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CELANESE CHEMICAL COMPANY Chemcel Plant Bishop, Texas PLAINTIFFS | EXHIBIT I CEL-236 To: C. W. Harrison From: W. H. Meyer' WHM-19-77 February 16, 1977 Laboratory Department Summary January, 1977 DISTRIBUTION C h e m i cal J. H. Frick G. D. Boyd W. J. Derocher T. N. Dowdy H. A. Ducote K. G. Gallimore M. D. Harvey J. M. Hodges M. A. John B. C. Kerr C. W. Lee Dr. C. E. Loeffler Dr. R. P. Lowry W. W. Massey J. T. McMahon R. A. Mickelson J. M. Sawyer G. R. Scholz G. C. Seaman W. L. Sharp R. W. Swanbeck O. Towery P. J. Volpe J. D. Walker 002950 J. N. Gann - Bay City J. W. Dunn - Clear Lake J. M. Ramey New York Dr. J. C. Trebellas - New York J. E. Sanborn - Bayport Termin W. H. Tuke - Pampa F. B. McAndrews - Summit Dr. F. Zitomer - Summit Plastics J. L. Merian A. C. Abshier C. A. Amond W. C. Beyer R. L. Bunkley E. Munoz C. S. Schmaltz CCCTC W. E. Heinz Dr. C. C. Hobbs W. J. Humphrey W. T. McNair Dr. D. R. Napier Dr. L. Starr W. E. Taylor > / Central Files (2) File: 716. 0 CELANESE CHEMICAL COMPANY Chemcel Plant Bishop, Texas To: C. W. Harrison From: W. H. Meyer WHM-19-77 February 16, 1977 Laboratory Department Summary January, 1977 Bishop Plant Laboratory activities during January are attached. Section I contains a summary of the Analytical Group activities with a table of analytical and sample shipping statistics. Section II contains a Quality Assur ance Summary and a table listing shipments, quality waivers and quality complaints. Section III describes the status of Special Problems Group projects by Unit Chemist assignment. A table listing the priorities, justifications'and estimated completion dates of current Special Problems projects is also in cluded in Section III. WHM/jm Attached Report W. H. Meye^ 002951 WHM-19-77 -2- February 16, 1977 I. ANALYTICAL GROUP Competitive Evaluations: A sample of tech grade PE obtained from Mobile Chemical Co. was analyzed and compared to typical Chemcel production. The manufacturer is unknown, but Mobile stated a preference for this material in their use. Major differences observed were a higher di-PE content (10. 0 versus 7. 5 Chemcel average), and a smaller particle size (12% through 200 mesh versus 4-6% Chemcel average). Polyol TMP - Analytical support was provided for a trial, five-day, loss accounta bility study in the TMP unit. The additional work load of approximately 10 analyses per day was absorbed by the Group. Base case data was again generated (TMP reactor and T-202 column) for the proposed increased formaldehyde feed concentration trial. This project has been delayed due to a shortage of inventory) A Sartomer Chemical Co. method for benzene-sulfuric acid wash color was applied against TMP lot retain samples. Potential customer specification (Sartomer and Ware Chemical Co. 's) of 10 max. Gardner color units was not met by our product. Results of 12 lots checked ranged from 11-15 Gardner units. Ware Chemical Co. has been sampled with our typical product for their evaluation. 1,3-BG - Extensive analytical support was provided for the determination of the acetal impurity in our 1,3-BG product (100 hours technician overtime). An inordinate level of acetal make in hydrogenation was carried through to the finished product. Methodology firm-up is underway while the unit is down. Coverage will be provided for startup. DAA - Analysis was provided for reactor samples as part of the ongoing study for optimization of acetone conversion. Variation of reactor temperature (current study) was interrupted for sales demand. PE - Typical tech grade and pure grade PE product was checked against Ash land Chemical Co. special specifications for Melt Color and Phthalic Ester Color. Their spec = 1 max. Gardner units. Results of the testing indicate that we do not routinely meet these parameters. We have requestedAshland's evaluation of our product. 