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Improved AMS 14C Dating of Shell Carbonates Using High-Precision X-Ray Diffraction and a Novel Density Separation Protocol (Cards)

Published online by Cambridge University Press:  18 July 2016

Katerina Douka ,
Robert E M Hedges  and
Thomas F G Higham
Katerina Douka*
Affiliation:
Research Laboratory for Archaeology and the History of Art, University of Oxford, Dyson Perrins Building, South Parks Road, Oxford OX1 3QY, United Kingdom Oxford Radiocarbon Accelerator Unit, Research Laboratory for Archaeology and the History of Art, University of Oxford, Dyson Perrins Building, South Parks Road, Oxford OX1 3QY, United Kingdom
Robert E M Hedges
Affiliation:
Research Laboratory for Archaeology and the History of Art, University of Oxford, Dyson Perrins Building, South Parks Road, Oxford OX1 3QY, United Kingdom
Thomas F G Higham
Affiliation:
Oxford Radiocarbon Accelerator Unit, Research Laboratory for Archaeology and the History of Art, University of Oxford, Dyson Perrins Building, South Parks Road, Oxford OX1 3QY, United Kingdom
*
Corresponding author. Email: [email protected]
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Abstract

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One critical variable in the successful application of radiocarbon dating is the effective removal of carbonaceous contaminants. In the case of marine carbonates, contamination appears usually in the form of secondary low-magnesium calcite, the stable polymorph of calcium carbonate and byproduct of the post-mortem recrystallization or replacement of the autochthonous phase, originally in the form of high-magnesium calcite or aragonite. Depending on the nature of the depositional environment, the secondary phase may be contemporary in age with the original shell carbonate and may have even been derived from it by dissolution-recrystallization processes, or can be an exogenous contaminant of younger or older age. The limited ability of current pretreatment protocols to detect and remove the secondary mineralogical phases prior to dating carbonates has been one of the reasons marine shell and coral 14C determinations are often difficult to validate in terms of their reliability. We have developed a new pretreatment protocol designed to achieve greater reliability and accuracy in the dating of this material. The method entails 2 steps. The first one involves the improved detection and quantification of secondary calcite in aragonite using X-ray diffraction, at a precision of ∼0.1% and ∼0.8%, respectively. Next, where this is required, a novel density separation step using non-toxic heavy liquids (CarDS) is applied to the diagenetic sample. This enables the clear separation of calcite and aragonite, with only the latter kept for dating. We have applied the new steps, screening and separation, on standard and archaeological examples and our initial results suggest that it is successful and reproducible. In this paper, we describe the method and initial results.

Type
Methods, Applications, and Developments
Information
Radiocarbon , Volume 52 , Issue 2: 20th Int. Radiocarbon Conference Proceedings , 2010 , pp. 735 - 751
Copyright
Copyright © 2010 by the Arizona Board of Regents on behalf of the University of Arizona 

References

Addadi, L, Joester, D, Nudelman, F, Weiner, S. 2006. Mollusk shell formation: a source of new concepts for understanding biomineralization processes. Chemistry -A European Journal 12(4):980–7.CrossRefGoogle ScholarPubMed
Allan, JR, Matthews, RK. 1982. Isotope signatures associated with early meteoric diagenesis. Sedimentology 29(6):797–817.CrossRefGoogle Scholar
Allison, PA, Pye, K. 1994. Early diagenetic mineralization and fossil preservation in modern carbonate concretions. Palaios 9(6):561–75.CrossRefGoogle Scholar
