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
In standardising the chromate solution, the standard lead nitrate
solution is used. A quantity containing about as much lead as the assay
is supposed to contain is measured off, rendered alkaline with dilute
ammonia, and then neutralised with acetic acid, using a small piece of
litmus paper dropped into the solution as indicator. Then dilute, boil,
and titrate. When the lead in the assay has been separated as sulphate
and dissolved in sodic acetate, less chromate is apparently required,
and in this case it will be necessary to precipitate the lead in the
standard with an equivalent of sodic sulphate and redissolve in sodic
acetate just as in the assay. In these solutions (although there is
considerable chromate in excess) a further addition of 5 or 6 c.c. of
the chromate solution will cause a further precipitate. The following
experiments show the effect of variation in the conditions of the
assay:--
~Effect of Varying Temperature.~--Twenty c.c. of lead nitrate solution
and 10 grams of sodium acetate were used; diluted to 200 c.c., heated to
the desired temperature, and titrated. The results were:--
Temperature 15° 30° 50° 100°
"Chromate" required 19.8 c.c. 19.5 c.c. 19.3 c.c. 19.2 c.c.
The first two of these filtered badly, the precipitate coming through
the filter; the last was very satisfactory in the working.
~Effect of Varying Bulk.~--Using 20 c.c. of lead nitrate, and 10 grams
of sodium acetate as before, diluting to the required bulk, heating to
boiling, and titrating, the results were:--
Bulk 100.0 c.c. 200.0 c.c. 500.0 c.c. 1000.0 c.c.
"Chromate" required 19.6 " 19.3 " 19.4 " 19.4 "
~Effect of Varying Acetic Acid.~--Since the experiments are carried out
in the presence of sodic acetate, acetic acid is the only acid whose
effect need be considered. Working as before, but with 200 c.c. bulk and
varying amounts of the acid, the results were:--
Acid present -- 10.0 c.c. 20.0 c.c. 40.0 c.c.
"Chromate" required 19.7 c.c. 19.1 " 18.5 " 17.3 "
These experiments show that only slight quantities of acid are
admissible.
~Effect of Varying Sodium Acetate.~--With the same conditions as before,
but with varying weights of sodium acetate, the results were:--
Sodium acetate present -- 5 grams 10 grams 25 grams 50 grams
"Chromate" required 19.7 c.c. 19.6 c.c. 19.6 c.c. 18.8 c.c. 17.8 c.c.
These experiments show that excessive quantities of sodium acetate must
be avoided. Ammonium acetate interferes to a greater extent, and if
both acetic acid and this salt are present, each exerts its disturbing
influence. With 10 grams of ammonium acetate, 19.4 c.c. of the chromate
solution were required instead of 19.7 c.c. in the absence of this salt;
with 10 grams of the acetate and 10 c.c. of acetic acid, only 18.6 c.c.
were required.
Public-domain text, read in full here on John Shaqi.
Reviews
Reviews
No reviews yet
Be the first to share your thoughts on this work.
Elsewhere in the archive
Join the Discussion
Join the discussion
Sign in to leave a comment or review.
Sign InorCreate an account