Document a41rR0Q8Q1491VyRbVKB6gKqB

CELANESE CHEMICAL COMPANY Chemcel Plant Bishop, Texas To: Dr. R. R. Graham From: G. D. Boyd GDB-149-81 November 6, 1981 Laboratory Department Summary - October 1981 Attached is the Laboratory's monthly summary for October. The summaries are by groups. A table listing priorities, justifications, and estimated completion dates of Special Problems projects is also included. GDB:j r Chemical J. J. Fritsch W. H. Brough J. B. Brown G. L. Cade R. R. Carpenter M. W. Clifton R. S. Hahn W. A. Heenan A. A. Miller B. C. Kerr C. W. Lee D. E. Lockwood A. G. McGehee W. H. Meyer D. G. Pausky J. C. Rubiano 0. W. Schnellenberger G. R. Scholz D. D. Siemonsma W. L. Sharp K. R. Stelts H. H. Thigpen F. R. Dow G. D. Boyd Distribution Plastics R. G. Brandt A. C. Abshier R. L. Bunkley H. L. Davis D. A. Reck E. J. Heinz CCCTC G. J. Fisher W. E. Heinz W. T. McNair Central Files (2) J. N. Gann, Bay City J. E. Sanborn, Bayport J. L. Paul, Clear Lake D. W. Harris, Pampa T. H. Golson, Dallas 003600 File No: 303.3 HOY 13.81 GDB-149-81 Page Two November 6, 1981 Highlights Treatment of steady state polyol effluent at low BOD unit loading has been demonstrated in a laboratory unit. Successful treatment of variable strength VCI waste continues in a laboratory unit. Preliminary vacuum truck waste characterization indicates that much of this waste is treatable in BOD II. A Plant trial for use of phosphoric extracted Oxo catalyst has been planned for December. A Plant trial for use of C. Itoh TPP has also been scheduled for December. Studies indicate that some quantity of 2-ethylhexylamine (2EHA) will have to be left in the VCI wiped-film evaporator (WFE) residue before our proposed PE recovery process will be effective on that stream. Studies are underway to determine the amount of 2EHA required. The discrepancy between the Celanese and Acme Resins HCHO assay methods was resolved. The Celanese method is the more accurate of the two. 003601 GDB-149-81 Page Three November 6. 1981 I. ANALYTICAL GROUP Methanol Oxidation (MO) Unstabilized 37% HCHO produced with a minimum level of antifoam is bein shippped to Dow Chemical, Freeport, Texas. This is an attempt to alleviate "solids scum" formation problem in the customers process. Approximately 92 gallons of product on hand in Dow's tanks will be returned to the Plant for claiming. Polyol Area Pentaerythritol (PE) - The Instrument Section is providing analytical support for a project to evaluate potential processes for separating di and tri-PE from PE unit product. Utilities and BOD BOD analysis were provided for the CCCTC pilot study of the Celrobic system. The CCCTC study is to evaluate prospective customers effluent in tl system. The results were forwarded to Susan Smith for evaluation. Chemical Oxygen Demand (COD) analyses are being run daily on the Polyol effluent sump. This is to establish base case data prior to feeding this material to the BOD system. Customer Complaints 9- 29-81 - Hooker Chemical, N. Tonawanda, N.Y. - 50% HCHO - 20 M Gal. ca Complained of arrival with 20 color. 10- 1-81 - American Cyanamid, Kalamazoo, Michigan - 52% HCHO - 20 M Gal. Complained of arrival with assay of 51.7% HCHO. 10-1-81 - Dow Chemical Co., Freeport, Texas - 37% HCHO - 92 M Gal. in ci inventory - Complained of formation of "scum" in process when using this proc 10-27-81 - Hooker Chemical, N. Tonawanda, N.Y. - 50% HCHO - 20 M Gal. cs Arrived with 15 color. Quality Waivers 9- 30-81 - iso-BuAc to Celanese, Argo Terminal - iso-butyl propionate at wt.% vs. max. of 0.01 wt.% - 192,770 lbs. - QD. 10- 1-81 - iso-BuAc to Celanese, Celriver Terminal - iso-butyl propionate 0.02 wt.% vs. max. of 0.01 wt.% - 192,150 lbs. - QD. 10-1-81 - PE-Tech (Lube grade) to Reichhold Chemical Co., Oakdale, La.15,000 lbs. - SQD - Note: This Lube grade PE shipped as Tech grade as per manufacturing agreement. 003602 GDB-149-81 Page Four November 6, 1981 10-2-81 - iso-BuAc to Celanese, San Pedro Terminal - n-BuOH content @ 0.08 wt.% vs. max, of 0.05 wt.% - 147,460 lbs. - QD. 10-8-81 - iso-BuAc to Celanese, Newark Terminal - iso-butyl propionate @ 0.02 wt.% vs. max. of 0.01 wt.% - 194,220 lbs. - QD. 10-28-81 - iso-BuAc to Celanese, Argo Terminal - iso-butyl propionate @ 0.02 vs. max. of 0.01 wt.