The phosphoric acid is determined in one-half of the filtrate and in
the remaining half the iron is reduced with zinc and determined with
potassium permanganate in the usual way. The phosphoric acid and iron
having been thus determined the alumina is estimated by difference. The
chief objection to this process is in the excessive quantity of acetic
acid used and the danger of solution of the precipitated phosphates
caused thereby.
=43. Estimation of the Lime and Magnesia.=—The filtrate and washings
from the first precipitation, (paragraph =41=,) of iron and alumina
in the method of Krug and McElroy, above described, are collected and
sufficient ammonium oxalate is added to precipitate the calcium. The
precipitated calcium is very fine and should be collected on a gooch,
under pressure. The filtrate and washings from the calcium precipitate
are again collected, and a solution of sodium phosphate added to
precipitate the magnesia. The solution must be kept cool and slightly
alkaline with ammonia during the above operations in order to prevent
the separation of molybdic anhydrid.
=44. Estimation of Sulfuric Acid.=—As a rule, sulfates are not abundant
in mineral phosphates. In case the samples are pyritiferous, however,
considerable quantities of sulfuric acid may be found after treatment
with aqua regia.
The acid is precipitated with barium chlorid, in the usual way, in an
aliquot portion of the filtrate first obtained. The precipitate of
barium sulfate is washed with hot water until clean, dried, ignited,
and weighed. If the portion of the filtrate taken represent half a gram
of the original material then the weight of barium sulfate obtained
multiplied by 0.6858 will give the quantity of sulfur trioxid in one
gram.
=45. Estimation of Fluorin by the Method of Berzelius as Modified by
Chatard.=—The method of estimating fluorin as proposed by Berzelius,
has been found quite satisfactory in the laboratory of the Geological
Survey, with the modifications given below.[34]
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