Document 4YNn8ppn79R1yeLr3V896q0x
CELANESE CHEMICAL COMPANY Chemcel Plant Bishop, Texas
To: C. W. Harrison From: W. H. Mever - AT
WHM-380-80
PLAINTIFFS EXHIBIT
CEL-256
April 8, 1980
Chemical
P. E. Hime G. D. Boyd W. H. Brough R. R. Carpenter J. Chervenka K. G. Gallimore B. P. Hanson M. D. Harvey J. M. Hodges R. W. James B. C. Kerr C. W. Lee D. E. Lockwood Dr. R. P. Lowry A. G. McGehee D. G. Pausky G. R. Scholz D. D. Siemonsma W. L. Sharp H. H. Thigpen P. J. Volpe
DISTRIBUTION
Plastics
A. C. Abshier R. G. Brandt R. L. Bunkley H. L. Davis H. W. Hill E. Munoz
CCCTC
G. J. Fisher W. E. Heinz W. T. McNair Central Files
(2)
J. N. Gann J. E. Sanborn J. W. Dunn T. H. GoIson A. J. Branecky W. H. Tuke F. B. McAndrews Dr. J. Zitomer
Bay City Bayport Term: Clear Lake Dallas Edmonton Pampa Summit Summit
003332
\e: 716.0
APR 23 80
CELANESE CHEMICAL COMPANY Chemcel Plant Bishop, Texas
To: C. W. Harrison From: W. H. Meyer
WHM-380-80
April 8, 1980
Laboratory Department Summary March, 1980
A summary of each Groups' Monthly Report is attached. Section I contains a summary of the Quality Assurance and Analytical Group Activities with tables of analytical statistics, shipments, quality waivers, quality complaints and sample shipping statistics. Section II describes the status of Special Problems Groups and Staff Chemist projects by Chemist assignment. A table listing the priorities, justifications, estimated completion dates of current Special Problems projects and a graph of the Laboratory Effort Analysis is also included in Section II.
WHM/as Attached Report
003333
WHM-380-80
-2- April 8, 1980
I. ANALYTICAL GROUP
Competitive Evaluations
A sample of 1,3-Butylene Glycol manufactured by VEB Chemische Werke Buna (East Germany) was received from P. W. Schmidt of Amcel, Brussels. A competitive analysis report will be issued.
One sample of a tank car of Isobutyl Alcohol received from Rhom & Haas was forwarded to the Bay City Plant for competitive evaluation.
MO Units and Formaldehyde Blending
Formaldehyde Blending - The new Methocel Stabilizer Addition equipment that was installed last month has operated very erraticly. Results of the blend tanks has ranged from 1.8 to 28 ppm. The desired level of stabilizer in the preblend tanks is 12 ppm.
Oxo Butyraldehyde
Propylene - The Propylene pipe line to the Chemcel Plant was placed in service on March 18, 1980, providing about half of the Oxo Unit feed. Routine laboratory analyses thus far show the material to be spec. Polymer grade Propylene. The Laboratory will continue to monitor the quality of this material on a routine basis.
A sample of Propylene received from Texaco was analyzed in the Instrument Laboratory. The material met all our purchase specifications. Tank car shipments from Texaco have begun, and samples from each ship ment thus far have met our specs. Routine analysis of this material will continue.
Polyol Area
Pentaerythritol (PE) - Manpower assistance is being furnished to the Special Problems Group for 24 hr operation of the PE AML Extractor operation. This is in support of the organics recovery project prior to sale of PE AML to Virginia Chemicals Co.
003334
WBM-380-80
-3- April 8, 1980
Analytical Group General
The Review of the Bishop Plant Manufacturing Control Specifications has been completed locally. Final recommendations to Company Quality Assurance will await the Specifications format meeting to be held in Dallas, April 8, 1980.
The decision was made to proceed with the purchased solutions project. Ready-made solutions will be employed both in house (Laboratory) and dispensed to Unit operations pending contractural agreements with the vendor of choice. La Mar Ka of Baton Rouge, La. One technician headcount is expected to be saved via this project.
