A Manual of Clinical DiagnosisTodd, James Campbell
Science
A Manual of Clinical Diagnosis
Todd, James Campbell
Diagnosis, Laboratory
It is essential that all apparatus used be lead-free. Five hundred
cubic centimeters of the urine are acidified {97} with 70 c.c. pure
sulphuric acid, and heated in a beaker or porcelain dish. About 20 to
25 gm. of potassium persulphate are added a little at a time. This
should decolorize the urine, leaving it only slightly yellow. If it
darkens upon heating, a few more crystals of potassium persulphate are
added, the burner being first removed to prevent boiling over; if it
becomes cloudy, a small amount of sulphuric acid is added. It is then
boiled until it has evaporated to 250 c.c. or less. After cooling, an
equal volume of alcohol is added, and the mixture allowed to stand in
a cool place for four or five hours, during which time all the lead
will be precipitated as insoluble sulphate.
The mixture is then filtered through a small, close-grained
filter-paper (preferably an ashless, quantitative filter-paper), and
any sediment remaining in the beaker or dish is carefully washed out
with alcohol and filtered. A test-tube is placed underneath the
funnel; a hole is punched through the tip of the filter with a small
glass rod, and all the precipitate (which may be so slight as to be
scarcely visible) washed down into the test-tube with a jet of
distilled water from a wash-bottle, using as little water as possible.
Ten cubic centimeters will usually suffice. This fluid is then heated,
adding crystals of sodium acetate until it becomes perfectly clear. It
now contains all the lead of the 500 c.c. urine in the form of lead
acetate. It is allowed to cool, and hydrogen sulphid gas is passed
through it for about five minutes. The slightest yellowish-brown
discoloration indicates the presence of lead. A very slight
discoloration can be best seen when looked at from above. For
comparison, the gas may be passed through a test-tube containing an
equal amount of distilled water. The quantity of lead can be {98}
determined by comparing the discoloration with that produced by
passing the gas through lead acetate (sugar of lead) solutions of
known strength. One part of lead acetate crystals contains 0.54 part
of lead. Hydrogen sulphid is easily prepared in the simple apparatus
shown in Fig. 30. A small quantity of iron sulphid is placed in the
test-tube; a little dilute hydrochloric acid is added; the cork is
replaced; and the delivery tube is inserted to the bottom of fluid to
be tested.
[Illustration: FIG. 30.--A simple hydrogen sulphid generator.]
Mercury.--Traces can be detected in the urine for a considerable time
after the use of mercury compounds by ingestion or inunction.
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