(3) _Potassium Sulfate, Kainit, Etc._—In the analysis of kainit,
dissolve ten grams of the pulverized salt in 300 cubic centimeters of
boiling water, add ammonia to slight excess, then a sufficient quantity
of ammonium oxalate to throw down all lime present; cool and make up
to half a liter, mix thoroughly, and filter on a dry filter; from
twenty-five cubic centimeters, corresponding to a half gram, proceed
to remove the ammonia, as in the analysis of superphosphates; dissolve
the residue in hot water, plus a few drops of hydrochloric acid, and
add fifteen cubic centimeters of platinum solution. In the analysis
of high-grade sulfate and of double-manure salt (potassium sulfate,
magnesium sulfate, containing about twenty-seven per cent of potassium
oxid), make up the solution as above, but omit the precipitation,
evaporation, etc.; to an aliquot part equal to a half gram add fifteen
cubic centimeters of platinum solution. In all cases special care
must be taken in the washing with alcohol to remove all the double
platinum sodium chlorid which may be present. The washing should be
continued some time after the filtrate is colorless. Twenty-five cubic
centimeters of the ammonium chlorid solution are employed instead of
ten cubic centimeters, and the twenty-five cubic centimeters poured
through at least six times to remove all sulfates and chlorids. Wash
finally with alcohol; dry and weigh as usual.
=252. Alternate Method for Potash.=—Boil ten grams of the prepared
sample for thirty minutes with 300 cubic centimeters of water, and,
after cooling and without filtering, make up to one liter and filter
through a dry filter. If the sample have ten per cent of potassium
oxid, use fifty cubic centimeters of the filtrate; if less than ten per
cent of potassium oxid (ordinary potash fertilizers), use 100 cubic
centimeters of the filtrate. In each case make the volume up to 150
cubic centimeters, heat to 100°, and add, drop by drop with constant
stirring, a slight excess of barium chlorid, and, without filtering,
in the same manner add barium hydrate in slight excess. Filter while
hot and wash until the precipitate is free of chlorids. Add to the
filtrate one cubic centimeter of strong ammonium hydrate, and then a
saturated solution of ammonium carbonate, until the excess of barium is
precipitated. Heat and add, in fine powder, a half gram of pure oxalic
acid or 0.75 gram of ammonium oxalate. Filter, wash free of chlorids,
evaporate the filtrate to dryness in a platinum dish, and ignite
carefully over the free flame, below red heat, until all volatile
matter is driven off.
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