Silver catalyst samples entering the Laboratory will be weighed in and out in support of the precious metals accounting system. Laboratory inventories of silver will be reported to the Accounting Dept, on a monthly basis.
One technician was transferred to the Special Problems Group to provide assistance in personnel environmental sampling and associated analysis.
Customer Complaints
March 14, 1980 - Plastics Engineering Co., Sheboygan, Wise. - 52Z HCH0 car CELX 13252 - Car arrived with "an amber color". Customer used product and returned a sample for evaluation. Returned sample had a yellow color of ^200 Pt-Co Units and an iron level of 2.6 ppm. .Apparent car lining failure. Tank car will be inspected for patching need upon its return. Complaint classed as valid.
March 25, 1980 - DuPont Chem. Co. - Louviers, Colo. - complained that PE Lot 80-29-3P arrived in a "chunky and junky" condition. Company Q.A. will not support return of material and has requested DuPonts sieve test specifications for review. Complaint classed as non valid.
Quality Waivers and Delays Delays - None Waivers - None
003335
WHM-380-80
-4- Aprll 8, 1980
Analytical Statistics
Sample Count Chemical Section Instrument Section Total
Technican Overtime Chemical Section Instrument Section Total
Mar. 4683 2451 7134
Mar. Y-T-D
15020
7970
22990
Previous Y-T-D 12859
7093
19952
110 170 165 44 148 122
154 318 287
Sample Shipping and Quality Assurance Statistics
Sample Shipping
Statistics For
March Month
Domestic Export Plastics Other
Total
76 2
11 11 100
Quality Assurance Statistics
Shipments (No. of Orders)
Delayed
w-,vr__
Internal
External
Complaints (Total)
Complaints (Legitimate)
Complaints (Non-Legitimate)
Complaints - Outstanding (Unresolved)
Month 1036
0
0 0 2 1 1
0
1980
YTD
221 6
20 27 274
Previous YTD
200 8 4
40 252
YTD 2881
2
0 3 11 3 8
0
Previous YTD 2725 4
3 6 20 7 5
8
003336
WttI-380-80
5- April 8, 1980
II. SPECIAL PROBLEMS GROUP
Mechanol Oxidation, Formaldehyde Blending T. A. Jasek, M. E. Harris
.MO Efficiency Improvement with .Trace Amounts of Halogenated Hydrocarbons The Laboratory Microunit is being refitted and revamped for resumed studies. (Jasek)
Metals in MO Air Supply - No progress due to priorities. (Jasek)
MO Silver Catalyst Screening - A particle size distribution determination was conducted op a sample of reground used catalyst. The catalyst had been topped with a- layer of fines. No significant difference was found between the particle size distribution of the new catalyst versus the reground used catalyst.
A silver inventory was conducted to determine the amounts and types of silver catalyst needles present in the Laboratory. Any unnecessary amounts of silver were returned to the silver warehouse. (Jasek)
Analysis of Surface Contamination of Silver Catalyst from Third MS Cude to MO Plant Trial - No progress due to priorities. (Jasek)
Methyl. Formate Make Study - A study is currently underway to determine the amount of methyl formate various aged and types of catalyst produces. Reactors at MO-II and MO-IV are being utilized in the study. Also being determined are the actual amounts of methyl formate produced by MO-II and MO-III, since both units receive methanol streams with methyl formate present. The amount of methyl formate is necessary to determine the individual reactor efficiencies. (Jasek)
Improved Formaldehyde Stabilizers - A report documenting work performed to date, along with recommendations for a plant trial have been submitted for review. Plans are to implement a stabilizer system containing 2-5 ppm polyvinyl alcohol and 10 ppm Methocel^ (carboxymethylcellulose). Tom Powanda at Summit has been contacted and he does not anticipate any particular problems in end use applications. I am presently searching for a supplier of polyvinyl alcohol of the correct molecular weight (8,000 to 14,000). Follow up work on this project continues. (Harris)
003337
Wai-380-80
-6- April 8, 1980
Utilities, BOD S. G. Smith, G. R. Stasney, B. W. Wise
Anaerobic-Aerobic Testing of Chemical Wastes - A report outlining the status and scheduling of remaining objectives for the Laboratory anaerobic-aerobic pilot studies was submitted (co-authored with Process Engineering).
