Numerical calibration of the Devonian-Carboniferous boundary:

Two new U-Pb isotope dilutionthermal ionization mass

spectrometry single-zircon ages from Hasselbachtal
(Sauerland, Germany)
Endres Trapp Zentrallabor fur Geochronologie, Institut fur Mineralogie, Universitat Munster, Corrensstrasse 24, 48149 Munster,
Germany

Bernd Kaufmann Institut fur Geowissenschaften, Universitat Tubingen, Sigwartstrasse 10, 72076 Tubingen, Germany
Klaus Mezger Zentrallabor fur Geochronologie, Institut fur Mineralogie, Universitat Munster, Corrensstrasse 24, 48149 Munster,
Germany

Dieter Korn Museum fur Naturkunde, Humboldt-Universitat, Invalidenstrasse 43, 10115 Berlin, Germany
Dieter Weyer Lowestrasse 15, 10249 Berlin, Germany
ABSTRACT
The Hasselbachtal section (Sauerland, Germany) is an auxiliary global stratotype of the
Devonian-Carboniferous boundary and one of the most important reference sections for
the evolution of the latest Famennian to earliest Tournaisian pelagic fauna. Biostratigraphically well controlled altered volcanic ash layers (metabentonites) intercalated in the section afford a perfect opportunity for a numerical fixing of this important Paleozoic period
boundary. We have performed U-Pb isotope dilutionthermal ionization mass spectrometry (ID-TIMS) analyses on (sub)microgram-sized single zircons and zircon fragments
extracted from two metabentonites (beds 79 and 70) in the lowermost Tournaisian part
of the section. Bed 79 metabentonite is positioned directly above the DevonianCarboniferous boundary within the Siphonodella sulcata conodont zone. Five concordant
analyses form a cluster with a 206Pb/238U concordia age of 360.5 6 0.8 Ma. Zircons of the
next younger metabentonite (bed 70), in the lower Siphonodella duplicata conodont zone,
yielded a tightly grouped cluster of 10 concordant analyses with a 206Pb/238U concordia
age of 360.2 6 0.7 Ma. On the basis of these two new single-zircon ages and previously
published late Famennian U-Pb ID-TIMS ages, the Devonian-Carboniferous boundary is
reinterpolated herein to 360.7 6 0.7 Ma.
Keywords: Devonian-Carboniferous boundary, metabentonites, U-Pb, zircon, absolute age.
INTRODUCTION
Period boundaries such as the one between
the Devonian and the Carboniferous are defined biostratigraphically. Marine sedimentary
successions crossing these boundaries and
well documented by index fossils are thus selected as global stratotype section and point
(GSSP) sections. For an accurate chronological calibration, isotopic ages have to be acquired from intercalated volcanic rocks situated in the immediate vicinity of the
boundary.
The Hasselbachtal auxiliary global stratotype section (Sauerland, Germany) offers such
an opportunity by intercalated volcanic ashes
(metabentonites) that are biostratigraphically
precisely fixed. Previously, zircons extracted
from the bed 79 metabentonite, directly above
the Devonian-Carboniferous boundary, were
dated by the U-Pb sensitive high-resolution
ion microprobe (SHRIMP) method as 353.2 6
4.0 Ma (Claoue-Long et al., 1992) and later
slightly changed to 353.7 6 4.2 Ma (ClaoueLong et al., 1995). This dating was used
to define the absolute reference age of the
Devonian-Carboniferous boundary as 354 Ma

