A text-book of assaying : $b for the use of those connected with mines.Beringer, C. (Cornelius)
Science
A text-book of assaying : $b for the use of those connected with mines.
Beringer, C. (Cornelius)
Assaying
~Effect of Foreign Salts.~--As already stated, sulphates interfere.
Twenty c.c. of the lead nitrate solution were taken, precipitated with
sulphate of soda, and the precipitate dissolved in 10 grams of sodium
acetate and titrated as before. Duplicate experiments required 18.6 c.c.
and 18.7 c.c. of the chromate solution. A similar experiment with 40
c.c. of lead nitrate required 37.4 c.c. of chromate. If the sulphate had
not been present, the results would have been 19.7 c.c. and 39.4 c.c.
respectively.
~Effect of Varying Lead.~--In these experiments the conditions were as
before, but with varying amounts of lead.
Lead nitrate solution present 10.0 c.c. 20.0 c.c. 50.0 c.c. 100.0 c.c.
Chromate solution required. 9.4 " 19.7 " 48.8 " 98.2 "
~Determination of Lead in Galena.~--Weigh up 1 gram of the powdered and
dried ore, and boil in an evaporating dish with 10 c.c. of dilute
hydrochloric acid. When the action becomes sluggish, dilute with an
equal bulk of water, and add a weighed piece of zinc rod about 1 inch
long and quarter-inch across. Keep up a moderate action by warming till
the ore is seen to be completely attacked and the lead precipitated.
Decant off the solution, wash once, strip off the lead, wash and weigh
the remaining zinc. Dissolve the lead in 5 c.c. of dilute nitric acid,
and 5 c.c. of water with the aid of heat. Dilute and transfer to a pint
flask; add a slight excess of dilute ammonia, and render faintly acid
with acetic acid. Dilute to 150 c.c., heat to boiling, and run in the
standard chromate in slight excess, noting the amount required, and make
up to 250 c.c. with water. Boil the solution, allow to settle for a
minute or so, filter off 50 c.c., and determine the excess of chromate
colorimetrically. As an example, 1 gram of an impure galena was
precipitated with 75 c.c. of standard chromate (100 c.c. = 1.020 gram
lead). The excess found in 50 c.c. was 0.3 c.c., which, multiplied by 5,
gives 1.5 c.c. as the excess in the whole solution. The remaining 73.5
c.c. of "chromate" required by the assay, are equivalent to 0.7497 gram
of lead. The zinc used up weighed 1.5 grams, and contained 0.0165 gram
of lead. Thus we get--
Lead in the assay 0.7497 gram
Lead from the zinc 0.0165 "
------
.'. Lead in the galena 0.7332 "
Equivalent to 73.3 per cent.
Another sample, in which the galena was accompanied with a large
quantity of pyrites, gave the following results:--Three grams were
treated with 30 c.c. of dilute hydrochloric acid and a rod of zinc. The
zinc and lead were carefully transferred to another vessel, the zinc
cleaned, and the lead (dissolved in 5 c.c. of dilute nitric acid and 20
c.c. of water) treated as before.
14.5 c.c. of the chromate were required = 0.1479 gram lead
Lead in 2 grams of zinc = 0.0220 "
------
.'. Lead in 3 grams of the ore = 0.1259 "
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