Anaerobic-Aerobic Pilot Unit #1 - Feed to filter #1 contains equalization basin material, oxo and polyol sumps, T-312 Residue (Na+ source) and nutrients (NH4OH and H3PO4). Feed COD concentration = 6000 to 8000 ppm. Following removal of solids from the filter by nitrogen agitation of the filter bed, organic removal efficiency increased by approximately 15Z.
For the month of March: anaerobic organic loading =0.6 lb COD/ft-tyday, anaerobic organic removal efficiency averaged 70Z. Aerobic outfall COD content ranged between 220 and 280 ppm, at a feed hydraulic detention of 2.5-2.8 days. The detention time necessary to maintain outfall of COD <230 ppm is to be determined. Plans for April are to eliminate polyol sump material from the anaerobic feed.
Samples across the anaerobic-aerobic system were collected and sent to CCCTC for priority pollutant analysis.
Anaerobic-Aerobic Bench Scale Unit #2 - A Laboratory simulation of the switchover from the current aerobic system to the expanded anaerobicaerobic system has been in progress since March 4.
The lab filter was charged with 0.5 vol. Z of BOD I sludge blowdown and 4.5 vol. % San Antonio Anaerobic digestor sludge (Rilling Road Plant). Startup feed contains equalization basin material (0.18-0.28Z HCHO), T-312 Residue (Na+ soucre) and nutrients, NH4OH and H3PO4. Initial organic loading averaged at 0.01 for the 1st week of operation^ No gas-make was observed until after the 8th day of the startup. Currently, after 4 weeks of operation, the organic loading is at 0.10 lb COD/ft^/day, organic removal efficiency = 80Z.
The aerobic feed is being gradually switched from equalization basin material to anaerobic outfall, in proportion to increases of organic loading to the filter. Outfall COD content has remained low, usually less than 200 ppm. Aerobic detention time has been held at 3 to 3.5 days.
Filter control has been manual. Problems with computer vent rate measurement have prevented use of the computer for process control during the startup simulation. This is to be corrected, if possible.
003338
WHM-380-80
-7- April 8, 1980
Ammonia Nutrient Addition - Ammoium hydroxide is now added to anaerobic feedstocks at a level of approximately 25 ppm as NH3. This level of addition is sufficient for anaerobic requirements only. The aerobic sections are fed NH4OH separately. At the 25 ppm NH3 addition level, a complete reaction with HCHO would produce ^50 ppm MNTA. Analysis for HMTA across the anaerobic-aerobic system has shown <10 ppm HMTA in the feed, anaerobic recycle, and aerobic outfall.
Further studies now in progress entail measuring HMTA formation and pH effects in anaerobic feed and recycle samples at NH3 addition levels >25 ppm.
Evaluation of TOD (Total Oxygen Demand) Analyzer - The TOD analyzer is to be interfaced with Filter #1 for continuous on-line analysis of feed and recycle TOD. The Laboratory will assist the Instrument group in evaluation of the TOD analyzer and determination of TOD/COD correlations.
BOD Unit Support - The unit method for analysis of NH3-nitrogen is Eeing crosschecked by a specific ion electrode analysis.
Environmental Health C.' E. Gary, K. V. Parker
Celanese maintenance and Arthur Bros, personnel were monitored for formaldehyde exposure (short term exposure levels - STEL/30 min) during the Paraform shutdown. Twenty of twenty-one people were exposed to >1.0 ppm HCHO. Fifteen of thirty-eight samples were >2.0 ppm (Corporate guidelines are 8 hour time weighted average (8 Hr TWA) - 1.0 ppm and STEL/30 min - 2.0 ppm.) (Report in prep.)
A "rough-draft" administrative policy covering respiratory protection to formaldehyde exposure has been written. (Under review-to be presented to the Formaldehyde Task Force.)