% - 192,720 lbs. - QD. Product Para F-Powder Para C-Powder Diacetone Alcohol Formaldehyde n-Butyl Acetate Sodium Formate Pentaerythritol-Tech* *(Lube as Tech) iso-Butyl Acetate ji-Butyraldehyde Para 95% Flake . % QD1 Month 0 0 0 0 0 0 0 100.0 0 0 % QD YTD 0.9 0 1.2 0.2 4.2 0 0 10.9 0 0 % SQD2 Month 0 0 0 0 0 0 0.6 0 0 0 % SQD YTD 2.3 5.5 0 0 1.4 1.1 1.4 0 0.5 7.3 1 Lbs. of product shipped out of Manufacturing Control Specification vs. total lbs. of that product shipped for month and YTD. 2 Lbs. of product shipped out of Sales Specification vs. total lbs. of that product shipped for month and YTD. 003603 GDB-149-81 Page Five November 6, 1981 Sample Count Chemical Section Instrument Section Total Technician Overtime Chemical Section Instrument Section Total Analytical Statistics Oct. Oct. YTD 4416 2757 7173 45914 26975 72889 28 ____ 9 37 538 330 868 Sample Shipping Domestic Export Plastics Others Total 42 593 2 52 1 11 13 102 58 758 QA Statistics Shipments Waivers (QD) Waivers (SQD) Complaints 605 6479 5 ' 24 1 13 4 15 Previous YTD 45586 22971 68557 627 325 952 655 27 77 77 836 7288 15 23 29 003604 GDB-149-81 Page Six November 6, 1981 II. STAFF CHEMISTS Process Technology B. C. Kerr Technology Manual Revision - The revision of the Chemcel Plant Technology Manual is approximately 80% complete. Text sections for the new MO IV con version and expansion and some parts of Utilities remain to be completed. Several Process Flowsheets are still needed from Process Engineering. First draft typing for the manual is approximately 60% complete. Groundwater Contamination - URM, Inc., has supplied the Plant with copies of their analyses of groundwater quality. These analyses are being reviewed in preparation for the 18 month review required for the Texas Water Quality Control Board. A review meeting with URM, Inc. is planned for November 2, 1981. Di-PE Recovery Project - A study has been started of potential methods for separating commercial quantities of di-PE from the existing PE Unit operation. At present, all effort is being devoted to an investigation of separation tech niques. If a commercially applicable method is found, then it will be necessary to determine how to produce the additional di-PE. Currently, Laboratory work is centered on trying to utilize the nearly 20-fold difference in solubilities between mono-PE and di-PE. Although it is possible to obtain a di-PE enrichment by the addition of water to Tech grade PE, the resulting slurry is difficult to filter and the enrichment is less than theoretical solubilities would indicate. Another technique which is being studied is to slurry PE in a solvent which has a low solubility in water and then emulsify water into the slurry with an inten sive blender. This procedure appears of giving di-P.E enrichment much closer to the theoretical solubility limits. Work with both n-butyl acetate and methylal have shown that Tech grade PE with an initial di-PE content of about 11% can be enriched in excess of 85% by sequential emulsion extractions. It should be noted that there is a concurrent concentration of tri-PE in these procedures. Combined di- and tri-PE concentrations of approximately 95% have been obtained in this manner. So far attempts at using elevated temperatures to reduce the volume of water required to remove the mono-PE have not been very successful. At 70C, it has been difficult to maintain the emulsion characteristics which lessen the filtration problems at lower temperatures. Work is continuing on this project. Production of Crotonaldehyde in the BG Unit - The Plant has received inquiries concerning the availability of crotonaldehyde for sale. While this product is not currently available, the potential exists in the BG Unit to produce some quantity of a relatively crude grade of crotonaldehyde concurrently with BG production. This potential has been discussed with the Technical Center and Process Engineering. A letter outlining the operational equipment requirements for co-producing BG and crotonaldehyde is being planned by H. H. Thigpen. Special Analytical F. R. Dow Polyol Feed to BOD II (Dow, Wise) - Analytical procedures have been finalized and documented for analysis of Polyol components in the BOD System. Routine analysis will be transferred to the Instrument Laboratory. 