Abstract
The application of H 2/Pd electrodes as generator and indicator electrodes is described for coulometric titrations of alkali metal halides and trivalent metal sulphates in acetic anhydride with potentiometric end-point detection. In acetic anhydride, sodium fluoride is a strong enough base to be titrated directly with H + ions obtained by anodic oxidation of hydrogen dissolved in palladium. Other halides (NaCl, KCl, LiCl, KBr and NaBr) can be determined, after reaction of halides with mercury (II) acetate, by coulometric titration of the liberated base. Potentiometric end-point detection with a H 2/Pd-mercury(I) acetate electrode pair is satisfactory. Sulphates of Fe(III), Cr(III) and Al(III) are determined by back-titrating the excess of barium acetate after precipitation of barium sulphate. The errors in these determinations are < 1% for concentrations ranging from 0.001 to 0.003 M.
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