414 Thornton, Jr. — Separation of Titanium from Iron, etc. 



acid in one operation — so that the time required for the 

 estimation of titanium in the presence of iron, aluminum, and 

 phosphoric acid is no greater than the time required for the 

 estimation of titanium when associated with iron only ; since 

 after filtering off the ferrous sulphide the technique is exactly 

 the same in either case. The precipitate comes down imme- 

 mediately and quantitatively in the cold in flocculent and 

 readily filterable condition, has little tendency to include 

 alkalies, and after drying can be easily converted to titanic 

 oxide of a high degree of purity. The entire procedure is so 

 simple that the attainment of good results by the analyst is 

 almost inevitable. 



In order that analytical chemists may have at hand directions 

 for the preparation of the ammonium salt of nitrosophenyl- 

 hydroxylamine* an abstract of Baudisch'sf instructions for its 

 synthesis is here appended.. 



Sixty grms. of nitrobenzene, 1000 om3 of water, and 30 grms. 

 of ammonium chloride are stirred rapidly to an emulsion. 

 Eighty grms. of zinc dust is added in small portions to the 

 stirred emulsion by means of a knife blade ; the temperature 

 being kept between 16° and 18° C. by the occasional addition 

 of a little shaved ice, until there is no longer an odor of nitro- 

 benzene and the precipitate is gray. The reduction is accom- 

 plished in about one-half hour. The solution is filtered from 

 the zinc hydroxide, which is washed a few times with iced 

 water. The filtrate, cooled to nearly 0° C, is saturated with 

 sodium chloride. Whereupon phenylhydroxylamine crystal- 

 lizes out in white needles. These are collected on a perforated 

 funnel and dried by being pressed between filter papers. The 

 yield is generally 70-85 per cent of the theoretical. This body 

 is a skin poison and if spattered on the hands or face should 

 be at once washed off with water and then with alcohol. The 

 crystals are dissolved in 300-500 cmi of commercial ether and 

 the solution filtered from any residual sodium chloride. The 

 ethereal solution, cooled to 0° C, is saturated with dry ammonia 

 gas. While still at 0° C, the calculated weight of fresh amyl 

 nitrite (one molecule to every molecule of nitrobenzene) is 

 added. The vessel is immediately filled with glistening white 

 crystals of the ammonium salt of nitrosophenylhydroxylamine4 

 After filtration and washing with ether, the crystals are dried 

 by filter paper, and kept in a closely stoppered bottle in which 

 is also placed a small lump of ammonium carbonate. 



February 18, 1914. 



* Kahrbaurn's salt can be purchased from Messrs. Eimer & Amend, New 

 York. 



•f Chem. Zeitung., xxxv, 223, 1911. 

 % C6H5NO.NONH4. 