Arnarson, TS, Keil, RG. 2001. Organic–mineral interactions in marine sediments studied using density fractionation and X-ray photoelectron spectroscopy. Organic Geochemistry 32(12):1401–15.CrossRefGoogle Scholar
Balmain, J, Hannoyer, B, Lopez, E. 1999. Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction analyses of mineral and organic matrix during heating of mother of pearl (nacre) from the shell of the mollusc Pinctada maxima. Journal of Biomedical Materials Research B 48(5):749–54.Google ScholarPubMed
Bard, E, Hamelin, B, Fairbanks, RG, Zindler, A, Mathieu, G, Arnold, M. 1990. U/Th and 14C ages of corals from Barbados and their use for calibrating the 14C time scale beyond 9000 years B.P. Nuclear Instruments and Methods in Physics Research B 52(3–4):461–8.CrossRefGoogle Scholar
Bard, E, Arnold, M, Fairbanks, RG, Hamelin, B. 1993. 230Th/234U and 14C ages obtained by mass spectrometry on corals. Radiocarbon 35(1):191–9.CrossRefGoogle Scholar
Basford, JR, Coscio, MR. 1973. An improved method for rapid, low loss density separations with heavy liquids. American Mineralogist 58:1094–5.Google Scholar
Bathurst, RGC. 1971. Carbonate Sediments and Their Diagenesis. Amsterdam: Elsevier. 620 p.Google Scholar
Bell, MS, Hörz, F, Reid, A. 1998. Characterization of experimental shock effects in calcite and dolomite by X-ray diffraction (abstract #1422). 29th Lunar and Planetary Institute Conference. URL: http://www.lpi.usra.edu/meetings/LPSC98/pdf/1422.pdf.Google Scholar
Bish, DL, Post, JE. 1993. Quantitative mineralogical analysis using the Rietveld full-pattern fitting method. American Mineralogist 78(9–10):932–40.Google Scholar
Brock, F, Higham, TFG, Ditchfield, P, Bronk Ramsey, C. 2010. Current pretreatment methods for AMS radiocarbon dating at the Oxford Radiocarbon Accelerator Unit (ORAU). Radiocarbon 52(1):103–12.CrossRefGoogle Scholar
Burr, GS, Edwards, RL, Donahue, DJ, Druffel, ERM, Taylor, FW. 1992. Mass spectrometric 14C and U-Th measurements in coral. Radiocarbon 34(3):611–8.CrossRefGoogle Scholar
Callahan, J. 1987. A nontoxic heavy liquid and inexpensive filters for separation of mineral grains. Journal of Sedimentary Petrology 57(4):765–6.CrossRefGoogle Scholar
Chappell, A, Polach, HA. 1972. Some effects on partial recrystallisation on 14C dating Late Pleistocene corals and molluscs. Quaternary Research 2(2):244–52.CrossRefGoogle Scholar
Chave, KE, Deffeyes, KS, Weyl, PK, Garrels, RM, Thompson, ME. 1962. Observations on the solubility of skeletal carbonates in aqueous solutions. Science 137(3523):33–4.CrossRefGoogle ScholarPubMed
Chiu, T-C, Fairbanks, RG, Mortlock, RA, Bloom, AL. 2005. Extending the radiocarbon calibration beyond 26,000 years before present using fossil corals. Quaternary Science Reviews 24(16–17):1797–808.CrossRefGoogle Scholar
Edwards, RL, Beck, JW, Burr, GS, Donahue, DJ, Chappell, JMA, Bloom, AL, Druffel, ERM, Taylor, FW. 1993. A large drop in atmospheric 14C/12C and reduced melting in the Younger Dryas documented with 230Th ages of corals. Science 260(5110):962–8.CrossRefGoogle ScholarPubMed
Enmar, R, Stein, M, Bar-Matthews, M, Sass, E, Katz, A, Lazar, B. 2000. Diagenesis in live corals from the Gulf of Aqaba. I. The effect on paleo-oceanography tracers. Geochimica et Cosmochimica Acta 64(18):3123–32.CrossRefGoogle Scholar
Folk, RL. 1974. The natural history of crystalline calcium carbonate; effect of magnesium content and salinity. Journal Sedimentary Petrology 44(1):40–53.Google Scholar
Folk, RL, Assereto, R. 1976. Comparative fabrics of length-slow and length-fast calcite and calcitized aragonite in a Holocene speleothem, Carlsbad Caverns, New Mexico. Journal Sedimentary Petrology 46(3):486–96.Google Scholar
Foster, LC, Andersson, C, Høie, H, Allison, N, Finch, AA, Johansen, T. 2008. Effects of micromilling on δ18O in biogenic aragonite. Geochemistry Geophysics Geosystems 9: Q04013, doi:10.1029/2007GC001911.CrossRefGoogle Scholar
