You are on page 1of 2

34 INDUSTRIAL AND ENGINEERING CHEMISTRY VOL. 9, NO.

is, in most cases, sufficient to indicate the true value of the


iL. A best cure.
v 93
5 VOLS. p'
Elongation
--
None 5
TABLE
10
I1
Gas Black Content of Stock, Volumes:-
20 25 30 35
GAS BLACK : %
NONE 350 11.3a 16.Ba 28.W 56.3a 58.8" 44.5O (62Ia
280 7 . i a 10.4a 16.qa 2 9 . P 30.9Q 24.4Q 30.7''
; IOVOLS. Test Piece Width, Mm.:
-6,3----- 5 3
".0-0-0 n' 200 Experimental Factors
: 7
- 4.2- 5.3 - 8 . 7 ~ -
A' Energy Storage Capacity
CURE 47b 71b 121b 232b 3126 3876 (452)a
I 1 I I 1 1 0 0 350
250 32b 44b 65b 122b 164b 212b 267b
Modulus
300 15C 270 56C llOc 148c 175C 185C
a Scale reading (per cent energy absorbed).
'A b Vaiues marked multiplied by the corresponding faotors.
Q

0 Modulus (kg. per sq. cm.), calculated from values marked b.

Following is a comparison of results obtained a t 50 cm.


per minute with those a t more than 25,000 om. by impact;
the cures were 35, 50, 70, 100, and 140 minutes a t 260' F.:
d
-At
-- Ratings in % of Lowest Cure Values-
low speed- -By impact-
Stock Gas Black 50- 70- 100- 140- 50- 70- 100- 140-
C U R E C MINS. > No. Loading min. min. min. min. mm. min. min. min.
CURE I I I I I Vol.
I II 1 I 55 9 70 100140 35 50 70 100 140
35 50 70 100140 v-92 None 116 118 128 132 108 113 106 101
93 5 169 228 295 340 118 123 110 104
94 10 163 234 267 297 132 152 146 126
ENERGY ABSORBED AT RUPTURE 95 20 157 207 237 243 110 116 104 83
0 BY IMPACT 96 25 140 206 192 178 104 99 90 68
97 30 131 178 138 119 100 98 77 62
A A T LOW SPEED 0- 98 35 128 147 128 112 99 97 75 47

10. ENERGY
FIGURE ABSORBEDAT RUPTURE,
IN RELATIOK
TO Acknowledgment
CURE '
The author desires to express his thanks to R.P. Dinsmore
mination of the energy storage capacity at 250 and 350 per and L. B. Sebrell for permission to publish this paper, and
cent elongation and t o modulus a t 300 per cent is shown in to W. W. Vogt and M. J. DeFrance for valuable criticism.
Figure 9 and in Table 11. Literature Cited
ENERGY ABSORPTIONAT BREAK. The energy storage
capacity at break in relation to best cure is shown in Figure 10. (1) Beadle, C., and Stevens, H. P., Proc. Intern Rubber Congr.,
London, 1911,pp. 344-50.
Probably one of the most useful applications of the impact (2) Van Rossem, A., and Beverdam, H. B., Rubber Chern. Tech., 4,
test is the determination of the best cure, from the standpoint 147-55 (1931).
of energy storage capacity. The difference between cure is, RECEIVEDJune 18, 1936. Presented before the Division of Rubber Chem-
in some cases, not very accentuated and almost on the limit istry a t the 91st Meeting of the American Chemical Society, Kansas City,
of the errors involved in the test. However, the general trend Mo., April 13 to 17, 1936.

A Standard Quinhydrone Electrode


VERNER SCHOMAKER AND D. J. BROWN
Avery Laboratory of Chemistry, University of Nebraska, Lincoln, Nebr.

