Hostname: page-component-8448b6f56d-wq2xx Total loading time: 0 Render date: 2024-04-19T19:56:05.378Z Has data issue: false hasContentIssue false

Single step Production of graphite from organic Samples for Radiocarbon Measurements

Published online by Cambridge University Press:  25 November 2019

K L Elder*
Affiliation:
Woods Hole Oceanographic Institution, Woods Hole, MA 02543USA
M L Roberts
Affiliation:
Woods Hole Oceanographic Institution, Woods Hole, MA 02543USA
T Walther
Affiliation:
Woods Hole Oceanographic Institution, Woods Hole, MA 02543USA University of Maine, Orono, ME 04469USA
L Xu
Affiliation:
Woods Hole Oceanographic Institution, Woods Hole, MA 02543USA
*
*Corresponding author. Email: kelder@whoi.edu.

Abstract

We present a new low-cost, high-throughput method for converting many types of organic carbon samples into graphite for radiocarbon (14C) measurements by accelerator mass spectrometry (AMS). The method combines sample combustion and reduction to graphite into a single procedure. In the Single Step method, solid samples are placed directly into Pyrex containing zinc, titanium hydride and iron catalyst. The tube is evacuated, flame sealed, and placed in a muffle furnace for 7 hr. A variety of organic samples have been tested including oxalic acid, sucrose, wood, peat, collagen, humic acid, and contamination swipe samples. The method significantly reduces the time required to produce a graphite sample for 14C measurement, with analytical precision and accuracy approaching that of traditional two-step combustion and hydrogen reduction methods. The details and applicability of the method are presented.

Type
Conference Paper
Copyright
© 2019 by the Arizona Board of Regents on behalf of the University of Arizona 

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

Footnotes

Selected Papers from the 23rd International Radiocarbon Conference, Trondheim, Norway, 17–22 June, 2018

