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AMOUNTS OF POTASSIUM*
Equilibrium Studies
E$ect of Silver Concentration-In this series of experiments we
studied the effect of the amount of the silver that participates
in the reaction upon the composition of the reaction product.
The pure potassium sulfa.te employed was put up in 0.22276 per
cent, st’ock solution, containing 1 mg. of potassium per cc. ; dilu-
tions were made as needed in these and subsequent experiments.
The following reagents2 were rcquircd.
1. Sodium cobaltinitritc, prepared as follows: 150 grn. of
sodium nitrite arc dissolved in 150 cc. of hot water; after the solu-
tion is cooled to about 40”, 50 gm. of cobalt nitrate crystals arc
1 Our equilibrium studies (see Fig. 1) show that this equation does not
represent the true course of the reaction. Regardless of this fact, how-
ever, our experiments bear out the assumption t,hat the concentration of
silver seriously affects the course of the reaction.
2 We used hlallincltrodt A. R. grade reagents, which were consistently
satisfactory.
Weichselbaum, Somogyi, a’nd Rusk
3 The 15 cc. Pyrex centrifuge tubes must be prepared for use by treat-
ment with hot chromic-sulfuric acid solution and thorough rinsing with
tap water and then with ammonia-free distilled water. The tubes arc
inverted to drain on a clean sheet of filter paper; they must drain without
the breaking of the film of water or else the acid treatment is to be repeated.
No ammonia must be used in proximity to the work bench.
346 Potassium Determination
had assumed the temperature of the bath, there was added,
dropwise with stirring, 0.5 cc. of a freshly prepared 12.5 per cent
solution of sodium cobaltinitrite (temperature IS-20’). The
tubes were allowed to stand in the water bath for from 10 to 20
minutes and then centrifuged for 10 minutes at 3000 R.P.M.~
The supernatant fluid was removed by suction, a finely drawn
glass tube with the end curved upward being used. At all times
when the tubes were not in the centrifuge or in manipulation, they
were kept in the water bath. Three washings with 5 cc. portions
the fluid in the cup was just above the capillary. The cup was
then washed with 0.5 cc. of 10 per cent urea solution, which was
also lowered into the extraction chamber. From this point on,
the only deviation in our procedure from that of Kramer and
Gittleman was that we deaerated the solution in the extraction
chamber before adding the 1 cc. of 8 N sulfuric acid. We have
found that this deaeration makes a difference of from 2 to 3 mm.
of pressure in our final reading. A blank analysis was per-
formed on each batch of the reagents used in the potassium de-
2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19
MG. SILVER ADDED
4.25-
3.85-
3.65-
G
+ 3.45-
c
h 3.25-
9a 3.05-
&OS-
a
fJ& 2.6 5-
5&
yF- 2.65-
z
zZ p 2.45-
;$ 2.25-
2 y 2.05-
F”o 1.05-
uurn + 1.65-
z
“: 1.45-
0.0.5- 0
0.65- *
0
0.45 , , , , , , , , , , , , , , ( ( , , , , , , , , ,
.04 .05 .D6 .07 .08 .09 .lO .11 .I2 3.3 .I4 .15 .16 .17 .10 .19 .20 .21 .22.23 .24 .25 .26 .27 .26.29 20
MG. POTASSIUM ADDED
mg., both the nitrite and silver contents of the reaction product
maintain a constant ratio to the potassium.
Effect of Potassium Cancel-kation-In the following experi-
ments we maintained the amount of the added silver as a constant.
In three series of experiments, 10, 12, and 15 mg. of silver re-
spectively were employed as constant quantities. These are
t,he silver concentrations located at the beginning, the middle,
and the end of the horizontal zones of both curves in Fig. 1. Other
350 Potassium Determination
(2) sodium tungstate, 3 per cent solution, and (3) silver nitrate,
0.2 M solution.
.With a 1 cc. Ostwald pipette (“to contain”), 1 cc. of serum is
measured into a Pyrex test-tube containing 6.2 cc. of water and
the content,s are mixed well. 1 cc. of 3 per cent sodium tungstate
is admixed; then 1 cc. of 5 per cent cupric sulfate is added, and the
tube is stoppered and thoroughly shaken. Following this, 0.8
cc. of 0.2 M silver nitrate is added, the tube is again stoppered
and thoroughly shaken, and the contents are filtered through a
TABLE I
Comparative Serum Potassium Determinations by Manometric Nitrite and
Titrimetric Silver Procedures
mg. ml.
18.9 18.7
18.2 18.3
19.5 19.3
24.0 23.8
24.5 24.1
TABLE II
Comparative Potassium Determinations on Blood Serum by Silver Potassium
Cobaltinitrite Method, with 0.5 cc. of Serum, and Chloroplatinate
Macromethod of MacKay and Butler, with 10 Cc. of Serum
Accuracy of Method
Comparison of Gasometric and Tit&metric Determination--In
Table I are presented comparative &rum potassium values ob-
tained by parallel determinations of the nitrite and silver content
of the precipitates. As may be seen, the agreement between the
two sets of results is satisfactory, so that the two procedures are
practically interchangeable. For our own part we prefer the
gasometric technique for its precision; the titrimetric technique,
on the other hand, is more rapid and easier to perform.
Comparison with Chloroplatinate Method-The data given in
Weichselbaum, Somogyi, and Rusk 355
TABLE III
Recovery of Potassium Added to Blood Serum (Mg. per 100 Cc. ofserum)
0 18.3 0
5 23.2 4.9
TABLE IV
Serum Potassium Content of Normal Subjects
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