Gaffey, SJ, Kolak, JK, Bronnimann, CE. 1991. Effects of drying, heating, annealing, and roasting on carbonate skeletal material, with geochemical and diagenetic implications. Geochimica et Cosmochimica Acta 55(6):1627–40.CrossRefGoogle Scholar
Given, RK, Wilkinson, BH. 1985. Kinetic control of morphology, composition, and mineralogy of abiotic sedimentary carbonates. Journal Sedimentary Petrology 55(1):109–19.Google Scholar
Grant-Taylor, TL. 1972. Conditions for the use of calcium carbonate as a dating material. In: Rafter, TA, Grant-Taylor, TL, editors. Proceedings of the 8th International Conference on Radiocarbon Dating. Wellington: Royal Society New Zealand. p G56–59.Google Scholar
Green, OR. 2001. A Manual of Practical Laboratory and Field Techniques in Palaeobiology. Dordrecht: Kluwer Academic Publishers. 538 p.CrossRefGoogle Scholar
Gross, KS. 1965. X-ray line broadening and stored energy in deformed and annealed calcite. Philosophical Magazine 12(118):801–13.CrossRefGoogle Scholar
Gussone, N, Böhm, F, Eisenhauer, A, Dietzel, M, Heuser, A, Teichert, BMA, Reitner, J, Wörheide, G, Dullo, W. 2005. Calcium isotope fractionation in calcite and aragonite. Geochimica et Cosmochimica Acta 69(18):4485–94.CrossRefGoogle Scholar
Henderson, GM, Rendle, RH, Slowey, NC, Reijmer, JJG. 2000. U-Th dating and diagenesis of Pleistocene highstand sediments from the Bahamas slope. In: Swart, PK, Eberli, GP, Malone, MJ, Sarg, JF, editors. Proceedings of the Ocean Drilling Program, Scientific Results 166:61–76.Google Scholar
Henderson, GM, Slowey, NC, Fleisher, MQ. 2001. U-Th dating of carbonate platform and slope sediments. Geochimica Cosmochimica Acta 65(16):2757–70.CrossRefGoogle Scholar
Ijlst, L. 1973. A laboratory overflow-centrifuge for heavy liquid mineral separation. American Mineralogist 58:1088–93.Google Scholar
Klug, HP, Alexander, LE. 1974. X-Ray Diffraction Procedures: For Polycrystalline and Amorphous Materials. New York: John Wiley & Sons. 992 p.Google Scholar
Krukowski, ST. 1988. Sodium metatungstate: a new heavy-mineral separation medium for the extraction of conodonts from insoluble residues. Journal of Paleontology 62(2):314–6.CrossRefGoogle Scholar
Lécuyer, C. 1996. Effects of heating on the geochemistry of biogenic carbonates. Chemical Geology 129(3–4):173–83.CrossRefGoogle Scholar
Lowenstam, HA, Weiner, S. 1989. On Biomineralization. New York: Oxford University Press. 324 p.CrossRefGoogle Scholar
Magnani, G, Bartolomei, P, Cavulli, F, Esposito, M, Marino, EC, Neri, M, Rizzo, A, Scaruffi, S, Tosi, M. 2007. U-series and radiocarbon dates on mollusc shells from the uppermost layer of the archaeological site of KHB-1, Ra's al Khabbah, Oman. Journal of Archaeological Science 34(5):749–55.CrossRefGoogle Scholar
McGregor, HV, Gagan, MK. 2003. Diagenesis and geochemistry of Porites corals from Papua New Guinea: implications for paleoclimate reconstruction. Geochimica et Cosmochimica Acta 67(12):2147–56.CrossRefGoogle Scholar
Milliman, JD. 1974. Marine Carbonates. Berlin: Spinger-Verlag. 375 p.Google Scholar
Morse, JW, Mackenzie, FT. 1990. Geochemistry of Sedimentary Carbonates. New York: Elsevier. 707 p.Google Scholar
Morse, W, Wang, Q, Tsio, MY. 1997. Influences of temperature and Mg:Ca ratio on CaCO3 precipitates from seawater. Geology 25(1):85–7.2.3.CO;2>CrossRefGoogle Scholar
Munsterman, D, Kerstholt, S. 1996. Sodium polytungstate, a new non-toxic alternative to bromoform in heavy liquid separation. Review of Palaeobotany and Palynology 91(1–4):417–22.CrossRefGoogle Scholar
Northwood, DO, Lewis, D. 1970. Strain induced calcitearagonite transformation in calcium carbonate. The Canadian Mineralogist 10:216–24.Google Scholar
