Document VJMNga7qY4ypZmaLLzqQoG8wK
Exhibit 17
October Continuous Plant Run: Extraction Studies
of PVC Sheet by Gollob Analytical Service
Exhibit 17
^Gollob Analytical Service Corp.
-- Mass Spectrometry Gras Chromatography Leak Detection_________ -
47 INDUSTRIAL ROAD
BERKELEY HEIGHTS. NEW JERSEY 07922
TO: Mr. Michael F. Saggese
TO.. (201) 4644331
Tenneco Chemicals, Inc. Plastics Division Nixon Lane
ANALYTICAL REPORT NO. G.A.S. 34847
Nixon, N. J. 08818
Date Reported: 12/2/75
Date Requested:
11/11/75
P.O. No. Verbal
MATERIAL SUBMITTED: Three PVC Film Samples - Continuous Plant Run
Tenneco Proprietary Technique
INFORMATION REQUESTED: Gas Chromatographic Analysis
NOTEBOOK REFERENCE: NB 363, pages 31-32
RESULT OF INVESTIGATION: This vinyl chloride monomer extraction study was under
taken at the request of Tenneco Chemicals; see letters from F. V. Owens dated November 10*i> and 141>, 19 75.
Procedure
Subject samples have been analyzed at the Gollob Analy tical Service laboratory by Flame Ionization Gas Chromatography for extracted vinyl chloride monomer as follows:
A measured portion of the supplied film (.75 in 2 ) was placed into 2-dram vials containing 7.5 ml of the solvent re quested: a. 50/50 ethanol and water, b. hexane and c. distilled water. The vials were sealed with special Teflon lined septums and stored upright at the required temperature. After 1, 3 and every 5 days thereafter, the samples were analyzed by injecting 25 ul of the indicated solvent into a gas chromatograph: hexane onto a 15 ft. x %inch SE-30 column; water and ethanol-water onto a 20 ft. x k inch Carbowax 20 M column. All columns were main tained at ambient conditions.
Continued Page 1 of 3 Pages -
TEN4170
By GOLLOB ANALYTICAL SERVICE CORP.
Mr. Michael F. Saggese Tenneco Chemicals, Inc.
-2-
G.A.S. 34847
The Varian 1860 Gas Chromatograph was standardized by injecting freshly prepared standards of vinyl chloride gas into each of the extraction solvents. The standards were prepared as follows:.
A stock solution with a concentration of 520 ppb was prepared by adding 200 ul of vinyl chloride gas to 100 ml of the required solvent. This stock was further diluted to produce a 260 ppb vinyl chloride standard by injecting 100 ul of the stock into a special Teflon stoppered glass vial containing 1.9 ml of the required solvent. 25 ul of this standard produced a peak height of approximately 100 divisions on the gas chromato graph. Theoretically, each division is equivalent to 2.6 ppb. However, due to interferences by solvent impurities and chromato graphic base line instability, values below 20 ppb are not con sidered reliable.
dm 12/2/75
TEN 4171
E x h ib it 17
nyl Cn|^:ide Monomer Concer. ration opb Weiqht/Vclume
Analysis Extraction
Tate
Time {Days)
HEXANE 7329-40 7685-15
t --.79-15
ETOH/WATER 7329-40 7685-15 7779-15
WATER 7329 -40 7685 -15 7779
~ov. 19 21 26
ec. 1 6 10
'otes:
1 3 8 13 18 22
LT 20 LT 20 LT 20 LT 20 LT 20 LT 20
LT 20 LT 20 LT 20 LT 20 LT 20 LT 20
LT 20 LT 20 LT 20 LT 20 LT 20 LT 20
LT 20 LT 20 LT 20 LT 20 LT 20 LT 20
LT 20 LT 20 LT 20 LT 20 LT 2C LT 20
LT 20 LT 20 LT 20 LT 20 LT 20 LT 20
LT 50 LT 20 LT 20 LT 20 LT 20 LT 20
LT 50 LT 20 LT 20 LT 20 LT 20 LT 20
LT 50 LT 20 LT 20 LT 20 LT 20 LT 20
2T = less than
Values below the 20 ppb level are not considered reliable due to interferences by solvent impurities and chromatographic base-line instability. During the initial water extraction test an increase in the instrument noise level increased the less than value to 50 ppb. Samples prepared for study il/19/75.
Extraction Temperatures
Hexane
- 72F j
50/50 Ethanol - Water 120F
Distilled Water - 120F
ch
TEN 4172
Gollob Analytical Service Corp.
Mass Spectrometry Gas Chromatography Leak Detection
TO: Mr. Michael Saggese Tenneco Chemicals, Incorporated Plastics Division Nixon Lane, Nixon, New Jersey 08818
MATERIAL SUBMITTED: PVC Film-Sample No
47 INDUSTRIAL ROAD BERKELEY HEIGHTS. NEW JERSEY 07922 TEL. (201) 464-3331
ANALYTICAL REPORT NO. G.A.S. 35068
Date Reported: Date Requested: P.O. No.
12/15/75 12/11/75 Verbal
7330 #30 Tenneco No. D079-176-1.
INFORMATION REQUESTED: Mass Spectrometry Analysis.
NOTEBOOK REFERENCE:
NB 374 page 21.
RESULT OF INVESTIGATION:
Object
The purpose of this study was to determine the presence and amount of vinyl chloride monomer in subject sample. Conclusion
Tenneco PVC film Sample No. 7330 #30 Tenneco No. D079-176-1 has been heated to 130C for 3 hours, and the gaseous constituents
evolved have been analyzed by mass spectrometry for residual
vinyl chloride mgnomer. Based upon the analysis discussed below, it is concluded that there is no indication of the presence of vinyl chloride.
Sample Designation
Vinyl Chloride Monomer Concentration ppb
Sample No. 7330 #30 Tenneco No. D079-176-1
None Detected*
*Test sensitivity 1 ppb.
fEN 4173
By ____________ __ GOLL&B ANALYTICAL SERVICE CORP.
Mr. Michael Saggese Tenneco Chemicals, Incorporated
2- -
G.A.S. # 35068
Procedure
10.0 gms. of subject film was placed in a special glass con
tainer and sealed with a Teflon septum. The container was placed in a Gas Chromatographic oven at 130C for 3 hours. After the heat
ing period the container was removed from the oven and the gaseous
contents of the 10. ml container were removed, by vacuum into a glass
trap refrigerated at
temperature. The contents of the trap
were then desorbed at 100C into the mass spectrometer and scanned.
Prior to the analysis of the PVC film, known quantities of
vinyl chloride gas in air were prepared and analyzed using the same
procedure.
Quantities as low as 10 nanograms were successfully detected
by mass spectrometer.
ach 12/16/75
TEN 4174