Document YkG9EZr1GNZazykK0e26V55D

CELANESE ENGINEERING RES INS Bishop, Texas TO: D. A. Reck FROM: E. J. Heinz EJH-15-83 February 8, 1983 LABORATORY DEPARTMENT MONTHLY REPORT Bishop Mr. C. A. Amond Mr. W. S. Allen Mr. G. Arcripe Mr. L. L. Bennect Mr. R. G. Brandt Mr. R. L. Bunkley Mr. S. Carlile Ms. N. A. Flaten Mr. B. R. Garza Mr. L. J. Gilliam Dr. R. R. Graham Dr. R. M. Gronner Mr. C. B. Halmess Mr. R. G. Hilbrich Mr. H. W. Hill Mr. G. I. Ille Ms. P. S. Maryan Mr. A. B. Milam Mr. M. A. Purcell Ms. A. E. Retherford Mr. R. G. Rothenberg Mr. A. G. Salinas Mr. F. Soliz Mr. D. W. Steele Mr. D. L. Wallen File: 1021.1 JANUARY, 1983 DISTRIBUTION - Chatham Mr. T. C. Bohrer Dr. M, J. Hannon. Summi t. Dr. R. Dix Mr. J. Chen Central Files (3) - CCCTC 009694 -M--O--N--T--H--L-Y----S--U--M--M--A--R-Y---------J--A--N--U--A-R--YT I. SAFETY There were no accidents reported during January. A small fire resulted when a heater bar became dislodged from a one inch extruder allowing molten Celcon purge to fall .on the heater. The polymer caught fire and was quickly extin guished with a CO2 extinguisher. No damage was sustained and measures have been taken to secure the heaters. January EMS crew training centered around a review of caring for the trauma patient. II. ROUTINE ANALYTICAL GROUP A. Physical property testing on miscellaneous Summit generated samples continues with 78 sets completed in January. There are 174 sets backlogged. Samples compounded in Summit as part of the CAO-5 stabilizer replacement .study continue to be analyzed in the Bishop Laboratory. Both routine and physical property analyses are being conducted. B. The instrument lab began analyzing the fresh formaldehyde feed tanks to TO-2 daily for sodium content. High sodium levels were suspected of causing reactor conversion problems in early January. Sampling will continue until a good data base has been developed. C. Product Recovery Program POUNDS RECOVERED POUNDS RECOVERED JANUARY YTD ESTIMATED SAVINGS, YTD Celcon 6,300 6,300 2,772 Nylon 1,200 1,200 1,104 Celanex 3,300 3,300 3,201 009695 EJH-15-83 2 CELCON RECOVERY February 8, 1983 -- 31,400 ^4 S3.960 S3.520 -- S3.080 : -J S2.640 S2.200 iSI.760 i SI.320 $880 . -$440 NYLON RECOVERY 009696 EJH-15-83 I .. ____ I --"1`fr ioooch 3 CELANEX RECOVERY ------ U------- !- EM; .. t -- . . i- i February 8, 1983 hL -is? -^.TOO III. SUE ABSENTEE STATISTICS (As of 1-23-83) Head Count Straight Time Hours 26 3656 3656 Sick Hours Z of Straight Time 192 Jan. 192 YTD 5.3 5.3 Absent Other Hours 7. of Straight Time 0 Jan 0 YTD 0 0 Overtime Hours Z of Straight Time 331 Jan. 331 YTD 9.1 9.1 Jan. YTD Jan. YTD - Jan. YTD Jan. YTD 009697 EJH-15-83 -4- February 8, 1983 1983 SNE ABSENTEEISM YTO STATISTICS 0- Ovrtlo A- Absent Ocher Hours a - sick Hour* IV- SAMPLE COUNT AND OVERTIME DISTRIBUTION - SaLinas The sample count for both the Specification and Color Labora tories for January is summarized on Tables I and II. The total laboratory sample count, Specification Laboratory sample count and the Color Laboratory sample count are graphed on Figures I, II and III respectively. The overtime distribution for this month and the Calcium Fluoride (CaF2) inventory are shown below: January Overtime Distribution ECA Training Safety Meeting Vacation Sick Leave Instron Evening Relief Work Load 10 8 64 106 104 88 17 397 009698 EJH-15-83 -5- February 8, 1983 NYLON NUCLEANT PRODUCTION INVENTORY ' --' "` m..,,-- i.i ,- Raw Macerials *f Potassium Fluoride Calcium Ac~<;ate 64 drums (32,000 lbs.) 65 drums (33,735 lbs.) Nucleant (CaF2) In Process (CaF2) 13 drums 17 drums V. PERSONNEL A. Mr. R. de Vaudrecourt returned to work from sick leave January 20, 1983. B. Mr. B. Garza, Laboratory Supervisor received his 15 year service award. C. Ms. Lucy Lopez and Ms. Sarah Perez were hired as Laboratory Technicians effective January 3, 1983. VI. SPECIAL PROBLEMS GROUP - R. G. Hilbrich 1. Process Analyzers - Allen, Cunningham r Specifications for the analyzers will be completed in early February. Analyzer house and sample system specifications will follow and should be ready in early March. 