Three Ecolyzer 9000 00 dosemeters were evaluated for carbon momoxide monitoring in the laboratory. A mixture containing 50 ppm CO and 459 ppm of a mix of methane, ethane, propane, and propylene indicated that 3.0-4.8 ppm HC will read as 1 ppm 00. A mix containing 552 ppm H2 and 50 ppm CO and a sample containing only 264 ppm H2 in Nitrogen showed that 3.0-6.7 ppm H2 will read as 1 ppm CO. These dosimeters are not acceptable for CO monitoring. (Report in prep.)
003339
WIM-380-80
-8- April 8, 1980
A canister type full-face mask was evaluated for respiratory protection in formaldehyde service. Both canister and cartridge type masks should be used for a maximum of 1 hour in HCHQ concentrations up to 15-20 ppm. CTo be reported.)
Oxo, Butanol J. D. Presley
Reactor Stability/Accountability - The composition of the Oxo reactor has been stable during the month. However* low TP? values have persisted. A cross-check of the G.C. derived value (using the titration method) showed the G.C. method to be in error by about 7.5% absolute. Plans are to use the titration method on a more regular basis.
Rhodium Accountability - On March 21, 1980, rhodium accountability was about 80% for Rian 6. This represents a loss for the second month in a row. The method of rhodium determination is now suspected. An alternate method used on a triplicate determination late last month showed 101% accountability (instead of the reported 85%). Work continues.
Total rhodium loss in T-210 Res is 12.8 pounds for Run 6.
Improved Rhodium Recovery - Testing of a second sample of T-4 residue concentrate from Bay City yielded low intrinsic activities. However, a third Bay City sample gave activity results similar to those reported in January, 1980. These tests, additional base case tests, T-210 residue concentrate tests, and retests of the first Bay City sample have been carried out with a much improved temperature control system on the autoclave. This data was reported at the Rhodium Technology Exchange held at CCCTC this month. Also, a letter detailing results will be written.
An extraction method for rhodium removal from hydroformylation products is correctly being tested for application to Oxo catalyst. Work continues.
Oxo Unit Support - Final analtyical work on the pipeline propylene has been completed. The propylene has continued 994-% purity. Results will be reported.
BuH, contaminating the oxo compressor (C-322) bearing oil, apparently increased over February. Work is still in progress to quantify the levels. Tenative sampling will be once each month. Work continues.
003340
WHM-380-80
-9- April 8. 1980
A letter has been written giving analytical results of Oxo interstage cooler condensate samples. The results will be used to determine disposition of liquid from a proposed in-line separator ahead of C-322.
Special Analtyical Assignments F. R. Dow
PE Monitor - Attempts have been made with the L.C. to trap a pure sample of Di-PE to determine linearity and purity of Di-PE in the PE monitor.
Initial attempts to trap Di-PE from high purity sample (98+Z by the SMA GC method) have indicated that an unknown component is present which is separated by L.C. but is not separated by the SHA G.C. procedure. The unknown component is in the monitor and is a portion of the reported value for Di-PE concentrations in PE.
Since the L.C. can make the necessary separation, the unknown is being trapped for potential identification.
Competitive MeOH - No progress due to other priorities.
Impurities in Plant Air - Plant air was monitored during the week-end of March 1 and 2, 1980. Observations previously reported (wind direction effects air purity) were again confirmed. A strong norther blew in 'v. midnight on February 29, 1980, and immediately high concentrations of impurities were recorded.
During that same week-end it was also observed that the air impurities did not increase during the 3 a.m.-5 a.m. time period. However, at about this time frame on Monday morning (March 3, 1980) the impurities did increase. The a.m. increase has been observed during the Monday through Friday air monitoring periods.
Methanol Synthesis J. E. Russell
MS-II Unit Support - The Selas Reformer was shut down for maintenance on March 4 and March 19. Ni(00)^ analyses were required for each shutdown. The Ni(GO)^ level was below the OSHA limit on both occasions, and a letter documenting the results of the analysis was issued for each shutdown.
