 ± 7 1.008
4. Starogród 1 Kie³p clays St1-2 TOR-41 Glaciofluvial sands 21 ± 3 41 ± 5 1.931
Kie³p clays St1-1 TOR-40 Glaciofluvial sands 27 ± 5 36 ± 6 1.329
5. Starogród 2 Rzêczkowo Fm. Sa2-1 TOR-38 Fluvial sands 47 ± 7 62 ± 9 1.325
Rzêczkowo Fm. Sa2-2 TOR-39 Fluvial sands 49 ± 5 60 ± 6 1.221
6. Che³mno Rzêczkowo Fm. Ch-1 TOR-33 Fluvial silts 45 ± 5 76 ± 8 1.685
Rzêczkowo Fm. Ch-2 TOR-34 Fluvial sands 46 ± 5 47 ± 5 1.028

*) The data obtained prior to the present project and published in Wysota et al. (2000).

Fig. 2. Synthetic section and

sedimentary environments of Vistulian
deposits in the southern part of the
Lower Vistula region. The numbers
column means TL dates in ka.

139
 CHRONOLOGY OF THE VISTULIAN (WEICHSELIAN) GLACIAL EVENTS ...
Fig. 3. Histogram of eleven TL dates obtained for samples
representing Rzêczkowo formation, the bar width is 7 ka.
Fig. 4. The set of eleven TL dates obtained for Rzêczkowo
formation and the weighted average value with its uncertainty,
T± σ.
4. PALAEOGEOGRAPHIC EPISODES
The Vistulian deposits in the Lower Vistula region
were deposited during five palaeogeographical episodes
(Fig. 2). During the preglacial period of the Early
Vistulian Upper fluvial series of the Lower Vistula For-
mation was accumulated. Deposition of deposits was
developed in a braided river environment.
During the next stage Che³mno clays were formed.
Sedimentary processes took place in a glaciolacustrine
environment. The environment was formed as a result of
the first ice sheet advance in the Lower Vistula region at
the beginning of the Middle Vistulian (~65–70 ka). It is
supposed that the ice sheet reached the Grudzi¹dz Basin.
140
As the ice sheet was retreating, depositional processes
were gradually changing their character from glacio-
lacustrine sedimentation to fluvial deposition. Rzêczkowo
formation was deposited in the environment of a sand-
bed braided river (Wysota et al., 1996 and Wysota, 2002).
The obtained TL dating suggests that the deposition of
Rzêczkowo formation developed during a long ice-free
period of the Middle Vistulian, between 65 and 30 ka.
Glacial, glaciolacustrine and glaciofluvial sedimenta-
tion characterised the succeeding depositional episodes.
They were connected with two ice sheet advances, which
covered the studied area during the Late Vistulian. The
older glacial event was related to the first Late Vistulian
maximum, ca 22–20 ka (the Leszno Phase). The younger
one represented ice sheet readvance connected with the
second Late Vistulian maximum, ca 19–18 ka (the Poznañ
Phase).
5. CONCLUSIONS
The obtained results of the studies indicate that there
was no glacial event in the southern part of the Lower
Vistula region during the Early Vistulian as it had previo-
usly been assumed (Makowska 1980, 1992 and 1994).
Pelaeogeographical and especially palaeoclimalological
conditions recently recognized in the Polish Lowland, also
deny ice sheet existence on the Lower Vistula at that time
(Mojski, 1999).
The first glacial advance in this area occurred as late
as at the beginning of the Middle Vistulian. This advance
corresponds to the Toruñ glacial horizon distinguished
earlier by Makowska (1979, 1980, 1992 and 1994) in the
Lower Vistula region. The collected lithostratigraphic
data have not confirmed that the ice sheet reached Toruñ,
as she presumed. The Middle Vistulian ice sheet anvanced
to the northern, and probably to the middle part of the
Lower Vistula region. Only proglacial deposits (Che³mno
clays) are related to this advance in the southern part of
the Lower Vistula region.
The obtained TL dates substantiated higher chrono-
stratigraphic position of the younger Vistulian units than
it had previously been stated (Makowska 1980, 1992 and
1994; Wysota et al., 1996). It is presumed that Rzeczkowo
Formation linked before to the Gniew Interstadial of the
Early/Middle Vistulian period, represents a younger warm
unit – the Grudzi¹dz Interstadial of the Middle Vistulian.
Overlying it, the lower glacial horizon of Starogród for-
mation (£¹¿yn till), which formerly has been interpreted
as the Middle Vistulian glacial episode unit (the Œwiecie
stadial), is related to the first Late Vistulian maximum (ca.
22–20 ka). The ice sheet readvance connected with the
second Late Vistulian maximum (ca. 19–18 ka) has not
been recognized in the Lower Vistula region yet.
ACKNOWLEDGEMENT
The research project has been financially supported
by the Nicholas Copernicus University – grant no. 457-F
and the Committee for Scientific Research – grant No.
6 P04D 022 14.
 W. Wysota et al.
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in the SW Margin of the Che³mno Moraine Plateau). Acta Univ.
Nic. Coper., Geografia 28: 39-63.
CHRONOLOGY OF THE VISTULIAN (WEICHSELIAN) GLACIAL EVENTS ...

142
 GEOCHRONOMETRIA Vol. 21, pp 143-150, 2002 – Journal on Methods and Applications of Absolute Chronology

SOME PROBLEMS IN THE STUDY OF THE CHRONOLOGY

OF THE ANCIENT NOMADIC CULTURES IN EURASIA
(9TH - 3RD CENTURIES BC)

A.YU.ALEKSEEV1, N.A.BOKOVENKO2, YU.BOLTRIK3, K.A.CHUGUNOV4, G.COOK5 ,

V.A.DERGACHEV6, N.KOVALIUKH7, G.POSSNERT8, J.VAN DER PLICHT9, E.M.SCOTT10,
A.SEMENTSOV2, V.SKRIPKIN7, S.VASILIEV6 AND G.ZAITSEVA2
1
The State Hermitage Museum, St.Petersburg, Russia
2
The Institute for the History of Material Culture of Russian Academy of Sciences, St.Petersburg, Russia
3
The Institute of Archaeology of the National Academy of Sciences of Ukraine, Kiev, Ukraine
4
The Institute of Cultural and Natural Heritage, St.Petersburg, Russia
5
Radiocarbon Laboratory, SUERC, East Kilbride, Scotland
6
The Physical-Technical Institute of the Russian Academy of Sciences, St.Petersburg, Russia
7
State Scientific Centre of Environmental Radiochemistry of National Academy of Sciences of Ukraine, Kiev, Ukraine
8
Svedberg Laboratory of Uppsala University, Uppsala, Sweden
9
Radiocarbon Laboratory of Groningen University, Groningen, the Netherlands
10
Department of Statistics, University of Glasgow, Glasgow, Scotland

Key words
words: Abstract: This research is focused on the chronological investigations of ancient nomads
NOMADS, belonging to the Scythian cultures which occupied the steppe and forest-steppe zones of Eurasia
SCYTHIAN TIME, during the 9th-3rd centuries BC. The 14C dates for the pre-scythian and early scythian time in
EURASIA, both Europe and Asia are presented and compared to their chronological position based on
RADIOCARBON archaeological evidence. The first 14C dates have been produced for the Scythian time monu-
DATES ments located in the Lower Volga River basin, Urals and Transurals regions. Their chrono-
logical positions are compared with the position of the monuments of Southern Siberia and
Central Asia. It was shown that the nomadic cultures belonging to the Scythian culture began
to exist over the wide territory of Eurasia from the 9th-8th centuries cal BC and there are some
monuments which may be synchronous to the Arzhan royal barrow (the oldest monument
known). A list of new 14C dates and a map of the monuments are presented.