003605 GDB-149-81 Page Seven November-6, 1981 Rainwater Runoff (Dow, Wise) - Daily samples from Chemical and Plastics Co. rainfall runoff were composited and analyzed for COD and identifiable components. During the period from 10-5-81 to 10-29-81 the Chemical Co. COD range was from 15,680 to 55,760 ppm and the Plastics Co. COD range was 322 to 1317 ppm. The major component contributors from the Chemical Co. were sodium formate, 1,3-BG and PE. Analysis of GE-60 (Antifoam) in Formaldehyde (Dow) - A complaint was received from Dow Chemical, (Freeport) stating that a "scum" formed on their versene when it was made with Celanese formaldehyde, but the "scum" did not form when Monsanto formaldehyde was used. Dow also stated that analysis by mass spectrometer showed the "scum" contained a high concentration of silicone. With this information it was concluded that the potential problem may be with the addition of GE-60 antifoam in the MO distillation columns or the addition of GE-60 with metolose stabilizer. The Chemcel Plant Method B-l-30 to analyze GE-60 [poly(dimethylsiloxane)] was evaluated and found to be unacceptable for the analysis of Si in formalde hyde. Further work determined that any ashing procedure would volatilize the GE-60 before it could be properly ashed. An alternate procedure is being investigated to extract the GE-60 and to analyze the extract for Si by AA. III. SPECIAL PROBLEMS - H. H. Thigpen, 0. W. Schnellenberger Methanol Oxidation, Formaldehyde Blending T. A. Jasek, J. F. Glenister, R. L. Day, B. K. Huelle, J. E. Russell Analytical AMR* s (Glenister) M0 III Start-Up "A" Train September 30, 1981 Indicated 0.80-0.83 0.80 MO I Start-Up October-20, 1981 Analytical* 1.45 1.60 1.32 1.37 1.28 0.990-1.0 0.999 0.993 0.954 0.952 * Unit was starting up a low methanol feed, therefore, throughput for analysis was low causing higher than expected analytical-AMR's. 003606 GDB-149-81 Page Eight November^, 1981 Specific Gravity Using Westphal Balance (Jasek) - The Laboratory provided Operations with a backup method for determining the specific gravity of the methanol-water solution in the vaporizers at MO IV. The backup method uses a Westphal specific gravity balance. A foinnula was developed which will calculate the percent water (wt.%) in a range of 35-55% and 10-30C. Tech nicians at the Laboratory and Operations personnel were trained in the use of the Westphal balance. GC/MO Reactor (Jasek) - The new Varian chromatograph was set-up and plumbed, for the GC/MO reactor. The reactor will be installed shortly. Studies utilizing the GC/MO reactor will then begin. Precipitate in Unstabilized 37% Formaldehyde, Tank '2603 (Glenister) The Analytical group noted the presence of a precipitate from the check for methocel in 37% unstabilized HCHO from Tank 2603. The precipitate varied in appearance from samples of a white, red mixture of particulates to presence of a red colored precipitate. An increase in this precipitate occurred around October 12, after MO IV shutdown and when MO III product was started into Tank 2603. Analysis of limited quantities suggest the presence of Dacalite, a filter aid used in the Blending Unit- Tank 2603 was cleaned the week of 10/2610/30.' The Laboratory will follow-up-on. results following the cleanout. Presence of Substances in 37% Stabilized HCHO Causing "Scum" Formation in Dow Versene 100 (Glenister) - Dow Chemical Co. reported the formation of a "scum like" layer in their versene (50% water solution of EDTA) when made using Celanese 37% inhibited formaldehyde. A sample of this versene was received and the scum isolated using a procedure suggested by Dow. An IR spectra of the unknown material was obtained and compared to the IR's of MeCl2 extractions of some components of the Celanese formaldehyde. Various extractions of GE-60, stabili zer and versene scum were analyzed by capillary gas chromatography by B. Wise. The Laboratory also received a sample of Celanese 37% inhibited formaldehyde used by Dow, it was extracted with MeCl2 and the separate layers analyzed by capillary gas chromatography. These results were compared to those obtained for the MeCl2 extractions of GE-60, stabilizer mix, and the versene "scum". No conclusions can be drawn to date. The study continues. Dow conducted a Plant trial using unstabilized 37% formaldehyde successfully and are currently using the unstabilized 37% in their process. The Laboratory is checking the stability of the 37% unstahilized formaldehyde at lower temperatures, to examine the effect of lower temperatures on storage. MO Catalyst Sinter Test (Glenister, Jasek) - Operations has placed a charge of Engelhard-198, fair sintering silver in MO II and MO III respectively. The Laboratory will monitor its performance. Formaldehyde Assay Discrepancy Between Acme and Celanese (Huelle, Russell)Work has been completed and results reported in a letter published in late October (BKH-08-81, JER-35-81). The study showed the pH adjustment of the sodium sulfite to be the key difference between the methods. Acme-s adjustment of the sulfite solution before the addition of HCHO causes approximately .24 wt.