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CELANESE CHEMICAL COMPANY Chemcel Plane Bishop, Texas
To: R. R. Graham ,j.l
From: G. D. Boyd
GDB-93-81
January 9, 1981
Laboratory Department Summary December, 1980
Chemical
J. J. Fritsch W. H. Brough J. B. -Brown R. R. Carpenter K. G. Gallimore R. S. Hahn J. M. Hodges R. W. James B. C. Kerr C. W. Lee D. E. Lockwood R. P. Lowry A. G. McGehee D. G. Pausky 0. W. Schnellenberger G. R. Scholz D. D. Siemonsma W. L. Sharp H. H. Thigpen W. H. Meyer W. L. Wallace Bishop Files
DISTRIBUTION
Plastics
A. C. Abshier R. G. Brandt R. L. Bunkley H. L. Davis H. W. Hill E. Munoz 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 Terminal J. L. Paul, Clear Lake W. H.' Tuke, Pampa T. H. Golson, Dallas
File No: 303.3
003447
1381
CELANESE CHEMICAL COMPANY Chemcel Plane
Bishop, Texas
To: R. R. Graham From: G. D. Boyd
GDB-93-81
January 9, 1981
Laboratory Department Summary December, 1980
* A summary of each Group's 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 assign ment. A table listing the priorities, justifications, estimated completion dates of current Special Problems projects and a graph eff the Laboratory Effort Analysis is also included in Section II.
GDB:jr
G. D. Boyd
003448
Page Two January 9, 1981
I. ANALYTICAL GROUP
Competitive Products
No competitive products were evaluated in December.
Polyol Unit
Pentaerythritol - Analytical Group support continues in efforts to determine the cause of high UV absorbance in Pure PE product. Lot selection is necessary to meet the DuPont special specification.
Corpus Terminal
Barge Shipping - After two barge loads (approximately 840M Gal.) of MeOH contaminated with hydrocarbons arrrived at the Bayport Terminal, special inspection of the new type barge in service (NMS 1496) revealed an unblinded vapor collection header as the probable cause of contamination. Follow up shipments in standard barges have arrived on test and the product has been blended to specification.
Special Analytical Services
Lube Grade PE (F. R. Dow, B. W. Wise) - A meeting in Fords, N. J. with representatives from Hatco Chemical Corp. was attended (December 8, 1980) to discuss the PE composition Hatco requires to produce Lube Esters. This meet ing had the same objectives as the one with Emery Industries in November, 1980. Both customers desire approximately 85 wt.% mono-PE and a minimum di-PE of approximately 12 wt.%. The tri-PE concentrations should be < 3 wt.%.
Samples of purified PE by-products and two PE samples (pure and tech) were given to each customer for analysis and exchange of analytical data.
Identification of Solar Pond and Monitor Well Components (F. R. Dow, B. W. Wise) - Capillary GC analysis of the solar pond and monitor wells for the Texas Water Quality report was completed and submitted for incorporation into the final report.
Ion Exchange Chromatograph (J. E. Russell) - The Ion Exchange Chromato graph was used for quantifying the Cl"in the AML, VCI centrate and VCI NaFo product streams. Additionally, NH44", PO42. and N03~ were determined for wastewater nutrient analyses on several screams. Several other special anal yses were performed to explore the capabilities of the instrument. Analytical methods for nutrient analyses have been defined, but need some problem solving before they are instituted. One particular problem is precluding microbial growth in the resin columns.
003449
GDB-93-80 Page Three January 9, 1981
Quality Waivers and Delays
Delays - None
Waivers
12-4-80 - Methyl Formcel - 15M Gal. to American Cyanamid, Wallingford, Conn. - Assay 54.9 vs. special customer spec, of 55.3 wt.% minimum.
12-12-80 - n-Butyraldehyde - 20M Ga. to Monsanto Co., Indian Orchard, Md. - n BuOH < 0.16 vs. M.C.S. of 0.10 wt.% maximum.
