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Quaternary International 432 (2017) 98e99

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Quaternary International
journal homepage: www.elsevier.com/locate/quaint

Further comment on: “Uraniumethorium dating method and


Palaeolithic rock art” by Sauvet et al. (2015, in press)
Maxime Aubert a, b, *
a
Research Centre of Human Evolution, Environmental Futures Research Institute, Griffith University, Brisbane, Queensland 4111, Australia
b
Place, Evolution and Rock Art Heritage Unit (PERAHU), Griffith University, Gold Coast, Queensland 4222, Australia

In Volume XXX of Quaternary International, Sauvet et al. (in coupled with the high level of precision required for such
press) write a critique of the application of uranium-thorium measurements.
dating to Palaeolithic rock art. These authors misrepresent key as- Sauvet et al. (in press) also write: “A more precise sampling
pects of the dating method they are criticising, as illustrated in the protocol was implemented by Aubert et al. (2007) in East Timor
comment by Pons-Bronchu et al. (in press). Furthermore, they using laser ablation MC-ICPMS (multicollector-inductively coupled
present a flawed understanding of the sampling methodology used plasma mass spectroscopy). A core sample “excavated” through the
in some of the cited case studies. In this comment, I draw attention calcite layer overlying the paintings was later subdivided by laser
to these critics' faulty interpretation of the sampling methodology ablation into layers about 100 mm thick to obtain a micro-
employed in Aubert et al. (2007, 2014). stratigraphy. A thin layer of pigment imbedded in the deposit could
Apart from the three concepts discussed in Pons-Bronchu be bracketed between 24 and 29.3 ka […]. Recently, U/Th dating of
et al. (in press), Sauvet et al. (in press) stipulate that: “the ura- paintings at Sulawesi (Indonesia) was performed using the same
nium/thorium dating method gives reliable and relatively precise technique of laser ablation MC-ICPMS (Aubert et al., 2014). Dates in
results in the case of massive speleothems, because the sampling the range of 35e40 ka were obtained for the lowest sublayer of
is carried out at the heart of the material where the hypothesis of calcite less that 1 mm thick overlying several hand stencils”. This is
a closed system (that is, no exchange with the outside environ- incorrect, as laser ablation MC-ICPMS was not employed to date the
ment) is justified in most cases. Unfortunately, the situation is rock art in Aubert et al. (2007, 2014).
quite different in the case of thin layers of calcite that overlie In East Timor, “laser ablation inductively coupled plasma mass
Palaeolithic cave drawings”. This concept is also incorrect as the spectrometry (Eggins et al., 2003) was used to profile a series of
closed system behavior of the calcium carbonate deposit has elements along individual layers of interest. Uranium concentra-
more to do with crystal structure and porosity than size. In fact, tion was measured to establish sample size requirements for the
in the cited example of Plagnes et al. (2003), the samples came determination of the U and Th isotopic ratios. Under 30
from a large and porous cave drapery and was selected and magnification the fine carbonate laminations were ground into
sampled by non-dating specialists who had limited under- fine powders using a micro-drill and dental burrs, maintaining
standing of these concepts (P. Setiawan, Pers. Comm.). It is true control over the micro-stratigraphic level (Watchman, 2000). An
that “the protactinium-231 (231Pa) dating method may be used to area measuring approximately 1 cm  1 cm was removed to a
check the results obtained by U/Th dating of calcite” but Sauvet depth of about 0.1 mm per sample and the powder collected on
et al. (in press) argue that the method has not been used for aluminium foil. Each sample was then dissolved in nitric acid,
rock art “because the concentration of Pa is much lower than that spiked and prepared according to the method described by Luo
of Th”. In fact, the greatest strength of measuring 231Pa/235U is its et al. (1997). Isotopic ratio measurements were made on a Fin-
use in combination with 230Th/234U-238U data in identifying and nigan Neptune multi-collector ICPMS equipped with desolvating
potentially dating open-system. The problem with the use of the nebuliser” (Aubert et al., 2007: page 994). Further on we write:
method relies in the difficulty in obtaining a spike for the accu- “This technology also enables the potential use of laser ablation
rate measurement of protactinium-231 by mass spectrometry for in situ uranium series dating of rock art where U concentra-
tions are higher then 1 ppm (Eggins et al., 2005)” (Aubert et al.,
2007: page 994).
DOIs of original article: http://dx.doi.org/10.1016/j.quaint.2015.03.053, http:// In Sulawesi, “each coralloid sample was sawn in situ so as to
dx.doi.org/10.1016/j.quaint.2015.10.016, http://dx.doi.org/10.1016/j.quaint.2015.10. produce a continuous microstratigraphic profile extending from
015. the outer surface of the coralloid through the pigment layer and
* Place, Evolution and Rock Art Heritage Unit (PERAHU), Griffith University, Gold
into the underlying rock face […]. In the laboratory, the samples
Coast, Queensland 4222, Australia.
E-mail address: m.aubert@griffith.edu.au. were microexcavated in arbitrary ‘spits’ over the entire surface of

http://dx.doi.org/10.1016/j.quaint.2016.04.020
1040-6182/© 2016 Elsevier Ltd and INQUA. All rights reserved.
M. Aubert / Quaternary International 432 (2017) 98e99 99