(e.g., Fordham, 1992; Gradstein and Ogg,

1996; Menning et al., 2001). In contrast,
Tucker et al. (1998) suggested a significantly
older boundary age of 362 Ma on the basis of
two U-Pb isotope dilutionthermal ionization
mass spectrometry (ID-TIMS) zircon ages
(multigrain analyses) of the Piskahegan Group
(New Brunswick, Canada). The significantly
younger SHRIMP age of the Hasselbachtal
bed 79 metabentonite was caused by a recently detected heterogeneity in the SL 13 zircon reference material and by the erroneous
inclusion of youngest data points (as later assumed to have lost Pb) in the weighted-mean
age (Compston, 2000). A reexamination of
zircons from this ash bed by application of the
more precise U-Pb ID-TIMS method is thus
required. First attempts were made by Kramm
et al. (1991), whose multigrain analyses of
abraded crystals yielded a maximum 206Pb/
238U age of 346.6 6 1.6 Ma. However, because of high amounts of common Pb (mainly
derived from apatite inclusions) and low
amounts of radiogenic Pb, the analytical uncertainties of the 207Pb/235U ages were so high
that the observed concordance could not be

considered meaningful. The 206Pb/238U age of

346.6 6 1.6 Ma was thus regarded as a minimum age affected by significant Pb loss
(Kramm et al., 1991). Consequently, the purpose of this study is the dating of the Hasselbachtal bed 79 metabentonite and the next
younger bed 70 metabentonite in the lower Siphonodella duplicata conodont zone by analyzing single zircons or zircon fragments. The
results are the first U-Pb ID-TIMS ages from
basal Tournaisian strata that can be used for a
recalibration of the Devonian-Carboniferous
boundary.
HASSELBACHTAL SECTION
The Hasselbachtal auxiliary global stratotype section is located at the northern margin
of the Rhenish Massif near the town of Hagen
(Sauerland, Germany). Because of its rich fossiliferous record, it is one of the best investigated successions across the Devonian-Carboniferous boundary worldwide (Korn and
Weyer, 2003, and references therein). Hasselbachtal is also a reference section, particularly
with regard to the ammonoid and conodont
biozonations (Groos-Uffenorde and Uffenorde, 1974; Becker et al., 1984; Becker, 1996;
Korn and Weyer, 2003) (Fig. 1). The section
contains six whitish or greenish (fresh) or yellowish (weathered), #1-cm-thick metabentonite horizons in the boundary interval (Korn
and Weyer, 2003). Their wide spatial distribution supports the interpretation of these layers as primary airborne products of explosive,
acidic (rhyolitic to rhyodacitic) volcanism. In
the lowermost Tournaisian part of the section
(Hangenberg Limestone), three metabentonites are intercalated. Of these, the older two
have been sampled for zircon extraction: bed
79 metabentonite, which was already dated by
Claoue-Long et al. (1992, 1995), is only 43
cm above the Devonian-Carboniferous boundary in the upper part of the S. sulcata conodont zone (Fig. 1). The next younger bed 70
metabentonite is intercalated 57 cm above bed
79 in the lower part of the lower S. duplicata
conodont zone (Fig. 1).

q 2004 Geological Society of America. For permission to copy, contact Copyright Permissions, GSA, or editing@geosociety.org.
Geology; October 2004; v. 32; no. 10; p. 857860; doi: 10.1130/G20644.1; 3 figures; 1 table.

857

Figure 1. Lithologic column of Hasselbachtal

section including conodont and ammonoid
stratigraphy and showing positions of bed
79 (a1) and 70 (a2) metabentonites (modified after Korn and Weyer, 2003).

ANALYTICAL METHODS
U-Pb data were acquired at the Zentrallabor
fur Geochronologie, Institut fur Mineralogie,
Universitat Munster (Germany). Zircons were
isolated from bed 79 and bed 70 metabentonites using refined procedures as described by
Winter (1981). Investigations of the zircons,
using an optical microscope and a scanning
electron microscope, revealed mostly euhedral
crystals of short- to normal-prismatic shape
(2:1 to 4:1; see also Winter, 1993), and a distinct oscillatory magmatic growth zonation is
visible in cathodoluminescence images. The
maximum length of the zircons is ;200 mm;
their maximum width is ;100 mm. In the zircon population of the bed 79 metabentonite,
magmatically corroded zircons are also a characteristic constituent.
Zircons selected for analyses were subjected to air abrasion (Krogh, 1982), and most
samples were additionally cleaned for 2 h in
concentrated HF-HNO3 (4:1) at 80 8C to remove attached impurities. After washing in
7N HNO3 at 80 8C for 25 min, individual
858