12-29-80 - 52% HCHO - 20M Gal. to Plastics Engineering Co., Sheboygan, Wisconsin - Acid < 0.017 at shipping vs. special customer spec, of 0.015 wt.% max.
Customer ComDlaints
12-1 and 12-8-80 - MeOH - 840M Gal. to Bayport Terminal. Product arrived contaminated with hydrocarbons.
ANALYTICAL STATISTICS
Sample Co'unt Chemical Section Instrument Section
Total
Technician Overtime Chemical Section Instrument Section
Total
Dec.
4051 2263 6314
Dec. YTD
53797 27720
81517
53 720
5~17
455
-
110 1175
Previous YTD
60413 32570 92983
980 507 1487
003450
Page Four January 9, 1981
Analytical Group General Approved, revised Manufacturing Control Specifications for all Plant products have been received from Company QA Group. They will be disseminated and implemented during the first quarter 1981. SNE employee K. D. Pratt resigned 12-19-80. Yvonne Trevino transferred from the Plastics Co. Laboratory to the Analytical Group 12-29-80. J. E. Russell attended a Dionex Seminar on ion exchange chromatography.
003451
Sample Shipping and Quality Aaauranca Statistics
Statistics For Porpwhpr 1980
Sample Shipping
Domestic Export Plastics Other
Month
Total
40 5 1 5
51
YTD
735 35 78 88
936
Previous YTD
782 30 18 79
909
Quality Assurance Statistics
Shipments (NO.of Orders) Delayed
Internal External Comolalnts (Total) Comolaints (Legitimate) Complaints (Non-Legitimate) Complaints - Outstanding
(Unresolved)
Month__________
YTDPrevious YTD
936 8903 07
11167 31
0 23
7
3 28
40
1 34 1 15 0 19
47 19 28
00
0
003452
Page Five January 9, 1981
II. SPECIAL PROBLEMS GROUP
Process Technology B. C. Kerr
Solar Pond Disposal Study - This project received very little attention this month due to higher priority work.
Enforcement Compliance Directive Report - The report was completed and delivered to the Texas Department of Water Resources Wednesday, December 31, 1980. My work for the month was nearly 100% devoted to this project.
Methanol Oxidation, Formaldehyde Blending T. A. Jasek
GC/MO Reactor - New heaters were received and installed. No further progress due to priorities.
MO Silver Catalyst Modifiers - A test sample of silver crystals were grown from a silver nitrate solution containing 1000 ppm bismuth (Bi). These crystals had a spongy appearance, which were different from the crystals previously grown. The Tech Center plans to evaluate the crystals in the micro unit. Also, the crystals will be analyzed for Bi content.
Methane Slip in the PPG and Selas - The Laboratory was requested to confirm the methane slip in the DPG and Selas outlet indicated by the pro cess analyzer. Using the same standards (prepared by CCCTC) used to calibrate the process analyzers, the Laboratory confirmed the process analyzer results. However, CCCTC analysis of the DPG sample did not agree with the Laboratory results. CCCTC analysis of the standard used by the Laboratory showed it to be lower than thought. Reanalysis by the Laboratory of the DPG sample against a Bishop prepared standard confirmed the Tech Center results. A new standard was prepared by CCCTC for calibration of the process analyzer on the DPG and Selas outlet.
November MO Color Problem - Ethyl ether extracts were obtained from T-280 SS and MO-IV vaporizer blowdown. These were analyzed on a capillary GC. Numerous peaks were observed. The samples will be sent to CCCTC during the next month, to determine (by GC-Mass Spec) if some of the compounds present are or could form colored species.
