Document JNjejZ8VgKdnneERzK8pY57a2

CELANESE CHEMICAL COMPANY Chemcel Plant Bishop, Texas To: C. W. Harrison From: W. H. Meyer WHM-89-77 September 12, 1977 Laboratory Department Summary August, 1977 Chemical DISTRIBUTION J. H. Frick P. E. Heime J. N. Gann G. D. Boyd J. W. Dunn J. Chervenka J. M. Ramey W. J. Derocher Dr. J. C. Trebellas T. N. Dowdy J. E. Sanborn H. A. Ducote K. G. Gallimore W. H. Tuke R. S. Hahn F. B. McAndrews M. D. Harvey Dr. F. Zitomer J. M. Hodges M. A. John Plastics B. C. Kerr J. L. Merian Dr. C. E. Loeffler A. C. Abshier Dr. R. P. Lowry C. A. Amond W. W. Massey W. C. Beyer A. G. McGehee R. L. Bunkley J. T. McMahon E. Munoz R. A. Mickelson K. A. Rose J. M. Sawyer C. S. Schmaltz G. R. Scholz W. L. Sharp CCCTC R. W. Swanbeck W. E. Heinz H. H. Thigpen Dr. C. C. Hobbs 0. Towery W. J. Humphrey J. L. Trumbley W. T. McNair P. J. Volpe Dr. D. R. Napier J. D. Walker Dr. L. Starr W. E. Tavlor Central Fi1r~T7i*t^*i - Bay City - Clear Lake - New York - New York - Bayport Terminal - Pampa - Summit - Summit r lie: 71 o. 0 003091 CELANESE CHEMICAL COMPANY Chemcel Plant Bishop, Texas To: C. W. Harrison From: W. H. Meyer WHM-89-77 September 12, 1977 Laboratory Department Summary August, 1977 The Bishop Plant Laboratory activities during August, 1977, are attached. Section I contains a summary of the Analytical Group activities with a table of analytical statistics. Section II contains a Quality Assurance Summary and a table listing shipments, quality waivers, quality complaints and sample shipping, statistics. 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 included in Section III. WHM/jm Attached Report W. H. M^fer 003092 WHM-89-77 -2- September 12, 1977 I. ANALYTICAL GROUP Competitive Evaluation Methyl Formcel - A sample of Borden-produced 55% Methyl Formcel was obtained from Rohm and Haas. An evaluation report will be issued. Polyol TMP - Analytical support was provided for the preparation of Labora tory re crystallized TMP. Samples were sent to Sartomer and PPG for evaluation. PE AML - The PE AML storage tank number 2458 is now being analyzed daily for sodium formate. These analyses will be used for charging of product transfers to Virginia Chemical Company. Pa raf orm Methyl Formcel - Support was provided for efforts to establish minimum concentration of caustic additive necessary to maintain low methylal build in Methyl Formcel product. To date, lOOppm sodium combined with one hour reactor cook time has proven successful. Lower para meters have not yet been tried. MO Units MO-III and IV - Analytical support was provided for rate run calculations around these two units. The runs will be repeated due to feed unit (MS) upsets. Stabilizer - Methocel stabilizer addition tanks and pumps have been re located. Methocel analysis in sales grade formaldehyde will be per formed three per week until conditions stabilize. Current levels range from 3 to 11 ppm with a target of lOppm. Oxo Area Propylene - Four Bayport Terminal propylene samples were analyzed for ppm 02 for the purposes of cross-checking the Bayport unloading and in ventory system. 003093 WHM-89-77 -3- September 12, 1977 Utilities and BOD The Texas Water Quality Board representatives were in the Plant August 9, 1977, for a 24-hour sampling of the two permit outfalls. Samples taken were split between the TWQB consultant, Ernst Davis, and the Plant Laboratory. A letter report will be issued when resuits from all sources are in hand. Plant Laboratory results indicate all parameters are well within permit levels. A nalytical Statistic s Sample Count Chemical Section Samples Instrument Section Samples Total Technician Overtime: Chemical I n s t r um e n t Total August 4, 334 2. 115 6,449 August Y-T-D 39,541 18.458 57,999 Previous Y-T-D 32,210 14.971 47, 181 24 559 50 544 74 1, 103 52 7 423 950 003094 WHM-89-77 -4 September 12, 1977 II. QUALITY ASSURANCE DAA - On August 10, 1977, we received word that GATX 69682 loaded with DAA and shipped on July 19 to Alvi, Mexico, arrived with a high color (color unknown). This tank car was a Union Carbide car, and the customer Union Carbide's. The product shipped out at less than 2 5. Current status in not known. Methanol - During the month, the Chemcel Laboratory evaluated U.S.I. specifications for methanol as related to the ultraviolet (U. V.) absor bance. Chemcel MS product meets the U. V. absorbance requirements as follows: Does not exceed 0. 60 at 240 m/a; 0. 40 at 250 m/u; 0,15 at 260 m/u; and 0. 