A direct method for determining Pb in free-cutting steel without preliminary separation of the Pb from the large amounts of Fe has been studied. Interference of Fe (III) is avoided by reduction with N
2H
4·2HCl and H·COONa, the latter also acting as the supporting electrolyte. Factors affecting the wave-height were investigated-that is, the amount of reagent, acidity, time of heating, interference of other metals, etc. -and as a result, the following procedure was established: a sample (2.5g) is dissolved in HCl (1+1, 30cc) and H
2O
2 (10%, 5cc) with gentle warming, heated to decompose the excess of H
2O
2, and diluted to 50cc. Ten cc is aliquoted into the measuringflask (50cc), then neutralized by dropping NH
4OH (1+2) to a slight permanent precipitation, and clarified with HCl (1+1, 3cc). Then N
2H
4·2HCI (20%, 10cc), H·COONa (50%, 10cc), and starch (2%, 3cc)are added, in that order, and the mixture is heated over a boiling water bath for 5 minutes. After cooling and diluting to the mark, Pb is then polarographically determined in the usual way. Cu(0.4%), As(0. 1%), Sn(0.05%), Cr(2%), Mo(0.1%), and the other elements encountered in the analysis of ordinary free-cutting steel do not interfere.
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