grains were placed in multisample Teflon microcapsules and dissolved for at least 4 days
in concentrated HF-HNO3 (4:1) at 180 8C.
Subsequently, dissolved zircons were spiked
with a mixed 233U-205Pb tracer solution, dried
at 80 8C, redissolved in 6N HCl, and equilibrated at 180 8C for 1 day. After drying at 80
8C, the samples were loaded on a single Re
filament using a mixture of silica gel and 6N
HCl0.25N H3PO4.
Isotope ratios of Pb and U were measured
with a Daly-type detector in ion-counting
mode on a VG Sector 54 TIMS. Low radiogenic Pb concentrations required isotope analyses by peak jumping. Pb and U (as UO12 )
were run sequentially on the same filament at
temperatures of 12501350 8C and 1300
1450 8C, respectively. Average measured precision (2s error) of Pb isotope ratios was 1.2%
(206Pb/204Pb), 0.22% (207Pb/206Pb), and 0.1%
(206Pb/205Pb). Individual ratios were corrected
for mass fractionation on average by 0.23%/
amu (207Pb/206Pb, 206Pb/205Pb), and 0.09%/
amu (206Pb/204Pb), on the basis of multiple
analyses of the NBS 982 standard. The 233U/
238U ratio was measured more precisely than
0.24% (2s), and mass fractionation was individually corrected on average by 0.03%/amu
based on analyses of the NBS 500 standard.
For each charge of samples, the maximum Pb
blank was assumed to be equivalent to the total amount of nonradiogenic Pb in the analysis
of the most radiogenic sample. It was required
to analyze radiogenic Pb amounts as low as
0.6 pg due to low to moderate U concentrations (,100450 ppm) and small sample volumes. It was thus necessary to reduce the Pb
blank as much as possible (K1 pg) by extremely careful sample handling. In nearly all
samples, 206Pbrad/206Pbtot was sufficiently high
to obtain precise 206Pb/238U ages. The U blank
was too small to be measured and was thus
assumed to amount to 20% of the individual
Pb blank, based on experience with the analysis of milligram-sized samples. Uncertainties
in 206Pb/238U, 207Pb/235U, and 207Pb/206Pb
were calculated by using the algorithm of
Ludwig (1980), and errors are given at the 2s
level. Software Isoplot/Ex, rev. 2.49 (Ludwig,
2001), was used for the concordia plot.
U-Pb SINGLE-ZIRCON AGES
Bed 79 Metabentonite (Upper Part of
sulcata Conodont Zone)
On the basis of 13 analyses (single zircons
or zircon fragments), a younger zircon generation of 5 analyses is distinguished from
older zircon generations (Table 1). The latter,
obviously inherited, yielded 207Pb/206Pb ages
of 444 to 2044 Ma (Table 1). The abundance
of Precambrian ages is a remarkable feature;
note that no inherited zircons were detected in
the study of Claoue-Long et al. (1992). The
error ellipses of the older zircons are clearly
separated from a tight concordant cluster of