Utilities, BOD S. G. Smith, P. G. Welling, G. R. Stasney
Anaerobic-Aerobic Pilot Studies
Start-Up Study/Upflow Velocity Study (Welling, Stasney, Smith) - For over five months, two anaerobic-aerobic units have been operated to study the effects of upflow velocity on start-up and solids accumulation in the
003453
sjv*d-- j j--yw
Page Six January 9, 1981
filter bed. Filter it2 was operated at an upflow velocity of 1-2 ft/hr (to maintain the 10:1 recycle to feed ratio), while filter #3 was operated at an upflow velocity of 10 ft/hr (to simulate the upflow expected in the commercial unit). The feed to the filters contained Polyol sump, Oxo sump, equalization basin material, nutrients N and P, and V-312 residue (Na+ source for filter buffering). The anaerobic filtershad attained an organic loading of 0.45 lbs C0D/ft3/day, with resulting kinetic efficiencies of 63-65% and COD removal efficiencies of 84-86%. Following aerobic treatment at a feed hydraulic detention of 3 days, final outfall COD's were 130-140 ppm.
Little or no difference was observed between the startup or perfor mance of the two filters. The effect of upflow velocity on solids accumu lation was measured by determination of filter void volumes. Void volumes were measured in two ways: (1) addition of a tracer and subsequent calcu lation of tracer dilution volume, and (2) by draining filter liquid for actual volume measurement. In the tracer measurement, 10 mis of 3.35% t-butanol (a water soluble refractory not present in our feed) was added to the filter. After recycling filter liquid by 4 filter volumes, a sample of filter liquid was obtained and analyzed for t-butanol. The volume by which the filter liquid had diluted the t-butanol is the void volume. Original (packing only) void volumes of the filters were 20.38 liters for it2 and 20.20 liters for it3. By tracer measurement, void volumes of the filters were 18.97 liters (#2) and 19.35 liters (it3). Actual volume measurements showed filter void volumes of 16.94 liters (#2) and 16.92 liters (#3). Using either method it is observed that there was little difference in solids accumulation between the two filters operated at 1 and 10 ft/hr liquid upflow velocity.
The filters were filled with river water and restarted, and both are now bein operated at a 10:1 recycle to feed ratio. Organic loading to the filters as of 12-30-80 is approximately 0.15 lbs C0D/ft3/day. Kinetic efficiencies are approximately 60 to 70%.
During the draining and restarting of the filters, the aerobic tanks were fed anaerobic filter feed with a detention time that gradually reduced from 10 days to 4 days. The outfall CODs are 85-155 ppm for it2 and 95-135 ppm for it3 at the 4 day detention.
A report detailing laboratory startup studies for the anaerobic-aerobic system has been submitted. (Smith)
Solar Pond Treatability - Basic feed to Tanks #4, it5, and #6 continued as in November. The first part of the month the tanks were given feed con sisting of 119 parts equalization basin material to 1 part solar pond material + water or equalization basin. The outfall CODs at this dilution were 400 to 415 ppm for #5 (94.5% removal) 375 to 390 ppm for it6 (94.5 - 94.7% removal) with a control COD of 220-250 ppm (96.5 - 97.0% removal). By the middle of the month, the feed was changed to 87 parts equalization basin to one part solar pond + water or equalization. The outfall CODs at this dilution were 385 to 420 ppm for #5 (94.4 - 94.8% removal), 375-405 ppm for it5 (94.4 - 94.75% removal) with a control COD of 165 to 180 ppm (97.5 - 97.75% removal). The dilution has been reduced to 71 parts equalization to one part solar pond + water or equalization. It is too early to see results of this increase in solar pond concentration. Work continues.
003454
GDB-93-80 Page Seven January 9, 1981
El^lgac^n^^ductio^of^Sola^Pond^Odor (Smith, Jasek)
A report detailing work completed on this project is being written.
Methane in Monitor Wells
(T. A. Jasek) - Six different monitor well head
yyauea wary analyzed" Tut methane (CHi*) and carbon dioxide (CO2). Methane
concentrations ranged from 2.4 ppm to 9500 ppm. Work will continue to deter
mine the amounts and changes in the amounts of CH4 and CO2 observed in each
of the monitor wells.