003341
WHM-380-80
-10-
April 8, 1980
The monoethanolamlne was analyzed to determine the 00 loading In resonse to continued poor scrubbing performance. The analyses on both the 5 MM and 2 MM Girdler MEA Systems suggested leaks in the respective rich amine-lean amine heat exchangers. Corrective maintenance confirmed the leaks in the heat exchangers and these have been repaired. The leaking 5 MM heat exchanger, one of 5 shell and tube units required for that service, has not been returned to service.
Sediment from the corroded 2 MM rich MEA-lean MEA heat exchanger was analyzed for Ni, Cr, and Fe. The sediment sample contained approximately 27% by weight Fe, 5% Cr, and .08% Ni.
Waste Stream Viscosities - The lab completed the determination of the viscosities of several liquid waste streams and blends of those streams for use by CE Lummus. A letter was issued reporting the values obtained.
CO2 Injection Plant Trial - The Lab is assisting operations in determining the effects of C02 injection into the Selas Reformer. Base case values for the composition of Crude MeOH will be compared to those same values after CO2 injection begins. An earlier attempt this month led to no useful data due to various operating problems.
The OO2 injection trial will continue into April.
BuDH Purification Improvement - The Lab work has been completed on the one column BuOH purification. A letter will be issued this month.
Formic Acid Removal - No progress due to priorities.
1,3-Butylene Glycol P. J. Buras
Unit Support - None provided.
Improved Aldol Consensation and AcH Recovery - No progress due to priorities.
003342
WIM-380-80
-11-
April 8, 1980
DiAcetone Alcohol R. L. Day, P. J. Buras
H2O Addition to Acetone Feed to Reduce Mesityl Oxide Losses - Water was added continuously beginning the first day following startup on March 6, 1980. Recycle acetone to the reactor was raised to 60 gpm on the second day of the catalyst run. Mesityl oxide In the reactor product was less than 0.1 wt. % for virtually the entire run. Mesityl oxide in T-284 residue averaged ,'<1.0 wt. %.
In addition to raw material savings, there were indications that the quality and stability of DAA are improved through water addition. The color of T-285 residue was less than normal (25 vs >35 Pt-Co Units). No trace of nonsymmetrical phorone isomer (the suspected cause of water immiscibility) was detected. 1-285 residue consistently passed miscibility whereas previously in 1979 it failed most of the time.
A report detailing the results of the plant test, project economics, and final design was issued with Process Engineering. Cost of the proposed permanent water addition system is estimated at $6.2 M. Annual savings for 1980 are conservatively estimated at $7.3 M/year based on raw material savings alone. Additional savings may result from improved stability of DAA. (Buras, Day)
DAA Color - Studies were continued this month to determine the effect of the plant air blanket on the color of the DAA Inventory tank, and to determine the best type of blanket to use. So far, the best blanket to minimize color build is an inert blanket, such as bottled nitrogen or cryogenic nitrogen. Data also indicate that most color bodies form through an air oxidation process.
Studies were also continued on the effect of water on inhibiting color formation.
A report documenting DAA color studies is in progress. (Day)
DAA Miscibility - A status report outlining DAA color and water miscibility investigations was written (PJB-24-80, RLD-08-80). All laboratory work conducted thus far indicates that color and miscibility problems are caused by impurities in DAA. Some of these impurities are formed in the reactor. Since water addition to the acetone feed to the DAA unit reduces by product formation in the reactor, the stability of DAA should be improved. A detailed report on identified impurities in DAA and their impace on water miscibility is in preparation. (Buras)
003343
WHM-380-80
-12-
April 8, 1980
Acetates L. M. Harvey, M. E. Harris
Low Efficiencies in Acetate Unit - Low acid and alcohol efficiencies were experienced during n-Butyl Acetate production in March. Analyses have been completed on daily composite samples of T-103 residue, V-1583 and V-862 WIP tanks. Evaluation of results will be coordinated with Process Engineering and a report will be issued in April. (Harvey)
Corrosion Inhibitor - The cupric phosphate (Cu3(P04>2) corrosion control system recommended by CCCTC for the reactor column reboiler has been checked out by the Bishop Lab. A report has been published (MEH-40-80) recommending a plant trial. Chemicals are on order and the tests should begin in mid-April. (Harris)
Paraform,
Products
M. E. Harris
Paraform Unit Support - T. Jasek applied two samples of 'high' and 'low' molecular weight paraffins to be tested for cloud time effects in liquid 'para'. At 10 ppm the 'low* molecular weight material showed no appreciable effect (cloud time of 45 min. vs. blank of 55 min.). The 'high' molecular weight material at 10 ppm was very detrimental, giving v 0 cloud time. This may have been caused by other material contained in the paraffins. Plans are to run further experiments with pure paraffin samples.