1. INTRODUCTION For a long time, the chronology of the Eurasian

The chronology of the nomadic tribes, which occupied
the steppe and forest-steppe zones of Eurasia during the
1st millennium BC is very important. The tribes are tradi-
tionally connected with the Scythian cultures which have
different names in different regions of Eurasia: the
Scythians in Europe, the Suoromathian in the Lower
Volga River Basin and Southern Ural regions, the Tasmola
in the Transural regions and the different mosaic cultures
in Altai, Southern Ural and Central Asia. The majority
of sites associated with these cultures are located between
~ 40 °-55°N and 30°-110°E. The connections between
European and Asian Scythian cultures, and their interac-
tion is testified by the similarities between both European
and Asian Scythian artefacts, the dynamics of these
interactions can be solved on the basis of chronological
research.
Scythian cultures was based on a variety of different ar-
chaeological approaches due to a lack of 14C dates for the
European monuments. Recently the first radiocarbon
dates for these monuments have been produced by AMS
dating.
It is necessary to note that about 20 years ago,
M.P.Gryasnov picked out 11 geographical zones in the
history of Early Scythian cultures (9-7 centuries BC):
1) Northern Black Sea region, 2) the Northern Caucasus
region, 3) the Aral Sea region, 4) Central and Northern
Kazakhstan, 5) Semirech’e, Tien Shan and the Pamirs,
6) steppe and forest-steppe zones to the North and West
from Altai Mountains, 7) Altai Mountains, 8) South Si-
beria, 9) Tuva, 10) Mongolia, 11) Ordos (Gryasnov, 1983).
It was found that these local zones contained features
of later chronological periods, but it was necessary to add
two additional geographical zones – the Lower Volga and
 SOME PROBLEMS IN THE STUDY OF THE CHRONOLOGY OF THE ANCIENT...
Southern Urals regions – to the list of zones. These latter
additions may be considered as distinctive intermediate
points for cultural and ethnic pulses between the two main
macro-regions of the Scythian World – Western and
Eastern.
One should also not forget that the Lower Volga no-
mads have close relations with European Scythians to the
west, on one hand, and that Southern Urals barrows have
many similar features with the Aral Sea region,
Kazakhstan, and Southern Siberia materials to the east,
on the other hand (Ochir-Gorayeva, 1988).
Such conclusions have been drawn on the basis of ar-
chaeological evidence. Now we have produced the first
14
C dates for the monuments in these regions and can
compare the radiocarbon chronology of the key Scythian
monuments for Eurasia focusing special attention on de-
termining the first appearance of the Scythian culture.
2. RESULTS
In total, samples for dating have been collected from
about 40 Eurasian Scythian monuments, many of them
having not been previously dated. As well, additional 14C
dates were produced for some well-known Scythian monu-
ments: Oguz, Solokha, and Chertomlyk, the Pazyryk group
barrows, Arzhan, Dogee-Baary-2 and others. The map of
monuments dated is presented in Fig. 1. The 14C dates
produced during the last two years and dates which were
not published previously now are presented in Table 1.
Earlier there was a broad sweep of territory in which the
Scythian monuments had not been dated including
144
the Lower Volga River basin and the Southern Ural
regions. Now this gap has begun to be filled. There have
also been a considerable number of samples collected for
Scythian time monuments in Southern Siberia. It is
important to note that before the end of 1990»s, only the
elite barrow Arzhan, Dogee-Baary-2 and Kopto barrows
had been 14C dated (Alekseev et al., 2001). Now there are
about 10 Scythian-time monuments in this region dated
by 14C. Discussion of the interpretation of these results
now follows.
3. DISCUSSION
Steppe and Forest-steppe regions of Europe
For the prescythian time of European Scythia, the
monuments of the so-called Chernogorovka culture dated
by archaeological finds to pre-scythian time play the most
important role. Until recently there were no 14C dates for
this culture. In 1971 the Vysokaja Mogila barrow (graves
number 2 and 5) was excavated in the Lower Dnieper
River basin (steppe area). At first this monument was
dated by archaeological materials. Grave number 5 dates
to the late Chernogorovka period (900-750 BC accord-
ing to Terenozhkin, 1976) and grave number 2 to the
younger Novocherkassk period (750-650 BC). There are
contradictory opinions on the absolute chronology of
these two monuments: for example, 25 years ago
A.I.Terenozhkin dated them both to ca middle 8th century
BC, but S.A.Skory together with other archaeologists now
date Vysokaja Mogila, grave 2 from the late 8th to the early
7th centuries BC (Skory, 1999). 14C dates of both graves
Fig.1. Map of location of the
Scythian time monuments
dated by 14C.
 A.Yu. Alekseev et al.
produced recently are very close and give earlier results:
grave 5, Ki –8425, 2765±50 BP (calibrated 1007-815 cal
BC, 2σ), and grave 2, Ki-8424, 2740±50 BP (calibrated 997-
805 cal BC, 2σ). This evidence would suggest that the mod-
ern archaeological “short” chronology is not quite correct.
Another important monument for European Scythia
also dated to the early period is barrow 15 of the Steblev
group located in the forest-steppe area. This was esta-
blished as the oldest Scythian grave and dated by archae-
ologists to the late 8th century BC (Klochko and Skory,
1993). The 14C dates produced for this barrow (2620-2580
BP) testify to the earlier Scythian association (the late 8th
century cal BC).
For a long time, the oldest monument for all Eurasia
was the royal barrow Arzhan (Central Asia and Tuva
Republic). About 30 14C dates were produced which lay
in the interval from 2800-2666 BP, testifying that this
monument was erected during the 9th century cal BC
(Zaitseva et al, 1998). Now there is the possibility to com-
pare the radiocarbon chronology of the Arzhan barrow
and European prescythian time monuments (Vysokaja
Mogila and Steblev, grave 15). One can unter the same
time intervals for their existence (Table 1).
Very interesting results have been obtained for the
classical Scythian royal tomb Solokha, one of the four
greatest Scythian barrows in the northern Black Sea re-
gion. Because the construction of any tomb occurred over
a rather short time, it was very important to obtain a pre-
cisely calibrated calendar interval for 14C dates and to com-
pare the archaeological data and radiocarbon chronology.
According to archaeological data, this barrow can be dated
to 400-375 BC (Alekseev, 1992). Eleven 14C dates for this
famous barrow have been produced. Taking into account
the complicated character of the calibration curve, which
has a wide plateau for the intervals 2600-2400 BP, and
impossibility of using in this case the wiggle matching
method to establish the more precise calendar time of this
tomb construction, we used the combine dates obtained
by the OxCal calibration program. The combined 14C date
from the eleven individual dates is 2333±15 BP which cor-
responds to 400-395 cal BC (1σ) and to 403-390 cal BC
(2σ) (Fig. 2). These results are generally in good agree-
ment with the archaeological dates.
The Lower Volga River basin
The Lower Volga nomads have close relations with
European Scythians to the West. They also have many
similarities with the nomads of the Aral Sea region,
Kazakhstan and Southern Siberia to the East. Now we
present the first 14C dates for the monuments in these
regions (Table 1).
There are numerous nomadic graves of the Scythian
era in the Lower Volga River region belonging to the so-
called “Sauromatian” culture and one of them is the
Aksenovski burial ground discovered in 1966 by V.P. Shilov
(Shilov, 1997). According to archaeological data, the dates
of all Aksenovski barrows and graves lie in the range of
ca 450 – 375 BC.
Barrow number 10 (grave number 1, where two women
were buried) also dates back to this time. Two bronze
145
Fig. 2. Combined 14C date for the Solokha barrow and its
position on the calibration curve.
mirrors were found, however, which according to archaeo-
logical data belong to an earlier time – the 7th-6th centu-
ries BC and what is more, one of these mirrors belongs to
a special group of so-called “indicators” of the Early
Scythian culture (Alekseev, 1992).
A sample for AMS radiocarbon dating was taken
from wooden fragments of one of the mirror-cases. One
of the 14C dates (Ua-16869) gave us the general chrono-
logical period from the 9th to 5th centuries cal BC (2σ).
In more detail, the calibration intervals are the follow-
ing: 9th-6th century cal BC, early 5th century cal BC, or sec-
ond half of the 5th century cal BC. Each of these intervals
is in a good agreement with the known archaeological
date. A second 14C date (GrA-16832) is earlier – from the
9th to the beginning of the 8th century cal BC. It is impor-
tant to note that combined date (2640±41 BP) gives also
the same range. One explanation is that the samples per-
haps came from the central part of the trunk. In any case,
results of radiocarbon dating show that terminus ante quem
of the construction of this wooden artifact is the late 5th
century BC.
Southern Urals and Southern Transurals regions
The ancient nomadic culture in the Southern Urals was
located in the centre of the “steppe belt” of the Scythian
cultures and it was subjected to a certain influence from
the nomads from the West (the Pontic Sea area) and from
the East (Central Asia, Altai and Southern Siberia).
The most important and famous barrow for the late pre-
scythian and early Scythian periods is the Great Guma-
rovo barrow (grave number 3) excavated in 1980 by
R. Ismagilov (Ismagilov, 1988). This monument can be
archaeologically dated on the late 8th to the early 7th cen-
turies BC. Samples for 14C analyses (AMS) were taken
from four leather fragments and one wooden fragment
from the quiver.
The agreement between archaeological and 14C dates
is good, except sample Ua-16867, 2750±75 BP, which gave
an earlier chronological age – from the late 12th to the
 SOME PROBLEMS IN THE STUDY OF THE CHRONOLOGY OF THE ANCIENT...

Table 1. The 14 C dates produced for the Scythian time monuments of Eurasia.
14
No No Lab. index C Age Monument Material C alibrated age [BC]
on the [BP]
Map 1 2
Ukraine
Pre-Scythian time (Chernogorovskaya culture)
1 60 Ki-8424 2740±50 Visoka mogila Wood 910-826 990-806
2 60 Ki-8425 2765±50 Visoka mogila Wood 978-834 1000-814
Earlier Scythian time
3 Ki-7740 2490±50 Steblev, barrow 15 Animal bone 766-528 782-412
4 9 Ki-7741 2660±50 Steblev, barrow 15 Animal bone 892-794 906-778
5 9 Ki-8426 2620±60 Steblev, barrow 15 Wood 892-562 908-532
6 9 Ki-8427 2530±60 Steblev, barrow 15 Wood 794-534 804-414
7 9 Ki-8428 2580±60 Steblev, barrow 15 Wood 810-550 836-420
Scythian time
8 63 Ki-8454 2180±60 Vishneva Mogila, barrow 11, Organic remains 360-122 374-60
grave 3
9 63 Ki-8454 2230±60 Vishneva Mogila, barrow 11, Leather 368-202 396-120
grave 5
10 63 Ki-8455 2210±60 Vishneva Mogila, barrow 11, Wood 364-192 392-106
grave 5
11 63 Ki-8456 2170±70 Vishneva Mogila, barrow 11, Leather from shoes 358-110 382-44
grave 5
12 63 Ki-8457 2250±70 Vishneva Mogila, barrow 11, Leather 384-202 406-106
grave 4
13 6 GrA-10163 2170±40 Oguz, grave 9 Grass, 354-118 364-66
14 6 Ki-7717 2230±50 Oguz Skeleton bone 366-202 392-176
15 6 Ki-7718 2190±50 Oguz Grass 360-178 380-100
16 7 GrA-10164 2330±50 Pastak, barrow 10 Wood from sword 476-214 750-202
17 10 GrA-10059 2180±40 Chertomlyk Wood from arrows 356-166 368-106
18 10 GrA-10203 2320±50 Chertomlyk Wood from arrows 408-210 516-200
19 10 GrA-10204 2350±50 Chertomlyk Wood from arrows 514-368 756-208
20 10 Ki-7720 2290±50 Chertomlyk, embanment Horse bone 398-210 404-200
21 10 Ki-7721 2170±80 Chertomlyk, embanment Sheep bone 360-108 388-8
22 10 Ki-7722 2335±80 Chertomlyk, northern grave Animal bone 520-206 762-192
23 10 Ki-7723 2130±70 Chertomlyk, northern grave Sheep bone 348-44 366BC-10AD
24 10 Ki-7724 2210±70 Chertomlyk, northern grave Horse bone 368-190 394-66
25 10 Ki-7725 2170±60 Chertomlyk Wool from clothes 358-112 370-54
26 10 Ki-7726 2310±55 Chertomlyk Skeleton bone 406-208 512-196
27 8 GrA-10060 2325±40 Solokha, Wood from sword 406-264 484-206
28 8 GrA-10159 2270±50 Solokha Wood from sword 390-208 398-200
29 8 GrA-10160 2350±50 Solokha Wood from sword 514-368 756-208
30 8 Ki-7742 2370±55 Solokha Wood from sword 746-380 762-254
31 8 Ki-7743 2295±55 Solokha Wood from sword 400-208 474-192
32 8 Ki-7744 2310±55 Solokha Wood from sword 406-208 512-196
33 8 Ki-7745 2350±55 Solokha Wood from artefact 516-266 758-204
34 8 Ki-7746 2320±55 Solokha Wood from artefact 410-208 522-198
35 8 Ki-7747 2380±55 Solokha Grass rope 750-386 762-266
36 8 Ki-7748 2425±60 Solokha Leather 756-402 764-394
37 8 Ki-7749 2300±55 Solokha Wood from artefact 402-208 482-192
Northern Caucasus, Russia
38 11 Ki-7769 2510±50 Uashkhitu, barrow 1 Wood 780-530 796-416
39 11 Ki-7770 2570±50 Uashkhitu, barrow 1 Wood 806-554 816-526
Lower Volga River Basin
40 14. Ua-16869 2595±75 Aksenovski Wood from mirror 826-546 902-418
41 14 GrA-16832 2660±50 Aksenovski Wood from mirror 892-794 906-778
Southern Ural and Transural regions (Orenburg, Chelyabinsk oblasts, Bashkartostan)
42 15 GrA-15862 2320±50 Filippovka Wood from the gold deer 408-210 516-200
43 15 GrA-15860 2940±50 Filippovka Wood from the gold deer 1250-1046 1304-994
44 17 Ua-16866 2430±70 Gumarovo Leather 758-402 766-394
45 17 Ua-16867 2750±75 Gumarovo Organic 982-816 1112-796
46 17 GrA-12895 2500±70 Gumarovo Organic 774-524 792-412
47 17 GrA-16829 2500±50 Gumarovo Leather 770-530 792-414
48 17 AA-40434 2623±44 Gumarovo Wood from arrow bow case 822-780 898-554
49 18 Ua-16870 2590±85 Solonchanka Wood of shaft 830-536 900-414
50 64 AA-40432 2454±58 Small Klimovski Wood from shaft 760-410 766-404
51 21 GrA-16831 2250±50 Temir Wood 378-206 392-194
52 21 Ua-16868 2250±75 Temir Bark-birch 386-202 408-64

