Improved Quantitative Analysis of Metals by Spark Source Mass Spectrography

FUMIYA KONISHI

doi:10.5702/massspec1953.19.284

FUMIYA KONISHI

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1971 Volume 19 Issue 4 Pages 284-293

DOI https://doi.org/10.5702/massspec1953.19.284

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Published: December 29, 1971 Received: September 06, 1971 Available on J-STAGE: June 28, 2010 Accepted: - Advance online publication: - Revised: -
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Date of correction: June 28, 2010 Reason for correction: - Correction: DTRECEIVED Details: Right : 19710906

Date of correction: June 28, 2010 Reason for correction: - Correction: ABSTRACT Details: Right : Attempts have been made to improve the precision and accuracy of the analysis of metals performed with spark source mass spectrograph by using some standard samples(aluminum, steel, copper and lead matrix)that contained impurities in concentrations ranging from a few thousan down to ten ppm. Reproducibility expressed in terms of coefficient of variation of the analytical results obtained on repeated exposures can attain 5 to 15 per cent(Tables 1 through 4)provided that all source oonditions are maintained constant, especially the spark gap at a rather large value of ca. 50μ and all plots for calculation curves are corrected for line width variation. From the analytical results thus obtained and further subjected to correction for mass dependence of emulsion sensitivity, the relative sensitivity factors of impurity elements have been. determined at the values ranging from 0.48 to 3.6(Fe=1)(Table6. cf. Table5). The experimental relative sensitivity factors agree within ± 30% with the values calulated by the relation proposed by Kai et al. in which the sensitivity factor of an element is inversely proportional to the product of its ionization potential and sublimation energy(Fig.4).

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Right : J. S. Halliday, P. S. Swift and W. A. Wolstenholme, “ Advances in Mass Spectrometry ”, p. 143, Institute of Petroleum, London, 1966.
J. Franzen and K. D. Schuy, “ Advances in Mass Spectrometry ”, p. 449, The Institute of Petroleum, London, 1968.
W. H. Wadlin and W. W. Harrison, Anal. Chem., 42, 1399(1970).
H. J. Svec, R. J. Conzemius and G. D. Flesh, 15th Annual Conference on Mass Spectrometry, Paper45, p. 138, Denver, 1967.
J. Kai and M. Miki, Mitsubishi Denki Lab. Rept., 5, 175(1964).
M. Desjardins, R. Stefani, R. Bourguillot and A. Cornu, “ Advances in Mass Spectrometry ”, p. 131, The Institute of Petroleum, London, 1966.
J. Franzen and K. D. Schuy, Z. Anal. Chemie, 225, 295(1967).
P. F. S. Jackson and J. Whitehead, Anal. Chem., 39, 1737(1967).
R. Brown, P. G. T. Vossen, P. F. S. Jackson and J. Whitehead, “ Advances in Mass Spectrometry ”, p. 431, The Institute of Petroleum, London, 1968.
C. A. Evans and G. H. Morrison, Anal. Chem., 40, 2106(1968).
E. B. Owens and N. A. Giardino, Anal. Chem., 35, 1173(1963).
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R. D. Craig, G. A. Errock and J. D. Waldron, “ Advances in Mass Spectrometry ”, p. 136, Pergamon Press, London, 1959.
“ Questionnaire on Relative Sensitivity Factors ”, ASTM Committee E-14 on Mass Spectrometry.
R. M. Elliott, R. D. Craig and G. A. Errock, “ Instruments and Measurements ”, Vol. 1, ed. by H. Koch and G. Ljungberg, p. 271, Academic Press, New York, 1961.
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Abstract

Attempts have been made to improve the precision and accuracy of the analysis of metals performed with spark source mass spectrograph by using some standard samples(aluminum, steel, copper and lead matrix)that contained impurities in concentrations ranging from a few thousan down to ten ppm. Reproducibility expressed in terms of coefficient of variation of the analytical results obtained on repeated exposures can attain 5 to 15 per cent(Tables 1 through 4)provided that all source oonditions are maintained constant, especially the spark gap at a rather large value of ca. 50μ and all plots for calculation curves are corrected for line width variation. From the analytical results thus obtained and further subjected to correction for mass dependence of emulsion sensitivity, the relative sensitivity factors of impurity elements have been. determined at the values ranging from 0.48 to 3.6(Fe=1)(Table6. cf. Table5). The experimental relative sensitivity factors agree within ± 30% with the values calulated by the relation proposed by Kai et al. in which the sensitivity factor of an element is inversely proportional to the product of its ionization potential and sublimation energy(Fig.4).

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