Document evpeQDaY3q3nDNG1y6XgGq3Kq

M4 (SOM) INTER-OFFICE MEMO TENNECO CHEMICALS, INC To H.B. Carr AT Burlington f"om E.L. Kanyok ' AT Burlington subject Burlington Quality Control Manpower Date March 10, 1972 copy to P.R ,, Scarlto Mk- W. Williams ,/F:lie This memo is to advise you that the Burlington Quality Control testing workload has become increasingly backlogged, particu larly in the area of CRE's and special testing support. The reasons for this situation are: 1. Preparation of Columbia Records preshipment samples which is time-consuming (screening 5-lb. samples through 5 mesh screen, counting contamination and checking bulk density). 2. Pilot Plant is submitting special requests (8 to 10 weekly) for testing of packed bulk density, loose bulk density, PTU (using DOP) and PTU (using G-54). 3. Resins Group is submitting CRE*s (21 in the first J days of March) for complete analysis. Personnel 4. M. McGargile transferred to Production on 3/6/Y2 and has a 14-working-day trial period. At that time, another man will be brought into the lab who will also have a 14-working-day trial period which means we will not be up to maximum effic iency until 4/17/72. 5. In the past month, A. Gentilini was out sick for 9 days and J. Duffy for 7 days. 6. Of course, we were cut back 1 technician in mid-December, 1971 It should be noted that raw materials, in-process testing, fin ished product testing and bulk shipments have priority over CRE*s and special requests. I would recommend that: 1. PTU's, bulk density, etc. be run at the Flemington site. 2. We review current test frequency for standard products (ih-pro cess and finished products) and reduce where appropriate and if feasible. 3. Our manpower be increased to include the technician we lost in December if the addition to the budget can be approved. This man was assigned to day shift and handled most of the CRE's and special requests in addition to running testing rechecks, raw material tests' and equipment calibration check-outs. ELK/jt TENNECO CHEMICALS, INC. TENNECO INTERMEDIATES DIVISION ANALYTICAL & PHYSICAL TESTING MANUAL INDEX SECTION 300 Determination of Bound Vinyl Acetate in Vinyl Acetate/Vinyl Chloride Copolymers by Infrared Spectroscopy Determination of Residual Vinyl Acetate Monomer in Polyvinyl Chloride/Polyvinyl Acetate Monomer Method No. j500-l 500-2 4 COLOR!TE 016526 \ TENNECO CHEMICALS, INC. TENNECO INTERMEDIATES DIVISION T.A.M. 300-2 Specific Use: Burlington/Flemington Date Issued: March, 1972 DETERMINATION OF RESIDUAL VINYL ACETATE MONOMER IN POLYVINYL CHLORIDE/ POLYVINYL ACETATE MONOMER APPLICATION The level of residual vinyl acetate monomer is suspected to have a direct influence on the processability of the Copolymer. The analysis is accomplished by dissolving the polymer in tetrahydrofuran (THF) followed by precipitation with methanol, followed by gas chromatographic analysis of the supernatant liquid. The sensitivity for this method, as written, is to the 0.001$ (10 ppm) level. APPARATUS: 1. Hewlett-Packard gas chromatograph, F&M-5754A, or equivalent (equipped with a hydrogen flame ionization detector (FID) and septum covered, on column injection port). 2. Hamilton fixed needle syringe, 50 ul (Cat. No. 705N, Hamil ton Company, P.0. Box 307 > Whittier, California 90608). 3. Screw cap Erlenmeyer flask^ 250 ml. 4. Burrell wrist-action shaker (Cat. No. 21-6055, Ace Scientific, 1420 East Linden Ave., Linden, New Jersey 07036). 5. Aluminum foil. 6. Analytical balance with readout to 0. 1 mg. < 7- Volumetric flask, 50 ml. 8. Transfer pipette, 30 ml, 20 ml. 9. Graduated cylinder, 50 ml. HO 1/8" Swagelokinuts and ferrules. COLORITE 016527 \ 11. 1/8" 0D 316 stainless steel tubing. `T.A.M. 300-2 Page 2 12. 2-stage regulators for helium, hydrogen, air with secon dary gauge capacity 0-100 psig. 13. Glass wool. 14. Glass rod. 15. Evaporating disc, 200 mm diameter. 16. Vacuum oven. 17. Hot plate. 18. 60- and 80-mesh Tyler screen assembly. 19. Funnel, long stem, 75 mm upper ID. 20. Tygon tubing, 3/16" ID, 3/52" wall thickness. REAGENTS: 1. Silicone gum rubber, UCC-W-982 (methyl vinyl) (HewlettPackard, Cat. No. 8501-3840). 2. Diatoport S, 80-100 mesh (Hewlett-Packard, Cat. No. 85OI6302). 3. Methylene chloride, analytical reagent. 4. Vinyl acetate, monomeric. 5. Tetrahydrofurna, chromatoquality (THF). 6. Water, demineralized. COLUMN PREPARATION: For column preparation see T.A.M. 2-1 except use an 8-ft. length of 1/4" stainless steel tubing as the column. CONDITIONS: Column:. Carrier Gas: Air: Hydrogen: Injection Port: FID: 8-ft. x 1/4" stainless steel 10$ silicone gum rubber, UCC-W-982 on Diatoport S 60-80 mesh Helium, 47 cc/min, 50 psig in line 350 cc/min, 20 psig in line 60 cc/min, 40 psig in line 7QC 120 C COLOR!TE 016528 T.A.M. 300-2 Page 4 \ CALCULATION: (continued) ppm of residual vinyl acetate = PPm.in standard x peak height of sample peak height of standard (A typical chromatogram is shown in Figure 1.) Written By: F.W. Kanzler Issued By:________ _____________ H.B. Carr, Supervisor Quality Control COLORXTE 016529 I \ STANDARDIZATION: T.A.M. 300-2 Page 3 1. Using a 50^ul syringe, weigh approximately 15-30 mg of vinyl acetate monomer into a 5 ml volumetric flask. Record to the nearest +0.1 mg. (The vinyl acetate level should be close to the anticipated residual monomer le vel in the sample to be analyzed. The weights given above represent a residual monomer level from 3,750 to 7>500 ppm (4 gm sample). 2. Pipette 30 ml of THF into Ihe 5 ml volumetric flask. Shake well. 3. Make up to volume with water. 4. With a 50 ul syringe, inject 5jul of the standard into the gas chromatograph and attenuate the peaks as required. (The standard must be run at the same attenuation as the sample,) PROCEDURE: 1. Into a 250 ml Erlenmeyer flask, weigh 4.0 gms of sample. Record the weight to the nearest +0.1 mg. 2. Pipette 30 ml of THF into the Erlenmeyer flask. Cover with aluminum foil and cap. 3. Place the flask on the Burrell wrist-action shaker and allow it to shake for 4 hours. Make certain that the sample is completely dissolved. 4. Pipette 20 ml of water into the Erlenmeyer flask and place on the shaker for 1 hour to facilitate precipitation of the polymer. 5. After 10 minutes of standing, inject 5 ^wl of the superna tant liquid into the gas chromatograph. Attenuate the peaks as required. * CALCULATION: 1. Measure the peak height of the standard vinyl acetate peak (in millimeters). 2. Measure the peak height of the sample vinyl acetate peak. 3. Record the values from steps 1. and 2. and the ppm concen tration of the vinyl acetate standard. COLORITE 016530