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A volumetric method first described by SCHROEDER2» 2 5 6 utilizes an internal indicator (tetrahydroxyquinone) to detect the endpoint in the reaction between sulphate and barium chloride; the first slight excess of barium chloride causes a colour change from yellow to red but although the method is rapid the end-point is not particularly good. A popular volumetric method for the estimation of sulphate is based upon the precipitation of sparingly soluble benzidine sulphate* followed by the titration of the washed precipitate with standard sodium hydroxide using phenolphthalein as indi cator13» 16»134A» 257 .
An excellent discussion of the interferences and factors affecting the Nessler method is given in the book edited by BOLTZ 1 3 4 . In gasworks practice, a distinction is made between the 'free' ammonia and the 'fixed' ammonia content of an effluent. The free ammonia is estimated by a straightforward distillation without addition of an alkaline reagent, and the residual liquor is then 36 CHEMICAL 221 37 ANALYSIS 221 treated with sodium carbonate , magnesium oxide or caustic soda 20 and distilled to get the fixed ammonia.
This reading can then be deducted from that given by the direct o-tolidine test. Neither the potassium iodide test nor the o-tolidine test is specific for free chlorine.