% error in the assay. 003607 GDB-149-81 Page Nine November.6, 1981 A small ('''0.1 wt. %) error in the Celanese HCHO assay method caused by excessive indicator was found and corrected. Using caustic as a "substitute" standard, the Celanese method proved to be more accurate than the Acme method. The reproducibility of Acme's method was adversely affected by exposure of the calomel electrode to the sulfite solution. HCHO Stability Study (Day) - The HCHO stability study was full time this month. Samples were set up from MO I, MO II, MO III, MO IV, the blending unit, and unit storage tanks. Each sample was analyzed for assay, acid, color, sodium, and iron. Age of the HCHO was also noted. Twelve ppm metolose stabilizer was added in the Laboratory. The samples in the 49C oven have lasted longer than our spec, of 30 days. In the samples set up in the 40C oven a large range was seen in stability. Some samples lasted as few as 3 days, and some lasted as long as 24 days. A study is underway to attempt to correlate the presence of specific im purities with stability. An extraction of the HCHO followed by capillary GC analysis of the extract is used to indicate the presence of specific impurities. Several solvents were screened for use in the analytical procedure. Methylene chloride, chloroform, a butyl ester, a butyl ether, and 1,4-dioxolane were evaluated. Based solely on one data point, there may be several initial im purities that correlate with stability. Before any specific conclusions can be drawn, however, additional data must be collected. Monsanto HCHO (Day)- We are currently receiving Monsanto HCHO for resale and internal use while MO IV is down. Four quarts of this Monsanto HCHO were quick-frozen for future evaluation. The Monsanto HCHO was extracted with methylene chloride, and the extract was analyzed by capillary GC. There are differences in the GC scans of Monsanto .and Celanese HCHO. Some of the Monsanto HCHO is being evaporated down to isolate their stabilizer. This stabilizer will then be put back in our own HCHO, and its effect on HCHO stability determined. Trimethylolpropane R. L. Day Unit Support - None provided 747 Residue Methanolysis - No progress, full time on HCHO stability. Extractor Optimization - No progress, full on on HCHO stability. 003608 GDB-149-81 Page Ten October 6, 1981 Pentaerythritol L. M. Harvey, B. K. Huelle, J. E. Russell Recover PE Prom VCI Waste Stream (Harvey) - The process recently proposed by the Laboratory for the simultaneous recovery of PE and 2ethylhexylamine (2EHA) from VCI extract does not appear to be economically attractive due to its energy-intensive nature. VCI is proceeding with plans to recover the 2EHA using a wiped-film evaporator (WFE). Efforts to recover PE from the proposed WFE residue indicate that some amount of 2EHA must remain in the WFE residue to obtain a PE of suitable quality for recycle. The 2EHA in the WFE residue would function in the same way as in the proposed process using VCI extract (to extract impurities from the aqueous PE stream) . Since an azeotropic distillation step similar to the original proposal would be necessary in any PE recovery scheme (to insure complete removal of all 2EHA from the PE recycle stream), studies are in progress to determine the minimum amount of 2EHA which must be left in VCI's WFE residue in order to obtain a PE stream of suitable quality for recycle to the PE Unit. Efforts to simulate VCI's proposed WFE met with mechanical difficulties. As 2EHA was flashed from VCI extract material, PE precipitated on the walls and the blades of the laboratory-model WFE making steady-state conditions impossible to achieve. Mr. Joe L. Bush of VCI said they