146
 A.Yu. Alekseev et al.

Altai
53 35 Le-5788 2200±40 Bashadar dendro- sampl, Wood, 1-10 tree-rings 358-192 378-126
80 tree-rings
54 35 Le-5789 2200±20 Bashadar dendro- sampl, Wood, 11-20 tree-rings 355-195 359-191
80 tree-rings
55 35 Le-5790 2175±20 Bashadar dendro- sampl, Wood, 21-30 tree-rings 345-182 356-130
80 tree-rings
56 35 Le-5791 2145±25 Bashadar dendro- sampl, Wood, 31-40 tree-rings 194-118 342-64
80 tree-rings
57 35 Le-5792 2160±50 Bashadar dendro- sampl, Wood, 41-50 tree-rings 354-10 364-50
80 tree-rings
58 35 Le-5793 2152±25 Bashadar dendro- sampl, Wood, 51-60 tree-rings 198-118 350-68
80 tree-rings
59 35 Le-5794 2170±20 Bashadar dendro- sampl, Wood, 61-70 tree-rings 343-176 354-120
80 tree-rings
60 35 Le-5795 2190±40 Bashadar dendro- sampl, Wood, 71-80 tree-rings 358-184 372-116
80 tree-rings
61 36 GU-8355 2340±60 Pazyryk-2 Wood, all tree rings 516-254 758-200
62 36 GU-8356 2360±50 Pazyryk-2 Wood, all tree rings 516-376 760-210
Southern Siberia
63 40 Le-5838 2780±30 Tiger-Taidzhen, barrow1 Wood 980-848 992-838
64 43 Le-5646 2640±120 Kazanovka-3, barrow 2A, grave 2 Bone of skeleton 920-530 1030-400
65 45 Le-5669 2570±30 Taplaya, barrow 1, grave 2 Charcoal 802-610 806-552
66 46 Le-5679 2370±20 Cheremshino, barrow, grave 1, Wood 406-397 473-390
log, 4 layer from the centre
67 46 Le-5678 2400±20 Cheremshino, barrow, grave 1, Wood 484-401 516-399
log, 3 layer from the centre
68 46 Le-5677 2540±40 Cheremshino, barrow, grave 1, Wood 794-552 802-526
log, 2 layer from the centre
70 46 Le-5676 2710±60 Cheremshino, barrow, grave 1, Wood 900-812 990-796
log, 1 layer from the centre
71 46 Le-5680 2435±25 Cheremshino, barrow 1, grave 1, Wood 746-410 756-404
outside rings
72 46 Le-5670 2470±30 Cheremshino, barrow 1, grave 3 Wood 762-420 764-412
73 46 Le-5668 2530±25 Cheremshino, barrow 1, grave 2 Wood 786-554 792-542
74 46 Le-5671 2610±50 Cheremshino, barrow 1, grave 3 Wood 828-606 894-540
75 46 Le-5672 2660±60 Cheremshino, barrow 1, grave 1, Wood 898-792 980-556
outside rings
76 46 Le-5675 2700±50 Cheremshino, barrow 1, grave 1, Wood 898-808 926-796
central rings
77 47 Le-5651 2480±50 Pechische, barrow 3, grave 3 Bone of skeleton 764-518 770-412
78 48 Le-5652 2490±80 Sarala, barrow 2, grave 1 Bone of skeleton 770-516 790-410
Central Asia (Tuva)
79 49 Le-5848 2440±30 Aldy-Bel,branch grave Wood 752-410 760-402
80 49 GU-9181 2470±50 Aldy-Bel,branch grave Wood 762-418 766-412
81 50 Le-5446 2880±120 Arzhan Horse teeth 1210-910 1380-820
82 50 Le-5645 2750±35 Arzhan Wood, fragment 908-842 982-816
of upper log, 22 tree-rings
83 51 GU-8351 2310±60 Arzhan-Tarlag Wood, fragment 406-208 520-192
of upper log, 20 tree-rings
84 51 GU-8354 2360±50 Arzhan-Tarlag Wood, fragment 516-376 760-210
of upper log, 20 tree-rings
85 51 GU-8352 2410±70 Arzhan-Tarlag Wood, fragment 758-396 768-384
of upper log, 20 tree-rings
86 51 GU-8353 2470±60 Arzhan-Tarlag Wood, fragment of upper log 762-418 768-408
87 51 Le-5450 2455±25 Arzhan-Tarlag Wood, fragment of upper log 756-416 762-408
88 52 Ua-12968 2425±45 Dogee-Baary-2, barrow 10 Leather 752-404 762-396
89 52 Ua-12969 2435±45 Dogee-Baary-2, barrow 3 Textile 754-408 762-400
90 52 Ua-12970 2490±45 Dogee-Baary-2, barrow 1 Textile 764-528 782-414
91 52 Ua-12971 2420±45 Dogee-Baary-2, barrow 6 Textile 752-402 762-394
92 52 Ua-12972 2450±45 Dogee-Baary-2, barrow 15 Textile 758-410 764-404
93 54 Le-5603 2800±200 Suglug-Khem-1, part of artefact Wood 1260-790 1430-410
94 55 Le-5566 2300±50 Saryg-Bulun, barrow 1, grave 5 Wood 402-210 408-200
95 56 Ua-15270 2190±70 Ust’-Khadynnyg-1- barrow 37 Bone 366-162 384-58
96 56 Ua-15229 2635±70 Ust’-Khadynnyg-1, Wood from arrow 902-606 926-528
barrow 4, grave 3
97 56 Ua-15228 2805±70 Ust’-Khadynnyg-1, Leather from quiver 1016-844 1154-810
barrow 4, grave 3
98 57 Ua-12973 2360±45 Chinge-2, barrow 22, grave 2 Textile 510-380 756-256

147
 SOME PROBLEMS IN THE STUDY OF THE CHRONOLOGY OF THE ANCIENT...
early 8th century cal BC, but it turns out that all the dates
result in very wide calibrated intervals and so do not
allow a more accurate age definition. The combined date
(2562±25 BP) gives a “narrower” calibrated range: 798-
766 cal BC (1σ), 802-760, 676-662, 632-590 and 584-554
cal BC (2σ), and there is evidence that the quiver can be
attributed to the period ca 800-750 BC or to the period
from the 7th to the first half of the 6th century BC.
As one of the most famous monuments of this period
we can identify the so-called Filippovka “royal” burial
ground which was excavated in 1986-1989 by
A. Pshenichniuk (2000). The most important site is bar-
row number 1 which is of 7 m height. Different weapons,
horse bridles, golden plaques on wooden vessels, several
gold and silver Iran vessels and 26 large, extraordinary
wooden sculptures of deer which were covered by gold
and silver were found. The majority of these objects are
unique but at the same time, they demonstrate stylistic
similarity with objects from other regions of the Scythian
world – South Siberia, Altai Mountains, Central Asia, and
Northern Caucasus (Korolkova, 2000). According to the
archaeological data there are two similar dates proposed
for the Filippovka burial ground – the 5th century BC
(Korolkova (Chezhina), 1992) and the early 4th century
BC (Pshenichniuk, 2000). Samples for 14C analyses (AMS)
were taken from wooden fragments from inside the base
of the deer sculptures.
Radiocarbon dates give different chronological ranges
(GrA-15860, 2940±50 BP; GrA-15862, 2320±50 BP).
GrA-15862 date is in perfect correlation with archaeologi-
cal evidence. The combined 14C date 2630±35 BP, cali-
brated to 832 – 774 cal BC (2σ) is earlier than the archaeo-
logical dating.
The comparison of the radiocarbon age for the
Scythian time monuments of the Lower Volga River ba-
sin and the Southern Ural regions with the monuments
of the Sayan-Altai (the Arzhan and Pazyryk group) pre-
sented in Table 1 shows, that the radiocarbon age of these
monuments is significantly younger than the Arzhan bar-
row but closer to the Pazyryk group barrows.
Southern Siberia and Central Asia (Tuva)
As mentioned above the oldest monument for all
Eurasia is the royal barrow Arzhan (Central Asia and Tuva
Republic). In 2000 the first radiocarbon dates were pro-
duced for other monuments belonging to the prescythian
and early Scythian time.
The most interesting new date has been produced for
the monument Tigir-Taidzhen, barrow 1: 2780±30 BP (Le-
5838). It is very important that, according to this date and
to the archaeological finds, this barrow is synchronous with
the Arzhan barrow and can be dated to the 9th cal BC.
Another interesting monument of the Tagar culture
in the Southern Siberia (Minusinsk valley) is the
Cheremshino barrow. According to the archaeological
classification, this monument dates to the early stage of
the Tagar culture. Now the first radiocarbon dates have
been produced for this monument from the wooden bar-
row construction and have been used in the “wiggle match-
ing” method to produce a precise determination of the
148
calendar interval. According to these data this barrow can
be dated to the beginning of the 8th cal BC.
The so-called “aldy-bel” culture (Grach, 1983) existed
in Central Asia (Tuva). One should note that the earliest
Scythian barrow Arzhan is located in Tuva too. For a long
time only this monument was dated by 14C. Now 14C dates
have been produced for the Ust’-Khadynnyg-1 barrow.
Dates 2635±70 BP, wood from arrow (Ua-15229) and
2805±70 BP, leather from quiver (Ua-15228) for barrow
4, grave 3 excavated by A.D. Grach in 1980 (Grach, 1983)
can be correlated with the dates for the Arzhan barrow.
The key monument of the late stage of Scythian time,
the so-called the uyuk-saglynsk culture, is the Dogee-
Baary-2 barrow. A long series of 14C dates have been pro-
duced for this monument and the “wiggle matching”
method has been used to determine its position on the
calendar scale (Alekseev et al., 2001). The results con-
firmed the archaeological ideas about the existence of this
monument during the 5th-4th centuries BC. 14C dates for
the Arzhan-Tarlag (Gu-8351-8354) and the Chinge (Ua-
12973) barrows testify to their synchronicity. The Aldy-
Bel’ burial mound according to the 14C dates produced
from the wooden barrow construction (Le-5848, and GU-
9181) can be related to this time.
The first 14C dates produced for the monuments be-
longing to the pre-scythian and early scythian time of
Southern Siberia and Central Asia testify that some monu-
ments existed in this territory at the same time as the
Arzhan barrow.
4. CONCLUSIONS
Since the 9th-8th centuries BC the Scythian cultures
began to appear on the wide territory of the steppe and
forest-steppe zones of Eurasia. Now there are some monu-
ments, which, according to the radiocarbon dates, can be
demonstrated to be synchronous to the Arzhan royal bar-
row. The ages of monuments located in the Lower Volga
River basin, the Urals and Transurals regions are more
synchronous to the Pazyryk group barrows.
ACKNOWLEDGEMENTS
We are very grateful to the staff of the State Hermit-
age Museum and to the archaeologists from the
Chelyabinsk and Ekaterinburg Universities for the
samples presented for dating. This research is supported
by INTAS, project No 97-20362.
REFERENCES
Alekseev A.Yu., Bokovenko N.A.,.Boltrik Yu, Chugunov K.V, Cook
G,.Dergachev V.A, Kovaliukh N.N., Possnert G, van der Plicht
J, Scott E.M., Sementsov A.A, Skripkin V.V, Vasiliev S.S. and
Zaitseva G.I., 2001: A chronology of the Scythian Antiquities
of Eurasia based on new archaeological and 14C data. In:
The Proceedings of the 17th Radiocarbon Conference. Radiocar-
bon (in press).
Alekseev A.Yu., 1992: Scythian Chronicle. Scythians in the 7th-4th
centuries B.C. In: Historical and Archaeological Review. Saint
Petersburg: 206 pp (in Russian).
 A.Yu. Alekseev et al.
Gryasnov M.P., 1983: The Initial Phase of the Development of the
Scytho-Siberian Cultures. In: Archaeology of South Siberia.
Kemerovo: 3-18 (in Russian.).
Grach A.D., 1983: The historical-cultural population of the early
Scythian epoch in the Central Asia. Archaeological Journal of
the State Hermitage Museum 23: 30-42 (in Russian).
Ismagilov R.B., 1988: Burial of the Great Gumarovo Barrow in the
Southern Urals and the Problem of the Scythian Culture Ori-
gin. Arheologicheskii sbornik. The State Hermitage Museum. Saint
Petersburg: 29-47 (in Russian).
Klochko V.I., Skory S.A., 1993: Barrow No 15 near village Steblev
in Ros’ River region. Arkheologija (Kiev) 2 (in Ukrainian).
Korolkova E., 2000: The Filippovka Kurgans and the Animal Style.
The Golden Deer of Eurasia. Scythian and Sarmatian Treasures
from the Russian Steppes. Aruz J., Farkas A., Alekseev A. and
Korolkova E., eds, The Exhibition Catalogue. The Metropoli-
tan Museum of Art, New York: 69 - 71.
Ochir-Goriaeva M.A., 1988: Sauromation culture of Lower Volga
region in 6th-4th centuries B.C. Dissertation Thesis. Leningrad:
20 (in Russian)
149
Pshenichniuk A., 2000: The Filippovka Kurgans at the Heart of the
Eurasian Steppes. The Golden Deer of Eurasia. Scythian and
Sarmatian Treasures from the Russian Steppes. Aruz J., Farkas
A., Alekseev A. and Korolkova E., eds, The Exhibition Cata-
logue. The Metropolitan Museum of Art, New York: 21-30.
Shilov V.P. and Ochir-Goriaeva M.A., 1997: The Scythian Time
Tumuli in the Cemeteries Aksenovo I and II. In: Prescythian
and Scythian monuments in the South Eastern Europe. Moscow:
127-152 (in Russian).
Skory S.A., 1999: Cimmerians in Ukrainen Forest-steppe zone.
Kiev-Poltava (in Russian).
Terenozhkin A.I., 1976: Cimmerians. Kiev (in Russian).
Zaitseva G.I., Vasiliev S.S., van der Plicht J., Marsadolov L.S.,
Sementsov A.A., Dergachev V.A. and Lebedeva L.M., 1998: New
Investigations on the Cronology of the Key Sites of the Scythian
Epoch in the Sayan-Altai. Acte du colloque “C-14 Archeologie”:
315-318.
SOME PROBLEMS IN THE STUDY OF THE CHRONOLOGY OF THE ANCIENT...

