A Note on the Determination of Very Small Quantities of Hydroxylamine by Blom's Method

Abstract

In a study on the possible occurrence of hydroxylamine as an intermediate compound in the oxidation of ammonium salts to nitrites in sea water (see Cooper, 1937), the method of Blom was tried in order to estimate the hydroxylamine. The method consists in the oxidation of the hydroxylamine by a solution of iodine in acetic acid, removal of the excess of iodine with N/Io thiosulphate, and estimation of the nitrite so produced by the Griess method; the method has been used by several workers for the estimation of small amounts of hydroxylamine in biological material.The method had not been used for such small amounts of hydroxylamineas would be expected in sea water, and it was therefore tested at high dilutions. It was found that nitrite itself, however, could not be recovered after treatment with the above reagents, and it was noticed that in many cases a precipitate (probably sulphur) was produced, and a distinct smell of hydrogen sulphide was often apparent. It was thought probable therefore that the loss was due to the interaction of the nitrite or the red dye with the thiosulphate used for removing the excess of iodine. This view was confirmed by noting the removal of the red colour, the appearance of a precipitate, and the smell of hydrogen sulphide when a solution of thiosulphate was added to a solution of the dye.Experiments were therefore set up to determine the amount of thiosulphate that could be present in excess without interfering with the estimation.