had no evidence of a similar problem in their pilot-scale WFE; however, frequent washings of their WFE with water did improve their 2EHA-recovery efficiency. A simple batch flashing procedure is being used instead of the laboratory-model WFE in experi ments to determine the minimum amount of 2EHA required in the WFE residue for PE recovery. Evaluation of Filter Cloths for the A and B Belts (Huelle) - An evaluation of filter cloths for the A and B belts is near completion. Eight filter cloths were evaluated; three cloths with the best flow races were evaluated further at various cake thicknesses. None of the cloths had porosities great enough to allow fines to break through. The cloth .currently in use is among the top three candidates. PE Hydrolysis (Russell) - The final Laboratory report was issued. 1,3-Butylene Glycol J. E. Russell V-778 Residue Burning - The analyses of September samples of V-778 Residue were completed. The results were published. Acetaldol for Nepera - A one-gallon sample of T-219 Residue was collected and sent to Nepera's Harriman, New York facility at the request of Dallas Quality Assurance. The sample was not assayed, but is expected to contain 3040% acetaldol in water with samll amounts of crotonaldehyde and acetaldehyde. T-219 Analytical Method - A method is being developed to analyze T-219 over head and T-219 residue for acetaldehyde, crotonaldehyde, and acetaldol. A good 003609 GDB-149-81 Page Eleven November .-6, 1981 analytical method will enable the Laboratory, Operations and Process Engineering, to optimize T-219 operating conditions. At optimum conditions T-219 should strip enough acetaldehyde from the reactor product to minimize efficiency losses to ethanol, but conditions should not be severe enough to dehydrate the acetaldol to crotonaldehyde, which is an efficiency loss to BuOH. Currently, an analytical method is being developed which uses the Laboratory's liquid chromatograph. BOD - Utilities P. W. Young, D. R. Akin, J. C. Bustabad, G. R. Stasney BOD II Support-(Young) - Continued support was provided to BOD II operations. Input was given on the procedure to add polyol effluent to BOD II. Technical support will be given during this addition. Polyol Treatability In BOD II (Young, Stasney) - A Laboratory anaerobicaerobic system (No. 3) was acclimated to 7-8% steady state polyol effluent (C0D=3i,000) ("*25-30% COD). Operated at an organic loading (OL) of 0.2 lbs COD/ ft3/day and an aerobic detention time of 3.5 days. The aerobic outfall C0D= 160-180 ppm. At this time, 5.5% VCI effluent was added to the above feed (OL=0.28 lbs C0D/ft3/day, aerobic detention time = 2.9 days). The aerobic out fall rose to 300-500 ppm. Feed was lowered (OL'^0.2, det. time ^3.5 days). This upset probably occurred due to the rapid increase in F/M in the aerobic section. This shows that acclimation time and time for increase in biomass concentration is needed to include 5.5% (25 gpra) VCI in BOD II feed. Upon recovery, the OL of 0.28 and detention time of 2.9 days will be attained slowly, thus giving the bacteria acclimation time. Live polyol samples are being collected and analyzed for future laboratory pilot unit feed. VCI Waste Treatability (Young, Stasney) - Many different samples from VCI waste are being fed to the Laboratory anaerobic-aerobic system (No. 2) to see effects of variability in VCI effluent. No adverse effects are being seen so far. Plastics Laboratory Effluent (Young, Stasney) - Eighteen samples were col lected from CP & SC Laboratory. The results are as follows: flow rate: 600012000 gal/day, mean COD: 501 ppm, metals: Na: 145-300 ppm, Ni + Cu + Cr: 0.040.26 ppm. BOD II Aerobic Optimization-Sludge Age Study (Akin-, Stasney) - This study was completed during October. The 25 and 35 day sludge ages both had similar COD removal efficiencies, but by utilization of the 35 day sludge age, sludge waste age would be minimized. Settling velocities observed at both sludge ages were much higher than is required in the clarifier. The recommended sludge age for the BOD II system with its present feed is 35 days. This study will be documented and another study begun to determine the optimum sludge age for the BOD II system after the addition of polyol effluent. Aerobic Treatment of Polyol Sump (Akin, Stasney) - A study is underway to determine if polyol effluent