002952 WHM-19-77 -3- February 16, 1977 Paraform n-Butyl Acetate - TOC analysis was provided for water layer samples around T-103, the alcohol recovery column. This is preliminary to column optimi zation studies currently being considered. Trioxane - Customer complaint spotlighted benzene contamination in our pure grade TO product. Contamination has been quantified on all production back to and including November, 1976, and recall of customer inventory is under way. Temporary quality control procedures are allowing the packaging of replacement material while purchase specifications and equipment modifica tions are being expedited. The contaminations apparently occurred through leakage into transfer vessels and/or lines at the Plastics Co. production point. Then current methods of analysis at the Chemical Co. packaging level gave no indication of benzene. Benzene determinations are being made both before and after each transfer of TO product with a temporary specification of 10 ppm max. Sharing of analysis equipment and time have resulted in some loading delays and extensive manpower is required to monitor around-the-clock loadings, (85 hours technician overtime to date, with more expected). 'Oxo BuH/BuOH The change-over of one Corpus Christi terminal transfer line and tank from MeOH to n-BuOH service was effected this month. The first barge load of n-BuOH has been shipped with no apparent quality problems. Product mix and cutoff points were monitored via G. C. procedure with approximately 19 hours technician overtime involved. MS Unit Analytical assistance was provided for 4 column profiles this month on towers T-280 and T-288. A recurring low permanganate time problem is the main object of the search. ( Utilities-BOD Anaerobic Study - Additional effluent and/or process streams added to the list of those being composited for CCCTC study feed are: back ditch effluent and V-1331 overhead. Sample handling, compositing and analysis requirements are presently requiring 2 manhours per day from the Analytical Group. First samples of the system product returned from CCCTC indicate good conversion from the anaerobic filter. 002953 WHM-19-77 -4- February 16, 1977 Ge ne ra1 Recurring operation problems with the Instrument Lab computer have necessitated the loan of spare parts from the Tech Center. These will be returned as soon as ours can be repaired or replaced. A computer (EAI) representative will be requested to aid in pinpointing and solving our problems. See attached Analytical and Sample Shipping Statistics: I 002954 WHM-19-77 -5- February 16, 1977 Analytical and Sample Shipping Statistics Sample Count Chemical Section Samples Instrument Section Samples Total January 4,460 2.235 January Y-T-D 4, 460 2.235 Previous Y-T-D 3, 773 2.067 6,695 6,695 5,840 Overtime Technician Overtime: Chemical Instrument Total 69 140 209 69 140 209 32 28 60 Sample Shipping: Domestic Export Plastics Other Total NA* NA NA NA NA NA NA NA * NA= Not currently available. Will be included next month. 96 2 6 21 125 002955 WHM-19-77 -6- February 16, 1977 II. QUALITY ASSURANCE Methylal - Methylal storage inventory is borderline to off-test on water (spec is 1.5% max.). The methylal in TK1492 was over 3.0% water, and high in aldehydes at 0. 30% (spec 0. 10%). A tentative reprocessing run is scheduled for the current inventory of methylal while the acetate unit is down. Methanol - A water problem developed in our MS-II methanol inventory during the third week of January and the first week of February. No assignable cause was evident. Tank 386 had 0.36% water and tank car loadings were made out of MO inventory. The water level is now down to 0.02% . 1,3-BG - Efforts are being made to bring the purity of the product back to the 99. 5+%, Complaints - The major valid complaint during the month was from Van Brodie regarding benzene in TO. Replacement of the TO at Van Brodie is over 70% complete. All of the Sylvannia Delkit material has been re placed and we have since filled another order to Sylvannia. Formaldehyde Blending - Blending inhibited formaldehyde continues to be a problem because of problems with the in-line blender. Three out of seven inhibited blends were missed during the month, causing resampling, adjustment followed by resampling, and increased truck demurrage. We consider this to be a continuing and serious problem, which could affect product quality since we make calculated adjustments in the shipping con tainer. Engineering is working on the request to replace the blender. See attached Quality Assurance Statistics: 002956 WHM-19-77 -7- February 16, 1977 Quality Assurance Statistics Shipments (Number of Orders) Delayed Shipments Quality Waivers Quality Complaints Quality Complaints Accepted January 843 4 2 4 1 January Y- T-D 843 4 2 4 1 Previous Y- T-D 612 4 0 2 2 002957 WHM-19-77 -8- February 16, 1977 III. SPECIAL PROBLEMS GROUP Methanol Oxidation, Formaldehyde Blending A. J. Branecky MO Efficiency