Document Rpw8q92BGVKRwbLbDjEm26MGa
PROGRESS REPORT
ORGANIC CHEMICALS fIVISION
TECHNOLOGY DEPARTMENT
. . - w_ j, Litschgi w, M. Mees j, p. Mieure P.. S. Tucker
|.C
St. Louis - S. Second Street
..
Sept. 1971
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:*Ti 2 9-28-71
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2-21-760.01-13480. 85010, 16300
Tt. rtocumtM < if* property of MONSANTO COMPANV It aonulm CONFIDENTIAL INFORMATION which trust net tie rtp,cd,,cd
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DISTRIBUTION
-WITH DETAILS
RESTRICTED TO: H. S. Bergen M. W. Farrar
*P. B. Hodges W. K. Johnson
*R. E. Keller *R. H. Munch *W. B. Papageorge
T. M. Patrick
*R,Lidgett/H.Vodden/R.
*W. R. Richard
Baxter - Ruabon
*C. W. Roos
*J,R. Durland - Tokyo
J. E. Springgate
*E. S. Tucker/W. M, Mees/ J. P. Mieure/w. J.
Litschgi
*E. P. Wheeler/G. J. Levinskas
ENVIRONMENTAL ANALYTICAL STUDIES - RESEARCH AND DEVELOPMENT, MANUFACTURING AND OUTSIDE SUPPORT STUDIES
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Identify, locate and assess the magnitude of Aroclor pollution problems, help determine what needs to be done to control pollution sources, verify the effectiveness of proposed pollution control procedures, guide develop ment of recycle and/or disposal methods, and provide collaborative data for legal and regulatory purposes.
SUMMARY
During the month of September vfiO environmental and research samples have been analyzed for polychlorinated biphenyls (PCB's) by electron capture . gas chromatography. Analysis of these samples represents a minimum man power expenditure of 210 hours.
PCB's, typical of our Aroclors, have been found at levels below and above action levels in:
. Fish meal, soybean meal and meat meal (animal and poultry fed components)
. Paperboard and polyethylene film (food packaging materials) . Environmental samples from three customer sites (oil, sediment,
and water) . Two Monsanto products . Fish and sewer effluents from two Monsanto manufacturing sites
An over view of the analytical results is shown in Table I in the detail section.
MOWS 057138
2-21-760.01-13480, 65010, 16300 Page 2
Additional external and internal support has been provided in the form of:
. On site PCB methodology training for laboratory personnel from Raiston-Purina, St. Louis; St. Regis Paper Co., Dallas, Texas; and Monsanto, Ag Div., Nitro, West Virginia
. Attendance at pertinent meetings on PCB problems (Working Group on Pesticides, Washington, D.C.j National Broiler Council, Scientific Advisory Committee and Lake State's Governors Inter disciplinary Pesticide Conference)
. General internal and external analytical consultation
. Distribution of Aroclor methodology and reference standards
. Preparation of, and participation in, inter- and intra laboratory checks on PCB methods of analysis
FUTURE PLANS
1. J. F. Queeny monthly sewer effluent composites.
2. St. Regis Paper Company - Polyethylene film and paperboard samples.
3. Distribution of PCB's in whole milk (fat vs skim).
4. Complete PCT extraction and separation work.
5. Request pertinent plant effluent samples from Anniston for PCT analysis.
6. Complete recovery check and write up of methods for determination of PCB's in Santoquin and CaMHA.
7. Evaluate Dr. O.W. Berg's PCB perchlorination technique for quantita tion of altered PCB residues.
8. Analysis of MCS 1016 and Kanechlor for polychlorinated dibenzofurans.
9. Complete inter-laboratory PCB methodology check.
10. Participate in panel discussion of PCB methodology.
11. Analysis of USDA turkey tissue extracts to help establish contamination source(s).
W. J, Litschqi
E. S. Tucker db
HGNS 057135
1J details
Sample Source 1 Ralston-Purina j St. Louis, Mo,
CUSTOMER SERVICE
Sample Matrix
No. of Samples
Fish, meat 6 soybean 10 meal
Level Found
PPM
Associated Aroclor
A-1242
2-21-760.01-13480, 16300 Page 3
Support Objectives Determination of level and source of PCB contamination in animal feed components