the coralloids, creating a series of aliquots less than 1 mm thick […]. the rock art panels using a battery-operated rotary tool equipped
The uranium-series isotopes were measured on a Thermo Finnigan with a diamond saw blade” (Aubert et al., 2014: page 226). We used
Neptune Plus Multi-Collector inductively coupled plasma mass a rotary tool to make four incisions in the material and then used a
spectrometer […] (Aubert et al., 2014: page 226). flat-end micro screwdriver to carefully remove the sample. More-
In the first study, laser ablation ICPMS was used to determine over, each potential sample was assessed by a representative of the
the relative concentrations of 238Uranium and 232Thorium across Indonesian Heritage Department (who was also part of the Team)
the sample. This was then used to 1) identify areas with ‘clean’ and permission was given before collecting each sample, with the
calcium carbonate depositional layers; 2) determine the amount of collection process also supervised by representatives of the former
material (how many milligrams) needed to be micro-excavated institution. Since the age of the rock art was unknown and faced
using a micro-drill and burrs and; 3) determine the amount of serious threats from large-scale industrial activities (i.e., limestone
spike needed to accurately measure the isotopic ratios by solution quarrying) our Indonesian colleagues deemed it essential to pro-
based MC-ICPMS. In Sulawesi, laser ablation ICPMS was not ceed with sampling and dating speleothems already obscuring
employed. Instead, conventional solution based ICPMS was used to motifs. U/Th dating has established the extreme antiquity and
determine 1), 2), and 3). The powdered material was also collected global significance of the Sulawesi rock art and it is this discovery
using a micro-drill and burrs. that may ultimately save it from destruction.
Sauvet et al. (in press) further write: “The significant damage
caused by sampling, conducted by scraping with a scalpel or dril- References
ling with a carbide drill bit (Pike et al., 2012) is a matter of grave
concern. The alternative technique of core sampling with a rotating Aubert, M., O'Connor, S., McCulloch, M., Mortimer, G., Watchman, A., Richer-
LaFleche, M., 2007. Uranium-series dating rock art in East Timor. Journal of
diamond sawblade is probably also very invasive, as the excavated
Archaeological Science 34, 991e996.
section is very large (up to 200 mm2, corresponding to circular pits Aubert, M., Brumm, A., Ramli, M., Sutikna, T., Saptomo, E.W., Hakim, B.,
of 16 mm diameter) (Aubert et al., 2014) […]. Given the un- Morwood, M.J., van den Bergh, G.D., Kinsley, L., Dosseto, A., 2014. Pleistocene
cave art from Sulawesi, Indonesia. Nature 514, 223e227.
certainties of the U/Th method outlined above, a serious discussion
Eggins, S., Grün, R., Pike, A.W.G., Shelley, M., Taylor, L., 2003. 238U and 232Th
needs to take place among physical scientists, archaeologists, profiling and U-series isotope analysis of fossil teeth by laser ablation-ICPMS.
conservation specialists and authorities concerning the costs and Quaternary Science Reviews 22, 1373e1382.
benefits of such sampling”. Eggins, S.M., Grün, R., McCulloch, M.T., Pike, A.W.G., Chappell, J., Kinsley, L.,
Mortimer, G., Shelley, M., Murray-Wallace, C.V., Spo €tl, C., Taylor, L., 2005. In situ
“Core sampling through the calcite layer overlying the paint- U-series dating by laser ablation multi-collector ICPMS: new prospects for
ings” did not occur in East Timor. Instead “A test specimen (off-art) Quaternary geochronology. Quaternary Science Reviews 24 (23-24),
was collected from the cave wall near a painted figure. This sample 2523e2538.
Luo, X., Rehk€amper, M., Lee, D.-C., Halliday, A.N., 1997. High precision 230Th/232Th
contains the limestone bedrock covered by a ~2.5 mm thick calcite and 234U/238U measurements using energy filtered ICP magnetic sector
coating” (Aubert et al., 2007: page 994). The sample was already multiple collector mass spectrometry. International Journal of Mass Spec-
exfoliating and was near an Austronesian-type painting providing a trometry 171, 105e117.
Pike, A.W.G., Hoffmann, D.L., García-Diez, M., Pettitt, P.B., Alcolea, J., De Balbín, R.,
probable maximum age for the image. A red layer was subsequently Gonz alez Sainz, C., De Las Heras, C., Lasheras, J.-A., Montes, R., Zilhao, J., 2012.
observed within the micro-stratigraphy of the sample and we were U-series dating of Paleolithic art in 11 caves in Spain. Science 336, 1409e1413.
able to bracket its age. This red layer is possibly the remnants of a Plagnes, V., Causse, C., Fontugne, M., Valladas, H., Chazine, J.-M., Fage, L.-H., 2003.
Cross dating (Th/U-14C) of calcite covering prehistoric paintings in Borneo.
much older painted image […] but “specialised analysis of the red Quaternary Research 60, 172e179.
layer is required to identify the constituents, such as organic Pons-Bronchu, E., Fontugne, M., Michel, V., Valladas, H., 2015. Comment on: “Ura-
binders and mineral phases to confirm its anthropogenic origin as niumethorium Dating Method and Palaeolithic Rock Art” by Sauvet et al (in
press).
paint” (Aubert et al., 2007: page 995). This paper was a proof of
Sauvet, G., Bourrillon, R., Conkey, M., Fritz, C., G arate-Maidagan, D., Rivero, Vil a,
concept to show that thin natural calcite laminations can provide Tosello, G., White, R., 2016. Uraniume-Thorium Dating Method and Palaeolithic
the means for bracketing the age of cave paintings and no rock art Rock Art (in press).
was ‘damaged’. Watchman, A.L., 2000. Micro-excavation and laser extraction methods for dating
carbon in silica skins and oxalate crusts. In: Ward, G.K., Tuniz, C. (Eds.), Ad-
Similarly, core sampling was not used in Sulawesi. Instead, “a vances in Dating Australian Rock-Markings. Occasional AURA Publication 10,
small segment (100e200 mm2) of each coralloid was removed from pp. 35e39.

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