2. Analysis of Nylon Salt in Effluent - Allen A new analysis for nylon salt levels in the effluent is being investigated. This procedure combines a non aqueous and an aqueous titration to determine HMDA and salt concentra tion. Work continues. 3. Trioxane Reactor Monitoring - Gronner The first TO-2 reactor laboratory stripout following the mid-December start-up was done after four weeks of operation. Tar level was predictably low, at <0.1 wt.Z. A second stripout is currently underway. Reactor monitoring this month also included Na analyses of the reactor contents and HCHO feed tanks. High Na was the suspected cause for reactor conversion problems. Analysis showed 2300 ppm Na in the reactor on January 4 and 3700 ppm Na on January 28. Analysis of HCHO feed tanks showed 5-10 ppm Na early in the month. After CCC replaced their ion exchange resin bed for MOIV on January 18, the level dropped to 1-5 ppm, and when the MDII resin bed was re placed by CCC on January 25, Na levels dropped to <0.1 ppm. The reduced Na in the feed will greatly ''educe the rate of Na accumulation in the reactor. 009699 EJH-15-83 -6- February 8, 1983 4. Finished Trioxane Stability - Gronner A project was initiated to determine the necessity for adding 0.57. water to finished Tox, destined for sales, as a polymerization inhibitor. A literature search turned ap a 1965 CCC lab report (LD-7089-JMR) which showed that anhydrous Tox built up *2.5Z polymer in 24 hours, while Tox stabilized with water showed <100 ppm polymer. These experiments were repeated in the lab to determine polymer build-up rates in Tox which has under gone two-stage finishing. After 24 hours, the "stabilized" sample had 107 ppm polymer, while the anhydrous sample had 1120 ppm. In addition, a 3% month old anhydrous sample had 2460 ppm, while an 11 month old "stabilized" sample had only 260 ppm. While the two-stage finished Tox appears to polymerize less, water addition still improves stability. A report will be issued. 5. Analysis of KoKneader Contaminants - Gronner, Halmess Natural Finishing developed a problem with off-color pellets in M90-04 product from the KoKneader. Examination of the unit found light brown fines in the pellet water system, and dark brown material in -the pellet dryer. These materials were analyzed in the lab. The light brown material was identified as Celcon fines, by IR and HCHO determinations. The dark brown material was found to be mostly Acrawax C. A report is being written. 6. Analysis of Irg-259 in Celcon - Gronner Samples were collected around the KoKneader Crosshead extruder, during a C244 production run, for an Irg-259 material balance. Three samples each of product, C-244 rerun, and stabilizer blend were taken. The average Irg259 contents found were 0.48Z in product, 0.49Z in the rerun, and 16.3Z in the stabilizer blend. This data, along with the measured flow rates, yields 96Z accountability of the Irg-259 across the extruder. Because the percent Irg-259 in the stabilizer blend was low (20Z was expected), current work involves confirming the accuracy of this number. 7. CAO-5 Contamination in Irganox 259 Based M90-04' - Purcell The products produced in Special Products, to study the effects of CAO-5 cross contamination in Irganox 259 based M90-04 products, have been analyzed and the results compiled. Mold deposit levels increase as the CAO-5 contamination concentration increases. Thermal analyses results show Irganox based polymer thermal stability decreases as CAO-5 contamination increases. GPC results show smaller Mw increases after Kd as the CAO-5 level increases. It was recommended that 0.1 wt.Z CAO-5 be set as a limit in Irganox 259 based pioducts. 