Utilities Support (Smith)
At the request of Operations, small particles found in the SAC resin bed of the Demineralizer were analyzed for Calcium (Ca) and Magnesium (Mg). Analysis for Ca, Mg, and Iron (Fe) gave the following results:
0.8 wt.% Ca 1.0 qr.% Mg 7.2 wt.Z Fe
Further analysis showed approximately 45% (wt.) of the solids to be volatile, i.e.,probably organic in nature.
Methanol Synthesis J. C. Bustabad
MS-II Unit Support - Drager tube monitoring for H2S in CO2 from the MEA systems of the Girdler reformers continued. Monitoring began in November when there was evidence that Dow's corrosion inhibitor, ammonium thiocyanate, was degrading to form H2S. For several weeks of this month the passing of contam inated CO2 through a carbon guard bed resulted in a slow but steady decline in H2S levels. On December 22nd elevated H2S levels were noted. The elevated levels have continued since that time with the most recent recordings of Dec ember 29th being 3.5 ppm and 2.5 ppm for the 5MM and 2MM systems respectively. The levels previous to the elevations were 1.0 ppm and < 0.5 ppm for the 5MM and 2MM systems.respectively. The cause of these elevated levels is under investigation.
Information on the Celanese developed MEA corrosion inhibitor system was researched. Tests were conducted by Jim Russell to determine the effectiveness of the ion chromatograph in determining levels of molybdenum and nitrite, com ponents of the Celanese developed corrosion inhibitor. The ion chromatograph proved effective in determing molybdenum levels. Complications were encount ered with the determination of nitrite. Work is in progress on the reliability of a UV absorption method for nitrite in filtered MEA samples.
Arrangements were made through our MEA supplier, McKesson, for extensive testing of MEA in the Girdler and shift systems on a quarterly basis. These tests will be conducted by Union Carbide -at no cost to Celanese.
003455
GDB-93-80 Page Eight January 9, 1981
On December 29th, the nickel tetracarbonyl level determined on the nitrogen purge gas from the Selas .reformer was < .001 ppm/v. The Selas had been brought down for maintenance work on a leaking reformed gas pigtail.
Oxo, Butanol J. D. Presley
Reactor Stability/Accountability - December reactor stability was poor. Fluctuations of 32% to 43% BuH, 28% to 38% TPP, and 3% to 8% Tishchenko Esters were noted. The problem is believed to be a combination of analysis dif ficulties and of mid-month unit rate changes.
Average reactor accountability remained high at better than 83%.
Rhodium Accountability - Rhodium accountability for November was 100%. However, December's Rhodium accounting shows unexpectedly high results, 123%. The high accountability started about the time unit rates were lowered to 80%, indicating possible reactor level reading problems. This discrepancy will be investigated further.
Improved Rhodium Recovery - Phase four activities have been completed. Results indicate simple Oxygen reactivation of inactive Rhodium extracted from Oxo catalyst will not work. Three tests were performed varying operating parameters of temperature pressure, solvent base, and oxygen concentration.
Extraction project work remaining includes some analytical (GC and AA) and writing of the rough draft.
Oxo Unit Support - Analyses of samples from the Process Engineering test coalescer are almost complete. TPP and TPPO values have been obtained and Rhodium values will be completed on arrival of new AA accessories.
Environmental Health C. E. Gary, K. V. Parker
The personal exposure noise survey is being continued (approximately 60% complete.) (KVP)
Two batches of insulation were tested for asbestos content. Only one contained asbestos. (KVP, CEG)
Personal exposure carbon monoxide monitoring using long term Drager tubes is 95% complete. These have been significant carbon monoxide 8 hr TWA;s. (CEG)
Standards for validating the long term Drager tube for determining 8 hr TWA exposures have been obtained. Validation tests will be begun January 7, 1981. (CEG)
003456
UUD-5J-- ou Page Nine January 9, 1981
<8
Acetates, Paraform, Formcel Products R. L. Day, D. R. Akin
Corrosion Inhibitor In Ester Unit (Day) - The corrosion coupon test racks were removed from the acetate reactor kettle and kettle reboiler on December 22nd and sent to CCCTC for evaluation of the corrosion inhibitor. A flange was installed in the reactor kettle during this shutdown so that a corrosion probe could be used in the future.