1 Westinghouse ! S. Boston, Va.
! National Cash
Register Dayton, Ohio
Oil, water a sedi ment samples
a) NCR 24-hour sewer sediment
b) Wash solution from 14.3.1, wash job
7 PPB-PPM A-1242
1 PPB A-1242
1
PPM
A-1242
Pollution Control Pollution Control
Frigidaire Div., GM Corp. Dayton, Ohio
Monthly effluent composites from plants 2(3
4 PPB
A-1242
Pollution Control
St. Regis Paper Polyethylene film 2 ND*to
Co. paperboard
PPB
Dallas, Texas
A-1242
Pollution Control
Ag Division Nitro Plant
santoquin MHA
MANUFACTURING SUPPORT
7
PPB
A-1242
4
PPB
A-1242
Determination of level and source of contamination of animal feed additives
i J.F. Queeny j Pensacola, Fla.
Sewer effluent composites
Fish
8 PPB A-1242 Pollution Control
2 PPB A-1254 Determination of environmental contamination
( *ND = None Detected I
I
HONS 057140
DETAILS (Cont'd)
RESEARCH AND DEVELOPMENT
Sample Source
Sample Matrix
No. of Level Associated
Samples Found
Aroclor
Inter-plant Round Water spiked with
Robin
Aroclor
(WGK, Anniston,
& Applied Sciences)
8
A-1242 A-1254 A--1260
National Broiler Council Round Robin
Chicken fat spiked with Aroclor
4 - A-1242
2-21-760.01-13480, 16300 Page 4
|
Support Objectives
Insure the maintenance of precision and accuracy in Monsanto labs analyzing for PCB's
Cooperative government-industry PCB methodology check
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2
c/i o Vl
DETAILS (Cont'd)
2-21-760.01-13480, 16300 Page 5
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OUTSIDE SUPPORT STUDIES
Ralston-Purlna Company
The results of the analysis of 6 meal samples submitted by Ralston Purina were as follows:
Sample No. 661 662 663 664 665 666
Sample Description Fish Meal (69196) Meat Meal (69197) Soybean Meal (69200) Meat Meal (69201) Soybean Meal (69202) Soybean Meal (69203)
ppm PCB' s(Aroclor 1242)
Ralston
Monsanto
12 29
11 25
49
13 32
6 11
0.6
As the table indicates, with the exception of the lowest containing PCB sample, our results are not in agreement. The fairly consistent factor, 2-2.5X between the numbers leads me to believe that they are not extract ing the PCB quantitatively from the meal.
Subsequent analyses of four of these samples, spiked at a level equiva lent to that found, indicates that our procedure recoveries were in the range of 100-106%. The actual recoveries are shown in the following table.
Sample No.
661 662 664 665
Sample Description Fish Meal (69196) Meat Meal (69197) Meat Meal (69201) Soybean Meal (69202)
Level of PCB1s Added
21 PPM
11 PPM 12 PPM 11 PPM
Total Found
53 PPM 36 PPM 44 PPM 23 PPM
% Recovery
106 100 100 105
Approximately 1-1/2 days were spent in familiarizing D. Viviano, Supervisor, Fat Soluble Laboratory - Ralston-Purina, with Monsanto PCB methodology.
Frigidaire Division, GM Corporation
Sample No.
600 601
651 652
sample Description Plant 2 (June) Plant 3 (June) Plant 2 (July) Plant 3 (July)
PCB Level Found
<0.3 PPB 0.8 PPB
<0.1 PPB 1.2 PPB
1242 1242 1242 1242
The results shown have also been corrected for the 0.3 ppb background value.
HOftS 057142
DETAILS (Cont'd)
2-21-760.01-13480, 16300 Page 6
SCR - Dayton, Ohio
, Sample No. 667
Sample Description
Hash solution from 14.3.1, wash job, installation after one week use. Finishes Control Labs, NCR Co. 7-26-71
PCB Level Found
1.58 PPM
Aroclor 1242
653 NCR Sewer Composite (7-15-71)
<0.4 PPB
1242
Our calculated detection limit based upon observed background and sample size was 0.3 PPB. The results shown have been corrected for the 0.3 PPB blank. After orally reporting these results to Paul Henry, he indicated that they would not need much more support analysis. Possibly one more set to confirm the low PCB level observed in their 7-15-71 sewer composite sample.
