Abstract
The steel is dissolved in “Spekker Acid.” Manganese, chromium, and vanadium are oxidized to Mn7+, Cr6+, and V5+, respectively, by ammonium persulphate in the presence of silver nitrate. Manganese is titrated with sodium nitrite, the equivalence point being indicated at 890 mv. Chromium and vanadium are then titrated together with ferrous ammonium sulphate, the end point occurring at 500 mv. Vanadium is selectively re-oxidized at room temperature by potassium permanganate, and the excess is destroyed with sodium nitrite. The vanadium is then titrated with ferrous ammonium sulfate to the end point at 500 mv, as before.
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