Improvement with Trace Amounts of Halogenated Hydrocarbons - Preparations for the plant trial continue. Testing should begin in 2 - 3 weeks. MO New Catalyst Screening - A sample of Matthey-Bishop silver needles has been evaluated. The silver appeared acceptable for MO use based on sinter test, particle size, bulk density, purity and micro unit performance. A plant trial has been recommended as the next step in qualifying MattheyBishop as an approved supplier. Handy and Harmon's analytical method for copper in silver catalyst was evaluated and found comparable to the Celanese method. MO Catalyst Reuse - Contaminated silver catalyst from MO-III was subjected to four treatment schemes to attempt cleaning or regeneration of the catalyst. The contaminated catalyst performed at 87. 8% efficiency in micro unit test ing. Treatment and the resultant micro unit efficiency of the treated silver were: 3% HN03 for 2 minutes - ' 89. 5% 3% HC1 for 2 hours - 90. 3% 5% AgN03 for 18 hours - 90.6% Demineralized H20 wash - 90. 6% A complete reactor charge from MO-IV was washed with demineralized water in the lab. Before the catalyst was removed from MO-IV, it performed at 86% efficiency. After water washing the catalyst and placing it back in service in MO-IV, it performed at a level comparable to new catalyst. After 2 1/2 weeks on line, 89. 5% efficiency was demonstrated. MO Analytical Manual - The manual is complete and will be issued in the near future. MS-II Crude to MO - Work will begin now that MS-II has essentially reached steady state operation. MO-Support - Samples of MO-II catalyst were analyzed after an extended run. (One catalyst bed had been on-line for approximately 8 months. ) The catalyst showed relatively low levels of impurities compared to catalyst from MO-III and MO-IV that generally had been on-line a shorter time. This follows his torical data that shows MO-II can run longer without efficiency loss due to contaminated catalyst. 002958 WHM-19-77 -9- February 16, 1977 Efficiency losses in the MO-IV absorber were examined with the unit operat ing in a high concentration run (>52%). No significant increase in efficiency loss was observed. Pentaerythritol, Weak Formaldehyde H. H. Thigpen PE Efficiency - Unit efficiency for January was 75. 9% based on AcH versus a stretch objective of 73% for 1977. This was in spite of a power failure on January 2 7, which appeared to cause PE losses equivalent to 15-20 M lbs. The relatively high efficiency for January can probably be attributed to: a) The absence of major mechanical problems b) Continued satisfactory operation of the dam on the "A" filter c) Higher "A" evaporator gravity and better stripping of for maldehyde in T-2 86 than was typically maintained in 1976. Continuing laboratory studies of the effect of variables on efficiency during the "A" evaporation and crystallization steps have indicated that there is a maxi mum efficiency which can be approached by manipulation of these variables. This maximum efficiency is about 78% during pure production and may be as high as 84-85% during tech production. Studies of the tech PE system are continuing and will be completed in February. The maximum efficiencies are obtained when the crystallization drop temperature is 70 F, and the evaporator gravity results in 32-33% sodium formate in undiluted AML. Results of the lab study will be published, with recommendations, in March. The economic potential of maintaining better control of the gravity and temper ature during the "A" crystallizer process is 2 - 4% efficiency. Data from current studies indicate that impurities (primarily cyclic formals) significantly increase the solubility of PE in AML, and that the impurity level controls the maximum efficiency attainable in the unit. This could explain why the efficiency during tech production is significantly higher than during pure production. More cyclic formals are present during pure PE production since more of the linear formals are hydrolyzed to meet purity specs. Continuing studies will attempt to confirm and quantify the effect of cyclic formals on efficiency. If confirmed, studies of the hydrolysis step to minimize cyclic formal production will be initiated. If this is not successful, methods of re moving cyclic formals from the "B" mother liquor will be studied. The economic potential of minimizing cyclic formal formation may be equi valent to an additional 5 - 8% efficiency during pure PE production and 2 - 3% during tech production. 