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

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146 COMPLEX HALOGEN ACIDS AND SALTS.



  1. Heat a sample of the dry salt in a test-tube. In addition to
    a little water, mercuric iodide distils off and condenses in the yellow
    modification on the cooler part of the tube. After some time, or
    more quickly on touching it with a glass rod, the sublimate changes
    into the red form, and this can again be changed into the yellow
    condition by heating (cf. Prep. 17).

  2. Potassium Cobalticyanide, K.,[Co(CN) 6 ].
    Triturate 30 g. of cobalt carbonate with a little water until it is
    thoroughly wet; then suspend it in 100 c.c. of water and dissolve it
    by adding a solution of 110 g. potassium cyanide in 400 c.c. of
    water. Oxidize the potassium cobaltocyanide thus formed by
    drawing a vigorous current of air through the liquid for an hour.
    After filtering the dark-yellow solution, add to it 40 g. of glacial
    acetic acid and evaporate it to crystallization under a well-ven-


tilated hood outside of the general laboratory. Drain the crystals,
and wash them with alcohol of about 66% by volume. Work up


the mother-liquor repeatedly as long as a sample of the crystals


obtained gives a deep-blue solution when heated with concentrated


sulphuric acid. The easily soluble potassium acetate remains in
the residual liquor. Recrystallize the combined fractions from a


solution which is slightly acidified with acetic acid. Yield, about


60 g. The product may be used in No. 109.



  1. Hydroferrocyanlc Acid, H 4 [Fe(CN)e].
    Hydroferrocyanic acid can be obtained pure without difficulty, and dif-
    fers in this respect from most of the related acids which are only stable in
    the form of their salts. Hydroferrocyanic acid is easily soluble in water
    and alcohol; but it can be readily precipitated as an addition product with
    ether, and the ether can be removed from the compound by heating it in a
    current of hydrogen at 80° to 90°.


Treat a solution containing 42 g. of potassium ferrocyanide
(0.1 mol.) in 350 c.c. of water with 120 c.c. of concentrated hydro-
chloric acid; if any precipitate of potassium chloride separates,
redissolve it by adding a little more water. Cool and add about
50 c.c. of ether. After standing for several hours, colorless, glisten-
ing, microscopic crystals separate which should be drawn off and
washed with dilute hydrochloric acid containing a little ether. To
remove any admixed potassium chloride, dissolve the product in
50 c.c. of alcohol, filter, precipitate again with 50 c.c. of ether,
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