150
 GEOCHRONOMETRIA Vol. 21, pp 151-156, 2002 – Journal on Methods and Applications of Absolute Chronology

RADIOCARBON DATING OF THE NASCA SETTLEMENTS

LOS MOLINOS AND LA MUÑA IN PALPA, PERU

JOCHEN GÖRSDORF1 and MARKUS REINDEL2

1
Deutsches Archäologisches Institut, Eurasien-Abteilung, Postfach 330014, D-14191 Berlin, Germany
(e-mail: 14C@dainst.de)
2
Kommission für Allgemeine und Vergleichende Archäologie des Deutschen Archäologischen Instituts,
Endenicher Straße 41, D-53115 Bonn, Germany (e-mail: reindel@kava.dainst.de)

Key words
words: Abstract: The Palpa Archaeological Project PAP investigates the relationship between
RADIOCARBON the famous Nasca lines and ancient settlements in the Palpa region, in the desert of the south
DATING, coast of Peru. Chronology will be fixed in absolute terms by radiocarbon dating of sites of
NASCA CULTURE, Los Molinos and La Muña. As a first approximation we get for the Nasca 3 culture 60-280 cal
CHRONOLOGY, AD and for Nasca 4/5 and 5 culture 320-430 cal AD. That means the transition from Early
NASCA LINES to Middle Nasca is in the range between 280-320 cal AD.

1. INTRODUCTION
The Palpa Archaeological Project of the German In-
stitute of Archaeology and the Swiss-Liechtenstein Foun-
dation for Archaeological Research Abroad investigates
the relationship between the famous Nasca lines and an-
cient settlements in the Palpa region, in the desert of the
south coast of Peru (Reindel, 1997; Reindel and Cuadra-
do, 1998 and 2000; Reindel et al., 1998a,b). The Nasca
culture is known mainly from undocumented museum
materials excavated by grave looters. There have been few
excavations which produced well documented archaeo-
logical contexts. The Palpa project aims to enlarge the
archaeological data base concerning the cultural history
of the Nasca region with emphasis on settlement studies,
large scale excavations and stratigraphic investigations.
Chronology will be fixed in absolute terms by radiocar-
bon dating. Field work includes a detailed photogrammet-
ric and terrestrial mapping of the geoglyphs of the pam-
pas, their associated archaeological features, an exhaus-
tive survey of archaeological sites, test excavations and
large scale excavations in several settlements. More than
500 archaeological sites have been recorded in the valleys
of Rio Grande, Rio Palpa and Rio Viscas (Figs 1 and 2),
dating from Middle Formative (600 BC) to Inca times
(1530 AD). The archaeological evidence indicates that the
geoglyphs originated from petroglyphs at about 400 BC
and reached their apogee in Nasca times (200 BC – 600
AD). No later geoglyphs were identified (Fig.3).
The sites of Los Molinos and La Muña functioned as
administrative centres in the early and the middle Nasca
period (0 – 400 AD). This chronological assessment could
be confirmed by several radiocarbon dates, which we
present. Settlement patterns, architecture, burial prac-
tices, the ceramic findings as well as botanical and fau-
nistic remains show that the Nasca society was well
organised and stratified. Religious specialists must have
been in charge of the rituals concerning the nearby
geoglyphs. Small shrines directly associated with the
geoglyphs, where offerings of crop fruits, textiles and con-
siderable amounts of Spondylus shells were found, dem-
onstrate that water and fertility rites were practised in
a sacred landscape which was constantly modified by the
modelling of new geoglyphs. Our aim is to show the ra-
diocarbon dating results in the frame of archaeological
context.
 RADIOCARBON DATINGS OF THE NASCA SETTLEMENTS LOS MOLINOS ...

Fig. 1. The Nasca region at the south/

west coast of Peru.

Fig. 2. Map of the investigation area with PAP numbers of the archaeological sites.

152
 J. Görsdorf and M. Reindel
2. METHODS
The bigger samples were dated in the Berlin Labora-
tory (Bln). Chemical pretreatment of samples was done
by AAA treatment (Mook and Streurman, 1983). The dat-
ing was performed with gas proportional counters of the
Houtermans-Oeschger type, using methane at 133.3 kPa
pressure as filling gas. Measurement control and data
processing were done using computer controlled system
(Görsdorf, 1990; Görsdorf and Bojadþiev, 1996). A modern
electronics is used. The preamplifier, pulse amplifier,
comparator, pulse shaper and anti-coincidence unit are
located in a box (19cm x 10cm x 5cm), which is directly
connected to the counter. The detection of variation of
the environmental radiation and the inspection of the long
153
Fig. 3. Investigation area near
the sites PAP 47,48 and 53
with geoglyphs.
time stability of the electronics were required in order
to reach the measurement accuracy (Görsdorf, 2000).
The δ13C-measurements were done at the Leibniz-Labor,
University of Kiel, Germany and are reported in permil
relative to PDB-standard.
The smaller samples were dated in the Accelerator
Mass Spectrometry Laboratory in Erlangen (Erl).
3. RESULTS
The results with sample numbers, site names and da-
ting materials are shown in Table 1. The datings are cor-
rected for isotopic fractionation using the measured δ13C
values. The 14C ages are calibrated using the program Ox
Cal v.3.5 (Ramsey, 1995, 1998 and 2000) and employing
 RADIOCARBON DATINGS OF THE NASCA SETTLEMENTS LOS MOLINOS ...

the decadal calibration curve (Stuiver et al., 1998) as a first 4. COMMENTS AND CONCLUSIONS
approximation for all samples. A Southern Hemispheric
offset of 24±3 14C yr was taken into consideration (Stuiver The calibration results of the radiocarbon datings
et al., 1998). The calibration intervals were presented for agree with the general chronological table of the Palpa area
a confidence of 68.2 % and are rounded off to 10 years. (based on Menzel, 1977), which is shown in Table 2. Only
Fig. 4 shows the calibration results of the datings in chro- the dating results of the samples Bln-5239 seems to be
nological order. too young. No explanation was found for that up to now.

Table 1. Radiocarbon samples of the Palpa Archaeological Project and dating results.
Tomb*
Architectural Unit
Sector
Unit

Layer

Ceramic Phase
Sample no.

Site Context Material Weight Lab. No. ä13C 14

C Age Calibrated Agess
(68,2%)%
[g] [‰] [BP] [cal AD]

1 La Mu¼a C 2 R. N C Hearth 5 Charcoal 120 Bln-5234 - 25.0 1711 ± 30 290 - 420

2 La Mu¼a C 2 R. S A Hearth 5 Charcoal 160 Erl-3090 - 28.0 1816 ± 43 150 - 270
3 La Mu¼a B 5 R. 2 C Hearth 5 Charcoal 105
4 La Mu¼a B 5 R. 1 E Tomb 5 Wood 350 Erl-3091 - 26.0 1685 ± 39 340 - 440
5 La Mu¼a B 5 R. 1 C Hearth 5 Charcoal 80 Bln-5235 - 26.1 1691 ± 27 350 - 430

6 Los Molinos A 1 T1 D Tomb 4? Cane 90

7 Los Molinos A 2 T1 B Tomb 3 Wood 575 Bln-5236 - 24.4 1774 ± 25 250 - 340
8 Los Molinos A 2 T1 B Tomb 3 Cane 175 Erl-3092 - 25.0 1999 ± 40 20 cal BC - 80 cal AD
9 Los Molinos A 2 T1 B Tomb 3 Charcoal 95
10 Los Molinos A 2 R. 1 C Hearth 4/5 Charcoal 100 Bln-5237 - 25.9 1694 ± 27 350 - 430
11 Los Molinos A 2 R. 1A J Arch. Fill 3 Bean 10 Erl-3093 - 24.8 1858 ± 38 130 - 240
12 Los Molinos A 2 Pass. H Arch. Fill 3 Bean 10 Erl-3094 - 24.6 1934 ± 39 50 - 140
13 Los Molinos A 3 LT6 A Tomb 4/5 Wood 345 Bln-5238 - 23.4 1727 ± 30 270 - 390
14 Los Molinos A 3 AU4 F Floor 4? Cane and Wood 60
15 Los Molinos A 3 AU4 I Arch. Fill 3/4 Maniok 140
16 Los Molinos A 3 AU2 B Refuse 3 Seed of Huarango-tree 10
17 Los Molinos A 3 AU1 D Layer 4? Seeds 10
18 Los Molinos B 1 AU2 C-D Post 3 Wood 275 Bln-5239 - 23.5 1634 ± 30 400 - 490
19 Los Molinos B 1 AU2 D Hearth 3 Charcoal 100 Erl-3095 - 26.4 1836 ± 39 150 - 250
20 Los Molinos A 4 E Arch. Fill 8 Bean 10
21 Los Molinos A 4 D Arch. Fill 8 Bean 10 Erl-3096 - 29.2 1482 ± 35 570 - 650
22 Sitio PAP-11 A 1 T1 C Tomb Oc8 Wood 25
R. =Room, AU =Architectural Unit, T =Tomb, LT =Looted Tomb, Pass. =Passage.

Table 2. Chronological Table of the Palpa area (based on Menzel, 1977).