009700 EJH-15-83 -7- February 8, 1983 8. Irganox 259 Replacement: for CAP-5, Rerun - Regrind Studies - Halmess ' Twenty-four rerun and regrind study samples prepared in Summit were analyzed for moLecular weight, color, Kd, extractable HCHO, and melt index. The study was to compare rerun and regrind stability of CAO-5 and Irganox 259 based M90-04 products. The results did not indicate any problem in rerun or regrind stability due to the use of Irganox 259. A report was issued (CBH-1-83). 9. MH/SH Ratio - Maryan A study is underway to determine the maximum acceptable level of MH polymer in -04 products. Data from previous studies was compiled and evaluated for trends between routine analytical, mold deposit, color stability, special analytical and the level of MH polymer. Current laboratory work involves determining the effects of MH level on initial color, color stability and mold deposit. 10. Head Space Analysis - Maryan Samples of M90 polymer-from the polymer units are being analyzed by headspace analysis for Trioxane and Tetroxane levels. The initial results confirm that MH polymer has a higher level of Tetroxane and a lower level of Trioxane than SH polymer. Work continues. 11. Thermal Analysis - Purcell Isothermal TGA is being used to evaluate Irganox 259 based Celcon products. Present work involves analyses of various stabilizer packages for Color Services. Current work is also under way to study oxidative stabilities using a reduced purge gas flow rate. Work continues. 12. Thermal Analysis Instrumentation Evaluation - Purcell Several manufacturers of thermal analysis instrumentation were evaluated in the Bishop Lab. Our present Mettler TA 3000 system was designed primarily to perform routine analyses which require minimum data manipulation and reduction. The Perkin-Elmer and Dupont systems offer increased operational capabilities and flexibility, auto mated data analysis, data storage, and the ability to optimize data presentation. Numerous applications have been identified for polymer monitoring and additive analyses. Purchase of the Perkin Elmer TGS-2 TGA module along with the TADS Data Station will be recommended. 009701 EJH-15-83 -8- February 8, 1983 13. Effect of Rerun on Celanex 3300 Natural - Halmess A trial was run on Phase I on January 3-4 while producing Celanex 3300 natural. The objective of the trial was to determine what effect the addition of dried start-up material had on the physical properties of Celanex. The results of the trial indicate that feeding 20Z dried (<0.1 wt. 7. volatiles) rerun does not decrease physical properties. Throughout the trial the tensile values for the Celanex 3300 remained above 19,200 psi, which is ^1,400 psi higher than the 1981 yearly average. A report will be issued. 14. Celanex 3300 Black for Delco Electronics - Halmess During January a production run of Celanex 3300 black was made on Phase I for Delco Electronics. The melt rheometer results of the two railcars produced were above the specification of 3,000 poise minimum. Since there has been some difficulty meeting the melt rheometer specifica tion, the conditions during this production run were compared to previous production runs. Two differences noted were that during the current production run a slower screw speed was-used (70 vs 'WSppm) and a lower feed rate was used (3,200 vs. ^3,600 Ibs/hr). A trend in the analytical results was also noted. Railcars that had a tensile value above 18,500 psi typically passed the melt rheometer test while railcars with a tensile value below 18,500 psi failed the melt rheometer. A report will be issued. 15. EPA Toxicity Testing of Pigments - Flaten The results of the toxicity testing were received from Core Laboratories. The results of the testing show that when the pigments are encapsulated in polymer they are no longer classified as hazardous waste. A report discussing these results is being reviewed. 