CHLORIDES OF ANTIMONY. 77Honly necessary to remove the stopper a moment and push the
obstruction out of the way with a stirring rod.
Conduct chlorine into the flask, and at the same time intro-
duce phosphorus trichloride through the dropping funnel; the
two substances immediately combine. Care should be taken to
keep chlorine present in excess. At the end loosen the phos-
phorus pentachloride formed by means of a spatula, and allow
the flask, which is still filled with chlorine, to stand for some time
before removing the product. The yield is almost quantitative.
Dependent preparation: Thionyl Chloride, No. 151.
Phosphorus Oxychloride. Connect a 150 to 200 c.c. distilling
flask, containing 21 g. (one-sixth mol.) of finely powdered potas-
sium chlorate, with a condenser and receiver. Then allow 69 g.
of phosphorus trichloride (one-half mol.) to flow into the flask a
little at a time. After each addition of the chloride, wait until
the reaction, which is made evident by a gentle ebullition, has
ceased before adding more; at the start it is permissible to
warm slightly if necessary. Should a little liquid distil over into
the receiver during this operation, return it to the distilling. flask.
When the reaction is complete, distil the phosphorus oxychlo-
ride by heating with a large flame, holding the burner in the hand
and playing the flame around the bulb of the flask. A ther-
mometer is not necessary for this distillation. Clean and dry
the apparatus, and redistil the product, this time using a ther-
mometer. Collect the first few drops which come over separately.
Boiling-point, 110°. Dependent preparation: Triethyl Phos-
phate, No. 157.- Chlorides of Antimony.
Antimony Trichloride. Treat 100 g. of finely powdered stibnite,
in a 750 c.c. flask, with 400 g. of concentrated, commercial hydro-
chloric acid, shaking frequently and heating upon the water bath
until as much as possible of the material is dissolved. Boil the
solution five minutes in order to remove the greater part of the
dissolved hydrogen sulphide. Add five cubic centimeters more of
concentrated hydrochloric acid, and filter the solution through a
Biichner funnel containing a layer of asbestos-felt which has been
previously moistened with the concentrated acid.