002959 WHM-19-77 -10- February 16, 1977 Low Sulfate PE AML Sodium Formate - No laboratory work. PE "Fines'1 Problem - The production of "fines" in pure PE is being studied. A report with recommendations will be written this month. Methanol Synthesis _________F. R. Dow Fuel Gas Quality - Fuel gas quality has remained relatively unchanged during January, even though it was sampled twice during extremely cold weather. The Process Analyzer group has installed an on-stream Bendix Total Sulfur G.C. to monitor total sulfur in incoming fuel gas. Preliminary analyses have shown approximately 600 ppb total sulfur. The fuel gas to the MS carbon beds shows the total COS, H2S and S02 to be approximately 400 ppb. MS-II Analytical Support - Tower profiles of T-280 and T-288 were analyzed several times during the month in an attempt to monitor the fusal oil band and to obtain data on upper and lower drawoff streams. Analysis has shown that an upper drawoff may not be necessary to maintain the permanganate time spec, but lower drawoff of approximately 0. 8 gpm is necessary for removal of PrOH, s-BuOH, iso-BuOH and n-BuOH. This investigation was also attempting to quantify the by-product make of Lurgi catalyst. Due to the extremely low con centration of impurities in crude MeOH, direct analysis yields unreliable data. Future work should include a lab distillation of crude MeOH to accurately de termine by-product components and concentration. A report will be written showing all purification tower profile data. Esters, Methylal, Paraform, Formcels R. G, Hilbrich Methylal Build in Methyl Formcel - A new study has been initiated to determine if aluminum 6061-T6 in methylal Formcel storage causes increased methylal formation. In an initial study, the test samples were mistakenly destroyed. The original samples had shown no methyLal increase in 2 1/2 months contact with aluminum 6061-T6. Paraform Material Balance - Progress on this project is delayed due to the current lack of Process Engineering coverage on paraform. 002960 WHM-19-77 -11- February 16, 1977 Ester Unit Support - A recent n-butyl acetate run used n-butyl alcohol from T-67 and T-101 residue streams of the butyl alcohol unit. The run was closely monitored analytically by the Laboratory. No problems were en countered. Samples around the ester unit water recovery column (T-103) were analyzed in support of a Process Engineering project to determine the justification for continued operation of T-103. Alternate n-Butyl Acetate Process - Results of the latest laboratory run show 99% one pass conversion to n-BuAc based onHAc feed. Reactor column residue product analysis showed 0. 5% acetic acid, 4. 3% BuOH and approxi mately 94% n-BuAc by difference. Work continues in an effort to reduce acetic acid-concentration in the product. Paraform, Formcels and Ester Unit Analytical Manuals - No work due to priorities. Oxo, 1-Butanol, 1-Propanol A. J. Bacon Oxo Reactor Accountability - Through a continuous extraction procedure, a large portion of "unknowns" were separated from Oxo catalyst solution. It was approximately 85% P, M. W. TPP and contained 60:40 aliphatic to aromatic hydrogen. It was undoubtedly a mixture. Some progress has bee-, made in detection through thin layer and infra red methods. This work con tinues as time permits. PrOH Material Balance - No balance done. However, a loss analysis was : to try to explain low yield accounting efficiencies. All losses were norma.. Process traced the problem to lack of temperature compensation. The Lao worked with Production and the Computer group to finalize implementation : temperature compensation data into yield accounting. - T-229 Residue Aldol - No progress due to priorities. Aldol make remains * T-210 Residue Burning - Letter covering lab work on No. 1 boiler scale , completed. Similarities with residue at Bay City from a phosphorus con taining stream were reported. Oxo, n-BuOH, n-PrOH Unit Support - a) Reassay of catalyst ash from the July 6, 1976 dump was completed. Results showed 3. 95% rhodium as compared WHM-19-77 -12- February 16, 1977 to the 3. 