Paraform (Akin) - Assisted unit personnel in their GC analysis of methylal.
Trimethylolpropane ______ R. L. Day
ft T-312 Extractor Optimization - A second set of samples for a data base on the T-312 extractor was collected December 14-16. Analytical is 75% complete. A letter will be issued next month and will include base case data taken in July and in December.
IMP Color Problems - Laboratory support was provided during color prob lems in the IMP unit December 28 and 29. Abnormally high color was first observed in T-202 residue. This stream is usually only slightly colored, but during these two days, the color rose to as high as 850 Pt-Co units. (Color analysis was determined from a 10% solution diluted with water.) The cause of the problem was determined to be a faulty pH analyzer. This pH analyzer adjusts the pH of T-202 feed to slightly less than 7. This step neutralizes excess caustic in the reaction product. A condition of high pH and heat can cause color problems in IMP.
Diacetone Alcohol B. K. Huelle
Unit Support (Huelle) - None provided.
Pentaerythritol D. R. Akin, P. J. Buras, B. K. Huelle
Eliminate VCI Centrate Waste Stream (Buras) - Evaluation of alternatives to the previously identified extraction process continues. The initial ob jective is to non-selectively extract all organics from AML. This would improve recovery of sodium formate by VCI and hopefully eliminate the centrate waste stream. The organics removed from AML could be burned or PE could be selectively recovered for recycle to the PE unit.
Improved solvents identified from one-stage shake out data were eval uated in continuous laboratory extractions of AML and concentrated AML. A mixture of methanol and n-butyraldehyde appears to be the best solvent. Work continues to optimize extraction conditions (e.g., solvent ratio, AML concentration).
003457
GDB-93-80 Page Ten
January 9, 1981
PE Formal Hydrolysis (Akin) - Studies were continued using Amberlyst
15 ion exchange resin, as a co-catalyst
with a
contin
uously fed strong acid (sulfuric or formic). Amberlyst 15 exposure time
to date is 160 days. The conversion rates of linear formals remain good.
Variable studies of the effects of sodium concentration and acid concen
tration (with a constant residence time) on conversion of linear formals
were conducted on this resin. Studies will continue.
Development of a System to Monitor PE Reaction Conversion and Minimize PV Absorbance at 220 nm (Huelle) - A cakes were made from reactions which differ only in their caustic to acetaldehyde mole ratios. These A cakes were hydrolyzed and UV absorptions determined. As seen in the A cakes, the hydrolyzed products (B cakes) show decreasing absorbances as the mole ratio increases.
Attempts are being made to correlate the laboratory data to the unit. A cake from the unit on December 17 indicated a mole ratio of 1.04 on the A cake absorbance vs. mole ratio curve. This A cake was hydrolyzed in the laboratory. Hydrolyzed products' absorbance indicates a mole ratio of 1.04 on the B cake curve.
A and B cake unit samples are being taken daily fco see if absorabance * changes in A cake correspond to absorbance changes in B cake.
APE unit reaction mixture sample was divided into two parts. One part was neutralized and carried out through the laboratory PE preparation. The second part was treated with additional caustic and the reaction continued for 20 minutes. The second part was also neutralized and put through the laboratory process. Absorbances of A cakes from the two parts were very similar. Studies to explain the failure of additional cuastic to lower uv absorbance in the A cake are currently underway.
1,3-Butylene Glycol B. K. Huelle, P. J. Buras
Unit Support (Huelle) - None provided.
Improved Aldol Condensation and AcH Recovery (Buras) - No progress due to priorities.
Special Problems Group - General
Becky Day conducted a tour of the Paraform Unit for Dr. Susan Weiss from CCCTC on December 10. Dr. Weiss is the Project Analyst for the Para form piloting work planned at CCCTC. She also met with A. G. McGehee, H. H. Thigpen, R. L. Day and D. R. Akin to discuss Paraform analysis and potential ways to determine average molecular weight of Paraform.
003458
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