Summary
A method is described for determination of arsenic in organometallic compounds by oxygen-flask decomposition. Benzoyl peroxide is added to prevent the formation of platinum-arsenic alloys. The combustion products are absorbed in dilute iodine solution to ensure complete oxidation to As(V). The arsenic is determined spectrophotometrically as arsenomolybdenum blue produced by reduction with hydrazine sulphate. The method is simple and gives reliable and highly reproducible results both on the micro- and decimilligram scales.
Zusammenfassung
Eine Methode zur Arsenbestimmung in Organometallverbindungen nach Veraschung im Sauerstoffkolben wurde beschrieben. Um die Bildung von Platin-Arsen-Legierungen zu verhindern, setzt man Benzoylperoxid zu. Die Verbrennungsprodukte werden in verdünnter Jodlösung absorbiert, um die vollständige Oxydation zu As(V) zu gewährleisten. Das Arsen wird spektralphotometrisch als Arsen-Molybdänblau gemessen, das sich durch Reduktion mit Hydrazinsulfat bildet. Das einfache Verfahren gibt zuverlässige und sehr gut reproduzierbare Resultate im Mikro- und Dezimilligrammbereich.
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References
I. M. Kolthoff and P. J. Elving, “Treatise on Analytical Chemistry” Part II, Vol. 12, New York: Interscience. 1965. p. 330.
R. F. Milton and W. D. Duffield, Analyst67, 279 (1942).
T. T. Gorsuch, Analyst84, 135 (1959).
H. A. Williams, Analyst66, 228 (1941).
P. F. Wyatt, Analyst80, 368 (1955).
A. Sykes in C. L. Wilson and D. W. Wilson, eds. “Comprehensive Analytical Chemistry”, Vol. 1B, Amsterdam: Elsevier. 1960.
G. Ingram, “Methods of Organic Elemental Microanalysis”, London: Chapman & Hall. 1962. p. 297.
R. Belcher, A. M. G. MacDonald, and T. S. West, Talanta1, 408 (1958).
M. Corner, Analyst84, 41 (1959).
K. Eder, Mikrochim. Acta [Wien]1960, 471.
W. Merz, Mikrochim. Acta [Wien]1959, 640.
R. Püschel and Z. Stefanać, Mikrochim. Acta [Wien] 1962, 1108.
M. M. Tuckerman, J. H. Hodecker, B. C. Southworth, and K. D. Fleischer, Analyt. Chim. Acta21, 463 (1959).
R. Belcher and A. M. G. MacDonald, Talanta1, 185 (1958).
P. Fleury, J. pharm. chim.21, 385 (1920).
E. Schutzk and von Villecz, Z. analyt. Chem.76, 81 (1929).
R. Levy, Bull. soc. chim. France1956, 517.
P. S. Tutundžić and M. Mladenović, Analyt. Chim. Acta12, 390 (1955).
S. Meyer and O. G. Koch, Z. analyt. Chem.158, 434 (1957).
V. Vašák and V. Sedivec, Chem. Listy46, 341 (1952).
H. J. Morris and H. O. Calvery, Ind. Eng. Chem., Analyt. Ed.9, 447 (1937).
G. R. Kingsley and R. R. Schaffert, Analyt. Chemistry23, 914 (1951).
A. Crawford, J. G. Palmer, and J. H. Wood, Mikrochim. Acta [Wien]1958, 277.
E. B. Sandell, Colorimetric Determination of Traces of Metals, 2nd Ed., New York: Interscience. 1950. p. 178.
E. Celon and L. Sindellari, in the press.
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Celon, E., Degetto, S., Marangoni, G. et al. Determination of arsenic in organometallic compounds by the oxygen flask method on micro- and decimilligram-scale. Mikrochim Acta 65, 113–120 (1976). https://doi.org/10.1007/BF01218255
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DOI: https://doi.org/10.1007/BF01218255