鉄鋼分析を主とするカソーディックストリッピングボルタンメトリーの研究

概要

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Cathodic stripping voltammetry(CSV), based on electrodeposition from a sample solution was performed. Subsequently, cathodic dissolution was applied to the determination of trace manganese, selenium and sulfur in steel and lead in copper. By considering the operational simplicity and prevention of losses and contamination, a sample solution without separating the matrix was directly employed as an electrolyte, except for the sulfur determination. The CSV of sulfide was preceded by the conversion of sulfur into hydrogen sulfide, followed by its absorption in a sodium hydroxide solution. Manganese and lead were deposited on a platinum anode as manganese(IV) and lead(IV) oxides, respectively. In the case of the CSV of selenium and sulfide with a rotating silver disk electrode, the medium-exchange technique was adopted. Calibration graphs were linear down to ng ml^<-1> level, and the determination of manganese, selenium, sulfur and lead at the μg^<-1> level in samples with an RSD of 3 to 6% was achieved. The time required for each determination was less than 2.5h. For the analysis of steel and copper, the proposed methods are superior to commonly used JIS methods in terms of simplicity, rapidity, less experimental skill, without using harmful reagents, high sensitivity and excellent precision.
1997-10-05