10 from 2 70 m/a through 340 m/a. This evaluation was prompted by a recent barge shipment to Bayport which did not pass this special requirement for U.S.I. on methanol. The methanol was found to contain traces of toluene which increased the U.V. absorbance. Paraformaldehyde Fine Powder Dycho Co. Inc. (Niota, Tennessee)- The customer complained that the product appeared wet and caused lumping and balling in use. Three lots were involved in the complaint: Lot 2417 (January 10, 1977), Lot 2379 (April 1, 1976) and Lot 2378 (March 27, 1976). The original analyses and the analyses of the retains show that this pro duct met sales specs. Samples representing each of these three lots were returned to us on August 11, 1977. The returned samples were analyzed and found to meet all of our sales specifications, and no evidence of wet powder or lumps was observed. We understand the customer has used the material. Tennessee Eastman Co. (Kingsport. Tennessee)- The customer com plained of difficulties with Paraformaldehyde fine powder shipped to them on June 7, 1977, out of Lot 2442. The complaint involved "bal ling up" in their machine. They had checked several bags and found lumps the size of gravel. The customer asked that the 200 bags be replaced with a new lot, and this has been done. Analysis of the lot retain and a large sample returned to us met all sales specifications. We checked the sample returned to us from Tennessee Eastman, and found no lumps, as they had reported. The Charlotte Office handled the complaint. Disposition of the 200 bags from Tennessee Eastman is unknown. WHM-89-77 -5- September 12, 1977 n-Butyl Acetate - Texas Instruments Specification - Work has started on analyzing n-butyl acetate for residue after evaporation by the Texas Instruments method to determine if we can consistently meet their re quirements of 2 0ppm. We feel we must evaluate this further because we now take a residue product as a result of an energy conservation project. Paraform Flake - Lehn and Fink Products Co. in Toledo, Ohio, com plained that the product they have was low in assay. The lots in question are numbers 189-77 and 194-77. The customer reported an 80.8% for maldehyde on these two lots. We feel that this must be an assay problem with them as a value this low would be impossible to flake. A check of the retains of these two lots shows a range of 92-93%, which is normal. The customer has used all this material and has agreed to an exchange of retain samples for an assay check. We have not received the samples. Methyl Formcel - Recently Uniroyal Chemical at Geismar, Louisiana, has been concerned about the reported formaldehyde value versus the calculated formaldehyde value on the 55% Methyl Formcel + Acetic Acid blends sent to them. Asa result of a meeting with Production and Laboratory personnel, a letter (WHM-85-77) of recommendations on the future handling of this type product has been issued. Sample Shipping and Quality Assurance Statistics follow: 003096 WHM-89-77 -6- September 12, 1977 Sample Shipping and Quality Assurance Statistics Sample Shipping D ome stic Export Plastics Othe r ' Total August 61 8 4 10 83 August Y-T-D 785 77 59 702 1,623 Previous Y-T-D 796 129 101 171 1, 197 Shipments (Number of Orders) Delayed Due to Quality Quality Waivers Quality Complaints Quality Complaints Accepted 743 6, 762 6,086 0 22 25 4 33 11 4 42 15 0 12 9 NOTE: See attached copies of Quality Complaints and Delayed Shipments due to quality or quality waiver. 003097 WKM-39-77 September 12, 1977 "3 U ~ Z 3? ^ -- 7 V33. r c 3. -- w ax --233 *3?3 m V3 3.< 3. . 9 3. 3_ U 3. fEl <S33 3 i. - 32 " y 3 *5 3 a53 3 3. i,3 I! :4 i3 5" 1 j V2-f j Z l15 " ! mu -30 * * "3? a- - * 3 iO:; = : a - 2-- Z | | '5 ! - lill SJ a * 3 J 23 = 2lv5.2 S. j|='l! 3 J a a-a e ia r* *TO*33 --m3a2. w7ia3* -.3-01<3335*a3 -3 ? -- e IS.i* --3^--25 W a 32. J & 3 - .* w a a J 2 a 3 E 3 -i _ i2 aw a0 ^a 5 3 3*5 i 3- 1i a <33 ^aa oo* <-*eMr a a ^ -1 >N N a-- ^ *3 3 CJ -a "U j *3 u x * a a < * 3 J c30 a *a a 3 *3 "3 3 aa 3 y r :* t r ,*** t 330* a* a a u* v> a o J3 3 Ja a 3 - % i a - aa --5 ca a-- a- 4-3 a 3. 