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
Lead chromate precipitated in the cold is a lemon-yellow, light
precipitate, very difficult to filter: on heating to 40° C. the colour
becomes orange; at 60° C. it assumes a deeper hue, and becomes
flocculent; and at a boiling temperature it still further darkens and
settles readily. These changes in colour are not due to any chemical
change, as will be seen by testing the filtrate for chromium or lead:
this is an advantage to the assay, since it is only at the higher
temperature that the precipitate can be easily filtered. The lead is not
completely precipitated, but the amount remaining in solution is only 2
or 3 milligrams, which is just sufficient to give a dark coloration with
sulphuretted hydrogen.
_The standard chromate of potash solution_ is made by dissolving 7.13
grams of bichromate of potash and 2.0 grams of caustic soda in water,
and diluting to 1 litre; or 9.40 grams of the neutral chromate
(K_{2}CrO_{4}) may be dissolved and diluted to 1 litre: 100 c.c. will be
equivalent to 1.000 gram of lead.
_Standard Lead Solution._--16 grams of nitrate of lead (Pb(NO_{3})_{2})
are dissolved in water and diluted to 1 litre; 100 c.c. will contain
1.000 gram of lead.
_Acetate of Soda Solution._--250 grams of the crystallised salt
(NaAc.3H_{2}O) are dissolved, and diluted to 1 litre. Use 40 c.c. for
each assay.
In the titration the assay solution should measure 150 to 200 c.c., and
should be boiling or nearly so. It is best contained in a pint flask,
and the standard chromate solution used with an ordinary burette. Run in
the chromate solution in a steady stream until the whole of the lead has
been precipitated. The amount required for this may be calculated: for
example, 1 gram of an 80 per cent. ore would require 80 c.c. A little of
the assay may be filtered off, and if it does not show a yellow colour
in the filtrate run in 2 c.c. more of the standard solution and continue
this addition till a colour is shown. After this run in another c.c. to
ensure an excess, dilute to 250 c.c., and heat to boiling; allow to
settle for three or four minutes, filter off 50 c.c. into a Nessler
glass, and determine the excess of chromate colorimetrically. The excess
found in the 50 c.c. must, of course, be multiplied by five, and then be
deducted from the quantity of chromate originally run into the assay
solution. The quantity to be deducted should not exceed 3 c.c. Where a
number of determinations are made the colorimetric estimation is
facilitated by using a series of standard phials similar to those
described under the _Electrolytic Copper Assay_. The determination is
rendered sharper and less liable to error by the addition of a few drops
of acetic acid to convert the chromate into bichromate. The same
chromate solution must be used in this determination as was used in the
precipitation.
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