can be treated by aerobic methods alone. A Labora tory unit is removing 70% of COD from a feed with a COD concentration of 8800 ppm. 003610 GDB-149-81 Page Twelve November 6, 1981 This feed is 27% by volume polyol effluent and 63% effluent from another laboratory unit simulating BOD II. The COD contribution from polyol effluent is 90%. The feed detention time is 12 days. Further work will attempt to optimize the system. Oxygen Uptake Rates in Aerobic Systems (Akin, Stasney) - A study has begun to follow trends in oxygen uptake rates (OUR) versus mixed liquor volatile suspended solids (JILVSS) in aerobic systems. Three laboratory units and BOD II aeration basins have been monitored for changes in OUR/MLVSS. The OUR/MLVSS in creases in proportion to increases in feed to biomass (F/M) to the aerobic systems. Since the OUR/MLVSS increases in proportion to F/M the COD removal efficiency remains relatively constant. This trend only holds true up to a level where the excess feed becomes toxic to the biomass. At this point OUR/ MLVSS begins to drop. When the loading is reduced to a level that can be tolerated by the biomass, OUR/MLVSS resumes its normal level. A drop in OUR/ MLVSS is followed by a drop in COD removal efficiency. This was observed in anaerobic/aerobic system No. 3 treating polyol when VCI waste was added at too high an initial loading. As loading increased so did the OUR/MLVSS. COD removal efficiency was relatively constant as the VSS respiration rate kept up with the loading increase, but once the loading became too high, the OUR/MLVSS dropped drastically indicating a toxic affect from the excess feed. Two days later the COD removal efficiency began a steady decline. This would indicate that the OUR/MLVSS could given an advance warning of COD removal problems be fore they occur. This would allow the loading to be lowered based on OUR/MLVSS rather than COD removal efficiency, which could eliminate a larger upset than normally would occur. Published reports on this subject recommend an OUR/MLVSS of <10 mg Qz/g VSS x Hr. The BOD II system currently operates at a satisfactory level of 'V'7.5 mg Qz/g VSS x Hr. This study will continue indefinitely. Pre liminary information will be documented. Operations has been contacted to try to get the on line respirometer in service to aid in this work. Clarifier Operation (Akin) - The Laboratory has initiated a study into clarifier operation to determine the optimum operating controls. A report published by Environmental Dynamics, Inc. indicates in order to optimize clarifier operation (lower outfall TSS, settle solids, recycle solids) one must reach a balance of hydraulic loading to the clarifier and of solids recycle back to the aeration basins. The Laboratory will work with Operations to determine this balance. Vacuum Truck Content Characterization (Akin, Gonzalez) - In order to develop a system for disposal of vacuum truck wastes, a study was begun in late September to characterize vacuum truck contents. Analyses of these contents include pH, viscosity, specific gravity, specific filtration resistance, % solids, % oil layer, and COD. October composite COD concentration results of each unit that used vacuum trucks are as follows: 1) Paraform - 45,000 ppm, 2) M0 IV 580,000 ppm, 3) Polyol - 29,000 ppm, 4) Landfill - 77,100 ppm, 5) Oxo 27,610 ppm. 6) MS - 3,110 ppm, 7) MO III - 11,292 ppm, 8) Tank Car Cleaning - 23,400 ppm. Complete analytical results will be published when characterization has been completed. BOD II Sludge Hazardous Waste Determination (Akin) - Sludge from the BOD II aeration basins has been determined not to be a hazardous waste as determined 003611 GDB-149-81 Page Thirteen November. 