Spectrophotometric method using methylene blue was studied for determination of trace sulfate in salt.
The analysis procedure was as follows. Sulfate ion was reduced to hydrogen sulfide by a mixture of red-phosphorus, formic acid, and hydroiodic acid. Hydrogen sulfide was absorbed in solution of zinc acetate. Methylene blue was produced by addition of
N, N-dimethyl-
p-phenylenediamime solution and iron (III) chloride solution. The concentration of methylene blue was determined by spectrophotometry.
The effect of operating condition and precision in this method were studied and the following results were obtained:
1) The determination value was not influenced by flow rate of carrier gas in the range of 50 to 200 ml/min, a diameter of capillary in the range of 0.1 to 1.1 mm, pH of absorbing solution in the range of 5.1 to 5.8, light and heating time in the range of 30 to 120 min. The absorbance of methylene blue was constant within 6 h.
2) The determination value was influenced by temperature of absorbing solution. The value was stable at 20 to 30°C, was decreased at higher temperature, and was increased at lower temperature.
3) The volume ratio of reducing reagent to sample solution was adoptable at 2 to 1.
4) The linear relationship was obtained in the range from 2 to 200 micrograms of sulfate ion, and the coefficient of variation was 2.5%.
5) The accuracy and sensitivity of the methylene blue method were six times higher than barium chromate method.
Thus, determination of trace sulfate in high-grade salt was possible.
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