154
 J. Görsdorf and M. Reindel

p ( ); ; y( );

La Muña
La Muña and Los Molinos

Curve intcal98
Reservoir 24±3
Phase Nasca 3
Erl-3092 1999±40BP
Erl-3094 1934±39BP
Erl-3093 1858±38BP
Erl-3095 1836±39BP
Bln-5236 1774±25BP
Bln-5239 1634±30BP
Phase Nasca 4/5 and 5
Bln-5238 1727±30BP
Bln-5237 1694±27BP
Erl-3090 1816±43BP
Bln-5234 1711±30BP
Bln-5235 1691±27BP
Erl-3091 1685±39BP
Phase Nasca 8
Erl-3096 1482±35BP

500CalBC CalBC/CalAD 500CalAD

Calibrated date

Fig. 4 The calibration results of the dates from Los Molinos and La Muña sites.The confidence limit of the hatched
boxes is 68.2% and of the broader boxes 95.4%.

A recalculation of the calibration intervals, take into ACKNOWLEDGEMENTS

account the cultural order, with the help of the Gibbs
Sampling Method (Ramsey, 1995) gives the results in
Fig. 5. The sum of calibration results date the cultures in
a first approximation. For the Nasca 3 sum (probability
of 68,2 %) we get 60-280 cal AD and for Nasca 4/5 and 5
(probability of 68,2 %) we get 320-430 cal AD. That
means the transition from Early to Middle Nasca is in the
range between 280-320 cal AD.
We gratefully acknowledge Dr. H. Erlenkeuser and
colleagues (Leibniz-Labor, University of Kiel) for δ13C
measurements. Thanks are extended to E. Lau and D.
Teckenburg for assistance in the preparation and measure-
ment of samples in the Berlin Laboratory (German Insti-
tute of Archaeology, Eurasian-Department). For the
Accelerator Mass Spectrometry datings we thank Prof. Dr.
W. Kretschmer and colleagues (University of Erlangen).

155
 RADIOCARBON DATINGS OF THE NASCA SETTLEMENTS LOS MOLINOS ...

( ) ( )

Sequence La Muña and Los Molinos

Sequence La Muna and Los Molinos {A=89.5%(A'c=60.0%)}

Sum Nasca 3
Erl-3092 100.0%
Erl-3094 101.2%
Erl-3093 102.2%
Erl-3095 105.3%
Bln-5236 90.3%
Sum Nasca 3
Sum Nasca 4/5 and 5
Bln-5238 101.9%
Bln-5237 101.4%
Erl-3090 64.5%
Bln-5234 101.6%
Bln-5235 100.4%
Erl-3091 101.3%
Sum Nasca 4/5 and 5
Phase Nasca 8
Erl-3096 100.7%

1000CalBC 500CalBC CalBC/CalAD 500CalAD 1000CalAD

Calibrated date
Fig. 5 The calibration of dating results with the Gibbs Sampling Methode. The confidence limit of the hatched boxes
is 68.2% and of the broader boxes 95.4%.

REFERENCES Archäologische Forschungen im Ausland (1996). Zürich und

Görsdorf J., 1990: Die Interpretation von 14C-Datierungen im Ber-
liner 14C-Labor. Zeitschrift für Archäologie 24: 27-34.
Görsdorf J. and Bojadþiev J., 1996: Zur absoluten Chronologie der
bulgarischen Urgeschichte. Berliner 14C-Datierungen von bulga-
rischen archäologischen Fundplätzen. Eurasia Antiqua 2: 105-173.
Görsdorf J., 2000: Datierungen im Berliner 14C-Labor. Berliner
Beiträge zur Archäometrie, Band 17: 121-131.
Menzel D., 1977: The Archaeology of Peru and the Work of Max Uhle.
Berkeley.
Mook W. G. and Streurman H. J., 1983: Physical and chemical as-
pects of radiocarbon dating. Journal of the European Study
Group on Physical, Chemical and Mathematical Techniques
Applied to Archaeology. PACT 8: 31-55.
Ramsey C. B., 1995: Radiocarbon Calibration and Analysis of
Stratigraphy: The OxCal Program. In Cook G. T., Harkness D.
D., Miller B. F. and Scott E. M., eds., Proceedings of the 15th
International 14C Conference. Radiocarbon 37(2): 425-430.
Ramsey C. B., 1998: Probability and Dating. Radiocarbon 40(1):
461-474.
Ramsey C. B., 2000: OxCal Program v.3.5. (www.rlaha.ox.ac.uk/
orau/06_01.htm).
Reindel M., 1997: Archäologische Untersuchungen zur Nasca-
Kultur und ihren Bodenzeichnungen in Süd-Peru. Jahres-
bericht der Schweizerisch-Liechtensteinischen Stiftung für
Vaduz: 79-94.
Reindel M. und Cuadrado J.I., 1998: Ausgrabungen in Los Molinos
und La Muña: Ergebnisse der Grabungskampagne 1998 des
Archäologischen Projektes Nasca-Palpa, Süd-Peru. Jahres-
bericht der Schweizerisch-Liechtensteinischen Stiftung für
Archäologische Forschungen im Ausland (1998). Zürich und
Vaduz: 123-152.
Reindel M. und Cuadrado J.I., 2000: Ausgrabungen in Los Molinos
und La Muña: Ergebnisse der Grabungskampagne 1999 des
Archäologischen Projektes Nasca-Palpa, Süd-Peru“. Jahresbe-
richt der Schweizerisch-Liechtensteinischen Stiftung für Archäolo-
gische Forschungen im Ausland (1999). Zürich und Vaduz: 67-95.
Reindel M., Cuadrado J.I. und Koschmieder K., 1998a:
Vorspanische Siedlungen und Bodenzeichnungen in Palpa,
Peru. Ergebnisse der Feldkampagne 1997 des Archäologischen
Projektes Nasca/Palpa. Jahresbericht der Schweizerisch-
Liechtensteinischen Stiftung für Archäologische Forschungen im
Ausland (1997). Zürich und Vaduz: 131-162.
Reindel M., Cuadrado J.I. und Koschmieder K., 1998b: Vorspanische
Siedlungen und Bodenzeichnungen in Palpa, Süd-Peru. Beiträge
zur Allgemeinen und Vergleichenden Archäologie 19: 313-81.
Stuiver M., Reimer P.J., Bard E., Beck J.W., Burr G.S., Hughen K.A.,
Kromer B., McCormac F.G., v.d. Plicht J. and Spurk M. 1998:
INTCAL98 Radiocarbon Age Calibration, 24,000-0 cal BP.
Radiocarbon 40(3): 1041-1083.

156
 GEOCHRONOMETRIA Vol. 21, pp 157-162, 2002 – Journal on Methods and Applications of Absolute Chronology

DATING OF THE GRAVE COMPLEX IN DACHARZÓW,

MA£OPOLSKA
HALINA TARAS1, NIKOLAJ KOVALJUKH2 and VADIM SKRIPKIN2

1
Institute of Archaeology University of Lublin, Curie-Sk³odowska 4 square, 20-031 Lublin, Poland
(e-mail: koliber@klio.umcs.lublin.pl)
2
State Scientific Centre of Environmental Radiogeochemistry, Palladin 34, 142 Kiev, Ukraine

Key words
words:
RADIOCARBON DATING,
BONES, DACHARZÓW
SITE, MA£OPOLSKA
Abstract: Radiocarbon dating has confirmed the division of the period when the grave com-
plex in Dacharzów was used into two stages, between which there was a distinct gap.
In the second stage the graves appeared in cycles, after longer breaks (100 years or more).
The cemetery was used from the end of the 17th to the 10th or 10th/9th centuries BC.

1. INTRODUCTION In the central part of the barrow was found a stone

Dacharzów (Sandomierz district) is situated in the
north-eastern part of the Sandomierz Upland (Fig. 1). In
1991 one barrow was discovered here, marked as site 1
(Florek, 1994). It is situated on the edge of the Opatówka
river valley, rising 50 metres above the flat bottom of the
valley. In the years 1994-1995 archaeological excavations
were carried out on the barrow and its surroundings
(Florek and Taras, 1996). As a result, a whole complex of
graves was uncovered, dating from the Bronze Age, from
the period of the Trzciniec Culture (Florek and Taras,
1997; Florek, 1998).
structure consisting of two chambers (Fig. 2). They had a
wooden rafter structure, which supported the walls, and
a wooden (oak) floor; the remains of the wood have been
used in radiocarbon dating.
Inside the bigger chamber there were bone remains
of six people – four women and two children. The skel-
etons, badly-preserved, were not lying in the anatomical
order, and some of the bones in the northern part were
burnt out. In the smaller chamber there were scattered
less burnt bones of, most probably, a man. The bone ma-
terial coming from all the people buried here was radio-
carbon-dated.

Fig. 1. Dacharzów, site 1. Location of the site (S – Sandomierz, D – Dacharzów).