2a Z SO v* rr- a 003098 /*r?s a n d S h i |> m e n U D e l a y e d D u e t o Q u a l i t y 003099 WHM-89-77 -9- September 12, 1977 m. SPECIAL PROBLEMS Methaaol Oxidation, Formaldehyde Blending _______ A. J. Branecky, J. D. Presley MO Efficiency Increase with Trace Amounts of Halogenated Hydrocarbon - The data from the methylene bromide and methylene chloride plant tests is being collected and analyzed. A report will be issued this month. MO Catalyst Reuse - Work will continue as time permits. MS-II Crude to MO - Awaiting piping modifications for plant trial. Water Injection to MO - No progress due to priorities. Pampa Pipeline Grade Methanol to MO - A report was written in August, and will be issued this month (JDP-03-77). As reported in the last monthly summary, the test methanol showed standard micro unit efficiency and con version. Final analysis shows that the odor causing agent in the Pampa methanol is ethyl acrylate. Further investigation revealed that this com pound is not normally found in pipeline grade methanol, and that is was possibly introduced as a contaminant via the sample container used. The quality of the pipeline methanol appears to be sufficient for use in Bishop MO units. A plant trial is recommended (following the procedure outline in the report) before plant use is accepted. MO New Catalyst Screening - Further work on spun silver fiber is pend.-.; arrival of new samples. A lot of Engelhard standard silver needle cata.. containing 14ppm tin was received recently. The present specification : r tin is < lOppm. A sample of the lot (Lot 36, July 6, 1977) demonstrates typical new catalyst efficiency and conversion in the micro unit. A report (JDP-01-77) was issued recommending that, if the catalyst shcw*s standard efficiency and conversion in the process units, the standard spec.fication for tin be raised to 14ppm. Performance of the catalyst will be followed by the Lab. Reduce Methylal Formation in the MO Distillation Columns - Initial lab work showed the following stability of 50% formaldehyde containing caustic; 003100 WHM-89-77 -10 September 12, 1977 Blank 240ppm caustic 480ppm caustic 720ppm caustic 960ppm caustic 21+ days 21+ days 21+ days 4 days 3 days Presently, it is believed that significant methylal formation reduction can be achieved by adding caustic in amounts resulting in fewer than lOOppm in the final product. Hence, no problems are anticipated for product sta bility. No further progress was made due to priorities. Work continues. MO Unit Rate Runs - The Lab aided Engineering in obtaining necessary data for MO-HI and MO-IV rate runs. No significant data was gathered for MO-II due to mechanical difficulties. A report will be issued by Pro cess Engineering. Nepera Blend - The Lab was asked to determine the feasibility of making a special product blend for Nepera. The blend consists of acetaldehyde, for maldehyde and methanol in the respective molar ratio 1:0. 75:0.25. Nepera indicates that almost any concentration of water could be tolerated in the final blend. However, it would be advantageous to both them and us to have as little water as possible. Initial lab work shows that the blend is (by physical appearance) quite stable at room temperature. Gas chromatogra phic analysis shows, however, that some chemical reactions are taking place. .An attempt will be made to quantify this. Nepera further indicates that they can withstand 1 to 2 total weight per cent variations in the final blend. Hence, side reaction products, if small, might be tolerable within the 1 to 2 per cent limits. Work continues. Utilities, Raw Materials, BOD S, G. Smith Purchase Specification Update - No progress due to priorities. BOD Unit Analytical Methods Manual - No progress due to priorities. Anaerobic Pilot Testing of Chemical Waste - An estimate of equipment costs was completed, and a company to build the anaerobic reactor was located. Work on this project is in abeyance until Process Engineering economics are published, and until the decision is made as to which system to use for the proposed BOD expansion. The systems under study are anaerobic, aerobic and the Union Carbide Unox process. 003101 WHM-89-77 -11- Septembe r 12, 1977 /??*>. DAA Color Stability - A laboratory simulation of T-285, the DAA heavy ends column, is being conducted to; 1) find optimum operating conditions of the column, and 2) determine if heavy ends (color precursors) are being passed over to the finishing column, T-294, causing color insta bility of the finished product. Elimination of Lamella Underflow - No progress due to priorities. OSHA Monitoring J. M. Jackson Samples of formaldehyde in air, received from Ms. M. R. Blankenship (E.I. duPont) have been analyzed.and the results returned. This data was obtained for the Test Method Sub-Committee of the SOCMA Task Force, and will be used to evaluate the NIOSH formaldehyde sampling and analytical method. Duplicate airborne formaldehyde samples were obtained in the Laboratory and Paraformaldehyde Unit for evaluation of the dimedone versus chromatropic acid formaldehyde