. Hydroxylamine : its quantitative determination and some double salts . e solution. +Ebler and Schott usey chis method and claimto get good results . About one-tenth of a gram of the hydroxylaminesalt is dissolved in a little water and a known weight of ferric sul-phate and a few of sulphuric acid are added. The solution isheated to 90° and kept at that temperature for five minutes. The hy-droxylamine in hot acid solution is oxidized by means of ferric salts ;to nitrous oxide and + Og =N20+3H20 and an equivalent amount of ferrous salts are +2Fe2(S04)3=4FeS04 +2H
. Hydroxylamine : its quantitative determination and some double salts . e solution. +Ebler and Schott usey chis method and claimto get good results . About one-tenth of a gram of the hydroxylaminesalt is dissolved in a little water and a known weight of ferric sul-phate and a few of sulphuric acid are added. The solution isheated to 90° and kept at that temperature for five minutes. The hy-droxylamine in hot acid solution is oxidized by means of ferric salts ;to nitrous oxide and + Og =N20+3H20 and an equivalent amount of ferrous salts are +2Fe2(S04)3=4FeS04 +2H2SO4+H2O ^NgO The amount of ferrous salts being determined by titration with perman-ganate. If only slightly more than theoretical amount of ferric saltis added, the oxidation of hydroxylamine takes placethus-2NH2OH +30=3H20 +2N0 So it is impossible to obtain accurate results. The potassium permanganate used contained .00489 g. avail-able 0 per , being standardized with ferrous ammonium sulphateand ammoriiJim oxalate. +Ber. 10, 1940-48 + J. prakt chem. 78, 289-342. -8- No. of Wt. of KllnO usedExpt. taken found . 1 .1931 g .1665 2 .1121 g .0971 3 .0737 g .0559 4 .1207 g .0924 5 .0935 g .0874 :02 =Xi (No c .0 KIviri04 used X factor) X = W$. of The most accurate quantitative method found and the oneused for all the later quantitative estimations of hydroxylaraine, wasthe one of Ststhler* where-by the hydroxylamine is reduced by meansof titantffius sulphate or oxide. Ti^Or^ + NHoOH = 2Ti0„ + NH, An excess of the titanium solu- tion is used and the excess titrated with standard permanganate. Theprocess is asfollowsi- To a small weighAd portion of hydroxylaminesalt, add about 50 c c. water and allow carbon dioxide to pass intoit for several minutes before adding the titanium solution. Letstand for some time to allow it to act, otherwise the action will bebetween the hydroxylamine and the permanganate, then tit
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