 DATING OF THE GRAVE COMPLEX IN DACHARZÓW (MA£OPOLSKA)
The stone graves with their immediate surroundings
were covered with an earthen mound; earth for the mound
was taken mainly from the area north of the barrow,
where, as a result, a semi-circular basin was created.
On the south-western part of the mound there was
observed a semicrescent-like ditch (Fig. 2). On the cir-
cumference of the mound, in its southern and eastern
parts, eight graves were discovered (No. 2, 5, 8-12, 14)
containing inhumation burials. The skeletons are poorly-
preserved, in some cases there are only single bones pre-
served. The bone remains from all the graves but one –
No. 14 – have been radiocarbon-dated.
2. METHODS OF RADIOCARBON DATING
OF BONE SAMPLES
In the research was used the technology developed
in Kiev Radiocarbon Laboratory. This technology makes
it possible to produce lithium carbide production from
collagen or bone without preliminary deposition of them
in a pure kind (Skripkin and Kovaljukh, 1998).
The bones for this purpose are reduced to fragments, and
158
after washing with trisodium phosphate solution they are
processed by 1-3% hydrofluoric acid. This acid transforms
carbonate and partly calcium phosphate into fluoride.
Calcium fluoride practically does not dissolve in weak
acids, but change of CO3-2 and PO4-3 volumetric anions
for compact F- leads to genesis of mineral matrix which is
porous and cleaned from organic-silicate complex. Col-
lagen in this case exists in semi-bound non-hydrated state.
The essential advantage of hydrofluoric acid is its ability
to dissolve silicates and humic acids as well as products
of bacteria vital activity absorbed on them. It makes it
possible to remove introduced organic substances and
carbonic carbon, to wash and dry the processed sample
easily and qualitatively. As a result of running processes
the collagen is converted into volatile organic combina-
tions and into bone coal. The addition of manganese
dioxide plays an important role. When the temperature
is above 550oC the manganese dioxide disintegrates with
active oxygen liberation all over the volume of mixture.
Oxygen liberation runs quietly, under the broad range of
temperatures (550-940 oC). Fine-dispersed bone coal
therewith is oxidised till carbon oxide and dioxide,
Fig. 2. Dacharzów, site 1.
Grave complex of the Trzciniec
Culture: 1 - boundaries of the
investigated area, 2 – stones,
3 - human bones, 4 – original
circumference of the base of
the barrow, 5 – traces of
ploughing, 6 - range of the
basin created after taking earth
for erecting the mound,
7 – ditch, 8 – pits, 9 – hole left
by a post, 10 - pottery; I-V -
bones of individual people
buried in the graves; No 1-13
– features; A-G - pottery
(after Florek and Taras 1996).
 H. Taras et al.
and in such a kind it is absorbed by melted metallic lithium.
An essential feature of manganese oxides is their ability
to link phosphorus and sulphur in thermal stable combi-
nations. This allows getting lithium carbide of high qua-
lity, and what is more - practically from the whole carbon
content of bone organic substances. Lithium carbide
is subjected to hydrolysis, and gassing acetylene is con-
verted into benzene on vanadium catalyst. The vacuum
system for benzene syntheses is made from materials,
which adsorb not all acetylene and benzene. Constructive
particularities mentioned above allow one reach 95-97%
benzene output to the total exclusion of the memory
effect. As a result of summation of new complex techno-
logy advantages there appears a possibility for bone
samples dating carried-out with collagen total contents
up to 250-300 mg.
Measurement of benzene is carried out into the spe-
cially developed vials with the help of “Quantulus” - low-
background spectrometer.
As a result of biological processes, which have been
going on within the system bone - soil microorganisms,
the natural relation between three main carbon isotopes
(12C, 13C and 14C) undergoes certain changes. In evaluat-
ing radiocarbon age the correction is being taken in ac-
count for biological isotopic fractionation. Undertaking
such an operation is possible due to well-defined relation-
ship between the deflection of 13C isotope concentration
and the degree of 14C isotope fractionation. For this aim
the determination is made on variation in concentrations
of 13C isotope in the ready benzene by mass-spectro-
metric method. This factor usually falls within the limit
-20.7<δ13C <-18.5‰. Correction entering for the isoto-
pic fractionation is currently central for bone samples.
3. STATISTICAL APPROACH
For receiving reliable dates of bone material from the
Dacharzów settlement the statistical approach of the ra-
diocarbon dating was used. Big separate bones were cut
to several parts and then all necessary procedure steps
were made quite separately. The received dates were cal-
culated for average value. Averaged dates are much more
reliable and may be used for good evaluation of the main
historical periods.
4. ARCHAEOLOGICAL DATING RESULTS
The site in question has clear, stratigraphically con-
firmed stages of use:
1. Construction and use of the stone graves and their
surroundings. The smaller chamber, situated on the then
ground level, was added to the already existing larger one,
slightly sunk in the loess.
2. Building the mound.
3. Construction and use of the ditch surrounding the
barrow from the south-west. The ditch cut into the west-
ern periphery of the basin created by digging earth for
the construction of the mound, thus pointing to the
sequence of the events.
159
The area around the ditch continued to be used, how-
ever, there is no stratigraphic evidence that would point
to the chronological order of the following events:
– filling the ditch and using it for two burials,
– the appearance of further graves on the circumference
of the mound that together with the ditch formed a ring.
The only certain thing that was found was that graves
No. 11 and 12 – just like No. 2 and 5, that were uncovered
in the ditch – appeared after the mound was made be-
cause they are situated in the eastern part of the basin
created as a result of erecting the mound (Fig. 2). Since
the flat graves form a regular ring on the circumference
of the mound, the logical conclusion is that all of them
were built after the barrow was made.
It has been assumed that the ditch was filled at one
go. The claim is supported by the homogenous character
of the filling material, both in its colour and texture, and
the absence of clear pit contours as in the case of grave
No. 2, which would point to a later digging of the grave in
the filled ditch. As far as grave No. 5 is conserved, the
situation is more complex: the contour of a rectangular,
shallow pit is visible only on the level and it not possible
to see the contour. Under the circumstances, it seems that
graves No. 2 and 5 were built during the using (grave No.
5) and filling (grave No. 2) of the ditch.
The objects found in graves 1A and 1B and in their
surroundings are connected with the first stage of using
the cemetery, namely the period before the mound was
built. The identical style of their production enables one
to date them to the first half of phase II of the Bronze
Age (16th – 16th/15th centuries BC) and also suggests that
the period in which they were being deposited in the graves
did not last too long.
The second stage in the use of the cemetery is con-
nected with material coming from the graves built after
the erection of the mound, on its circumference. The
material consists of the equipment from graves No. 2, 5
and 11. The formal features of the pottery found in these
graves are typical of the late or terminal stage of the
Trzciniec Culture, both in Ma³opolska (Górski, 1994) and
in other regions (Taras, 1995), which are dated to the end
of phase II and phase III of the Bronze Age (14th/13th –
12th centuries BC), and in eastern Poland even longer
(Górski, 1998; Taras, 1998).
The analysis of the objects found in individual graves
shows that between the stage of using the stone graves
and the appearance of graves on the circumference of the
mound there was a considerable time gap, possibly even
200 – 300 years.
5. RADIOCARBON DATING RESULTS
Radiocarbon dating was carried out in the Kiev Labo-
ratory. The calibrated age was obtained using three cali-
brations programs worked out in: Groningen (Van der
Plicht, 1993), Oxford (OxCal, v. 3.5) and Cologne (We-
ninger, 1986 and 1993). In the case of well-preserved ma-
terial (remains of wood from the central graves, skeletons
in good condition) between 2 and 5 samples were dated,
in other cases single dating were done. The obtained dates
 DATING OF THE GRAVE COMPLEX IN DACHARZÓW (MA£OPOLSKA)

Table 1. Age of samples from Dacharzów, site 1.

14
Lab. Code Place of origin C Age Cal Age [BC] Point dating [BC] Cal Age [BC]
(material) [BP] (van der Plicht, 1993) (Weninger, 1993) (Ox Cal v.3.5)
Ki-8548 Feature 1A 3340±60 1σ 1685-1599 1595±73 68.2% 1690-1520
(wood) 1587-1577
2σ 1747-1495 95.4% 1770-1490
Ki-8106 Feature 1A 2830±70 1σ 1053-899 958±95 68.2% 1130-890
(wood) 2σ 1131-829 95.4% 1220-820
Ki-8610 Feature 1A 3335±45 1σ 1587-1581 1580±62 68.2% 1690-1580
(wood) 2σ 1693-1523 95.4% 1700-1510
Ki-8614 Feature 1A 3350±50 1σ 1687-1601 1599±66 68.2% 1690-1580
(wood) 1585-1583
2σ 1699-1521 95.4% 1750-1510
Ki-8615 Feature 1A 3450±80 1σ 1829-1683 1745±109 68.2% 1890-1680
(wood) 2σ 19451-1599 95.4% 1950-1520
Ki-8089 Feature 1A-I 3445±90 1σ 1833-1681 1740±120 68.2% 1890-1630
(bone) (women) 2σ 1957-1523 95.4% 1980-1520
Ki-8090 Feature 1A-I 3340±160 1σ 1775-1435 1604±187 68.2% 1780-1430
(bone) (child) 2σ 2035-1260 95.4% 2150-1200
Ki-8091 Feature 1A-II 2800±80 1σ 1023-891 923±90 68.2% 1050-840
(bone) (women) 2σ 1131-805 95.4% 1220-810
Ki-8092 Feature 1A-II 2820±80 1σ 1051-895 937±100 68.2% 1080-890
(bone) (child) 2σ 1133-823 95.4% 1220-810
Ki-8314 Feature 1A-III 3270±70 1σ 1621-1491 1521±79 68.2% 1630-1490
(bone) 2σ 1689-1411 95.4% 1690-1400
Ki-8315 Feature 1A-III 3220±70 1σ 1527-1411 1465±75 68.2% 1530-1410
(bone) 2σ 1639-1375 95.4% 1690-1370
Ki-8316 Feature 1A-III 3310±70 1σ 1641-1519 1566±82 68.2% 1690-1510
(bone) 2σ 1699-1435 95.4% 1750-1430
Ki-8094 Feature 1A-IV 3340±70 1σ 1593-1525 1593±81 68.2% 1690-1520
(bone) 2σ 1773-1491 95.4% 1780-1440
Ki-8317 Feature 1A-IV 3415±70 1σ 1775-1679 1679±99 68.2% 1780-1620
(bone) 2σ 1833-1597 95.4% 1890-1520
Ki-8318 Feature 1A-IV 3360±70 1σ 1693-1599 1605±84 68.2% 1700-1580
(bone) 2σ 1777-1497 95.4% 1780-1490
Ki-8549 Feature 1B 3320±70 1σ 1643-1521 1579±81 68.2% 1690-1520
(wood) 2σ 1745-1437 95.4% 1750-1430
Ki-8107 Feature 1B 3390±200 1σ 1925-1445 1674±241 68.2% 1940-1440
(wood) 2σ 2205-1255 95.4% 2300-1100
Ki-8611 Feature 1B 3280±45 1σ 1621-1515 1537±61 68.2% 1630-1500
(wood) 2σ 1641-1489 95.4% 1690-1440
Ki-8616 Feature 1B 3300±50 1σ 1623-1521 1554±63 68.2% 1630-1510
(wood) 2σ 1689-1491 95.4% 1690-1440
Ki-8095 Feature 1B-V 3340±60 1σ 1587-1577 1594±73 68.2% 1690-1520
(bone) 2σ 1747-1495 95.4% 1770-1490
Ki-8319 Feature 1B-V 3270±70 1σ 1621-1491 1521±79 68.2% 1630-1490
(bone) 2σ 1689-1411 95.4% 1690-1400
Ki-8096 Feature 2 2840±60 1σ 1051-915 975±85 68.2% 1120-900
(bone) 2σ 1131-891 95.4% 1220-830
Ki-8320 Feature 2 2820±60 1σ 1049-897 942±80 68.2% 1050-890
(bone) 2σ 1127-831 95.4% 1130-830
Ki-8097 Feature 2 2790±70 1σ 1003-891 907±78 68.2% 1010-830
(bone 2σ 1127-811 95.4% 1130-800
Ki-8098 Feature 5 3270±70 1σ 1621-1491 1521±79 68.2% 1630-1490
(bone) 2σ 1689-1411 95.4% 1690-1400
Ki-8321 Feature 5 3160±70 1σ 1517-1387 1408±80 68.2% 1520-1380
(bone) 2σ 1537-1261 95.4% 1610-1250
Ki-8322 Feature 5 3180±70 1σ 1521-1393 1438±75 68.2% 1530-1390
(bone) 2σ 1617-1295 95.4% 1620-1290
Ki-8617 Feature 5 3290±60 1σ 1637-1515 1544±72 68.2% 1640-1510
(bone) 2σ 1689-1435 95.4% 1690-1430
Ki-8099 Feature 8 2940±70 1σ 1217-1043 1116±107 68.2% 1260-1010
(bone) 2σ 1319-973 95.4% 1320-970
Ki-8100 Feature 9 6980±70 1σ 5913-5785 5806±83 68.2% 5920-5770
(bone) 2σ 5927-5727 95.4% 5930-5720

160
 H. Taras et al.

Ki-8101 Feature 10 2770±80 1σ 977-831 897±80 68.2% 1000-830

(bone) 2σ 1127-801 95.4% 1130-790
Ki-8102 Feature 10 2980±70 1σ 1315-1125 1175±111 68.2% 1320-1110
(bone) 2σ 1325-1005 95.4% 1400-1000
Ki-8323 Feature 10 3070±70 1σ 1411-1259 1311±92 68.2% 1420-1250
(bone) 2σ 1463-1185 95.4% 1500-1120
Ki-8324 Feature 10 2995±70 1σ 1317-1187 1196±112 68.2% 1320-1120
(bone) 2σ 1405-1041 95.4% 1410-1010
Ki-8103 Feature 11 2950±70 1σ 1261-1047 1127±108 68.2% 1270-1040
(bone) 2σ 1321-995 95.4% 1320-970
Ki-8104 Feature 11 2595±80 1σ 687-659 689±132 68.2% 700-540
(bone) 2σ 901-513 95.4% 910-480
Ki-8325 Feature 11 2800±70 1σ 1015-893 916±82 68.2% 1020-890
(bone) 2σ 1129-815 95.4% 1130-810
Ki-8105 Feature 12 3050±70 1σ 1405-1257 1293±98 68.2% 1410-1250
(bone) 2σ 1445-1123 95.4% 1450-1050

Table 2. Dacharzów, site 1. Average 14C ages and calibration results.