the five youngest zircon analyses, which yield

a 206Pb/238U concordia age of 360.5 6 0.8 Ma
(Fig. 2A). This age is interpreted as the crystallization age of the comagmatic zircon population and thus the time of eruption of the
ash. Comagmatic zircons are only a small
fraction of the total zircon population. It is
possible that the youngest zircon generation
occurs as micrometer-sized rims around inherited zircons as well, but these new growth
zones were removed by the air-abrasion procedure prior to the dissolution of the grains.
Bed 70 Metabentonite (Lower Part of
Lower duplicata Conodont Zone)
The bed 70 metabentonite yielded a precise
age with the U-Pb ID-TIMS single-zircon
method. A 206Pb/238U concordia age of 360.2
6 0.7 Ma was obtained from a tight concordant cluster of 10 analyses (Fig. 2B; Table 1).
Six ages of this cluster are based on pyramids
broken off from whole zircon crystals, and
these fragments are typically free of inherited
core material. The analyses of the grains B-0,
H.III-2, H12-0, H12-2, and K29-0, despite being concordant within analytical error, plot
slightly below the cluster (Fig. 2B), and are
not included in the age calculation. These
grains have probably lost some Pb with respect to the primary radiogenic Pb content.
Signs of inheritance or reworked (older) crystals are documented by the analyses K29-3
and K14-2 (Fig. 2B). The error ellipses of
these zircons are also separated from the cluster, yielding older apparent 206Pb/238U ages of
363.4 and 366 Ma, respectively. The 206Pb/
238U concordia age of 360.2 6 0.7 Ma for the
bed 70 metabentonite harmonizes well with
the age of the stratigraphically slightly older
bed 79 metabentonite.
CALIBRATION OF THE DEVONIANCARBONIFEROUS BOUNDARY
The two new earliest Tournaisian geochronological constraints presented here and two
previously published late Famennian ages constitute a methodically consistent data set of four
U-Pb ID-TIMS zircon and monazite ages. This
result allows a unique, accurate geochronological bracketing of the Devonian-Carboniferous
boundary by stratigraphically younger and
older strata. The two late Famennian ages are
(1) Piskahegan Group (New Brunswick, Canada), 363.6 6 1.6 Ma, uppermost marginifera
to upper expansa conodont zone (Tucker et al.,
1998; Streel, 2000), and (2) Nordegg Tuff of
the Exshaw Formation (Alberta, Canada),
363.3 6 0.4 Ma, middle expansa to lower
praesulcata conodont zone (Richards et al.,
2002). For interpolation, the isotopic ages are
plotted against a relative biostratigraphic time
scale (Fig. 3). The scale used here was derived
from the conodont-bearing Lali section (Ji and
Ziegler, 1993), which fits the following requirements: (1) it is well documented by coGEOLOGY, October 2004

TABLE 1. U-Pb ZIRCON DATA OF HASSELBACHTAL METABENTONITES

Sample*

Bed 70 metabentonite
AW20-1: 60 mm, 2:1, fr, 2a, hf
B-0: 200 mm, 3.5:1, fr, 2a, hf**
B-1: 150 mm, 1:1, fr, 2a, hf
B-2: 80 mm, 1.5:1, fr, 2a, hf
B-3: 150 mm, 3.5:1, 2a, hf
H.III-1: 110 mm, 2.5:1, 1a, hf
H.III-2: 120 mm, 3:1, 2a, hf**
H.III-3: 100 mm, 2.5:1, fr, 2a, hf
H12-0: 100 mm, 1:1, fr, 2a, hf**
H12-2: 50 mm, 1.5:1, fr, 1a, hf**
K14.2: 150 mm, 4:1, 2a
K14-6: 100 mm, 3:1, 2a
K29-0: 80 mm, 2.5:1, fr, 2a, hf**
K29-3: 60 mm, 2:1, 1a, hf
M2-0: 60 mm, 2.5:1, 1a, hf
M2-1: 130 mm, 3:1, fr, 2a, hf
M2-3: 70 mm, 1:1, fr, 2a, hf
Bed 79 metabentonite
H.II-1: 50 mm, 1.5:1, 1a, hf
H.II-3: 50 mm, 1.5:1, 1a, hf
H1-1: 70 mm, 1.5:1, 1a, hf
H1-3: 60 mm, 3:1, 1a, hf
H21-0: 60 mm, 2:1, 1a, hf
H21-2: 50 mm, 2:1, 1a, hf
H29-0: 100 mm, 2:1, 1a, hf
H29-1: 80 mm, 2:1, 1a, hf
H29-2: 100 mm, 1.5:1, 1a, hf
H29-3: 200 mm, 2.5:1, 1a, hf
H30-0: 150 mm, 1.5:1, 1a, hf
H30-2: 100 mm, 2:1, 1a, hf
H30-3: 120 mm, 1.5:1, 1a, hf

Concentrations

Isotopic ratios
206

204

Pb/

Pb

206

238

207

Pb/

Isotopic ages (Ma)

235

Pb/

207

206

Pb/

Pb

206

238

Pb/

Pb/235U#

207

Pb/206Pb#

Pb rad.
(pg)

