File:Image from page 368 of "Practical methods of organic chemistry" (1901) (14791526853).jpg

Identifier: practicalmethods00gatt Title: Practical methods of organic chemistry Year: 1901 (1900s) Authors: Gattemann, Ludwig. [from old catalog] Subjects: Publisher: [n.p.] Contributing Library: The Library of Congress Digitizing Sponsor: The Library of Congress

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Text Appearing Before Image: ith nitric acid,sp. gr. 1.3, and heated gently on a wire gauze with a free flame(under the hood). In order to condense the nitric acid carriedalong with the gases, an empty wash-bottle, cooled by cold water,is employed. (See Fig. 81.) 7. PHOSPHORUS TRICHLORIDE Under water, in a porcelain mortar, cut 40 grammes of yellowphosphorus, with a knife or chisel, into pieces which will con-veniently pass into the tubulure of a 300 c.c. retort. After the airin the retort has been displaced by dry carbon dioxide (Fig. 87),each single piece of phosphorus is taken from the water by pincers,and dried quickly by pressing it between several layers of filter-paper, and immediately placed in the retort, care being taken toprevent it from becoming ignited by friction in the opening ofthe tubulure. As soon as all the phosphorus has been transferred PHOSPHORUS TRICHLORIDE 349 to the retort, the tubultire is connected with a delivery tube whichmust move easily in the cork, and a moderately rapid current of

Text Appearing After Image: dry chlorine passed over the phosphorus; phosphorus chloride isthus formed with evolution of heat and light. If crystals of phos-phorus pentachloride should collect in the neck of the retort, the 35o SPECIAL PART delivery tube is pushed somewhat farther into the retort. If, onthe other hand, phosphorus distils to the upper part of the retort,the tube is somewhat raised. The phosphorus trichloride con-densing in the receiver is distilled from a dry fractionating flask.Boiling-point, 740. Yield, 125-140 grammes. 8. PHOSPHORUS OXYCHLORIDEi To 100 grammes of phosphorus trichloride, contained in a largetubulated retort connected with a condenser, add gradually, insmall portions of about 2-3 grammes,32 grammes of finely pulverised potas-sium chlorate. After each addition,wait until the liquid bubbles up, beforeadding a new quantity. - If, on theaddition of the first portion, no reac-tion takes place, it is started by a gentlewarming. During the addition, noliquid should distil into the rece

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