6,1981 by EPA methodology. EP toxicity result levels were well below maximum permissable levels. Corrosivity of the sludge was also well below the maximum allowable levels. Results of this determination will be published. Methanol Synthesis J. C. Bustabad, J. E. Russell Evaluation of Methods for Determing Microbial Biomass (Bustabad) - A cursory evaluation of the ATP method showed good reproducibility on duplicate samples. Evaluation of this method will continue when more of the required reagents are received. Familiarization of the literature on the dehydrogenase method of biomass determination has begun. Monitoring of H2S in Recycled CO2 (Bustabad) - An October 26th check of H2S and COS in recycled CO2 from the 5 MM Girdler amine system and the Shift amine system showed nondetectable levels (<35 ppb) by Tracor. Plant Trial of Sodium Metavanadate (NaVOa) as a MEA Corrosion Inhibitor Coordination of Laboratory support for a NaV03 Plant trial was provided. Monoethanolamine (MEA) in Storage - A further check of the MEA in storage in V-345 and V-346 showed the sulfur compounds detectable to be relatively stable sulfates (121 ppm SO4 and 41 ppm SO4 in V-346 and V-345 respectively) . Sulfates in the MEA system are not suspect of creating process problems. How ever, further Laboratory work was completed to determine the effect of reclaim ing on sulfate concentration. A laboratory distillation of MEA from V-345 showed that sulfates, as expected, concentrate in the bottoms. (Overheads were 4.3 ppm SO4; bottoms were 67 ppm SO4.) A letter will be issued shortly on this study. Syn Gas to Oxo - Atypical analyses in the Oxo Unit prompted a check on October 26th of syn gas going to Oxo. An effort was coordinated with CCCTC to determine the concentrations of major components in the syn gas sample. Re sults showed no abnormalities. Amines in Clear Lake MeOH (Russell) - Three samples of MeOH were received from Mallinckrodt, one of which was rejected for high odor. Mallinckrodt had purchased the MeOH from Clear Lake through Transchem. The other two samples were free of odor and one also came from Clear Lake while the other was GeorgiaPacific MeOH. An analysis of the high odor MeOH on the ion chromatograph showed approximately 10 ppm monomethylamine. The odor-free MeOH samples showed less than 1 ppm amines. The results were published. Oxo, Butanol J. D. Presley Reactor Stability/Accountability - We continue to have^.analytical problems providing consistent TPP concentrations in Oxo catalyst. The reactor is operating well. 003612 GDB-149-81 Page Fourteen November 6, 1981 Graphing percent of design capacity versus time for Oxo Runs I through VII indicates no cummulative relationship between the percent of time the unit was run above 90% rates and the length of the catalyst life. However, based on Runs I through IV it is believed that after the catalyst is older (e.g. six months), a rate versus time relationship is evident. Based on these runs, older catalyst should ideally not be run below 95% rates for more than 10 consecutive weeks. Longer, low-rate, run times are believed to cause excessive build-up of "foamers" in the catalyst which will necessitate catalyst change out. Work continues to better define these relationships. Rhodium Accountability - Reactor rhodium accountability for October is about 89%. As with last month, higher than normal reactor rousing causes in accurate level readings. Using an approximate correction factor the account ability is about 95%. Losses from T-210 Residue RTD are about 8.2 pounds of rhodium for the run-to-date. Improved Rhodium Recovery - In a meeting with Operations, Process Engineer ing, and the Laboratory it was decided to go ahead with a Plant trial to phosphoric acid extract 250 gallons of Run VI catalyst. Work continues. An RFPA for phosphoric acid extraction has been submitted. Various solutions are being used to extract Run VII catalyst to reduce foaming. No results have been obtained. Foaming tests will be run at CCCTC when all samples are ready. Work continues. Two stage propylene extractions have been used to isolate a catalyst solution fraction. The fraction is believed to contain high concentrations of foamers. Work continues to further concentrate and identify the foaming agent(s). An effort was made to prove that Run VI catalyst activity will improve as the 2-ethyl-2-hexenal is stripped as it is added to Run VII. A sample of the Run VI catalyst was maintained in a hydrogen atmosphere at reactor temperature and pressure to hydrogenate the 2-ethyl-2-hexenal. After about 3 hours the 2-ethyl-2-hexenal was dropped from about 40% to about 4%. Catalyst activity before hydrogenation was about 0.85 liters/mole-sec. Afterwards, the catalyst displayed an activity of about 0.92 liters/mole-sec. Industrial Health C. E. Gary, K. V. Parker Personal noise exposures were taken to obtain a better statistical base. Report in preparation. Additonal personal formaldehyde exposures sampling was done to provide a better statistical base. Report in preparation. A personal noise exposure survey of Maintenance personnel was begun.