A critical examination of commonly used semiquantitative techniques has been completed. Improved precision and accuracy have allowed analysis on sample sizes of 10 mg with no prior knowledge of chemical composition. A comparison of various matrices such as graphite, lithium carbonate, and lithium fluoride is included. Data on the precision and accuracy of each matrix in air and argon–oxygen atmospheres are also presented. A lithium fluoride–graphite matrix showed the best over-all results. The deviation from established values was approximately 15% and the coefficient of variation was also 15%. This study was completed under rigorous conditions with single determinations. Results were taken over a two year period and nearly 500 single determinations were used to complete the data.

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