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Quaternary Geochronology (Quaternary Science ReviewsL Vol. 13. pp. 563--567. 1994.

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COMBINATION OF A R C H A E O M A G N E T I S M AND T H E R M O L U M I N E S C E N C E FOR


P R E C I S I O N DATING

H. Becker,* H.Y. G 6 k s u t and D.F. R e g u l l a t


*Bayerisches Landesamt fiir Denkmalpflege, Abt. Vor- und Friihgeschichte, Hofgraben 4, D-80539 Mi~nchen,
Germany
t G S F - - Forschungszentrum, Institut fiir Strahlenschutz, Neuherberg, Postfach 1129,
D-85758 Oberschleissheim, Germany

Archaeomagnetic dating was applied to two chalk-burning ovens from an early medieval noble-cemetery. Usually
this method allows dating by the investigation of the geomagnetic declination and inclination through the
thermoremanent magnetisation of baked clay in situ. However, in this case the method resulted in multiple
dates since it was not possible to distinguish the branching of the geomagnetic secular variation curve.
Thermoluminescence dating was applied to the same samples to overcome the problem of multiple dates.
This first combined application of archaeomagnetism and thermoluminescence for dating yielded A.D. 670+30
for the two ovens, which dates the first stone-church at the site after a wooden predecessor archeologically
dated A.D. 620--630.

INTRODUCTION SITE AND SAMPLE DESCRIPTION

Archaeomagnetic (AM) and thermoluminescence The samples were collected from two ovens found
(TL) dating methods can, under certain conditions, inside an early medieval noble-cemetery, with a wooden
be applied to the same materials like baked clays and a stone-church, close to the town of Herrsching
(Aitken, 1970). There are two essential requirements in Bavaria, Germany, which was under excavation in
for this to remain true: the degree of heating should August 1982. The sampling could not cover the whole
be sufficiently high, and the material must have structure, because of the complete destruction of the
remained undisturbed since cooling down from its walls; but there was still burnt chalk left in the centre
last firing. of the floor. The samples originate from the floor of
A precision of up to +10 years may be achieved this oven which consists of a 5-10 cm thick layer of
with the AM dating method during the medieval baked clay containing many pebbles. The baked clay
epoch by the determination of geomagnetic inclination. was very wet when it was collected and rather soft.
However, the method has the drawback that it can The archaeomagnetic sampling procedure followed a
yield multiple dates over several centuries if one modified recipe of Thellier (Becker, 1978) using big
cannot distinguish the branch of the geomagnetic samples covered by gypsum plaster. The orientation of
secular variation curve. the samples as determined with a precision spirit-level,
Another problem for AM dating derives from the compass and sun-azimuth was better than 0.5 °.
distortion of the thermoremanent magnetisation of the The samples carried only a weak remanent magneti-
burnt structure due to magnetic refraction. During the sation, but they had a light red colour indicating a
acquisition of magnetisation while cooling down below high firing temperature and the presence of haematite.
the blocking temperature of the magnetic minerals the The carrier of the main thermoremanent magnetisation
geomagnetic field may be distorted by the magnetic might be maghemite. A rock magnetic investigation is in
field of the burnt structure itself (Schurr, 1986). At progress for the identification of the magnetic minerals.
the moment there are no direct criteria to realise this The surface of the oven was exposed to the sun for
effect and correct for it. several weeks during the excavation period. But, as the
In the present investigations the thermoluminescence samples were sufficiently thick, it was possible to find
dating method was, for the first time, used to overcome unaffected material inside for TL measurements.
the problem of multiple results of the AM method.
Prior to TL age determination the degree of heating was
measured by using the method of thermally activated ARCHAEOMAGNETIC DATING
sensitivity enhancement of the 110 °C TL peak
(TASE) (Sunta and David, 1982; G6ksu-Ogelman Six big samples, HR 1-4 and HE 5-6 (Table 1),
et al., 1989). from the two ovens were re-cut into smaller specimens

563
564 FI. Becker et al.