Nunn, PD, Peltier, WR. 2001. Far-field test of the ICE-4G model of global isostatic response to deglaciation using empirical and theoretical Holocene sea-level reconstructions for the Fiji Islands, southwestern Pacific. Quaternary Research 55(2):203–14.CrossRefGoogle Scholar
Reimer, PJ, Baillie, MGL, Bard, E, Beck, JW, Blackwell, PG, Buck, CE, Burr, GS, Edwards, LR, Friedrich, M, Guilderson, TP, Hogg, AG, Hughen, KA, Kromer, B, McCormac, G, Manning, S, Reimer, RW, Southon, JR, Stuiver, M, van der Plicht, J, Weyhenmeyer, CE. 2006. Comment on “Radiocarbon calibration curve spanning 0 to 50,000 years BP based on paired 230Th/234U/238U and 14C dates on pristine corals” by R.G. Fairbanks et al. (Quaternary Science Reviews 24 (2005) 1781–1796) and “Extending the radiocarbon calibration beyond 26,000 years before present using fossil corals” by T.-C. Chiu et al. (Quaternary Science Reviews 24 (2005) 1797–1808). Quaternary Science Reviews 25(7–8):855–62.Google Scholar
Richelle, LJ. 1964. One possible solution to the problem of the biochemistry of bone mineral. Clinical Orthopaedics and Related Research 33:211–9.CrossRefGoogle Scholar
Schmalz, RF. 1967. Kinetics and diagenesis of carbonate sediments. Journal of Sedimentary Petrology 37(1):60–7.Google Scholar
Sepulcre, S, Durand, N, Bard, E. 2009. Mineralogical determination of reef and periplatform carbonates: calibration and implications for paleoceanography and radiochronology. Global and Planetary Change 66(1–2):1–9.CrossRefGoogle Scholar
Shin, J-Y. 2007. Studies in extracting isotopic information from archaeological bone [unpublished DPhil thesis]. University of Oxford.Google Scholar
Takenaka, M, Ikeda, M, Terada, S. 1999. The use of microwave digestion method for the determination of chemical forms of sodium and chloride ions in seashell structures. Analytical Communications 36(3):109–11.CrossRefGoogle Scholar
Thommeret, J, Thommeret, Y. 1965. Quelques limitations a la méthode du carbone 14 pour la datation des coquilles. Bulletin du Musée d'Anthropologie Préhistorique de Monaco 12:17–22.Google Scholar
Tucker, ME. 2001. Sedimentary Petrology: An Introduction to the Origin of Sedimentary Rocks. 3rd edition. Chichester: Wiley-Blackwell. 372 p.Google Scholar
Ulm, S. 2006. Mort Creek Site Complex. Coastal Themes: An Archaeology of the Southern Curtis Coast, Queensland. Series Terra Australis 24. Canberra: Australian National University. Press. p 97–113.Google Scholar
Vandergoes, MJ, Prior, CA. 2003. AMS dating of pollen concentrates—a methodological study of late Quaternary sediments from south Westland, New Zealand. Radiocarbon 45(3):479–91.CrossRefGoogle Scholar
Vita-Finzi, C. 1980. 14C dating of recent crustal movements in the Persian Gulf and Iranian Makran. Radiocarbon 22(3):763–73.CrossRefGoogle Scholar
Vita-Finzi, C, Roberts, N. 1984. Selective leaching of shells for 14C dating. Radiocarbon 26(1):54–8.CrossRefGoogle Scholar
Walter, LM. 1986. Relative efficiency of carbonate dissolution and precipitation during diagenesis: a progress report on the role of solution chemistry. In: Gautier, DL, editor. Roles of Organic Matter in Mineral Diagenesis. Special Publication 38. Tulsa: Society of Economic Paleontologists and Mineralogists. p 1–12.Google Scholar
Webb, GE, Price, GJ, Nothdurft, LD, Deer, L, Rintoul, L. 2007. Cryptic meteoric diagenesis in freshwater bivalves: implications for radiocarbon dating. Geology 35(9):803–6.CrossRefGoogle Scholar
Welberry, TR. 2004. Diffuse X-Ray Scattering and Models of Disorder. IUCr Monographs on Crystallography 16. New York: Oxford University Press. 280 p.Google Scholar
Wolf, G, Günther, C. 2001. Thermophysical investigations of the polymorphous phases of calcium carbonate. Journal of Thermal Analysis and Calorimetry 65(3):687–98.CrossRefGoogle Scholar
Yokoyama, Y, Esat, TM, Lambeck, K, Fifield, LK. 2000. Last ice age millennial scale climate changes recorded in Huon Peninsula corals. Radiocarbon 42(3):383–401.CrossRefGoogle Scholar