Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
Determination
R. H. KIMBALL, H. H. WITTENBURG, AND D. E. MACFADYEN
University of New Hampshire, Durham, N. H.
!
JANUARY 15, 1937 ANALYTICAL EDITION 49
microbalance. After rolling between the fingers, the capsule is of nitric acid is reduced t o 1 cc. They are charged, heated, and
left on the balance pan for 10 minutes t o reach constant weight. opened, and the precipitate is transferred to the filter as before.
The bomb tubes are constructed of 10-mm. tubing and the amount Before the first weighing of any day the filter tube is wiped with
a dam cloth, placed in the adapter, and heated in the oven at
125’ 8 The adapter is closed with cork stoppers and allowed
to cool, and the filter tube wiped again with the damp cloth and
TABLEI. RESULTS
B Y SEMI-MICROMETHOD
left for a half hour on the pan of the microbalance before weighing.
Sample Halide Calcd. Found Difference After filtration the identical procedure is followed, and this
Mo . Mo . % % % weight can be used &sthe first weight of any succeeding analysis
p-Bromoacetanilide, BrCoHCVHCOCH3 on the same day. Obviously the drying block technic of Pregl
22.30 19.80 37.34 37.79 4-0.45 could be employed if desired.
23.25
48.50
20.30
42.30
37.17
37,12
-0.17
-0.22
The accuracy seems to be of the same order as the semi-micro-
46.20 40.25 37.08 -0.26 determinations. Slightly more time is required, so that economy
26.55 23.30 37.36 +0.02 of material is the only advantage of the micromethod.
58.25 50.65 37.01 -0.33
23.70 20.80 37.36 +o 02
p-Chloroacetanilide, CIC6H4NHCOCHa Analytical Results
39.45 33.20 20.92 20.82 -0.10
58.25 49.10 20.85 -0.07 The data given in Tables I and 11, obtained by under-
26.45 22.40 20.95 $0.03
43.10 36.00 20.66 -0 26 graduate students, indicate that the degree of accuracy is
p-Nitrochlorobenzene, C1CsH4NOz about that normally expected. It is worthy of note that the
41.75 37.90 22.51 22.46 -0 05 use of a larger sample brings no corresponding increase in
29.85 27.00 22.38 -0 13
101.20 92.20 22.54 +O 03 accuracy, showing that the errors in weighing are well within
61.05
45.75
54.75
41.95
22.18
22.68
-0 33
f0.17
those inherent in the method itself. Of the few failures en-
20.75 19.15 22.82 4-0 31 countered, only two were not traced to faulty manipula-
N-(7-bromopropyl) phthalimide, CaH4OnN-CHz-CHz-CHzBr tion.
31.45 22.00 29.82 29.77 -0.05
35.05 24.50 29.75 -0 07
37.15 25.95 29.73 -0 09 Summary
21.85 15.30 29.80 -0 02
63.00 44.05 29.76 -0.06
82.30 57.50 29.74 -0.08 A simplified Carius method is described for the semi-
Methyl-a-phenyl-8-bromo-@-benzoyl propionate (a), ClrHlaOsBr micro- and microdetermination of chlorine and bromine in
37.25 19.90 23.03 22.74 -0 29 organic compounds. The sample is weighed on a n ordinary
21.55 11.70 23.11 +o 08 analytical balance in a capsule of silver foil which dissolves
19.65 10.60 22.96 -0 07
21.55 11.60 22.92 -0 11 and allows the halide to be siphoned directly from the bomb
Methyl-o,r-diphenyl-o,8-dihydroxy-y-ohlorobutyrate (91, C I ~ H I ~ O L X tube onto a micro filter tube. The bomb tube is opened with
12.75 5.70 11.06 11.06 0
22.15 9.95 11.11 $0.05 a flame which eliminates the danger of glass chips falling into
20.80 9.25 11.00 -0.06 the precipitate. The method is reliable and convenient and
the results are of the usual order of accuracy.
TABLE11. RESULTSBY MICROMETHOD
Sample Halide Calcd. Found Difference Literature Cited
24-0. Mg. % % % Clark, J . Assoc. O f i c i d Agr. Chem., 17, 483 (1934).
p-Bromoacetanilide Kohler and Goodwin, J . Am. Chem. Soc., 49,226 (1927); Kohler
11.660 10.280 37.34 37.52 +o. 18 and Kimball, Ibid., 56, 730 (1934).
10.710 9.395 37.34 0 Ibid., 55, 4637 (1933).
10.666 9.370 37.39 +0.05
12.807 11.240 37.36 +0.02 Pregl, “Quantitative Organic Microanalysis,” 2nd English ed..
p-Chloroacetanilide tr. by Fyleman, p. 149, Philadelphia, P. Blakiston’s Son &
11.161 9.430 20.92 20.91 -0.01 Co., 1930.
7~ 156 6.095 21.07 +O. 15 I b i d . , 4th German ed., p. 129, Berlin, Julius Springer, 1935.
6.226 5.315 21.11 +o. 19
RECEIVED
August 20, 1936.