68% originally found. No reason for the discrepancy in known. Engelhard and Celanese have settled on the 3.95% value. A report was written. b) Sample bombs were prepared and sent to Clear Lake so that our lab can check the quality (chloride) of CLP pipeline propylene which may be used here for Oxo. c) Spec tests were begun on T-133 overhead as part of steam savings project in BuOH. Tr imethylolpropane D. W. Harris TMP Unit Analytical Manual - Revision of the TMP unit analytical methods manual is in progress. Increased Formaldehyde Feed Concentration to the TMP Reactor - The plant trial planned for January was not conducted. The unit operated at approximately 40MM rates and 25% formaldehyde feed concentration. The trial will be conducted after rates are reduced. TMP Daily Carbon Accountability - A plant trial of the carbon accountability procedure outlined in JRK-01, JWH-09 was conducted January 23 - 27. Carbon accountability for the 5-days averaged 102.2%. A report estimating the cost for implementing the procedure, and results of the trial will be issued. TMP Unit Support - Analysis of V-1331 overhead (NaFo concentrator) samples showed 0.8 wt. % ethyl acetate and 6 ppm Na+. Process Engineering is eval uating the feasibility of using this stream as make-up condensate to T-204 (solvent recovery column). A report is in progress. T-206 Receiver and V-759 Vent Emissions - Sampling of T-2 06 receiver vent has been delayed. Plans are to pipe the vent into the TMP concentrator (V-759) vent line. The combined vent will be sampled after piping is completed. 1,3-Butylene Glycol J. W. Hermann 1,3-BG Daily Carbon Accountability - A report on the results of a plant trial and estimated cost for implementation is in preparation. 002962 WHM-19-77 -13- February 16, 1977 1.3- BG Efficiency - Measurement of crotonaldehyde produced in V-1478 is underway to determine if there is significant efficiency loss due to residence time and temperature. 1.3- BG Unit Analytical Manual - No work due to priority given to unit support. 1.3- BG Unit Support - The unit experienced several major upsets between January 15 and 20, 1977: loss of air pressure, low 240 psi steam pressure, and loss of hydrogenation catalyst. These upsets resulted in an unusually large amount of the cyclic acetal of 1,3-BG and acetaldol in the hydrogenation system. The BG finishing system is unable to remove this impurity due to T-22 7 overhead recycle of BG light ends. On January 19 the finished product contained >1% of the acetal impurity. The unit broke the T-227. overhead recycle to remove the acetal and was correcting hydrogenation problems when a shutdown became necessary to reprocess off-test inventory. The Laboratory will continue to closely monitor the finished product when the unit is restarted. Special Problems will continue to monitor acetal make in the hydrogenation system, and assist operations in minimizing acetal production. Utilities Raw Materials BOD ________M. F. B~rady Purchase Specifications Update - A major revision in the format is under con sideration.' Work continues. Demineralizer Support - The plugged caustic distribution laterals in the weak anion resin bed were cleaned. The unit produced good quality water when put back into service. The material which plugged the laterals was identified as resin fines from the'strong anion bed. The unit has increased the backwash frequency of the strong anion resin bed to reduce fines carryover to the weak anion distribution laterals. As followup to this problem, the Laboratory showed the capacity of the weak anion resin to be acceptable. The triethyl amine demand of the demineralizer was determined at the request of Celcon. The triethyl amine demand was within acceptable limits. Utilities Support - Assistance was provided to the Utilities Department in im proving the test method for 02 in boiler feed water. Problems in obtaining consistent results proved to be technique related. A permanent sample tap was installed and procedural problems were corrected. 