Hostname: page-component-77c89778f8-vpsfw Total loading time: 0 Render date: 2024-07-19T18:01:54.308Z Has data issue: false hasContentIssue false

Ultra-Small Graphitization Reactors for Ultra-Microscale 14C Analysis at the National Ocean Sciences Accelerator Mass Spectrometry (NOSAMS) Facility

Published online by Cambridge University Press:  09 February 2016

Sunita R Shah Walter*
Affiliation:
Geology and Geophysics Department, Woods Hole Oceanographic Institution, 360 Woods Hole Road, Woods Hole, MA 02543, USA
Alan R Gagnon
Affiliation:
Geology and Geophysics Department, Woods Hole Oceanographic Institution, 360 Woods Hole Road, Woods Hole, MA 02543, USA
Mark L Roberts
Affiliation:
Geology and Geophysics Department, Woods Hole Oceanographic Institution, 360 Woods Hole Road, Woods Hole, MA 02543, USA
Ann P McNichol
Affiliation:
Geology and Geophysics Department, Woods Hole Oceanographic Institution, 360 Woods Hole Road, Woods Hole, MA 02543, USA
Mary C Lardie Gaylord
Affiliation:
Geology and Geophysics Department, Woods Hole Oceanographic Institution, 360 Woods Hole Road, Woods Hole, MA 02543, USA
Elizabeth Klein
Affiliation:
Geology and Geophysics Department, Woods Hole Oceanographic Institution, 360 Woods Hole Road, Woods Hole, MA 02543, USA
*
Corresponding author. Email: shah@fas.harvard.edu.

Abstract

In response to the increasing demand for 14C analysis of samples containing less than 25 μg C, ultra-small graphitization reactors with an internal volume of ∼0.8 mL were developed at NOSAMS. For samples containing 6 to 25 μg C, these reactors convert CO2 to graphitic carbon in approximately 30 min. Although we continue to refine reaction conditions to improve yield, the reactors produce graphite targets that are successfully measured by AMS. Graphite targets produced with the ultra-small reactors are measured by using the Cs sputter source on the CFAMS instrument at NOSAMS where beam current was proportional to sample mass. We investigated the contribution of blank carbon from the ultra-small reactors and estimate it to be 0.3 ± 0.1 μg C with an Fm value of 0.43 ± 0.3. We also describe equations for blank correction and propagation of error associated with this correction. With a few exceptions for samples in the range of 6 to 7 μg C, we show that corrected Fm values agree with expected Fm values within uncertainty for samples containing 6–100 μg C.

Type
Articles
Copyright
Copyright © 2015 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.)