52.9
315.7
204.6
108.9
365.6
17.5
12.8
21.1
159.7
46.0
19.1
66.8
154.0
53.9
54.5
76.5
54.4

2.6
17.7
11.3
5.7
21.9
0.9
0.6
1.1
8.9
2.6
1.1
3.9
8.8
2.8
3.2
4.8
3.1

141.6
717.0
548.3
392.1
338.4
343.5
274.2
354.3
959.4
245.7
182.0
295.8
427.7
340.2
139.0
133.6
146.0

6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6

1.3
12.2
6.6
5.8
5.9
5.0
2.7
2.7
14.4
2.0
0.9
1.4
3.7
4.5
1.6
1.1
1.3

0.05748
0.05714
0.05743
0.05749
0.05748
0.05745
0.05686
0.05755
0.05708
0.05690
0.05841
0.05745
0.05720
0.05800
0.05742
0.05752
0.05737

6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6

50
30
27
26
29
31
33
26
25
29
37
26
32
27
34
32
32

0.4200
0.4246
0.4256
0.4253
0.4232
0.4267
0.4213
0.4270
0.4204
0.4261
0.4352
0.4238
0.4245
0.4307
0.4225
0.4262
0.4261

6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6

147
44
43
67
78
108
112
65
31
72
131
48
46
78
159
131
126

0.05299
0.05389
0.05375
0.05365
0.05341
0.05386
0.05373
0.05381
0.05341
0.05431
0.05403
0.05350
0.05383
0.05386
0.05337
0.05374
0.05386

6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6

166
46
45
76
89
123
127
70
30
82
143
51
47
87
185
152
145

12.5
3.7
3.6
5.7
6.6
9.1
9.5
5.5
2.7
6.1
11.1
4.1
3.9
6.6
13.5
11.0
10.7

328
367
361
357
346
365
360
363
346
384
372
350
364
365
344
360
365

6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6

70
19
18
31
38
51
52
29
13
33
59
21
20
36
79
63
60

40.9
55.9
270.4
23.5
48.1
22.0
66.2
450.0
64.7
20.2
50.8
35.5
104.8

2.1
3.0
107.0
2.0
17.4
5.5
3.5
31.2
6.4
1.0
7.9
2.0
9.7

165.8
194.4
2479.1
97.2
164.6
205.6
479.0
3031.1
504.0
225.1
1820.3
709.2
1734.4

6
6
6
6
6
6
6
6
6
6
6
6
6

1.4
1.1
25.4
0.7
2.5
8.2
3.8
28.4
4.9
2.8
23.8
11.1
14.9

0.05745
0.05749
0.37259
0.06867
0.32704
0.28823
0.05748
0.07026
0.10088
0.05756
0.15507
0.05758
0.09218

6
6
6
6
6
6
6
6
6
6
6
6
6

34
27
130
44
191
292
23
25
38
40
62
22
33

0.4238
0.4302
6.4755
0.5438
4.9748
3.9764
0.4260
0.5404
0.8427
0.4226
1.5005
0.4261
0.7511

6
6
6
6
6
6
6
6
6
6
6
6
6

120
81
250
242
857
1557
45
23
72
186
73
56
33

0.05350
0.05427
0.12605
0.05744
0.11032
0.10006
0.05376
0.05578
0.06058
0.05325
0.07018
0.05367
0.05910

6
6
6
6
6
6
6
6
6
6
6
6
6

136
360.1 6 2.2
358.8 6 10.2
90
360.4 6 1.7
363.3 6 6.8
21
2041.6 6 7.1
2042.6 6 7.9
236
428.1 6 2.8
440.9 6 19.6
165 1824.0 6 10.6 1815.0 6 31.2
349 1632.7 6 16.5 1629.4 6 63.8
48
360.3 6 1.5
360.4 6 3.8
12
437.7 6 1.6
438.7 6 1.8
43
619.6 6 2.3
620.6 6 5.3
213
360.8 6 2.5
357.9 6 15.8
19
929.3 6 3.7
930.6 6 4.5
63
360.9 6 1.4
360.4 6 4.7
15
568.4 6 2.0
568.9 6 2.5