16. Nucleant Contamination in Non-nucleated Nylon Analysis - Flaten A method for screening nucleant contamination in non-nucleated natural nylon formulations has been developed. Significant interferances were found to occur in black formulations. The method is an AA determination of Calcium levels. Several attempts to overcome these interferances were studied. None gave satisfactory results so the method was deemed unsuitable for black formulations. Alternative methods for determining nucleation contamination in black formulations will be investigated. 009702 EJH-15-83 -9- February 8, 1983 17. Raw Material Program - Flaten t A program is being implemented to review each raw material used at CER. Required specifications, testing procedures and testing frequency will be determined for each raw material. VII. INDUSTRIAL HYGIENE - Pritchard 1. CER Monitoring Program The CER Industrial Hygiene Monitoring Program has been revised for 1983. Quarterly surveys will be conducted in each area for each contaminant found in those areas. This will result in better documentation of exposures due to variables in operational procedures as well as environ mental conditions (changes in wind direction, temperature, etc.). Previously "Block" sampling was used to documenc exposures in particular units over shorter periods of time. First quarter emphasis will be on formaldehyde monitoring as part of the Phase I formaldehyde reduction program. 2. Formaldehyde Monitoring Personnel in the SH-1/T0-1, SH-2/T0-2, and MH-2 units have been monitored for formaldehyde exposure. Additional monitoring will be conducted in these as well as other units with a potential formaldehyde exposure problem. 3. Asbestos Monitoring in Filled Resins Area Asbestos monitoring has begun in the Filled Resins Area in order to determine potential areas or tasks requiring the use of protective equipment and/or administrative controls Additional monitoring will be conducted in this and other areas where asbestos are used. 4. Number of Monitoring Samples by Area Month YTD SH-1/T0-1 SH-2/TO-2 MH-2 Special Ppoducts Black Concentrate Unit Natural Finishing Filled Resins Laboratory ABI 4 4 3 4 4 3 TOTAL 14 14 009703 EJH-15-83 -10- February 8, 1983 VIII. L--A--B--O--R--A--T--O--R--Y----P-R--O--J-E--C--T----A--S--S--IG---N--M---E--N--T-S-Project Tide <( Chemist Estimated Project Completion Date TO Process Analyzers Nylon Salt Effluent Analysis Allen, Cunningham Allen 6/1/84 4/1/83 Trioxane Reactor Monitoring Gronner Trioxane Stabilization Gronner Extractor Reactor Process Evaluation Gronner Analysis of Irganox 259 in Celcon Gronner As required 4/1/83 1/1/84 4/1/83 CAO-5 Contamination in M90-04 Purcell Thermal Analysis Method Development Purcell New Instrument Evaluation Purcell 2/1/83 9/1/83 1/1/84 MH/SH Ratio Study Maryan Irganox 259 Replacement of CAO-5 Maryan Headspace Analysis of Celcon Polymer Maryan 4/1/83 4/1/83 6/1/83 Celanex Physical Property Decline Gel Permeation Chromatograph Halmess Ha lines s 9/1/83 6/1/83 Raw Material Program Nucleation Contamination in Nylon Flaten Flaten 1/1/83 7/1/83 1983 Environmental Monitoring Pritchard 1/1/84 EJH/lat Attachments >X.i Heinz 009704 n o<To> > U J 3 (C0 x H OZ 2 >oz* oH 2 oCQ (X o cj O< w&J4 cn owCCOU oW u cm on -T <0n) icWao rU(40 e 009705 CER COLOi '"'ORATORY SAMPLE COUNT MONTH J a n u a ry , 1983 13,000 12,000 ...... 11,000 --10,000 9,000 8,000 7,000 6,000 5 ,000 4003 CER LABORATORY TOTAL SAMPLES 1 983 _________ Figure I 1982 AVERAGE AM 009707 S0N 0 cir jpzc:: [CATION LABORATORY TOTAL SAP.PL L2S.3 9,000 ---------------------- ------------------------- -------- 8,000 -- 7,000 - 6,000 - ' . ......... -"-1982 AVERAGE- ::: - -- 5,000 ---------- --------- ---=-'------------- _ A,000 3,000 --2,000-- ---------------------------------1 ,000 -- -- - ------- - 0 ) 009708 0 CER COLOR LABORATORY TOTAL SAMPLES ___________________ L3&J___________________ Figure 9,000 - 8,000 7,000 ..I_____ l_ 6,000 5,000 - 4,000 --------------------- !-- --,------- L -i-- :{=: -A-- ....... i - '982 averagb- 3,000 2,000 1,000 FM 009709 S ID