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
The following experiments show the effect of variations in the
conditions of the assay. A solution of stannous chloride equivalent in
strength to the "permanganate" was made by dissolving 19.06 grams of the
crystallised salt (SnCl_{2}.2H_{2}O.) in 50 c.c. of water and 10 c.c. of
hydrochloric acid and diluting to 1 litre with water freed from
dissolved oxygen. 100 c.c. contain 1 gram of tin. In the first
experiments tap water was used and no precautions were taken for
excluding air. Except when otherwise stated, 20 c.c. of the stannous
chloride were used in each experiment with 10 c.c. of hydrochloric acid,
and were diluted to 100 c.c. with water before titration.
~Effect of Varying Hydrochloric Acid.~
Acid added 1.0 c.c. 10.0 c.c. 20.0 c.c. 50.0 c.c.
"Permanganate" required 18.8 " 18.9 " 18.8 " 18.8 "
The only effect of the increase in quantity of acid was to give the
brown of perchloride of manganese instead of the pink of permanganic
acid to mark the finishing point.
~Effect of Varying Temperature.~
Temperature 15° C. 50° C. 70° C. 100° C.
"Permanganate" required 18.8 c.c. 18.7 c.c. 18.6 c.c. 18.4 c.c.
~Rate of Atmospheric Oxidation.~--Solutions ready for titration were
exposed to air at the ordinary temperature for varying lengths of time
and then titrated.
Time exposed 0 min. 5 min. 10 min. 20 min. 60 min.
"Permanganate"
required 18.8 c.c. 18.8 c.c. 18.8 c.c. 18.8 c.c. 18.6 c.c.
It is best to titrate at once, although the loss by oxidation is only
small after one hour's exposure.
~Effect of Varying Tin.~
Stannous chloride
added 1.0 c.c. 10.0 c.c. 20.0 c.c. 50.0 c.c. 100.0 c.c.
"Permanganate"
required 0.7 " 8.8 " 18.0 " 47.4 " 95.4 "
~Effect of Varying Bulk.~
Bulk 50.0 c.c. 100.0 c.c. 200.0 c.c. 500.0 c.c.
"Permanganate" required. 9.0 " 18.3 " 17.4 " 15.1 "
The two last series show an interference, which is due to the oxygen
dissolved in the water, as may be seen from the following similar
experiments, which were, however, performed with water freed from oxygen
and in which the titrations were effected in an atmosphere of carbonic
acid.
~Effect of Varying Tin.~--A new solution of stannous chloride was used.
Stannous chloride
added 1.0 c.c. 10.0 c.c. 20.0 c.c. 50.0 c.c. 100.0 c.c.
"Permanganate"
required 1.0 " 10.0 " 19.8 " 49.6 " 99.3 "
~Effect of Varying Bulk.~
Bulk 30.0 c.c. 50.0 c.c. 100.0 c.c. 200.0 c.c. 500.0 c.c.
"Permanganate"
required 19.8 " 19.8 " 19.8 " 19.8 " 19.8 "
It will be seen that in working under these conditions the results are
proportional and the method satisfactory.
Public-domain text, read in full here on John Shaqi.
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