14
Lab. Code Place of origin C Age Cal Age [BC] Point dating [BC] Cal Age [BC]
[BP] (van der Plicht, 1993) (Weninger, 1993) (Ox Cal v.3.5)
Ki-8548/8610/ 8614/ 8615 Feature 1A 3370±30 1σ 1673-1621 1636±52 68,2% 1690-1610
(wood) 2σ 1695-1601 95,4% 1740-1600
Ki-8314-8316 Feature 1A-III 3265±40 1σ 1537-1495 1500±56 68,2% 1610-1490
(bone) 2σ 1623-1437 95,4% 1640-1430
Ki-8094/8317/8318 Feature 1A-IV 3370±40 1σ 1693-1615 1620±62 68,2% 1700-1600
(bone) 2σ 1741-1599 95,4% 1750-1520
Ki-8549/8611/8616 Feature 1B 3300±30 1σ 1603-1525 1554±46 68,2% 1610-1520
(wood) 2σ 1637-1519 95,4% 1690-1510
Ki-8095/8319 Feature 1B-V 3305±30 1σ 1591-1525 1557±45 68,2% 1620-1525
(bone) 2σ 1637-1521 95,4% 1690-1510
Ki-8096/8320 Feature 2 2830±30 1σ 959-927 959±44 68,2% 1050-900
(bone) 2σ 1049-903 95,4% 1130-890
Ki-8098/ 8321/8322/ 8617 Feature 5 3225±35 1σ 1477-1455 1468±34 68,2% 1520-1440
(bone) 2σ 1521-1437 95,4% 1540-1410
Ki-8102/8323/8324 Feature 10 3015±40 1σ 1243-1213 1236±80 68,2% 1320-1210
(bone) 2σ 1323-1207 95,4% 1400-1120
Ki-8103/8325 Feature 11 2875±35 1σ 1055-999 1017±61 68,2% 1130-990
(bone) 2σ 1129-971 95,4% 1130-920

6. DISCUSSION

confirm the division into an earlier period connected with
the use of the stone chambers (dates from bone and wood
samples) and a later one (graves on the circumference –
dates from bone samples) and point to a distinct gap be-
tween the two stages. They do not, however, allow one to
state clearly the order in which the individual graves on
the circumference appeared, because the dates from single
samples are not fully credible – an extreme case is here
the date obtained from the bone sample from grave No. 9
(Fig. 1), while for another grave (No. 14) no date has been
established due to the insufficient amount of bone mate-
rial. The list of dates suggests that all the graves were built
in cycles between 1450 and 950 BC. Thus, between the
burials of people from graves 1A and 1B and the burials
of those from grave No. 5 (or, to be precise, between the
death of the last person to be buried in grave No. 5) appro-
ximately 50 years passed. During that time, the mound
was erected and the ditch was dug. Between the burial in
grave No. 5 and the next ones (graves No. 10 and 12)
a maximum of 150 – 200 years passed.
Radiocarbon dating confirms the dating of the first
stage of using the cemetery to the 16th century BC. The
average dates obtained are generally within the years 1630
– 1500 BC; a couple of dates based on single samples do
not fall into this period: the date obtained from the bone
sample of woman I (Fig. 2, feature 1A-I) – second half of
the 18th century BC – and that from woman and child II
(Fig. 2, feature 1A-II) – second half of the 10th century
BC. There is no justification for such dating in the stratig-
raphy of the site; the possibility of burying the bodies in
the grave at a later time has also been excluded.
Another surprise was the dates from feature No. 5
– the grave located in the ditch, which, after calculating
the average date, set the time of death of the person bur-
ied there (possibly also the time the grave was built) at
approximately 1450 BC. The average date for feature No.
2, another grave from the ditch, is much later – approxi-
mately 950 BC. In the light of the above, the ideas about
how the ditch was used and how it was filled should be
revised. It may have been filled at one go (which view is

161
 DATING OF THE GRAVE COMPLEX IN DACHARZÓW (MA£OPOLSKA)
Age BC Allocation of the averaged dates of bones for Dacharzów
1650
No 1A-IV
1550 No 1B-V
No 1A-III
No 5
1450
1350
1250
No 10
1150
1050
950
850
Fig, 3. Dispersion averaged radiocarbon dates of bones from Dacharzów, site 1.
supported by the character of the filling) as late as in the
10th century and that is when grave No. 2 appeared, while
grave No. 5 (a secondary burial?) comes from the period
of using the ditch. Another possibility is that the ditch was
filled already in the 15th/14th century BC, after grave No. 5,
was built and grave No. 2 was dug in the filling of the ditch
at a later time. If so, the process of filling the grave pit
must have been carried out in such a way that the earth
dug out from the grave was not mixed with the earth from
the area surrounding the ditch. There is a third possibility:
both of the graves were dug in the previously filled ditch at
different times and in such conditions that the earth from
the graves and that of the surrounding area did not mix.
The youngest dates obtained for graves No. 2 and 11
could point to the fact that some enclaves of Trzciniec
Culture settlement (or the religious tradition connected
with the culture) survived in central and eastern Poland
for a much longer time than was suggested by the hitherto
available sources, that is even till the end of phase IV of
the Bronze Age (Ha B1).
REFERENCES
Florek M., 1994: Cmentarzyska kurhanowe i kopce na lessach
sandomiersko-opatowskich. Stan badañ. Charakterystyka.
Próba okreœlenia funkcji i chronologii (Barrow cemeteries and
individual barrows on Sandomierz-Opatów loesses). Materia³y
i Sprawozdania Rzeszowskiego Oœrodka Archeologicznego za rok
1993 (Materials and Reports of Rzeszów Archaeological Centre
for 1993): 251-280.
Florek M., 1998: Recepcja “mogi³owych” wzorców kulturowych
w obrz¹dku pogrzebowym ludnoœci kultury trzcinieckiej na
przyk³adzie zespo³u sepulkralnego w Dacharzowie i innych
wybranych stanowisk z terenu Ma³opolski (The reception of the
Tumulus Culture elements in the funeal rites of the Trzciniec
Culture people. An example of the sepulchral assemblage at
Dacharzów and some other sites from the Little Poland). In:
162
No 11
No 2
Feature
Koœko A. and Czebreszuk J., eds, “Trzciniec” – system kulturowy
czy interkulturowy proces? (Trzciniec-culture system or interculture
process?). Poznañ: 135-144.
Florek M. and Taras H., 1996: Sprawozdanie z badañ zespo³u
grobowego kultury trzcinieckiej na stanowisku 1 w Dacha-
rzowie, gm. Wilczyce, woj. tarnobrzeskie (Report from the
explorations of the sepulchral complex of the Trzciniec Culture
in Dacharzów, Wilczyce Municipality, Tarnobrzeg Voivodeship).
Archeologia Polski Œrodkowowschodniej 1: 63-68.
Florek M. and Taras H., 1997: Möglichkeiten der Interpretation
von Bestattungsbräuchen und Gesellschaftlichen Fragen in der
Trzciniec-Kultur. Am Beispiel des Hûgelgrabs in Dacharzów.
In: Blajer W., eds., Beiträge zur Deutung der bronzezeitlichen Hort-
und Grabfunde in Mitteleuropa. Kraków: 65-89.
Górski J., 1994: Periodyzacja kultury trzcinieckiej na lessach pod-
krakowskich (Periodisation of the Trzciniec Culture on the loess
in the vicinity of Cracow). In: Czopek S., ed., Problemy kultury
trzcinieckiej (Problems of Trzciniec Culture). Rzeszów: 23-49.
Górski J., 1998: The foudations of Trzciniec Culture taxonomy
in western Ma³opolska. In: The Trzciniec area of the early Bronze
Age civilisation: 1950-1200 BC. Baltic-Pontic Studies 6: 7-31.
Skripkin V.V. and Kovalyukh N.N., 1998: Recent Developments in
the Procedures Used at the SSCER Laboratory for the Routine
Preparation of Lithium Carbide. Radiocarbon 40(1): 211-214.
Taras H., 1995: Kultura trzciniecka w miêdzyrzeczu Wis³y, Bugu
i Sanu (The Trzciniec Culture between the Vistula and Bug and
San Rivers), Lublin (in Polish).
Taras H., 1998: The bases for taxonomy of the Trzciniec Culture in
the southern part of the area between the Vistula and Bug
rivers. In: The Trzciniec area of the early Bronze Age civilization:
1950-1200 BC. Baltic-Pontic Studies 6:32-47.
van der Plicht J., 1993: The Groningen radiocarbon calibration
program. Radiocarbon 35(1): 231-237.
Weninger B., 1986: High precession calibration of archaeological
radiocarbon dates. Acta Interdisciplinaria Archaeologica IV.
Nitra: 11-53.
Weninger B., 1993: Radiocarbon Calibration <calKN>. April 1993.
Dendro and Archaeological Wiggle Matching. Koln.
 GEOCHRONOMETRIA Vol. 21, pp 163-166, 2002 – Journal on Methods and Applications of Absolute Chronology

DETERMINATION OF USAGE AND ABSOLUTE

CHRONOLOGY OF A PIT FEATURE AT THE EARLY
BRONZE I ASHKELON MARINA, ISRAEL,
ARCHAEOLOGICAL SITE

D.I. GODFREY-SMITH1 and S. SHALEV2

1
Department of Earth Sciences, Dalhousie University, Halifax, N.S., B3H 3J5, Canada (e-mail: DIGS@is.dal.ca)
2
Institute for Maritime Studies and Department of Archaeology, University of Haifa, 31905 Haifa, Israel

OSL AND TL DATING, Abstract: A study of the luminescence properties of one of several pit features removed from
BRONZE AGE, the Ashkelon Marina EB1 (Early Bronze I) archaeological site during a 1998 excavation
ASHKELON unequivocally determines their function in antiquity.
MARINA SITE The features are shallow (£ 50 cm) cup-shaped pits preserved in the ground. A hardened and
reddened layer of earth £ 3cm thick forms the shape of each pit, and a thin layer of white
calcite is observed to lie upon the hardened earth. The pit is filled with soft buff coloured,
quartz-dominated sediments, indistinguishable from the sediments which underlie it. This
feature, and several others at the site, are suspected to be putative fire pit installations, over
which crucibles for the melting of copper had been placed. However, the lack of any direct
association of copper residues or artifacts found at the site with any of the pit features leaves
this hypothesis unproven. Previous investigations, which included X-ray diffraction, differ-
ential thermal analysis, optical mineralogy studies, and FT-IR spectral measurements, have
been unable to confirm the association of the pit features with fire. Calibrated radiocarbon
dates place the use of the site at 5500-5300 BP.
We applied optical dating and thermoluminescence (TL) dating to the hardened red layer and
the overlying fill sediments, in order to determine the last time of firing and/or exposure to sun-
light of the two components of the feature. The premise driving our investigations is the fact
that heated sediments will give the correct TL age. In contrast, unheated sediments will give an
incorrect TL age far in excess of the depositional age, but will give a correct optical dating age.
The TL analyses yielded ages of 5160 ±380 years for the hardened rim and 24,600 ±1600
years for the fill. Optical dating of the fill yielded an age of 5260 ±380 years, which is in
excellent agreement with the TL age on the rim. These results fulfil the hypothesized results
precisely. On this basis, we conclude that the pit features at the Ashkelon Marina archaeo-
logical site were fire pits used in early copper smelting technology.

