a little above 100 deg.C., which, unless the ore has undergone
chemical change because of the wetting, should be the same before and
after shipment.
PROCEDURE.--Spread 25 grams of the powdered sample on a weighed
watch-glass; weigh to the nearest 10 milligrams only and heat at
105 deg.C.; weigh at intervals of an hour, after cooling in a desiccator,
until the loss of weight after an hour's heating does not exceed
10 milligrams. It should be noted that a variation in weight of 10
milligrams in a total weight of 25 grams is no greater relatively than
a variation of 0.1 milligram when the sample taken weighs 0.25 gram
DETERMINATION OF THE INSOLUBLE MATTER AND SILICA
PROCEDURE.--Weigh out two portions of the original powdered sample
(not the dried sample), of about 5 grams each, into 250 cc.
casseroles, and cover each with a watch-glass (Note 1). Pour over the
powder 25 cc. of water, and then add 50 cc. of dilute hydrochloric
acid (sp. gr. 1.12) in small portions, warming gently, until nothing
further appears to dissolve (Note 2). Evaporate to dryness on the
water bath. Pour over the residue a mixture of 5 cc. of water and
5 cc. of concentrated hydrochloric acid (sp. gr. 1.2) and again
evaporate to dryness, and finally heat for at least an hour at
a temperature of 110 deg.C. Pour over this residue 50 cc. of dilute
hydrochloric acid (one volume acid (sp. gr. 1.12) to five volumes
water), and boil for about five minutes; then filter and wash twice
with the dilute hydrochloric acid, and then with hot water until
free from chlorides. Transfer the filter and contents to a porcelain
crucible, dry carefully over a low flame, and ignite to constant
weight. The residue represents the insoluble matter and the silica
from any soluble silicates (Note 3).
Calculate the combined percentage of these in the limestone.
[Note 1: The relatively large weight (5 grams) taken for analysis
insures greater accuracy in the determination of the ingredients which
are present in small proportions, and is also more likely to be a
representative sample of the material analyzed.]
[Note 2: It is plain that the amount of the insoluble residue and also
its character will often depend upon the strength of acid used for
solution of the limestone. It cannot, therefore, be regarded as
representing any well-defined constituent, and its determination is
essentially empirical.]
[Note 3: It is probable that some of the silicates present are wholly
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