Document 3ebp3mDV80O54NL5m6xOpDeOE
PHOSPHATE DIVISION RESEARCH DEPARTMENT
Short Form Report No. 2026
Work Started:' March 25, 1946 Work Finished: April 2, 1946 Date Reported: April 3, 1946
File No. 138
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CC: R. Lo Jenkins - Cc B Durgin E. E. Hardy H. F. Weaver E, S,, Weatherly
^A, M,, Ellenburg * _ Po Logue Research File
Job No, 171-297
Investigators: P. A, Sanguinetti . A. M. Ellenburg
TITLE: BIPHENYL ANALYSES ON BAGS AND OIL MIXTURE FOR WAXSIDE PAPER COMPANY ST. LOUIS, MISSOURI,
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INTRODUCTION:
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The Sales Department requested by letter on March 8, 1946, that the amount of biphenyl be determined for Waxside on paper bags which were impregnated with biphenyl. Another letter on March 14, 1946, requested that the amount of biphenyl in a paraffin wax and mineral oil mixture from Waxside be obtained,
SUMMARY:
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Weighed squares of paper (5" x 5") were analyzed by extracting the biphenyl with distilled chloroform. Then the Intensity of the blue color produced when the extraction solution was reacted with sublimed A1C13 was matched with known standards. This method of analysis is reported in. a recent work by R, G,, Tompkins and F, A, Isherwood.
Originally only the Inner layer of the multiwall bag had been impregnated
and most of the biphenyl was found there, but some biphenyl was found in the
middle and outer layers of the bag. The table in the experimental section
shows these data.
;
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The oil mixture was fractionated in a 1" x 4' packed column in order to effectively cut out the biphenyl fraction. Material boiling at 252-254*0 was collected as the biphenyl fraction, which constituted 17.3$ of the mix,
CONCLUSIONS:
1. The method used to determine the biphenyl in the bags is only accurate to 25 per cent.
2. Based on the analyses, ths hags are not uniformly impregnated,
3. Some biphenyl has migrated to the outside layers of the bags.
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4a The biphenyl in the oil mixture is approximately 17.3 0,5$
RECOMMENDATIONS:
A more accurate micro method of analyzing for biphenyl is desirable in case more work of this nature is anticipated,
OS\N 330559
4/11/46
A. M. Ellenburg " STLCOPCB4077203
S&ort Form Report No, 2026 Page 2
PREVIOUS WORK:
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"The Absorption of Diphenyl by Oranges from Treated Wraps." R. G. Tomkins anil F. A. Isherwood. Analyst, 1945, 70, 330.
EXPERIMENTAL DATA:
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The analytical data are rounded off to show that the method used is only a cl&se estimate. The locality of the samples indicates that the squares were cut either above or below the middle of the bag and check analyses were * taken from the opposite side of the bag. All three layers were analyzed at each locality.
An area of'25 square inches was taken for each analysis. This weighed piece
was extracted with 25 co of distilled chloroform for 12 hours in tightly
covered bottles. The test was performed by using the color-reaction obtained
when A1C13 is reacted with the biphenyl and chloroform mixture. Color
intensity was compared to known standards and the total biphenyl present was
calculated.
Biphenyl Analyses of Bags - 25-Square-Inch Ssmples
Weight of' Bag No. 1 Paper, gms.
Total Mgi'' Biphenyl Found
Kg;'Biphenyl Per Sq. Inch
I-T 1.7085 1.6605
30 20
1.8 1.2 . 1.2 .8
M-T .
1.4198
3.5
.3
.14
1.5005
3
.2 .12
0-T 1.4401
3
.2 .12
1.5656
1.5
.1
.06
I-B 1.6610 1.6037
15 17.5
. .9
i.l
.6 .7
M-B
1.4930
. 7.5
.5
.3
1.4365
3
-2 .12
0-B
1.4660
.4
1.4445 2
.3 .16 .1 .08
DSW 330560 STLCOPCB4077204
Short Form Report No. 2026 Page 3
Weight of Bag No. 2 Paper, gms.
Total Mg. Biphenyl Found
$ Biphenyl
I-T
1.6390
. 20
1.6165,
15
1..29
M-T 1.4280 1.4330
5 S
.4 .4
O-T 1.4680 1.3910
4 r .3 4 .3 '
I-B 1.6310 1.5930
M--B 1.4110 1.4570
10 10
4,5 4
.
.6 *6
.3 .3
0-B 1.3615 1.4340
3.5 3
.2 .2
Note:
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I - Inner Layer M - Middle Layer 0 - Outer Layer . T - Top of Bag B - Bottom of Bag
Check analyses are from opposide side of bag.
Mg; Biphenyl Per Sq. Inch
.8 .6
.2 .2
.16 .16
.4 .4
.18 .16
.14 .12
The oil mixture containing biphenyt was fractionated in two distillationsc The boiling point difference between biphenyl and mineral oil allowed a very distinct break in the sample cut.
The first run showed 16.5 per cent biphenyl while the second run showed 18p7 per cent. An average of the two runs was 17.3$. The differnece in the two runs is no doubt due to some hold up in the column after the first distillations.
NOTEBOOK RESERENGES:
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33348-50
DSW 330561 STLCOPCB4077205