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TEHNECOINTER OFFICE MEMO CHEMICALS , INC.
To Route List fkom W.C. Champion subject Revised Test Methods
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At Burlington
V. date September 25, 1975
JCopy to File
Attached are two Test Methods which are to be inserted into your Quality Control Manuals. They are as follows:
Test Method Title
Manual Section
2-31
Determination of Hard Particles in Record Resin
2
4-104
Quantitative Analysis of Copolymer Recovered Monomer
4
Method 2-31 supersedes the issue of January, 1970. Please discard the ob solete procedure which this replaces. Method 4-104 is currently being used at Flemington. This technique will be employed at Burlington at a later date. In the meantime, please retain the copy of Method 4-104 issued January, 1975 in your Manual,
Attachments (2) WCC/o'st
Jf. t W. C. Champioh
Route List
W, D. Bord H.B. Carr D. Hershkowitz H.R. Horton F. W. Kanzler D.J. Krzywicki W. Miringoff G. I. Rozand P.R. Scarito A. C. Siegel J.T. Sweeney R&D - Flemington
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TENNECO CHEMICALS, INC, ORGANICS & POLYMERS DIVISION
TESTING METHOD
DATE; Se pte mber, 1975 METHOD NO: 2-31
TITLE: PURPOSE: APPARATUS:
CHEMICALS: PROCEDURE:
REPORT: SAFETY:
Determination of Hard Particles in Record Resin
This method is for determining the possibility of hard particles causing stamper damage.
Balance, 1,000 gm capacity Paper Cups . Timer, calibrated in seconds Hydraulic Press, steam heated (60,000 lb capacity) Q-Panels, aluminum Spatula, stainless steel, 6" length
Resin to be tested Standard resin (315 type)
1. Weigh 500 gms of resin to be tested and screen through a 40 mesh screen (.0165" in opening).
2. Press oversize particles with a spatula to determine if they are hard particles.
3. If the particles are found to be hard, mix the oversize par ticles with 3 gms of the standard resin and place between two aluminum Q-Panels.
4. Place in hydraulic press heated to 300F and close as rap idly as possible to 60,000 lbs pressure and hold for two minutes.
5. Remove aluminum Q-Panels from press to cool.
Carefully examine surfaces of aluminum Q-Panels for any small dents or scratches. Report number and nature of defect (e.g. scratches, nicks, dents).
Gloves should be worn when removing Q-Panels from the press.
WRITTEN BY: D.J. Krzywicki
ISSUED BY/
Supersedes Issue Dated 1/27/70
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TENNECO CHUM I CALS, INC.
ORGANICS & POLYMERS DIVISION
TESTING METHOD
'^
V
DATE; September, 1975
4
METHOD NO: 4-104
TITLE: PURPOSE:
Quantitative Analysis of Copolymer Recovered Monomer
To quantitatively determine the composition of copoly
mer recovered monomer
;
APPARATUS:
Gow-Mac Gas Chromatograph (Model 69-100) Carle Liquid Sampling Valve, 5/il inject (Model 2015) Whitey Sampling Cylinders, 150 ml capacity
CHEMICALS:
Sample to be tested Helium, high purity
INSTRUMENT CONDITIONS: Gow-Mac: 50-55C (temperature control set 25) Inject Port Heater: - off Detector Current: 150 maximum Liquid Sample Valve Oven Temperature: 30~40C Carrier Gas: helium 80 psig in line pressure
Note: The instrument is never to be turned off except during the change of helium cylinders or when a malfunction is noted.
SAFETY:
Vinyl chloride is a Cancer Suspect Agent. Avoid phys ical contact or breathing of vapor. The sample valve must be installed in such a way that it provides vent ing of the sample purge to a hooded area.
PROCEDURE:
1. Attach one end of the sample cylinder to the quick connect on the inlet side of the sampling valve.
2. Attach the other end of the sample cylinder to the quick connect on the helium pressurization line.
3. Open helium pressurization valve.
4. Open upper valve on sample cylinder (this will pressurize the sample cylinder with 80 psig of helium).
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METHOD NUMBER: 4-104 Page 2
5. Check helium flow rate through the gas chromat ograph column using a soap bubble meter and a stop watch (flow rate should be 13+2 seconds per
SO ml).
6. Open vent valve completely.
7. Open lower valve on sample cylinder and allow liq uid to purge through the liquid sample valve.
8. When there is complete flow through the vent line, close the vent valve completely and reopen the valve approximately 1/8 of a turn. (The liquid monomer flow rate, through the vent line, is prop erly adjusted when small droplets can be observed at the end of the line,
9. Start the chart drive and set the attenuation to 256x for VCM.
10. Turn the liquid sample valve handle to either the left or right position. (Each turn of the handle will automatically inject 5pl of sample into the gas chromatograph column.)
11. After the elution of the vinyl chloride, change the attentuation to 128x to accomodate the vinyl acetate -monomer.
12. When the VAcM has eluted, change the attenuation to 8x and wait for the TCE peak.
Note:
The order of elution is; a. vinyl chloride monomer b. vinyl acetate monomer c. trichloroethylene
13. After the completion of the test, close the upper valve on the sample cylinder and the helium pressur ization valve. Remove the pressurization line quick connect and open the upper valve on the sample cyl inder. Allow the residual monomers to purge from the cylinder and the liquid sample valve.
14. Remove the sample cylinder from the unit and install the special adapter between the pressurization line and the inlet side of the liquid sample valve.
15. Open the vent valve completely and open the helium pressurization valve and purge the complete system by rotating the liquid sample valve back and forth several times.
16. Leave the adapter in position to prevent any foreign material from entering the lines and shut the helium pressurization valve off.
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METHOD NUMBER: 4 -.101 Page 3
CATCH MATTOX'S:
(X) x (Y) x attenuation - peak area X = height of peak Y - width of peak at half the height B = MVC peak area C = MVAc peak area D = TCE peak area
Percentage of components by weight:
MVC = B x 100 x RF B+C+D
MVAc- C x 100 x RF B+C+D
TCE = D x 100 x RF B+C+D
RESPONSE FACTORS:
vinyl chloride monomer x 1 vinyl acetate monomer x 1 TCE x 1.6
WRITTEN BY: D.J. Krzywicki
ISSUED BY: W. C. C1lampioji^--'' Supervisor - Quality Control
Supersedes Issue Dated January, 1975
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