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The Practical Analysis of High-Purity Chemicals. VI. Emission Spectrographic Analysis of High-Purity Acids

Volume 25, Number 5 (Oct. 1971) Page 542-549

Kershner, N.A.; Joy, E.F.; Barnard, A.J.

The spectrographic analysis of volatile acids in a high-purity form is reviewed and a procedure presented that involves evaporation of a 100-g sample under temperature controlled contamination-free conditions and emission spectrography using dc-arc excitation under controlled atmosphere. In the evaporation, graphite (10 mg) is added as a collector, sulfuric acid to convert to less volatile sulfates (with acetic, hydrochloric, and nitric acids), and also mannitol to retain boron (with hydrochloric and hydrofluoric acids). Indium is added as a internal standard. Spectra are examined for 33 elements against a multielement standard in graphite containing indium as an internal standard. For the concurrent analysis of three samples, the elapsed time is 4-10 h and the actual working time 3-5 h. Recovery studies are reported as well as the use of the procedure in the assessment of the leaching of borosilicate glass by concentrated mineral acids.