Document Z4nwGLEzgKa9xNOr5GvNMRDkY
confidential
OTHER LOCATIONS
'' ">J. R. Savage - W.G.K. J. J. Luecken - W.G.K. H. C. Carder - W.G.K. H. L. Hubbard - Sou. Second
GENERAL OFFICES
J. A. Mullendore P. G. Benignus W. R. Richard
ANNISTON
W. B. Papageorge L. C. Furhmeister J. G. Bryant 'V. R. Haupt R. G ^ Moody
PROGRESS REPORT ANNISTON LABORATORY
JOB NO.
435-1-65
REPORT NO. 1
DATE: November 9, 1965
TITLE:
i
GLC Analyses of Aroclor 1242
OBJECTIVE:
Determine isomer distribution of Aroclor 1242 to detect any changes in Anniston production, and to compare Anniston material with competitive Aroclor.
REPORTED BY: J. A. Liddle
PERSONNEL: J. A. Liddle (0. E. Dolin)
SUMMARY:
Sihce the first progress report on the study, August 6, 1965, 36 lots of Anniston material have been analyzed by GLC. A statistical evalua tion of the data indicates no significant shifts in: the isomer distribu tion have occurred.
RECOMMENDATIONS:
Continue analyses of Aroclor 1242 to obtain sufficient data for a reliable factor analysis.
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DETAILS
Background
The main objective of this study is to determine the isomer distribution of Aroclor 1242 and to detect any shifts due to changes in process or equipment.
Thirty six Anniston lots and seven Krummrich lots have been analyzed since the first
report on this study*
'
Data; Graphs of isomer values for material produced at Anniston during 1965 are attached. The scale of each graph is based on an analytical reproducibility factor of + 1% of the amount present.
Isomer values for three lots of Aroclor 1242 produced at W.G.K. are listed.
Isomer Group
KE 432
KE 441
KE 446
1`
2 3, 4, & 5 6&7 8, 9, 10, & 11 12, 13, 14, & 15 16, 17, 18, 19, & 20 21, 22, 23, & 24 25, 26, & 27 28, 29, 30, & 31 32, 33, & 34 35, 36, 37, 38, 39, & 40 41 & 42 43, 44, & 45 46 47 48 49 & 50
0.10 0.15 0.06 3.58 11.35 27.66 31.76 6.94 9.87 4.81 2.53 0.80 0.25 0.13 0.01 Trace Trace NDA
0.06 0.09 0.03 2.97 9.70 26.23 32.67 7.45 10.14 6.96 2.65 0.73 0.21 0.11 0.01 Trace NDA NDA
0.11 0.13 0.04 2.97 9.54 24.99 32.37 7.56 10.50 7.74 3.47 0.17 0.27 0.13 0.01 Trace Trace NDA
The stability properties, electric properties, etc.. for typical Anniston material are listed below:
Property
AE-171
Specific Gravity
1.387
<a 25/15.5#C
Refractive Index
1.6245
<3 25 C
Monsanto Stability 0.08
Hydrolysis Stability 0.21
Thermal Stability
0.38
Dielectric Constant 4.90
@ 100C, 1000 Cycles
Q
Resistivity @ 100C "1035 x 10
OHM-CM @ 500 V.O.C.
Power' Factor
0.29
@ 1000 Cycles
Sampling Date
7-29
AE-204 1.391
1.6250
0.16 0.18 0.26 4.85
9 640 x 10
0.20
9-8
AE-213 1.388
1.6247
0.12 0.15 0.44 4.83
_
9 1550 x 10
0.20
9-19
AE-238 1.388
Specifications 1.381 - 1.392
1.6250
1.6240 - 1.6260
0.09 0.14 0.46 4.88
0.4 ppm.. Max. 1.0 ppm.. Max. 0.75 ppm.. Max. 4.70 - 4.90
9- Q 880 x 10 500 x 10* Min.
0.17
'
10-19
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DISCUSSION
Lots AE-171, AE-204, AE-213, and AE-238 are typical of Anniston production.
Starting with Lot AE-182, a new column was used in the gas chromatograph. A compari son of isomer distribution data obtained from the old and new columns indicates a slight shift in percentages due to the column change. Isomer groups 12 through 20 appeared to increase slightly, while isomer groups resolving after 28 appeared to decrease.
The decrease in random variability of isomer distribution is believed to be due to the fact that all samples are now being analyzed and calculated by one person. This minimizes errors arising from baseline corrections, integrator counting, etc. .
V
Comparing Anniston material with W.G.K. material, the following differences are noted:
Peaks 2 to 11 Peaks 12 to 15 Peaks 16 to 20
W.G.K., has a lower concentration W.G.K. has about a 2% higher concentration W.G.K. has about a 4% higher concentration W.G.K. has slightly lower concentration after Peak 24
CONCLUSIONS
No significant shifts in isomer distribution have occurred in Aroclor 1242 produced at Anniston. TSD will evaluate GLC data to obtain information for optimizing chlorination in reference to dielectric constant and stability. (Progress Report 370-340, No. 2)
Samples for the study of the effects of slow and fast chlorination rates on isomer distribution have not been obtained at the present time.
FUTURE
1. Continue GLC analyses of approximately 20% lot samples of Aroclor 1242.
2. Analyze additional samples of typical W.G.K. material.
3. Have Research run IR analyses of typical and abnormal (1956) samples.
4. Have Research run GLC-mass spectrometer analyses of typical material to identify additional isomers.
5. Analyze batch vs. continuous and slow vs. fast chlorlnatirmatfe samples when
received.
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