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Article contents

Factorial Design Techniques Applied to Optimization of AMS Graphite Target Preparation

Published online by Cambridge University Press:  18 July 2016

R. Michael Verkouteren
Affiliation:
Surface and Microanalysis Science Division, National Institute of Standards and Technology Gaithersburg, Maryland 20899 USA
George A. Klouda
Affiliation:
Surface and Microanalysis Science Division, National Institute of Standards and Technology Gaithersburg, Maryland 20899 USA
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Abstract

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Many factors influence the preparation and quality of graphite targets for 14C accelerator mass spectrometry (AMS). We identified four factors (sample size, H2 pressure, catalyst temperature and pretreatment time) as potentially critical, and investigated their effects on two particular characteristics: the integrated rates of CO2 reduction (to graphite) and methane production. We used a 2-level fractional factorial experimental design and determined chemical reduction yield rates through manometry and partial pressure monitoring of residual gases by mass spectrometry.

Chemical reduction yield rates ranged from 0.2% to 6.2% per hour. With respect to their influence on percent yield rate, the factors we studied were ordered as: sample size > level of hydrogen > pretreatment of the catalyst. The temperature of the catalyst, and the sample size × hydrogen (2-factor) interaction, were only marginally influential. Other interactions did not appear to be significantly important. We estimated uncertainty in the order of influence and magnitudes of the effects by the Monte Carlo method of error propagation.

We observed significant methane production in only one experiment, which suggests that methane originates from indigenous carbon in untreated iron catalyst only in the presence of hydrogen and only at thermodynamically favorable temperatures. This exploratory investigation indicates that factorial design techniques are a useful means to investigate multivariate effects on the preparation and quality of AMS graphite targets.

Type
I. Sample Preparation and Measurement Techniques
Copyright
Copyright © The American Journal of Science 

References

Adamson, A. W. 1973 A Textbook of Physical Chemistry. New York, Academic Press: 1079 p.Google Scholar
Box, G. E. P., Hunter, W. G. and Hunter, J. S. 1978 Statistics for Experimenters. New York, John Wiley & Sons: 653 p.Google Scholar
Carpenter, H. C. H. and Smith, C. C. 1918 Some experiments on the reaction between pure carbon monoxide and pure electrolytic iron below the A1 inversion. Journal of the Iron and Steel Institute, London 98: 139191.Google Scholar
Currie, L. A., Stafford, T. W., Sheffield, A. E., Klouda, G. A., Wise, S. A. and Fletcher, R. A. 1989 Micro-chemical and molecular dating. In Long, A. and Kra, R. S., eds., Proceedings of the 13th International 14C Conference. Radiocarbon 31(3): 448463.Google Scholar
Hammersley, J. M. and Handscomb, D. C. 1964 Monte Carlo Methods. New York, John Wiley & Sons: 178 p.CrossRefGoogle Scholar
Jull, A. J. T., Donahue, D. J., Hatheway, A. L., Linick, T. W. and Toolin, L. J. 1986 Production of graphite targets by deposition from CO/H2 for precision accelerator 14C measurements. In Stuiver, M. and Kra, R. S., eds., Proceedings of the 12th International 14C Conference. Radiocarbon 28(2A): 191197.CrossRefGoogle Scholar
Klouda, G. A., Currie, L. A., Verkouteren, R. M., Einfeld, W. and Zak, B. D. 1988 Advances in micro-radiocarbon dating and the direct tracing of environmental carbon. Journal of Radioanalytical and Nuclear Chemistry, Articles 123: 191197.CrossRefGoogle Scholar
Klouda, G. A., Barraclough, D., Currie, L. A., Zweidinger, R. B., Lewis, C. W. and Stevens, R. K. 1991 Source apportionment of wintertime organic aerosols in Boise, Idaho by chemical and isotopic (14C) methods. Proceedings of the 84th Annual Meeting, Air & Waste Management Association 15A: 131.2.Google Scholar
Manning, M. P. and Reid, R. C. 1977 C-H-O systems in the presence of an iron catalyst. Industrial and Engineering Chemistry, Process Design and Development 16: 358361.CrossRefGoogle Scholar
Matsumoto, H. and Bennett, C. O. 1978 The transient method applied to the methanation and Fischer-Tropsch reactions over a fused iron catalyst. Journal of Catalysis 53: 331344.CrossRefGoogle Scholar
McNichol, A. P., Gagnon, A. R., Jones, G. A. and Osborne, E. A. 1992 Illumination of a black box: Analysis of gas composition during graphite target preparation. Radiocarbon, this issue.Google Scholar
Olsson, R. G. and Turkdogan, E. T. 1974 Catalytic effect of iron on decomposition of carbon monoxide: II. Effect of additions of H2, H2O, CO2, SO2 and H2S. Metallurgical Transactions 5: 2126.Google Scholar
Polach, H. A. 1984 Radiocarbon targets for AMS: A review of perceptions, aims and achievements. In Wölfli, W., Polach, H. A. and Anderson, H. H., eds., Proceedings of the 3rd International Symposium on Accelerator Mass Spectrometry. Nuclear Instruments and Methods 233(B5): 259264.CrossRefGoogle Scholar
Sheffield, A. E., Currie, L. A., Klouda, G. A., Donahue, D. J., Linick, T. W. and Jull, A. J. T. 1990 Accelerator mass spectrometric determination of carbon-14 in the low-polarity fraction of atmospheric particles. Analytical Chemistry 62: 20982102.CrossRefGoogle Scholar
Slota, P. J. Jr., Jull, A. J. T., Linick, T. W. and Toolin, L. J. 1987 Preparation of small samples for 14C accelerator targets by catalytic reduction of CO. Radiocarbon 29(2): 303306.CrossRefGoogle Scholar
Thomsen, M. S. and Gulliksen, S. 1992 Reduction of CO2-to-graphite conversion time of organic materials for 14C AMS. Radiocarbon, this issue.Google Scholar
Turkdogan, E. T. and Vinters, J. V. 1974 Catalytic effect of iron on decomposition of carbon monoxide: I. Carbon deposition in H2-CO mixtures. Metallurgical Transactions 5: 1119.Google Scholar
Verkouteren, R. M., Klouda, G. A., Currie, L. A., Donahue, D. J., Jull, A. J. T. and Linick, T. W. 1987 Preparation of microgram samples on iron wool for radiocarbon analysis via accelerator mass spectrometry: a closed-system approach. In Gove, H. E., Litherland, A. E. and Elmore, D., eds., Proceedings of the 4th International Symposium on Accelerator Mass Spectrometry. Nuclear Instruments and Methods B29: 4144.CrossRefGoogle Scholar
Vogel, J. S. 1992 Rapid production of graphite without contamination for biomedical AMS. Radiocarbon, this issue.Google Scholar
Wagman, D. D., Evans, W. H., Parker, V. B., Schumm, R. H., Halow, I., Bailey, S. M., Churney, K. L. and Nuttall, R. L. 1982 The NBS tables of chemical thermodynamic properties. Journal of Physical and Chemical Reference Data 11(2): 392 p.Google Scholar
Walsh, P. J. 1962 Algorithm 127, ORTHO. Communications of the ACM (Association for Computing Machinery) 5: 511513.CrossRefGoogle Scholar
Wampler, R. H. 1969 An evaluation of linear least squares computer programs. Journal of Research of the National Bureau of Standards B 73: 5990.Google Scholar
Wilson, A. T. 1992 A simple technique for converting carbon dioxide to AMS target graphite. Radiocarbon, this issue.Google Scholar
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