Hostname: page-component-586b7cd67f-l7hp2 Total loading time: 0 Render date: 2024-11-24T09:00:09.687Z Has data issue: false hasContentIssue false

Testing sealed-tube Graphitization at the NERC Radiocarbon facility, east Kilbride

Published online by Cambridge University Press:  09 September 2019

Luz Maria Cisneros-Dozal*
Affiliation:
NERC Radiocarbon Facility, East Kilbride, G75 0QF, UK
Xiaomei Xu
Affiliation:
KCCAMS Laboratory, Department of Earth System Science, University of California, Irvine, CA, 92697, USA
Sheng Xu
Affiliation:
SUERC AMS Laboratory, East Kilbride, G75 0QF, UK Current address:Institute of Surface-Earth System Science, Tianjin University, Tianjin 300072, China
*
*Corresponding author. Email: malu.cisneros@glasgow.ac.uk.

Abstract

Graphitization of 0.5–1.5 mg C, and of smaller samples to a lesser extent, is routinely done at our Facility by reduction over zinc. The method yields low background, good accuracy but offers a limited throughput, requires dedicated equipment and considerable operator time. Sealed-tube graphitization is faster, easier and cost-efficient producing as many graphites as CO2 can be purified in one day with low background, good accuracy and precision, provided precise measurements of δ13C values can be attained by accelerator mass spectrometry (AMS) to correct for isotope fractionation (Xu et al. 2007). We tested sealed-tube graphitization on 0.1 to 1.0 mg C samples and found that while we were able to obtain low backgrounds of >57,000 ±1000 yr BP for ∼1.7 mg C and 41,230 ± 430 yr BP for ∼0.09 mg C (0.0008 ± 0.0001 and 0.0059 ± 0.0003 Fraction Modern, respectively), results were variable for sample sizes <0.5 mg C. Measurements of FIRI Belfast Cellulose and TIRI Barleymash showed 0.3–0.6% precision and 1% accuracy for most sample sizes. We found better results in our laboratory by introducing the following modifications: (1) shorter inner tube (2 cm long), (2) short flame-seal length (∼7–8 cm) and (3) keeping the inner tube with iron separate from the outer tube containing zinc and titanium hydride during cleaning.

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

Khosh, MS, Xu, X, Trumbore, SE. 2010. Small-mass graphite preparation by sealed-tube zinc reduction method for AMS 14C measurements. Nuclear Instruments & Methods in Physics Research Section B-Beam Interactions with Materials and Atoms 268:927930.Google Scholar
Macario, KD, Oliveira, FM, Moreira, VN, Alves, EQ, Carvalho, C, Jou, RM, Oliveira, MI, Pereira, BB, Hammerschlag, I, Netto, B, Seixas, AP, Malafaia, JVP, Moreira, L, Cunha, L, Assumpção, A, Mallet, P, Lima, L, Lopes, F, Diaz, M, Chanca, IS, Gomes, PRS. 2017. Optimization of the amount of zinc in the graphitization reaction for radiocarbon AMS measurements at LAC-UFF. Radiocarbon 59(3):885891.CrossRefGoogle Scholar
Rinyu, L, Molnar, M, Major, I, Nagy, T, Veres, M, Kimak, A, Wacker, L, Synal, HA. 2013. Optimization of sealed tube graphitization method for environmental 14C studies using MICADAS. Nuclear Instruments and Methods in Physics Research B 294:270275.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.CrossRefGoogle Scholar
Scott, EM. 2003a. The Fourth International Radiocarbon Intercomparison (FIRI). Radiocarbon 45(2):135291.CrossRefGoogle Scholar
Scott, EM. 2003b. Part 2: The Third International Radiocarbon Intercomparison (TIRI). Radiocarbon 45(2):293328.CrossRefGoogle Scholar
Slota, PJ, Jull, AJT, Linick, TW, Toolin, LJ. 1987. Preparation of small samples for 14C accelerator targets by catalytic reduction of CO. Radiocarbon 29(2):303306.CrossRefGoogle Scholar
Stuiver, M, Polach, HA. 1977. Discussion: reporting of 14C data. Radiocarbon 19 (3):355363.CrossRefGoogle Scholar
Vogel, JS. 1992. Rapid production of graphite without contamination for biomedical AMS. Radiocarbon 34(3):344350.CrossRefGoogle Scholar
Walker, BD, Xu, X. 2019. An improved method for the sealed-tube zinc graphitization of microgram carbon samples and 14C AMS measurement. Nuclear Instruments & Methods in Physics Research Section B-Beam Interactions with Materials and Atoms 438(1):5865.Google Scholar
Xu, X, Trumbore, SE, Zheng, SH, 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 & Methods in Physics Research Section B-Beam Interactions with Materials and Atoms 259:320329.Google Scholar
Xu, X, Gao, P, Salamanca, EG. 2013. Ultra small-mass graphitization by sealed tube zinc reduction method for AMS 14C measurements. Radiocarbon 55:608616.CrossRefGoogle Scholar
Supplementary material: PDF

Cisneros-Dozal et al. supplementary material

Cisneros-Dozal et al. supplementary material 1

Download Cisneros-Dozal et al. supplementary material(PDF)
PDF 87.7 KB
Supplementary material: PDF

Cisneros-Dozal et al. supplementary material

Cisneros-Dozal et al. supplementary material 2

Download Cisneros-Dozal et al. supplementary material(PDF)
PDF 69.7 KB
Supplementary material: File

Cisneros-Dozal et al. supplementary material

Cisneros-Dozal et al. supplementary material 3

Download Cisneros-Dozal et al. supplementary material(File)
File 12.8 KB