T A B L E 1. Number (N) of samples and number (n) of specimens between the 18th and the 7th century branch of the
H R 1--4 and HE 5-6 obtained from the two ovens near DEC/INC secular variation curve.
Herrsching
The rather poor fitting of the declination in this
Structure N n curve may be due to the very small horizontal
component of the thermoremanent magnetisation and
HR 1-4 4 34
HE 5-6 2 16 to magnetic refraction (Schurr et al., 1984). There is
only little chance to select the original thermoremanent
magnetisation of the hematite, which may carry the
undisturbed direction of the geomagnetic field, by
and embedded in 6 cm cubes of gypsum plaster for thermal demagnetisation over 580 °C. In the chalk-
measurement with a computerised big-sample fluxgate burning process at temperatures around 1000 °C with
spinner magnetometer. The stability of the natural a high production of CO 2 one would even expect the
remanent magnetisation (NRM) was checked by the original generation of magnetite.
Thellier test (Thellier and Thellier, 1959) and by The use of the inclination curve only for AM dating
thermal demagnetisation using a big oven in zero-field resulted into four possible ages, i . e . A . D . 670+30,
condition. The sample H R 2 had to be removed A.D. 880+10, A.D. 1640+20 and A.D. 1775+20
due to a viscosity coefficient greater than 1%. After (Fig. 2). There was no archaeological evidence for
the correction of the measured declination by the distinguishing between these dates.
azimuth of the sun-orientation the mean values for
geomagnetic declination (DEC) and inclination (INC)
were calculated with Fisher's statistics (Fisher, 1953) DETERMINATION OF FIRING TEMPERATURE
with a confidence circle of less than 2.5 ° with 95%
probability (Table 2). The firing temperature of the clay samples used in
The fit of these mean directions in the DEC/INC this experiment was determined by thermally activated
archaeomagnetic reference curve by The llier (1981) for sensitivity enhancement of the 110 °C TL peak. The
middle Europe during the last 2000 years is shown in 10 mg aliquots with grains between 90--t40 txm were
Fig. 1. Because of the compatible geomagnetic latitude exposed to a small test dose of 50 mGy after various
of Paris and Herrsching no dipole correction had steps of thermal activation. The details and the routine
been calculated. There was no clear decision possible procedure for this method are described by G6ksu et al.

T A B L E 2. Mean stable NRM directions of the samples H R 1-4 and HE 5-6

Structure INC (°) DEC (o) n a~ 5 (o) k Mean INC_+SD (°) Mean D E C + S D (o)

H R 1-4 70.5 352.7 21 2.2 210 70.1_+0.8 - 8.8_+2.8


HE 5--6 71.3 335.6 16 2.7 190 71.1 _+1.2 -24.6_+2.4

INC: inclination; DEC: declination: n: number of specimens: a,j~ radius of cone of confidence: k: precision parameter: SD: standard
deviation.

'¢¢ E
.¢~. O" t¢'~-

\
"\\

FIG. 1. Standard curve DEC/1NC for archaeo-secular variation compiled by Thellier (1981) for the last 21~) years with the plot of the
mean directions for Herrsching samples HR 1-4 and HE 5-6.
Archaeomagnetic and TL Dating 565

: blean TL date: A D 696 + 47 + 91]


AD 1640 :t:201

~
~'Mean AM date: A 0 670 + 30 AD 1775+20]
AD 880-+101

Q
,::1;::::::
~::.:.: •
:~,~:!~-'L-.:'
75' Mean Inclination:
_ _ HR 1 - 4
70" HE 5 - 6
70.60_+0.8°

I o
J
i1/1"/" \ 65"
Geomagnetic
Inclination

\ 60"

55 ~

0 2OO 4O0 6OO 8OO lOOO 200 1400 1600 1800 20OO
Years A D

FIG. 2. Results of A M and TL dating presented within the standard curve INC for the archaeosecular variation of the inclination
(Thellier, 1981) for the last 2000 years with the overall mean inclination for the ovens H R 1-4 and H E 5-6.

700 .... , .... ~ .... ~ .... , .... ~=.' acid in an ultrasonic bath to remove carbonate deposits.
• HR 1/7 • HE 6/1 The samples were dried and fine grain layers were
650 prepared as described by Zimmermann (1971). 24
• HR 3/2 r-t HE 5/4 II

600- • HR 4/17 @
stainless steel discs were prepared from each sample
ii
and kept at 60 °C for 24 hr before they were used for
550 - • •. ." TL measurements. 16 of them were used for first and
• • • 0
second glow measurements. Six samples were used for
500-
.'O a-value determination, and two were kept for testing
450-
e'
short term fading.
a
The TL glow curves were evaluated by using Riso
0,. 400-
# TL-DA-90 equipment with Schott BG-39 and Corning
350-
[] 7/59 filters placed in the optical pathway.
Additive dose curves were obtained by using a
300- •D 1.48 GBq (40 mCi)9oSr beta source which was cali-
brated at the Secondary Standard Dosimetry Laboratory
250"
at GSF (Eckerl and Nahrstedt, 1986). An alpha
2 0 0 . . . . i . . . . i . . . . i . . . . i . . . . , ' ' i
irradiator, type 721/B, manufactured by Littlemore
400 450 500 550 600 650 700 Sci. Eng. Co., Oxford, was used for a-value determi-
Temperatur [*C]
nation. The irradiator contains six 241Am alpha sources
FIG. 3. Determination o f firing temperature o f lhc clay f r o m with an activity of 6.66 MBq (180 ixCi) each.
Herrsching using T A S E

Archaeological Dose Assessment


(1991). A fresh aliquot was used for each thermal The samples were heated up to 450 °C with a heating
activation to avoid the sensitivity enhancement due rate of 5 °C/see in a high purity nitrogen flow of
to predose, As can be seen from Fig. 3 all samples 4 l/rain. The plateaU test and first and second growth
were baked well above 580 °C. curves were analysed by the 'TL-Plus' programme
developed at GSF for the Rista TL-DA-90 system
(Waibel, 1990).
THERMOLUMINESCENCE DATING The TL glow curves achieved from the fine grain
samples show two peaks at 180 °C and 330 °C. The
Sample Preparation and TL Measurements deviation in the plateau was found to be less than 10%
The samples obtained for TL measurements were between 280-320 °C.
already encased in 6 × 6 x 6 cm 3 gypsum plaster. The All samples exhibited a linear TL response in the
gypsum plaster was first removed by a chisel. The dose range of interest. The second growth curves were
blocks were squeezed in a vice. Grains below 90 Ixm found to be parallel to the first growth curves. Heating
were separated by sieving and washed with 1% HCI and irradiation have not affected the sensitivity of the
566 H. Becker et al.