002963 WHM-19-77 -14- February 16, 1977 A method was developed by A. E. Retherford for determining ammonia (ppm) in front ditch (001) outfall. A report will be written. Evaluation of Rohm and Haas IRA-94 for Formaldehyde Service - No progress due to priorities. BOD Unit Analytical Methods Manual - Revision of test methods have been written. A report is in progress. Anaerobic Pilot Testing Of Chemcel Waste Streams - Sampling of effluent streams has proceeded rela tively smoothly. The CCCTC Anaerobic Pilot unit was started January 6, 1977, and required eleven days to acclimate to 100% Chemcel feedstock. The system has operated smoothly since then. The aerobic polisher is operational and is in the process of acclimating to anaerobic outfall. Addition of Betz Neutrameen To the Plant Steam System - The Laboratory cooperated with Operations in locating sample points. A report has been issued describing the location of these points and sample schedule. Methods for determining amine levels in the steam system have been set up. Particular attention will be given to areas in which live steam contacts process streams. OSHA Monitoring J. M. Jackson The following personnel were monitored for 8-hour TWA exposure to benzene: Laboratory Janitor Technician Technicians (3) Technician Solutions prep, room, Main Lab Solutions prep, room, Main Lab Wet Analytical, Plastics , Main Lab Wet Analytical, Chemical, Main Lab Area benzene samples, 8-hour TWA, were obtained in the Solutions Prep room, Main Lab, and in the Plastics Company area of the Wet Chemical Section (Main Lab). The space velocity of all Main Lab hoods was determined. Out of 9 hoods, only 3 were capable of lowering employee exposure to airborne contaminants to approximately 1 ppm. A report will be written recommending corrective action. 002964 WHM-19-77 -15- February 16, 1977 Diacetone Alcohol A. E. Retherford DAA Unit Support - T-2 95 was opened for maintenance inspection, and the trays were found to be fouled with a fine, grey powder. Elemental analysis of the material showed 15.2% Ca, approximately 2.02% Fe, 1.2% Na, and approximately 4% P. The material also gave a positive carbonate test. T-2 95 had been showing abnormally high pressure drop. Reboiler and overhead con denser leaks were also suspected due to abnormally high water levels in T-295 overhead product. From this information the powder was concluded to be pre dominately CaC03, Na2C03, Ca(P04)2, and Na3P04. Source of the Ca and COf was probably cooling water and/or DAA catalyst. The Na+ and P045 proably came from cooling water. Reoccurrence of the problem is not likely since the new DAA catalyst charge has aged in, and the T-2 95 leaks have been repaired. The powder was removed by water blasting. DAA Reactor Temperature and Residence Time Study - A plant trial to deter mine the effects of temperature and residence time on the DAA reactors was begun January 2 5, 1977. The reactor (V-1266) was allowed to line-out at 80 ppm recycle rate and 70-72 F outlet temperature. Recycle was then cut to 40 gpm while holding the outlet temperature 70-72 *F. Plans were to follow conversion to DAA and MesOX make through these changes, then lower the reactor outlet temperature to 65-67F to determine the effect of reduced tem perature on conversion to DAA and MesOX. At this point refrigeration machine failure caused a unit shutdown. The study will resume when the unit is restarted. Miscellaneous B. C. Kerr Trioxane Quality - Customer Service Call - A customer service call was made to Van Brodie in Clinton, Mass, to help resolve a quality problem with trioxane. Laboratory work had shown that most of the trioxane shipped to Van Brodie was contaminated with benzene. The visit to Van Brodie on January 12 and 13 showed a more serious contamination than had been seen in plant retain samples. A discussion between Van Brodie personnel, Gary Kastor and Bob Kerr con cluded that the only safe solution to the customer's problems was to replace the contaminated trioxane with specification product. A full discussion of the service call is given in BCK-02-77, January 20, 1977. 002965 WHM-19-77 -16- February 16, 1977 Perstorp Formaldehyde Stabilizer Problem - Perstorp licenses the Celanese formaldehyde solution stabilizer to European customers. One of their cus tomers has experienced problems with ion exchanging stabilized formaldehyde from the ion exchanged product. A letter was written to Perstorp (BCK-04-77, January 28, 1977) recom mending a methanol wash to remove stabilizer from the ion exchange bed. However, the foaming problem associated with distilling resins was outside plant knowledge. Mr. J. M. Ramey was requested (BCK-03-77, January 28, 1977) to provide any data for foam control that the company can, without vio lation of confidentiality. Ester Unit Statistical Data for the November and December, 1976, Butyl Acetate Production Runs - A letter is being typed which gives a detailed examination of the unit data for the subject production runs. 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