Inorganic Syntheses: v. 1 by H S Booth

By H S Booth

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Sample text

The light-green trioxalatoferriate crystallizes in nearly quantitative yield. Any soluble ferric salt, in the presence of excess oxalate ion, yields the trioxalatoferriate. By using ferric sulfate and barium oxalate the elimination of foreign ions is rendered very easy. 2 g. 7 g. of potassium oxalate (K2CzO4-H20) in 500 cc. of hot water. 9 g. of lead dioxide (see synthesis 16) is added slowly, followed by 25 ml. of glacial acetic acid added a drop at a time. The stirring is continued for an hour, during which time the color changes from red t o deep green.

CHAPTER V 20. NITROSYL CHLORIDE SO, + HNO3 HOSOzONO + HOSO2ONO + HC1 + NOCl + H2S04 SUBMITTED BY GEORGEH. COLEMAN,* GERALDA. LILLIS,*A N D GILBERT E. GOHEEN* C E E C K E D BY C. v. H E R R M A N N t AND H. s. ~ The procedure described here is a modification of the last method. The reactants used can be prepared easily, and the principal impurity in the crude product is hydrogen chloride from which nitrosyl chloride can be separated readily. Procedure ' It is necessary to carry out the preparation under a hood.

The amount of boron trifluoride absorbed by the reacting organic compounds can be determined from time to time by turning the three-way stopcock S so as to by-pass the boron trifluoride through the shunt and closing the stopcocks S' to protect the contents of the flask R from the atmosphere. The part of the apparatus from G to G' can then be removed and weighed. Properties Boron trifluoride is a colorless gas which fumes in air and has a pungent suffocatingodor. I t melts at -127°C. and boils at - 101°C.

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