350
382
2044
508
1805
1625
361
444
624
339
934
357
571

6
6
6
6
6
6
6
6
6
6
6
6
6

57
37
3
91
27
64
20
4
16
91
5
27
5

360.3
358.2
360.0
360.3
360.3
360.1
356.5
360.7
357.8
356.7
366.0
360.1
358.6
363.4
359.9
360.5
359.6

6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6

207

U
(ppm)

3.1
1.9
1.7
1.6
1.8
1.9
2.1
1.6
1.5
1.8
2.3
1.6
2.0
1.7
2.2
2.0
2.0

356.0
359.3
360.0
359.8
358.4
360.8
356.9
361.1
356.3
360.4
366.9
358.7
359.3
363.7
357.8
360.5
360.4

6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6
6

*Sample description, i.e., 100 mm 5 length of grain; 2:1 5 length/width ratio; fr 5 fragment; 2a 5 slightly abraded (;10% reduction of crystal volume); 1a 5 strongly
abraded (;30% reduction); hf 5 HF cleaned.

Calculations based on estimated mass of grain.

Measured value corrected for mass fractionation.

#
Ratios and ages corrected for mass fractionation, spike, Pb blank, and initial common Pb (at 360 Ma from Stacey and Kramers, 1975).
**Denotes discordant zircon analyses caused by significant recent Pb loss.

Denotes zircon analyses with isotopic evidence for inheritance.

nodonts, (2) it shows a quite homogeneous

limestone lithology in the upper Famennian to
lowermost Tournaisian interval, and (3) it is
much less condensed than other conodontbearing Devonian-Carboniferous boundary

sections. The homogeneous lithology reflects

a more or less uniform rock accumulation rate
that, in turn, is the precondition for an approximately linear record of time. A biostratigraphic scale derived in this manner has, nev-

ertheless, incorporated many sources of bias;

there are facies changes, incomplete sampling,
taxonomic confusion, and diachronism of index taxa. Therefore, it cannot be anything
more than an approach to linearity in time.

Figure 2. Concordia diagrams of single-zircon analyses from Hasselbachtal metabentonites. 206Pb/238U concordia ages are calculated from
shaded analyses only. MSWD 5 mean square of weighted deviates.
GEOLOGY, October 2004

859

Figure 3. Calibration of Devonian-Carboniferous boundary.

However, we regard it as more reliable than a

bioscheme that is based on the erroneous assumption that biozones represent equal time
intervals. Figure 3 shows the result of the interpolation: a biochronometric time scale that
allows the assignment of a numeric age with
its error to each biozone boundary in the late
Famennian to earliest Tournaisian interval.
The tie points of the time-scale line are the
center of the overlapping ages of the Piskahegan Group and Nordegg Tuff and the center
of the bed 70 metabentonite age. The latter is
more strongly weighted than bed 79 metabentonite because it is based on more concordant
analytical points. Based on this construction,
the Devonian-Carboniferous boundary is calculated as 360.7 6 0.7 Ma. Future refinements
of this boundary age may depend on the dating of the four other volcanic ashes closely
tied to this boundary in the Hasselbachtal section. This study highlights the value of defining biostratigraphic stratotypes in the vicinity
of known dateable horizons.
ACKNOWLEDGMENTS
This study was funded by the Deutsche Forschungsgemeinschaft (DFG, grant BA 544/43) within the
scope of the main research Evolution des Systems
Erde wahrend des jungeren Palazoikums im Spiegel der
Sediment-Geochemie. Technical assistance was given
by Heidi Baier and Michael Feldhaus (both Munster).
We are very grateful to Dieter Meischner (Gottingen),
William Compston (Canberra), and two anonymous Geology reviewers, whose constructive comments improved the manuscript.

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Manuscript received 15 March 2004
Revised manuscript received 6 July 2004
Manuscript accepted 7 July 2004
Printed in USA

GEOLOGY, October 2004