TABLE 3. Results of thermoluminescencedating from clay samples. Dose rate calculations by assuming the samples to be water saturated
throughout the whole year
Sample Th, ppm U, ppm K. % Dose rate, AD(Q+I), Age BP Age A.D.
mGy/year Gy
HE 6/1 10.892 1.023 0.602 2.612 3.59 1375 619
HE 5/4 9.343 0.919 0.738 2.527 3.07 1215 777
HR 3/2 7.419 2.908 0.746 3.131 3.92 1252 740
HR I/7 8.485 1.157 0.650 2.595 3.47 1337 654
HR 4/17 9.491 1.614 0.763 2.873 3.76 1309 683

TABLE 4. Results of thermoluminescencedating from clay samples containing pebbles


Sample Th, ppm U, ppm K, % Dose rate, AD(Q+I), Age BP Age A.D.
mGy/year Gy
HE 3/2 1.602 4.071 0.746 3.144 3.92 1247 745
Big pebbles
HE 4/17 1.689 3.143 0.763 2.800 3.76 1342 650
Small pebbles

samples; however, a slight change in the colour of the The samples were assumed to be water saturated
samples was observed. The archaeological doses with the whole year. The water saturation content of the
intercept correction from second growth are given in samples was found to be in the range of 19-30%.
Table 3. The samples were pre-annealed at 150 °C Two samples were identified to contain pebbles with
for 100 sec. The T L peak area between 280-320 °C diameter varying from 1-10 mm and a saturation water
as measured one month and one year after irradiation content of 2 - 3 % . It was found that the U, Th content
was found to be stable. of the pebbles was different from the surrounding
clay (Table 4). The annual absorbed dose rates of
A n n u a l Dose Rate Assessment clay samples calculated with the assumption that the
The internal component of the annual dose rate was environment consists of pebbles only (see Table 4)
calculated according to the Bell conversion tables (Bell, were in good agreement with the earlier considered
1979) and revised data of Nambi and Aitken (1986) by clay samples without pebbles (see Table 3). It appears
using U, Th and K contents obtained from thick sample that the low water content of the pebbles compensates
alpha counting and atomic absorption measurements for the difference in the U, Th content.
respectively. Results of the U, Th and K content of clay
are given in Table 3. The a-values were determined for
5 samples and a mean of a = 0.13_+0.02 is used for the CONCLUDING REMARKS
later dose rate calculations.
The external gamma dose rates were assessed in The mean T L age of the five clay samples was found
situ with a portable scintillation dose rate meter of to be A.D. 694+57+ 110 respectively BP 1297+57_+ 110,
type D L 7908 manufactured by Halle, Braunschweig, with the standard error on the mean value and the
Germany. The instrument has been type tested by the overall error calculated according to Aitken (1976).
Physikalisch-Technische Bundesanstalt (PTB), Braun- From the two clay samples with pebbles a mean T L age
schweig, Germany. The measurements were performed of A.D. 696_+47_+91 respectively BP 1294+47-+91 was
by digging a hole of 50 cm depth inside of both ovens, evaluated. Both T L ages fit within the limits of error
from where the samples were collected. only one of the AM dates, this being A.D. 670-+30.
The readings of absorbed dose rate were 89.9_+ The ovens were obviously used for chalk-burning
5.6 nSv/hr (2~_+6%). Since the instrument is calibrated in order to produce mortar or plaster for building
in terms of the dosimetric quantity photon dose the stone-church. Hence the age of these ovens has
equivalent (Reich, 1990), the readings had to be a considerable importance for archaeologists since
first converted into absorbed dose rate in water. it marks the building time of the first medieval
Second, from the ratio of the mass energy absorption stone-church at the Herrsching site which is only one
coefficients of water and quartz an absorbed dose rate generation after a wooden predecessor archaeologically
in quartz of 70.00+3.92 nGy/hr has been calculated. dated A.D. 620-630 (Keller, 1993).
The environmental gamma absorbed dose rate was,
for verification, also calculated assuming a uniform
ACKNOWLEDGEMENT
distribution of U, Th and K in the clay. The calculations
yielded an absorbed dose rate in quartz of 72.32+ We would like to thank E. Keller for providing unpublished
9.92 nGy/hr (2cr+13%), a result in good agreement results of the excavation at Herrsching as well as for valuable
with the in situ measurements. discussion about the site.
Archaeomagnetic and TL Dating 567

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