methods. These samples were at the request of Mr. C.S. Laubly (Corporate Industrial Hygienist). One set of samples was analyzed by the Bishop Lab by the chromatropic acid method. The duplicate set was sent to Gliddin Durkee for the dimedone analysis. A re port will be issued when the dimedone results are received. Opacity of the TMP concentrator exhaust was determined. Follow-up opacities will be determined to verify results, and a report will be issued. A summary report on OSHA monitoring data is in progress and will be issued soon. Girdler Unit Monitoring For Nickel Tetracarbonyl A. R. Hancock Girdler unit nitrogen purge gas was monitored for nickel tetracarbonyl on August 7, following the planned girdler unit shutdown. No nickel tetra carbonyl was detected. Procedures and results are being reported. Esters, Methylal, Paraform, Formcels R, G. Hilbrich. K. B. Benkendorfer Feed Contaminants and Liquid Paraform Stability - The study has been completed, and a full report is being written. WHM-89-77 -12- September 12, 1977 Paraform Material Balance - Delayed, pending full-time Process Engineering coverage on the Paraform Unit. Acetate Catalyst Evaluation - Dibutyltin diacetate was evaluated in the laboratory as a potential replacement catalyst for MSA in the Acetate Unit. It was found to be unsatisfactory because of low acti vity. A report has been written. Alternate n-Butyl Acetate Process - No progress due to priorities. Paraform, Formcels and Ester Unit Analytical Manual - No progress due to priorities. Acetate Unit Support - A study is underway to determine if there is a correlation between the acid concentration in the organic layer and the conductivity of the water layer in the acetate reactor column (T-268) distillate. It is hoped that this will provide a method to continuously mon itor the acid level in the organic layer. Numerous samples have been taken and analyzed. Work continues. 1,3-Butylene Glycol, DAA A. R. Hancock_____________ 1,3-BG Unit Support - None required. Unit down. 1,3-BG Cost Reduction - It may be possible to replace the vapor sidestream from the BG finishing column (T-22 7) with a liquid sidestream or a residue stream. About $50M per year in steam savings would result. Data from the previous run period was promising. A plant trial will be proposed at the appropriate time, if data continues to indicate feasibility. DAA Unit Support - No lab support needed. DAA Laboratory Reactor Study - No progress. Pentaerythritol, Weak Formaldehyde H. H. Thigpen, G. R. Stasney PE Efficiency - No progress. PE Color - The carbon charged on June 25 continues to remove color sat isfactorily. However, there has been some color breakthrough indicated 003103 WHM-89-77 -13- September 12, 1977 by detectable amounts of color in the "B" filtrate. A filtrate color of 12 PtCo units showed up in the "B" filtrate on August 8. There has been a very slow increase to 17-18 PtCo units on September 7. Re moval will remain satisfactory until the "B" filtrate color increases to 2 5-30 PtCo units. The PE product will then have a color of about 5 PtCo units (5% solution). We have produced approximately 680 lbs. of PE per pound carbon on the current charge (through September 7). This is a satisfactory carbon bed life. Previous lab data indicated that a minimum of about 630 lbs. of PE product per pound of carbon would be obtained. Economics were based on that value. Current data from the unit confirms the-prediction based on previous lab data. We will continue to monitor the performance of the carbon bed. A de tailed report will be issued after the current charge is replaced. Lower Sulfate in PE "A" Mother Liquor (AML) - The acid digestor tem-i perature and pressure control systems were repaired and the temperature can be maintained high enough (240-250 F) to minimize the amount of sulfuric acid required. During the next month, we will continue efforts to tune this system so we can meet the Virginia Chemical request for 0. 5% or less sodium sulfate in the AML sodium formate (dry basis). Methanol Synthesis F. R. Dow Fuel Gas Quality - A sample of fuel gas analyzed August 17 contained 97. 3 vol. % methane. This was about 0. 5 vol. % higher than the June and July analysis. Sulfur was not monitored by the Lab because CCCTC was using the Tracor sulfur analyzer. A letter will be issued outlining plans for resolving dis crepancies in sulfur analyses between the various process analyzers. MS-II Analytical Support - DPG, Selas and the combined reformer gases have been analyzed in the lab for comparison with the process analyzer data from the MS-II computer output. The process analyzer and Lab G. C. analysis of reformer gas compo sition shows excellent agreement for CO and CH4, but the Lab shows about 1% more COz than the process analyzer for the reformer streams. This difference is unexplainable at this time. Work will continue. 