IT
,
WAS the authors' purpose to prepare a n electrode readily
without use of balance or volumetric apparatus. Of those
Since the authors were attempting to prepare a half cell for
general laboratory use, ordinary distilled water was used.
studied, a quinhydrone half cell in which the solution is potas- Eastman's quinhydrone was carefully recrystallized from,water.
However, observations made using the quinhydrone as received
sium tetroxalate, saturated a t 0", was found to be very satis- varied less than 0.1 mv. from the purified product.
factory. A sample of the best grade of potassium tetroxalate (Merck)
The saturated calonlel electrode was used as the reference was twice recrystallized. The resulting salt, the original material,
half cell. I n all the determinations the calomel half cells were and salts from other sources, including a very old sample (Eimer
and Amend), all gave the same results.
of the same reproducibility as those prepared by Samuelson, A solution of potassium tetroxalate nearly saturated at room
(b) and the same precautions were used in their preparation. temperature was placed in an ice bath, vigorously stirred for 2
The value +0.2446 +
0.00020 ( t - 25) was used to calculate or 3 hours, and then decanted through a glass tube which con-
tained a plug of carefully washed cotton.
the values for the guinhydrone electrode (1, g ) . However,
if the temperature coefficient of the hydrogen electrode at A "nest" of half cells, similar t o those used by Samuelson (6),
was prepared for each type of solution, and these half cells were
all temperatures is called zero, the temperature coefficient measured against one another. The average deviation in milli-
of the saturated calomel half cell is -0.66 mv. per degree (6). volts during a series of observations is included in Table I. One
Values on this basis are also included. of these was then compared with one of a nest of calomel half
JANUARY 15, 1937 ANALYTICAL EDITION 35
cells which had been likewise interchecked and found to have a
very small average deviation.
A sufficient quantity of the tetroxalate solution for several half TABLEI. QUINHYDRONE
ELECTRODE
cells was saturated with quinhydrone, and several half cells were Average E. m. f .
filled. The balance of the solution was used t o wash the platinum E. m. f. Devia- of Calomel E. m. f .
foil electrodes, which were prepared as directed by Morgan, Temp. Observed tion 10 IIb 10 116
MV.
Lammert, and Campbell (4) and kept in water. Before use they 0 0.36566 0.07 0.2396 0.24625 0.60526 0,61191
were thoroughly washed with the solution of the half cell, but 26 0.35236 0.04 0.2446 0.2446 0.59696 0.69595
when transferred from one solution t o another they were washed 35 0 34743 0.06 0.2466 0.2380 0.59403 0.5854
thoroughly with the latter solution only. To detect possible
misbehavior of the electrodes, they were checked against one _
*Ex- -0.31 mv. degree
another in some of the solution before each run, and were not AT
used until they agreed within 0.02 mv.
The liquid junction between the nest of calomel electrodes and
of the quinhydrone electrodes was effected by means of “glass-
a
b
Absolute.
Relative to hydrogen electrode.
“aE;
- -.I - -0.1.17 mv. degree
stoppered” salt bridges built according to the directions of
Irving and Smith (3).
A Leeds & Northrup Type K potentiometer equipped with a
ty e R galvanometer was used in connection with a calibrated that of the half cells to be measured, and, since in ordinary
d s t o n cell. work the temperature coefficients are not considered, the
observed values will be more nearly true than if the com-
The potential of the tetroxalate-quinhydrone electrode was parison half cell had a lower value. For these reasons the
calculated a t 25’ C. and its temperature coefficient expressed authors believe this quinhydrone-potassium tetroxalate
either absolutely (Ij a) or relatively to the hydrogen electrode electrode is very suitable for ordinary laboratory work.
at all temperatures as zero (6).
The resistance of the cell was found to be comparatively Literature Cited
low. If a current of 0.1 microampere, sufficient to deflect the (1) Ewing, W. W., J . Am. Chem. SOC., 47, 301 (1925).
galvanometer 3 cm. on the scale, flowed for 20 seconds, the (2) Fales and Mudge, Ibid., 42, 2434 (1920).
maximum effect was 0.05 mv. This polarization disappeared (3) Irving and Smith, IND.ENG.CHEM., Anal. Ed., 6, 480 (1934).
(4) Morgan, Lammert, and Campbell, J . Am. Chem. Soc., 54, 910
within 20 seconds, or more quickly if stirred. (1932).
The new half cell is very easily prepared without use of ( 5 ) Samuelson, G. J., Ibid., 57, 2711 (1935).
balance or volumetric apparatus. The materials are easily (6) Vellinger, E.,A w h . phys. biol., 2, 119 (1926).
obtainable. While the temperature coefficient is high, so is RECEIVED
August 8, 1936.

Determination of the Ash Content of


Sugar Products
A Standardized Sulfated Ash Method
R. VALDEZ’ AND F. CAMPS-CAMPINS,2 Massachusetts Institute of Technology, Cambridge, Mass.

Experiments showed that the sulfated ash method is affected by the partial and variable loss of
ash method needed to be standardized as to chlorine, nitrogen, and sulfur from the sample during in-
cineration. Thus the percentages of these constituents so
the time and temperature of heating of the
lost vary according to the method of burning and the nature
resulfated ash. A standard method was of the bases with which these elements are combined. This
worked out, based on the thermal decompo- means that the method is unsuitable for the determination of
sition of pure sulfates. A technic was de- comparable values of the ash content a t various stages of
vised for ashing large amounts of low-ash the fabrication process or before and after treatment with
some ash adsorbent. For these reasons the use of the method
samples. The method is suitable for ash
has been discontinued.
adsorption studies, etc., where precision SULFATED ASH METHOD. I n this method (1) the partly
measurements are necessary. dried sample of sugar product is moistened with concentrated
sulfuric acid and then incinerated till a white ash is obtained,
This ash is taken up with a few drops of sulfuric acid-i. e.,

T HE methods for the determination of the ash content


of sugar products are of two types-i. e.: gravimetric
and conductometric. As the latter is interpreted in terms of
resulfated. The excess acid is driven off by heating and
the weight of ash recorded.
All the volatile constituents of the ash are driven off by
the former, it is obvious that gravimetric methods are the the acid treatment. Obviously, owing to the variation in
basis of all quantitative ash measurement. There are two the composition of the sulfatable salts as well as the amounts
gravimetric methods-the carbonated ash method and the of the inert matter present, there is no correlation between
sulfated ash method. the sulfated and carbonated ash values.
CARBONATED ASHMETHOD.Browne and Gamble (2) have
shown that the ash content as measured by the carbonated Purpose of Resulfation
1 Present address, Central Valdez, Guayas Prov., Ecuador. I n the ash obtained by the decarbonization of the sulfated
* Prasent address, National Adhesives Corp., New York, N. Y. sugar product, qualitative tests have shown (1) the presence

You might also like