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Spectrochemical Analysis by the Copper Spark Method

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Abstract

A system of spectrochemical analysis is described in which 0.1 ml of a hydrochloric acid solution of the sample is evaporated on the ends of a pair of flat-topped copper electrodes which are then excited in a spark. Absolute sensitivities for different elements ranging from 10−10 to 10−6 gram have been obtained. The lower limits measurable by visual comparison with standard plates are given for 64 elements. The visual method gives results accurate to a factor of two over a range from the lower limit up to about 10 micrograms. The accuracy can be increased, with some loss in sensitivity, by densitometry with an internal standard, an average deviation from the mean of 3 to 8 percent being obtained depending on whether a spectroscopic buffer is used. In addition to high sensitivity the method has the advantage that a great many elements can be determined in one exposure, so that almost any sample which can be obtained in hydrochloric acid can be analyzed for impurities without special calibration. The method was developed for the analysis of plutonium samples and is the result of considerable cooperative effort. The original stimulus was due to Professor G. K. Rollefson of the University of California at Berkeley, whose work was then considerably expanded at Chicago by the authors. Valuable contributions were also made by Dr. Raymond G. Russell, Dr. Wayne W. Marshall, Miss Irene Corvin, and the many analysts who used the method during its evolution. No special mention of the plutonium application is made in the present paper.

© 1947 Optical Society of America

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