1. SITE DESCRIPTION holes or pits (“installations”) of hardened sediment in

Between 1996 and 1998 a rescue excavation uncovered
an Early Bronze Age I (EB I) site at 18.5 m.a.s.l., above
the Marina Beach in Ashkelon, Israel (Fig. 1). The re-
mains of human activity included pottery shreds, animal
bones, metal objects, amorphous small metal lumps and
copper droplets, copper slag, and crucible fragments. The
scattered archaeological material represents an intensive
copper melting and refining activity and is the first metal
workshop discovered in the Levant. The material remains
clearly belong to the Early Bronze Age I cultural phase.
The major and almost the only architectural features
unearthed were several small and empty shallow conical
the ground.
No metals or any residues of metal activity, as well as
no other archaeological remains nor any archaeological
debris were found within or in connection with the instal-
lations in the ground. The slag and crucible fragments
were found at a distance of at least 3 m from any of these
installations. Thus, there is no archaeological proof that
these totally clean and partially preserved installations
were a part of the copper melting process. They are, how-
ever, the only man made features that could have served
in this process.
Two AMS radiocarbon dates measured at the Instute
of Physics, University of Aarhus, Denmark place the use
 DETERMINATION OF USAGE and ABSOLUTE CHRONOLOGY...
Fig. 1. Location of Ashkelon, Israel.
of the site at 5580-5330 cal BP and 5450-5300 cal BP; both
are 1 standard deviation ranges.
2. PIT FEATURES
The features are shallow (<50 cm) cup-shaped pits
preserved in the ground (Fig. 2). A hardened and red-
dened layer of earth 3 cm thick forms the shape of each
pit, and a thin layer of white calcite is observed to lie upon
the hardened earth. The pit is filled with soft, buff
coloured, quartz-dominated sediments that are indistin-
guishable from the sediments which underlie it. The instal-
lations appear in clusters; for example, three were found
in a single excavation unit during the 1999 field season.
All appear to be similar in composition. This suggests that
all may have been deliberately constructed in the same man-
ner, and/or that all served the same function.
The feature illustrated, and several others at the site,
are suspected to be fire pit installations, over which cru-
cibles for the melting of copper would have been placed.
However, the lack of any direct association of copper resi-
dues or artifacts found at the site with any of the pit fea-
tures leaves this hypothesis unproven. Previous investi-
gations on seven installations which had been removed
intact from the site included X-ray diffraction, optical
mineralogy studies, differential thermal analysis, FT-IR
164
Fig. 2. The top and side outlines of pit feature INS-6,
showing the locations of the samples collected for
luminescence analyses.
spectral measurements, and phytolith analysis. These
methods, however, have been unable to confirm the
association of the pit features with fire (Palatnik, 1999).
3. MOTIVATION FOR THE ANALYSES
We undertook this study in an attempt to conclusively
determine the origin of the pit features at this site. The
premise driving our investigations is the fact that a heated
sediment should give the correct TL age (Aitken, 1985).
However, since the TL signal is not completely erased by
exposure to light, an unheated sediment will always give
a TL age well in excess of the depositional age. In con-
trast, the same unheated sediment should give a correct
optical dating age, provided that the rate of sedimenta-
tion was sufficiently slow to allow complete zeroing of the
optical signal (Godfrey-Smith, 1994).
We therefore applied optical dating (OSL) and ther-
moluminescence dating (TL) to quartz grains extracted
from the hardened red layer and the overlying fill sediment,
in order to determine the last time of firing and/or expo-
sure to sunlight of the two components of the feature.
In addition to the principles generalized above, we also
predicted that, if the rim sample had indeed been exposed
to a high temperature, and if the infilling was reasonably
rapid following the abandonment of the pits, as may be
expected on the highly exposed coastal plain of the eas-
tern Mediterranean Sea, then the optical age of the fill
should closely match the TL age of the rim.
 D.I. Godfrey-Smith and S. Shalev

TL measurements create reference TL curves for quartz, typically 10°/s.

For each sample, six aliquots were prepared, each com- These shapes are typical of fired quartz (ex. from pottery)
posed of ~5 mg quartz on a 1cm Al disk. Half of these and unheated quartz (ex. from sediment), respectively.
were irradiated with a calibrated gamma dose of 10 Gy. The plateau tests, also shown in Figs 3 and 4, yield
After a few days of rest in complete darkness, the TL of mean De’s which differ by a factor 4.5 for the two samples.
all aliquots was measured at 3°/s to 450°C. The mean De for ASHK-1 = 8.0±0.4 Gy (280-330°C
The TL glow curves were mass normalized. Thermally- plateau), while for ASHK-2 the mean De = 36.2±1.2 Gy
shifted glow curves were aligned to the rest of the data (280-335°C plateau).
set. For each 5° TL integral, a two-point De was computed
using the least-squares linear fit, with the data points Single Aliquot Optical Dating
weighed inversely with respect to intensity. A plateau test The data shown in Figure 5 demonstrates that some
was constructed for each sample using the TL and De data aliquots represent grains which were more completely
between the 200-375°C range. bleached by exposure to sunlight than others. The best
De quoted below is based on the aliquots that were most
Optical dating measurements completely bleached to light. Here, it is an average of the
Single aliquot analysis on 15 aliquots of ~5mg was lowest four points on the graph, or 7.6±0.4 Gy.
performed, using restricted green light stimulation, and
detection in the near-UV region, a preheat of 230°C, held Table 2. Age results.
for 60 seconds, a shine of 0.5 s at 120°C, and cumulative Sample Dose De Dose rate R Apparent age
[Gy] [Gy/ka] [ka]
radiation doses of 5,10, 20, 30, 40, 55, and 70 Gy. A post-
ASHK 1 Rim TL 8.0 ± 0.4 1.55 ± 0.08 5.18 ± 0.38
additive preheat correction was applied.
ASHK 2 Fill TL 36.2 ± 1.2 1.45 ± 0.08 24.9 ± 1.58
The past dose De was deduced on the basis of the linear
ASHK 1 Rim OSL minimum 7.2 ± 0.5 1.45 ± 0.08 4.93 ± 0.43
least squares fit to preheat-corrected data. The resulting
ASHK 2 Fill OSL best 7.6 ± 0.4 1.45 ± 0.08 5.26 ± 0.38
De’s were plotted against each aliquot’s mass-normalized
natural luminescence intensity.
S a m p le A S H K -1 , ri m o f p it f e a t u r e
8 ,0 0 0
4. DOSIMETRY
N a tu ra l

Bulk material was crushed to a fine powder using a N + 10G y

T h e r m o lu m in e s c e n c e
(c o u n t s / 5 K - m g )

tungsten carbide ball mill, and allowed to rest for 1 month 6 ,0 0 0

prior to analyses. Th and U activities were measured on
loose powders using thick source alpha counting. The
values quoted are the averages of sealed and unsealed 4 ,0 0 0
counts. K2O concentrations were obtained by atomic ab-
sorption at a commercial laboratory (Bondar-Clegg of
Vancouver, BC). Water contents were assumed based on
2 ,0 0 0
known information on the site’s location and typical mois-
ture regimes in coastal Israel today.

Table 1. Values used to compute dose rates. 0

200 225 250 275 300 325 350
Sample Depth K2O Total α Th α
[m b.s.] [%] [ks-1 cm-1] [ks-1 cm-1] T e m p e r a t u r e (° C )
ASHK-1 Rim 0.70 0.51 0.537 ± 0.011 0.220 ± 0.033
14
AASHK-2 Fill 0.58 0.27 0.585 ± 0.011 0.241 ± 0.035
12
Water content = 0.06±0.05.
Average grain size 120 mm, etched with concentrated HF.
10
b-value = 0.
D e (G y)

8
5. RESULTS
6
Thermoluminescence
There is a clear distinction in the natural intensities 4
and the glow curve shapes of the two samples, shown in
Fig. 3 and 4. ASHK-1 has a peak TL intensity approxi- 2
mately one sixth as high as ASHK-2. ASHK-1 shows A S H K -1 , rim o f p it fe a tu re
a maximum TL peak which falls at the nominal 325°C TL 0
200 225 250 275 300 325 350
peak, and has a very low 375° C nominal TL peak, while
T e m p e ra tu re (° C )
ASHK-2 has its TL maximum at the nominal 375° C TL peak.
Note that these peaks are shifted to 307°C and 345°C Fig. 3. Thermoluminescence glow curves and plateau test
in our data due to a lower heating rate than that used to for ASHK-1.

165
 DETERMINATION OF USAGE and ABSOLUTE CHRONOLOGY...

A S H K -2 , f ill o f p it f e a t u r e 6. SUMMARY
2 5 ,0 0 0
The apparent TL age of the fill is 4.5 times older than
T h e r m o lu m in e s c e n c e (c o u n t s / 5 K - m g )

N a tu ra l
that of the underlying rim, even though their dose rates
N + 10 Gy
2 0 ,0 0 0 are nearly identical. Based on the simple natural laws of
stratigraphic succession, such a result is clearly not a rea-
sonable one if the two samples had identical thermal and
1 5 ,0 0 0 depositional histories. Thus, we must conclude that
sample ASHK-1 experienced a different thermal history
than ASHK-2. While ASHK-1 has only the radiation dose
1 0 ,0 0 0
De accrued since it was heated, sample ASHK-2, which
has not been exposed to heat also carries a large residual
5 ,0 0 0 dose of 28 Gy due to the unbleachable TL signal typical
of unheated sediments. Optical dating of the fill yielded
an age of 5260±380 years and is in excellent agreement
0 with the 5180±380 years TL age of the rim, indicating that
200 250 300 350 400 the infilling of the pit feature rapidly followed its creation
T e m p eratu re ( ° C ) and abandonment. These ages are also in an agreement
with the radiocarbon chronology.
50 These results precisely fulfill our hypotheses. We con-
clude that the pit features at the Ashkelon Marina EB1
archaeological site originated as fire pits used in early
40
copper smelting technology.

30
ACKNOWLEDGEMENT
D e (G y )

We thank Mr. Kevin Vaughan of Dalhousie Univer-

20 sity for technical assistance in the luminescence measure-
ments. The Thermally and Optically Stimulated Lumines-
cence Laboratory at Dalhousie Iniversity is supported by
10 the Natural Science and Engineering Research Council
P la t e a u t e s t
(NSERC) and the Social Sciences and Humanities
A S H K -2 , f ill o f p it fe a t u re
Research Council (SSHRC), both of Canada, through
0
200 250 300 350 400 research grants to D.I.G-S.
T e m p e ra t u re (° C )
REFERENCES
Fig. 4. Thermoluminescence glow curves and plateau test
for ASHK-2. Aitken M.J., 1985: Thermoluminescence dating. Academic Press,
London.
Godfrey-Smith D.I., 1994: Thermal effects in the optically stimu-
Optical dating of ASHK-2 fill, lated luminescence of quartz and mixed feldspars from sedi-
Single Aliquot analysis ments. Journal of Physics D 27:1-10.
Palatnik M., 1999: 5500 years old metal production in Ashkelon:
12 The meaning of the archaeological evidence. MSc thesis,
Weizmann Institute of Science, Israel.
10

8
De (Gy)

0
0 10000 20000 30000
Natural Luminescence ( counts / 0.5 s -mg)

Fig. 5. Single aliquot optical dating results for ASHK-2.

166