(KVP) 003613 GDB-149-81 Page Fifteen November 6, 1981 The Chemical Laboratory CEA-555 instrument was check-out to determine formaldehyde exposure concentrations. The unit pump failed and the instrument was sent to the factory for repairs. The CP & SC instrument has been borrowed and will be replumbed and checked out. (CEG) The Metronics Dynacalibrator has been installed and one familiarization run completed. A modified sampling system is being fabricated. (CEG) 0036-14 (1 cd -c Q CM rH CO CO ON ON M rH ^H CO CO CO rH rH 00 CM 00 43 >XJ rH ON M ON ON ON pH rH CM rH 00 ON ON rH rt 0 c 00 c * Vi * 00 e * 00 M *A ON * c^ m 0) *H C 0) P H Vi c> 3 a) VX V V4 3 43 XI X hi 4) k X Vi (U uX H (U CO rt E sE X E CO E W XJ C ?> o 3 XJ M CJ 3c "3 Q (U CO XJ pH CO X XcJ H rH CO 0) E <0 CO XJ o 0) > (0 co o a) f-4 XJ p Vi CO O pH xcj o u CL M HJ CO * Vi O 0) O cV u oj H > XJ 4-1 o 0) pH CO V( H < 3 Q. U o pH H Si CO W CM Cft CO > UH a *rl rH "3 Si :*. xj ac w XJ CQ CO CO 0) CO XJ >> *H >1 c (0 h a rH td CO *H CO 03 XJ 4h XJ o cd -i CO X H O Ed o CO . CO o CL CO H a XJ H o < XJ a CO >1 C C 00 o o Vi *H H ca) XJ XJ CJ a w CO 33 X3 XJ UB V (U rH Cd O Si XJ XJ 0o3 2 uo a> H (3 (1. CoQ 2 CO ao CO o u oCQ 2 CO CO c H > CO CO pH CO H U . o. H hi 0 4 V, cd a, CM pH CM rH rH rH CM M o 43 CL >XJ w CQ P4 sX c 0) <0-- 43 4} CO o 3 Vi > 43 4) pH 3o >v > Op Vi a CO X \ u Voi XJ <J U oo 0) c H CO (U cd c o H XJ CO > iH CO XJ C XJ CQ o <D CO o CU xj u *H Vt Hi u CO xj (0 X oc rHo *OH > C XJ rH CO CO XJ CO XJ N XJ H 01 H CO 4> lM O 2 *XHJ H XJ o 2 O a. ao O 2 < XJ o H "H c ff aX a CQ D 0X 43 XJ Cd V< Vi O Cd CL CL XJ C/3 3o D XJ co E M O *rH 0) pH pH XJ CL Ou H oX pH o ai Pi *H CO Vi e Eo C *H Vi CO XJ CJ Vi 43 QJ Ou O C/3 00 co CO cn pH *H Cl Pl Cd EpH CO *H CJ iH CJ 43 CO XJ Vi ?s jz 0) > oc 43 CL -tH C/3 XJ X .E X 43 XJ o pH 03 Vi O O 1-1 XJ <0 Vi 4) 43 60 3 CQ XJ rH CO XJ XJ 3 E Voi C Vi 3 H O oc <cuo rH CO > > O o H CO 1 CO E C3 43 3o 3 CO CL, 4 2' Voi pH 03 2 es U1 Cd Qo H 003615 0) <0 -o Q .0S)__ew d0 <" .-* C ** r* 0) 4J ^ 03 Q* W O o CM 00 9k JZ u u (0 CM CO CO on CO on CM r-* 00 on Ul "4 o >> JO U E CO X 4 a? xj 3u a. x <cu a; ai 3 CO *"0 CM . w CM oo 00 GOOs ON- ON *1 ^M * A >> }M U CO to 3 3W G O <uv Xe 0) O <0 0) 0) np CM CO On U to 3U JO 0) tu --M CO ON r_1 CO ON 9k **M --H Jm u oj CJ *JD eE 0) CJ au a CJ aQ r--4 00 ON CO Ui o O CJ CJ CJ n c 0 0] *J rt u o o u to Qh 3 CO c C 0) .a o PH P>s XJ Oh fM Pi O H rt U. CU u XJ (0 c CO 1) r-4 BC <0 11 u0 z u H cj > c (0 Cd = <0 ao (X - - CSI CM = r CQ Q o CoQ - ^M *--1 cP 0) k u Q to C3 v 00 c 3o ........... 3 u1 Jm o XJ a. H CO (U H (0 c o a 0) 1-4 X) XJ CO c rH *H c 0) 3 c> H 0J to j= 00 0) E CU U *-< (0 O 0) X w n fcu (J CO * o Ui (0 ao. H XJ >1 a XJ to 1-1 CO o X c o CO u a# tr tn-H a> Pm H Vj *o WC *->tir CJ C > >o c a co c CJ dir- 06 X < i-H oe XXtoJ 00 CD MC u o <4-1 pa(-0%j pS--4 C3O t0>oM) < .c o i-X*4J H XJ Xt<oD i-H to XtoJ HH >to H 1m CO X(0J XJ o T33 HC-4 xX01J 0) i-COi zO 0) U 00 cc (0 XCaJ> *UH XoJ C *H H C to O to 3 T--posl Po-I XJ Ou i-H &,CL (0 -H 3U co H o *H p o u 0) to <g XJ a 3 XJ C oo tX(0r0Ji) CO XJ to 0lM) H VrMo>H o i-4 OOi -ca to c % XJ XJ 3 (U X 1-1 C/3 3 *3 xj c w< c o *H XJ CJ 3 XJ CJ Oh XJ to u CO GcO > CO CO CO CO H J-4 CJ XJ tO PS XJ P^ CO o rj Tto V XJ CJ ---------CO Jm 3 Pm C o XJ CO 3 to > 'O Xo XJ - 0) VCoJ *H z c o u u X W CO *r4 u H ox Q M> c* 3 Cd 0) XJ CJ MM> 3 o o w 003616 t) <0 ^4 T3 Q CO CN CN On CO CO Jl fi H o\ Ox ^4 *4 (0 0 * c * h Q) 44 r~ CD Q* W 0 P s p a/ (0 X 3 P QJ XU 0) <u fa (3 AA PP 0) a) XI 0) QJ CJ O 0) QJ op ecia 003617 c c o o *H fH P w 44 rt CO a H ou <P H V H Q *44 r4 P P e co 44 P 3 u H to o a. 3 fa 3 O' CcO to C/3 0 H c tn CO C H CO 0) C/3 *H CQ jFt s Q 5X X 0 P tK CL P o H 4 J* H CN e o p CJ 3P T? P 0) O fa a a P3 <0 cn o oH fc (22 C/3 D2 CO o y oo X 3 sE CN H r4 a 44 w 03 4 44 `P s c r4 V T3 \ c 0c0 CO JO / rt 3 fa O CO V --7 < > CO 3 CQ l CO N QJ P CO H H rH CO c rH CO c P *H aX QJ *H 00 P o H o CO p oH p P CJ CO *3 P CO N *rt X p0) >> C X CO H oH QJ rH ccn o e *H X-N fa T3 p QJ < -ca o o fa cA P Oi <H O3 P PU H CO CO p o rH CHO W m foaC4 * afHa. OH CO JO 0) o <u0 *oH pa p p CO rH 0 cn pae) 3E T>3> O3 aO wP A O 0) P CO CO *T3 3O X fC>aO p<u X 3CJ O o rH P OaPO. 3 cn