003104 WHM-89-77 -14- September 12, 1977 Oxo Bataaol, Propaaol ______A. J. Bacon Oxo Reactor Accountability/Stability - Little work was done due to prior ities. Use of propylene in heavy ends separation scheme was tried on a larger scale and still looks good, though quantitative data is not available. A secrecy agreement has been sent to Witco Chemical Co. by J. W. Corley (Houston). Samples for foaming studies will be sent when the agreement has been received. Oxo, Butanol, Propanol Support - Support work centered around the Oxo run number 3 catalyst dump August-7, and drumming August 8. Sampling during drumming was coordinated and analytical work was carried out. Rhodium accounting and loss analysis reports will be issued in early September. Minor troubles after startup included uncertainty of reactor level (BuH concentration) and high T-163 overhead rates. We are setting up a unit lab analytical method to determine BuH levels in the reactor. In strument Lab personnel are running these analyses as needed until this is complete. High T-163 overhead rates could not be traced to any high inerts make through the reaction area. Raising the product separator base temperature seems to have diminished the problem. Quality Lab analyses of T-67 liquid sidestream product BuOH have shown that project to be a success so far. T-259 overhead samples were analyzed over approximately 4 days in the latest attempt to improve side fluctuations in daily yield accounting effi ciencies in PrOH. Data showed very minor changes in PrOH assay for this stream, revealing that its contribution to any WIP assay changes are minimal. Process Technology B. C, Kerr Technical Report Abstracting - Preparation of technical report abstracts is current. Abstract card files are current through July, 1977. Production Initiated Process Technology - It was reported last month that a simplified reporting form had been submitted to Production for comments and revisions. Only one report of six sent out has been returned with comments. 003105 WHM-89-77 -15- September 12, 1977 Chemcel Plant Process Technology Review for New Employees - A booklet has been prepared containing a short review of Chemcel unit operations. Simplified flow diagrams, process chemistry and other information is presented for each of the process units and the BOD system. Copies are available in Process Engineering and Plant Engineering and the Laboratory. M i seella ne ou s Jim Jackson and Gary Boyd attended a meeting in Houston to establish priorities on Chemical Company streams to be subjected to toxicity testing. Susan Smith reported as a Chemist to Special Problems on August 15. Her unit assignment will be Utilities, Raw Materials and BOD. Leanne Mayerle transferred from CCCTC to Chemcel as a Special Problems Chemist, effective September 1, 1977. Her assignment will be the TMP Unit. Bobby Briell accepted employment as a Chemist in the Special Problems section effective September 6, 1977. His unit assignment will be PE. Temporary summer employees, K. B. Benkendorfer, Mauro Castro and Randy Shafer, returned to their respective colleges during the month. EHM-89-77 a -3 Q *<v*d 0-c +s~4 --y4 WS o U r- r- qco iK' x " f4 "3 * E- J2 S 54a Cl* ^ 55v o- u u cVn 00 b >1 b 4pa4 a o u y <o -"i 0 1a a, 3 a s y A y9 41 > 00 (4 0 c - sJ 3*41*4 a, ><4 W y H41i HI (fl < 'O Vi X oo cO <4 y 41 (4 2 A 2 4>4. (4 <d 44 <d * w aU i4 fl, 05 3 cn X o Vi Q, Vi 0 N &4 n U y i cn >. >. Xy yA v B A i4 Vi A u CQ eg u A B O 4Q 0A yao y > o 44 S 0 Vi 3 *3 y --i |fl. e0 = o "I <, -O q, B a") y 44 cd f. A c _V Vi oh 5f u o 2 00 B hi B y y v cyn 41 A >* A u 5 v 2 O 2 r~ r- > O' 00 Sk0' B X-- " 5O-<' u . H g s sV .fl 44 Q*0 10 5 oy y 6O 10 Q >* V, 4o1 B y > B a oo B Hi >HI Vl y c(n4 > f4 cn (4 y y u c4n1 3 T3 y 03 <N Vo A 3 2 V 03 A >. 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A cn A B <, Q O CQ -Q 0 yM Vi y A B y x u <; y A A X y Vi 3 0, 5 o <U c D 0) A J B 0 44 41 A B M 003107 WHM-89-77 17 September 12, 1977 g U 003TTO P ro je c t R hodium A ccounting C u rre n t S p e c ia l P ro b le m s P ro je c ts P rio rity J u s tific a tio n Bacon M aintenance of Business C a ta lyst Savings E stim ated C o m p le tio n Date C ontinuing September 12, 1977 - -19- WHM-89-77