Pentaerythritol L. M. Harvey, P. J. Buras, M. E. Harris
Unit Support - None provided because of higher priority work and the lack of serious problems in PE. (Harvey)
Recovery of PE from VCI Centrate - A sample of PE AML collected during Tech-grade PE production was extracted with n-Hexanol and concentrated to <52% H^. Five gallons of concentrated, extracted AML and one gallon of the original AML were sent to VCI (Portsmouth, Va.) for evaluation in their Sodium Formate recovery process (IHH-72-80). An equivalent
003344
WHM-380-80
-13-
April 8, 1980
set of samples Is being prepared from AML collected during Pure-grade PE production and will be sent to VC1 In early April. VCI has agreed to return to us the centrate generated from their evaluation of our samples for further studies on stability and recycle of the material to the PE Unit. (Harvey)
Work Is In progress to optimize operating parameters of the AML extractor and back extractor. (Harvey, Buras)
PE Formal Hydrolysis - Work is starting for testing a potential PE hydrolysis scheme involving the Na+ form of a cation exchange resin, and a formic acid catalyst. This will be similar to previous studies on the Methanolysis of IMP formals in V-747 residue. The proposed hydrolysis scheme is a low corrosion. (Harris)
Trimethylolpropane P. J. Buras
Unit Support - None provided because of higher priority work and the lack of serious problems in IMP.
Leaking IMP Tank Car - A sample of liquid leaking from a tank car being loaded with molten TMP was identified as virtually pure water by refractive index and Karl Fischer titration.
Miscellaneous M. E. Harris
A conception record has been submitted for review concerning an earlier proposal of an alternate reactor scheme for producing 2-Ethylhexenal. Reaction kinetics are very good, and a preliminary energy balance indicates this scheme may be of commercial value.
Process Technology B. C. Kerr
Rhodium Recovery and Accountability - Current Laboratory work on this project is based on the use of a wiped-film evaporator. Spent Oxo Catalyst is being mixed with UCON 625 and run through the evaporator at
003345
WHM-380-80
-14-
April 8, 1980
high vacuum. The objective is to concentrate rhodium in the UCON oil and remove most organics. Mechanical and procedural problems are being investigated.
Organics Recovery from T-210 Residue - No progress this month.
Catalytic Removal of Formic Acid from HCHO - Awaiting delivery of fresh catalyst.
Rhodium Recovery Technology Review Meeting - A one-half day meeting was held at the Tech Center among personnel interested in rhodium recovery and conservation. Mr. Jim Thomas from Bay City will issue minutes of meeting.
General
1. Paul Buras attended the National ACS Meeting in Houston during March 24-27.
2. Leanne Harvey attended an Equality Committee Meeting in Clear Lake March 13.
3. Leanne Harvey attended the in-house "Professional Employee's Development Program" session on March 14.
4. Leanne Harvey and Hub Thigpen attended a meeting of Bishop Technical Department personnel with Virginia Chemical Co. personnel at Portsmouth, Virginia, on March 18.
5. Ronnie Hilbrich transferred to the production department (Area I), effective March 10, 1980.
6. Kathryn Parker transferred from the routine analytical section to the Special Problems Section to work with Chuck Gary in 0SHA monitoring. The transfer was effective March 17, 1980.
003346
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