References

Currie, LA, Polach, HA. 1980. Exploratory analysis of the International Radiocarbon Cross-Calibration Data: consensus values and interlaboratory error. Radiocarbon 22(3):933–5.Google Scholar
Drenzek, NJ, Montluçon, DB, Yunker, MB, Macdonald, RW, Eglinton, TI. 2007. Constraints on the origin of sedimentary organic carbon in the Beaufort Sea from coupled molecular 13C and 14C measurements. Marine Chemistry 103(1–2):146–62.Google Scholar
Gagnon, AR, McNichol, AP, Donoghue, JC, Stuart, DR, von Reden, K, NOSAMS. 2000. The NOSAMS sample preparation laboratory in the next millenium: progress after the WOCE program. Nuclear Instruments and Methods in Physics Research B 172(1–4):409–15.Google Scholar
Hua, Q, Jacobsen, GE, Zoppi, U, Lawson, EM, Williams, AA, Smith, AM, McGann, MJ. 2001. Progress in radiocarbon target preparation at the ANTARES AMS Centre. Radiocarbon 43(2A):275–82.Google Scholar
Hua, Q, Zoppi, U, Williams, AA, Smith, AM. 2004. Small-mass AMS radiocarbon analysis at ANTARES. Nuclear Instruments and Methods in Physics Research B 223–224:284–92.Google Scholar
Ingalls, AE, Shah, SR, Hansman, RL, Aluwihare, LI, Santos, GM, Druffel, ERM, Pearson, A. 2006. Quantifying archaeal community autotrophy in the mesopelagic ocean using natural radiocarbon. Proceedings of the National Academy of Sciences USA 103(17):6442–7.Google Scholar
Ingalls, AE, Ellis, EE, Santos, GM, McDuffee, KE, Truxal, L, Keil, RG, Druffel, ERM. 2010. HPLC purification of higher plant-dervied lignin phenols for compound specific radiocarbon analysis. Analytical Chemistry 82(21):8931–8.Google Scholar
Keigwin, LD, Gagnon, AR. 2015. Comparison of large and ultra-small Δ14C measurements in core top benthic foraminifera from the Okhotsk Sea. Radiocarbon 57(1):123–8.Google Scholar
Keigwin, LD, Guilderson, TP. 2009. Bioturbation artifacts in zero-age sediments. Paleoceanography 24(4):PA4212, doi:10.1029/2008PA001727.Google Scholar
Kirner, DL, Taylor, RE, Southon, JR. 1995. Reduction in backgrounds of microsamples for AMS 14C dating. Radiocarbon 37(2):697704.Google Scholar
Kitagawa, H, Masuzawa, T, Makamura, T, Matsumoto, E. 1993. A batch preparation method for graphite targets with low background for AMS 14C measurements. Radiocarbon 35(2):295300.Google Scholar
Le Clercq, M, van der Plicht, J, Gröning, M. 1998. New 14C reference materials with activities of 15 and 50 pMC. Radiocarbon 40(1):295–7.Google Scholar
Liebl, J, Ortiz, RA, Golser, R, Handle, F, Kutschera, W, Steier, P, Wild, EM. 2010. Studies on the preparation of small 14C samples with an RGA and 13C-enriched material. Radiocarbon 52(3):1394–404.Google Scholar
Liebl, J, Steier, P, Golser, R, Kutschera, W, Mair, K, Priller, A, Vonderhaid, I, Wild, EM. 2013. Carbon background and ionization yield of an AMS system during 14C measurements of microgram-size graphite samples. Nuclear Instruments and Methods in Physics Research B 294:335–9.Google Scholar
Mann, WB. 1983. An international reference material for radiocarbon dating. Radiocarbon 25(2):519–27.Google Scholar
McNichol, AP, Gagnon, AR, Jones, GA, Osborne, EA. 1992. Illumination of a black box: analysis of gas composition during graphite target preparation. Radiocarbon 34(3):321–9.CrossRefGoogle Scholar
Ohkouchi, N, Eglinton, TI, Keigwin, LD, Hayes, JM. 2002. Spatial and temporal offsets between proxy records in a sediment drift. Science 298(5596):1224–7.CrossRefGoogle Scholar
Ohkouchi, N, Xu, L, Reddy, CM, Montluçon, D, Eglinton, TI. 2005. Radiocarbon dating of alkenones from marine sediments: I. isolation protocol. Radiocarbon 47(3):401412.Google Scholar
Osborne, EA, McNichol, AP, Gagnon, AR, Hutton, DL, Jones, GA. 2000. Internal and external checks in the NOSAMS sample preparation laboratory for target quality and homogeneity. Nuclear Instruments and Methods in Physics Research B 92(1–4):158–61.Google Scholar
Pearson, A, McNichol, AP, Schneider, RJ, von Reden, KF. 1998. Microscale AMS 14C measurement at NOSAMS. Radiocarbon 40(1):6175.CrossRefGoogle Scholar
Pearson, A, Seewald, JS, Eglinton, TI. 2005. Bacterial incorporation of relict carbon in the hydrothermal environment of Guaymas Basin. Geochimica et Cosmochimica Acta 69(23):5477–86.Google 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):228–35.Google Scholar
Rosenheim, BE, Galy, V. 2012. Direct measurement of riverine particulate organic carbon age structure. Geophysical Research Letters 39:L198703, doi:10.1029/2012GL052883.Google Scholar
Rosenheim, BE, Day, MB, Domack, E, Schrum, H, Benthien, A, Hayes, JM. 2008. Antarctic sediment chronology by programmed-temperature pyrolysis: methodology and data treatment. Geochemistry, Geophysics, Geosystems 9:Q04005, doi:10.1029/2007GC001816.Google Scholar
Rozanski, K, Stichler, W, Gonfiantini, R, Scott, EM, Beukens, RP, Kromer, B, van der Plicht, J. 1992. The IAEA 14C intercomparison exercise 1990. Radiocarbon 34(3):506–19.Google Scholar
Santos, GM, Southon, JR, Griffin, S, Beaupré, 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.Google Scholar
Santos, GM, Southon, JR, Drenzek, NJ, Ziolkowski, LA, Druffel, ERM, Xu, X, Zhang, D, Trumbore, S, Eglinton, TI, Hughen, KA. 2010. Blank assessment for ultra-small radiocarbon samples: chemical extraction and separation versus AMS. Radiocarbon 52(3):1322–35.Google Scholar
Scott, EM. 2003. The Third International Radiocarbon Intercomparison (TIRI) and the Fourth International Radiocarbon Intercomparison (FIRI): Section 10. Radiocarbon 45(2):285–90.Google Scholar
Shah, SR, Pearson, A. 2007. Ultra-microscale (5–25 μg C) analysis of individual lipids by 14C AMS: assessment and correction for sample processing blanks. Radiocarbon 49(1):6982.Google Scholar
Stuiver, M. 1983. International agreements and the use of the new oxalic acid standard. Radiocarbon 25(2):793–5.Google Scholar
Stuiver, M, Polach, HA. 1977. Discussion: reporting of 14C data. Radiocarbon 19(3):355–63.Google Scholar
van der Borg, K, Alderliesten, C, de Jong, AFM, van den Brink, A, de Haas, AP, Kersemaekers, HJH, Raaymakers, JEMJ. 1997. Precision and mass fractionation in 14C analysis with AMS. Nuclear Instruments and Methods in Physics Research B 123(1–4):97101.Google Scholar
Verkouteren, RM, Klinedinst, DB, Currie, LA. 1997. Iron-manganese system for preparation of radiocarbon AMS targets: characterization of precedural chemical-isotopic blanks and fractionation. Radiocarbon 39(3):269–83.Google Scholar
Vogel, JS, Nelson, DE, Southon, JR. 1987. 14C background levels in an accelerator mass spectrometry system. Radiocarbon 29(3):323–33.Google Scholar
von Reden, KF, McNichol, AP, Pearson, A, Schneider, RJ. 1998. 14C AMS measurements of <100 μg samples with a high-current system. Radiocarbon 40(1):247–53.Google 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 targests: reducing background and attaining high precision. Nuclear Instruments and Methods in Physics Research B 259(1):320–9.Google Scholar
Yokoyama, Y, Koizumi, M, Matsuzaki, H, Miyairi, Y, Ohkouchi, N. 2010. Developing ultra small-scale radiocarbon sample measurement at the University of Tokyo. Radiocarbon 52(2):310–8.Google Scholar
Ziolkowski, LA, Druffel, ERM. 2009. Quantification of extraneous carbon during compound specific radiocarbon analysis of black carbon. Analytical Chemistry 81(24):10, 156–61.CrossRefGoogle ScholarPubMed