References

REFERENCES

Cruz, A, Childress, LB, Gagnon, A, McNichol, A, Burton, J, Elder, K, Lardie-Gaylord, M, Gospodinova, K, Hlavenka, J, Kurz, M, Longworth, B, Roberts, M, Trowbridge, N, Walther, T, and Xu, L. 2017. Advances in sample preparation at the National Ocean Sciences Accelerator Mass Spectrometry Facility (NOSAMS): Investigation of Carbonate Secondary Standards. Abstract in the 14th International Conference on Accelerator Mass Spectrometry, Ottawa, Canada, August 14–18 (Abstract ID: 400; Poster: SPT80). Available at https://hdl.handle.net/1912/10620.Google Scholar
Elder, KL, Roberts, ML, Lardie-Gaylord, MC. 2017. Single Step production of graphite from organic samples. Abstract in the 14th International Conference on Accelerator Mass Spectrometry, Ottawa, Canada, August 14–18 (Abstract ID: 180; Poster: SPT64). Available at https://hdl.handle.net/1912/10616.Google Scholar
Gagnon, A, Jones, G. 1993. AMS-graphite target production methods at the Woods Hole Oceanographic Institution during 1986–1991. Radiocarbon 35(2):301310. doi: 10.1017/S0033822200064985.CrossRefGoogle Scholar
Getachew, G, Kim, S-H, Burri, BJ, Kelly, PB, Haack, KW, Ognibene, TJ, Bucholz, BA, Vogel, JS, Modrow, J, Clifford, AJ. 2006. How to convert biological carbon into graphite for AMS. Radiocarbon 48(3):325336.10.1017/S0033822200038789CrossRefGoogle Scholar
Hua, Q, Barbetti, M. 2004. Review of tropospheric bomb 14C data for carbon cycle modeling and age calibration purposes. Radiocarbon 46(3):12731298.CrossRefGoogle Scholar
Khosh, MS, Xu, XM, Trumbore, SE. 2010. Small-mass graphite preparation by sealed-tube zinc reduction method for AMS C-14 measurements. Nuclear Instruments and Methods in Physics Research B 268:927930.CrossRefGoogle Scholar
Lardie-Gaylord, MC, Longworth, BE, Murphy, K, Cobb, C, McNichol, AP. 2019. Annual radiocarbon measurements in a century-old European beech tree (Fagus sylvatica) from coastal northeastern North America. Accepted to Nuclear Instruments and Methods in Physics Research B. doi: 10.1016/j.nimb.2019.03.029.CrossRefGoogle Scholar
McIntyre, CP, Lechleitner, F, Lang, SQ, Haghiour, N, Fahrni, S, Wacker, L, Synal, H-A. 2016. 14C contamination testing in natural abundance laboratories: A new preparation method using wet chemical oxidation and some experiences. Radiocarbon 58(4):935941.10.1017/RDC.2016.78CrossRefGoogle Scholar
Pearson, A, McNichol, AP, Schneider, RJ, von Reden, KF. 1998. Microscale AMS 14C measurement at NOSAMS. Radiocarbon 40(1):6175.10.1017/S0033822200017902CrossRefGoogle Scholar
Roberts, ML, Burton, JR, Elder, KL, Longworth, BE, McIntyre, CP, von Reden, KF, Han, BX, Rosenheim, BE, Jenkins, WJ, Galutschek, E, McNichol, AP. 2010. A high-performance 14C accelerator mass spectrometry system. Radiocarbon 52(2):228235.CrossRefGoogle Scholar
Roberts, ML, Elder, KL, McNichol, AP, Jenkins, WJ, Gagnon, AR, Xu, L, Hlavenka, JD, Longworth, BE. 2019. Determination of the 14C blank at the National Ocean Sciences AMS Laboratory. Radiocarbon. doi: 10.1017/RDC.2019.74.CrossRefGoogle Scholar
Santos, GM, Southon, JR, Griffin, S, Beaupre, SR, Druffel, ERM. 2007. Ultra small-mass AMS 14C sample preparation and analyses at KCCAMS/UCI facility. Nuclear Instruments and Methods in Physics Research B 259(1):293302.10.1016/j.nimb.2007.01.172CrossRefGoogle Scholar
Shah Walter, SR, Gagnon, A, Roberts, M, McNichol, AP, Lardie Gaylord, M, Klein, E. 2015. Ultra-small graphitization reactors for ultra-microscale 14C analysis at the National Ocean Sciences Accelerator Mass Spectrometry (NOSAMS) Facility. Radiocarbon 57:109122. doi: 10.2458/azu_rc.57.18118.CrossRefGoogle Scholar
Sookdeo, A, Wacker, L, Fahrni, S, McIntyre, CP, Friedrich, M, Reinig, F, Nievergelt, D, Tegel, W, Kromer, B, Buntgen, U. 2017. Speed dating: A rapid way to determine the radiocarbon age of wood by EA-AMS. Radiocarbon 59(3):933939.CrossRefGoogle Scholar
Vogel, JS, Nelson, DE, Southon, JS. 1987. 14C background levels in an accelerator mass spectrometry system. Radiocarbon 29(3): 323333. doi: 10.1017/S0033822200043733.CrossRefGoogle Scholar
Vogel, JS. 1992. Rapid production of graphite without contamination for biomedical AMS. Radiocarbon 34(3):344350.10.1017/S0033822200063529CrossRefGoogle Scholar
Xu, X, Trumbore, SE, Zheng, S, Southon, JR, McDuffee, KE, Luttgen, M, Liu, JC. 2007. Modifying a sealed tube zinc reduction method for preparation of AMS graphite targets: Reducing background and attaining high precision. Nuclear Instruments and Methods in Physics Research B 259:320329.CrossRefGoogle Scholar
Xu, XM, Gao, P, Salamanca, EG. 2013. Ultra small-mass graphitization by sealed-tube zinc reduction method for AMS 14C measurements. Radiocarbon 55:608616.CrossRefGoogle Scholar