PEROXYLAMINESU LPHONATES AND HYDROXÏ LAMINETRISULPHONATBS, ;;7 



the acid was obtained in characteristic crystals (Joe. cit. , 229), which 

 were somel imes weighed. 



The quantitative examination of the solution is a troublesome 

 and less satisfactory operation. The peroxylatninesulphonate can 

 hardly be obtained, for weighing in the dry and pure; state, because 

 of its instability. Therefore', after its composition had been found, from 

 concordant analyses of four different preparations, to be that ascertain- 

 ed by previous workers, the preparation of the solution and its 

 analysis after the salt had all decomposed wen; carried out in the 

 following way. The peroxylaminesulphonate, recry stall ised two or 

 three times from hot water made alkaline with potassium hydroxide, 

 was drained a short time on a tile from ils mother liquor, and at once 

 dissolved in suitable quantity in water to which had been added a 

 measured quantity of potassium hydroxide. The solution was 

 maintained at the boiling temperature until colourless through the 

 complete decomposition of the salt. The cold solution was weighed 

 off into four portions ; one of 5 per cent, of the whole, for estimating 

 the amount of peroxylaminesulphonate that had been dissolved ; 

 another of 15 per cent., for estimating the quantity of hydroxy lamine- 

 trisulphonate produced; a third and a fourth portion, each of 40 

 per cent., for estimating in one the quantity of sulphate and in the 

 other that of nitrite produced. The quantity of peroxylaminesulphon- 

 ate taken was determined by weighing as barium sulphate the total 

 sulphur in the solution. To ensure flic; hydrolysis of all the sulphouate, 

 the solution was heated with the hydrochloric aeid in sealed tubes for 

 •1-.") hours at 180°-200°. 



To determine tin; quantity of sulphate which had been produced, 

 very dilute hydrochloric acid was added with constant stirring 

 until the solution was left only barely alkaline to Phenolphthalein, 

 then much ammonium chloride was added before precipitating with 



