Laboratory Methods of Inorganic Chemistry, 2nd English Ed. 1928

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152 HETEROPOLYACIDS AND THEIR SALTS.


Copaux assumes that two atoms of hydrogen can also act as the central
atom. In this way the hypothetical acid H 2 « or H^H^Oe) is obtained,

from which metatungstic acid, Hio[H 2 (W207)6], is derived.



  1. Ammonium Phosphomolybdate, (NH 4 ) 3 PO4 • 13 MoO 3 • H 2 O.
    Treat a concentrated solution of 24 g. ammonium molybdate


with concentrated nitric acid until the precipitate of molybdic acid
first appearing has redissolved and the solution remains clear even


on boiling. On adding a solution of 3.6 g. of sodium phosphate the


well-known, yellow precipitate is produced. Wash this and dry


it in the steam closet. Yield, about 20 g.



  1. Silicotungstic Acid, H 8 [Si(W2O 7 ) 6 ] • 39 H 2 O.
    First prepare silicic acid hydrogel by dissolving 50 g. of com-


mercial, precipitated silicic acid in 12 g. of sodium hydroxide and


50 c.c. of water, diluting to 200 c.c, heating to about 100°, and
precipitating with hydrochloric acid. Dilute further with hot


water, drain the hydrogel on linen cloth in a large Biichner funnel


and wash with hot water. Stir up the hydrogel in a dish with


hot water and again drain it on the linen cloth.


Neutralize a solution of 50 g. pure, commercial sodium tungstate


in 200 c.c. of water with about 80 c.c. of 2-normal sulphuric acid,


using litmus paper as indicator. Have this solution boiling, add


the hydrogel above obtained, and boil the mixture until a filtered
sample no longer gives a yellow precipitate of tungstic acid when


acidified with hydrochloric acid. During the boiling add a little


2-normal sulphuric acid whenever the solution becomes alkaline


(in all about 20 c.c). This operation should take half to three-
quarters of an hour. Water should be added from time to time


to replace that lost by evaporation. Finally, filter the solution.


Cool the nitrate, which amounts to about 200 c.c. in volume, and


acidify it strongly by adding about 25 c.c. of concentrated sul-


phuric acid. Again cool and add ether, little by little with con-
stant shaking, until on settling in a separatory funnel three


layers are formed: on top an ethereal, in the middle an aqueous


solution, and underneath a thick, oily layer of a liquid compound


of silico-tungstic acid with ether. If this lowest layer does not
form, or forms but incompletely, more sulphuric acid must be


added. Allow the whole to stand over night, then draw off the

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