Wcstinghouse, S, Boston, Virginia
Sample No.
645 646 647 648
649
Sample Description
Oil skimmed from oil separator
Final effluent from oil separator
Effluent from neutralizer plant
Lawson's Creek
.
Dan River, above confluence with Lawson1s Creek
Dan River, below confluence with Lawson's Creek
PCB Level Found
8.06% 95 PPB
144 PPB 0.5 PPB 1.5 PPB
1.1 PPB
St. Regis Paper Company, Dallas, Texas
Paperboard and polyethylene extracts, used to package food products, were analyzed by EC/GC for PCB's. The polyethylene film extract contained no apparent PCB's while the paperboard contained M).5 PPM. J. Box and E. Albert visited our laboratory and were familiarized with Monsanto PCB
methodology.
MANUFACTURING SUPPORT WORK
Ag Division
Sample Description
Santoquin Composite 8-30-71 9-2-71
Santoquin Distillation Leg 9-3-71
Santoquin Composite 9-19-71
Detection Limit
PCB Level Found
146 PPB 108 PPB
91 PPB
111-405 PPB 89 PPB
Aroclor
1242 1242
1242
124 2 1242
MGNS 057143
DETAILS (Cont'd)
2-21*760.01-13480, 16300 Page 7
An attempt was made to decrease the PCB detection limit by Increasing the sample size by a factor of 10X. Matrix interferences were encountered which required that a maximum and minimum be reported (Santoquin composite 9-19-71).
GC/Mass analysis of the residues extracted from Santoquin verified that if PCB1s are present they would have to be at a level less than 0.5 PPM.
Spiking of three samples of Santoquin at the 1 PPM level with A-1242
yielded recoveries of 73%, 92% and 96%. A tentative method will now be
written but further research is planned in order to remove EC/GC inter
ferences .
PCB
Sample Description
Level Found
Aroclor
CaMHA:Na 09-46 CaMHArNa 09-46
18.5 PPB 237 PPB
1242 1242
Detection Limit
15 PPB
1242
Spiking of A-1242 at a 2 PPM level to CaMHA yielded a recovery of 96%.
PLANT SUPPORT
J, F. Queeny Plant
Sample NO. 589 599 591 654 655
Sample Description MSD Gatewell (June) Clean Acid Sewer (June) DC Sewer (June) Clean Acid Sewer (July) MSD Sewer (July)
PCB Level Found
12 PPB 14 PPB 13 PPB 22 PPB 99 PPB
Aroclor 1242 1242 1242 1242 1242
The sample "DC Sewer (June)" was supposed to be the "Clean Acid Sewer (June)" spiked with 'vlO PPB Aroclor 1242. As you can see, our analytical results do not reflect the added PCB's. I have talked to A1 Peterson about this apparent discrepancy and it was decided that spiked samples would be included with their August set to see if this problem can be worked out.
Pensacola, Florida
Sample Description Large Crappie (Fish) Small Shell Cracker (Fish)
PCB Level Found
494 PPB
130 PPB
Aroclor 1254 1254
Both fish were skinned and fileted and only the edible portion of each fish was used for analysis as requested.
MOMS 057144
DETAILS (Cont'd)
2-21-760.01-13480, 16300 Page 8
RESEARCH AND DEVELOPMENT
Inter-Plant PCB Methodology Check
Duplicate sets consisting of eight water and six fat samples spiked with production Aroclors at various levels have been prepared and distributed to the plant laboratories. The results of each laboratory analysis of these samples are to be compared to insure consistent internal reporting.
National Broiler Council Intra-Laboratory PCB Methodology Check
Ten sets of soybean oil and chicken fat samples were prepared by Monsanto for distribution by Ralston-Purina to government and industrial laboratories analyzing samples for PCB's. The objective of this intra laboratory check is to establish the validity of the different PCB methods currently being employed.
HQNS 057145