Document jg0ox84QbyZe3eL2w75kn7Zq9

MONSANTO COMPANY TEXAS CITY, TEXAS DEPTS. 233,4,5,7, 8,20, ,44, 45,46,48, 56,60 METHOD 602.009 (WC) Rev. 7/19/71 Page 1 of 3 MATERIAL Product SM, AN, MeOH, Bz, Toluene, EB and all other clear and colorless materials requiring an APHA color measure ment, - D0P, DIDP, -711- Other Alcohols, Caustic. ANALYSIS REQUIRED Color SAMPLE One quart bottle APPARATUS Nessler (short) tubes 100 ml marked at 150 mm from inside bottom. Lumetron Model 450 with color filter #B-420. REAGENTS Distilled water XXX APHA 500 Standard PROCEDURE 1. With switch off, set instrument to 0% transmission by means of the lever in the back. 2. Fill a tube to 150 mm mark with clear distilled water. Insert tube in machine and turn switch on. 3. Adjust the instrument to 100% transmission by raenas of the adjustment level at thetop. Turn switch off and remove tube. 4. Fill a tube with sample and place in instrument. Turn switch on and read % transmission from the scale. 7/20/71 Rsv 0014954 METHOD 602.009 (WC) Rev. 1 7/19/71 Page 2 of 3 PREPARATION OF REAGENTS None STANDARDIZATION AND/OR CALIBRATION Prepare standards by diluting APHA 500 stock at rate of 0, 1, 2, 3,4, & 5 ml to 100 ml with distilled water. The standards represent 0, 5, 10, 15, 20 & 25 APHA colors. Read the % transmission of these vs. the distilled water used. Plot the %-transmissions thus obtained vs. the cor responding APHA colors. Draw in the best representative line. Use this curve for routine work or prepare a chart from it showing 7.T vs. APHA color. SAFETY Use normal precautions in handling chemicals, glassware ar.d electrical equipment. ANALYTICAL TIME 5 minutes PRECISION OF RESULTS AND SIGNIFICANT FIGURES TO REPORT 957,, confidence limits are + 2 at a level of 10 APHA. Report results to the nearest 1 APHA. SCOPE The color of the sample is compared to the APHA scale. REFERENCES Method 31-16-6 /jw 7/20/71 RS V 0014955 LIGHT MUUSTSrcNT ON LKCTRGK METHOD 602.009 (WC) Rev. 1 7/19/71 Page 3 of 3 STEPS IN ADJUSTING LIGHT SOURCE 1. When bulb* bums out; remove light housing and, replace bulb. 2. Adjust iris diaphragm to 30% transmittance. 3. Adjust Bar A for maximum deflection to the right. 4. Loosen thumb screw B and adjust housing sideways for maximum deflection to the right and retighten. 5. Loosen thumb screw C and adjust backward or forward for maximum deflection to the right. 6. Adjust dark current to zero. 7. The instrument is ready to use. 8. Follow usual procedures for adjusting light source on a water blank for 100% transmittance. * The bulb used has a double contact on the base and is coded GE 1130. / jw 7/20/71 RSV 0014956 MONSANTO CHEMICAL COMPANY TEXAS CITY , TEXAS DEPTS. 10, 60 METHOD 602.016 Rev. 1 7/20/71 Page 1 of 4 (GC) MATERIAL 10-D7-OH, Gulf C2Ha, Humble C2H4, Dept. 2 & and Dept. 3 Meter Runs, Dept. 2 & 3 C2H4 Composite, Dept. 23 C2H4 Composite, Dept. 41 C2H4 ANALYSIS REQUIRED CHa, C2H2s C2H4, C2H6 SAMPLE 1.7 liter oxygen bomb with positive sample pressure. APPARATUS Perkin-Elmer Vapor Fractometer, Model 154B/or equivalent Gas charging valve with 1 cc sample loop 1/4'* O.D. aluminum or stainless steel tubing REAGENTS 30-60 mesh silica gel Methane, Phillips Research Grade Ethane, Phillips Research Grade Ethylene, Phillips Research Grade Acetylene, Commercial Grade - water scrubbed and dried. PROCEDURE A. Column Preparation 1. Pack a 1.5 meters column of 1/4'* tubing with 30-60 mesh silica gel. 2. Install the column in the Fractometer. Adjust the temperature to 50C. , determine optimum detector current and set at this value, and adjust the pressure such that the ethylene peak appears in 3-4 minutes after charging the sample. Allow the instrument to reach equilibrium at these conditions. RSV 0014957 METHOD 602.016 (GC) Rev. 1 7/20/71 Page 2 of 4 B. Analysis 1. Turn recorder on ar.d sec recorder range to 1. Recorder trace should show no drift for five minutes before Fractoneter is ready for use. 2. Purge 1 cc gas sample loop with sample to be analyzed, shut off valve from bomb, and enter 1 cc sample into Fractoneter. 3. Record peaks for air, methane, ethane, ethylene, and acetylene- or allow enough time for acetylene to appear as determined by retention times from a previous chart run under the same conditions. CALCULATIONS 1. Draw base lines for all peaks except air. 2. Use rule with 30 divisions per inch and measure peak height and width at one-half peak height for all peaks. Measurements should be made to the nearest one-tenth of a division. 3. Calculate corrected area for all peaks as follows: Corrected area h x v x rxF Where: h = peak height w width at one-half peak height r - recorder range F * calibration factor for that component 4. Caluclar.e mol percentage of each component in the sample as follows: Acorr. x 100 Mel X - ^ (Acorr. ) Where: Acorr. corrected area from Step 3 ^C(Acorr.) * total of all corrected areas calculated in Step 3. RSV 0014958 METHOD 602.016 (GC) Rev. 1 7/20/71 Page 3 of 4 PREPARATION OF REAGENT SOLUTIONS None necessary. CALIBRATION 1. Prepare at least two synthetics containing methane, ethane, and acetylene in approximately 957. ethylene. Allow to stand overnight to insure thorough mixing. 2. Analyze as in the procedure under Analysis. 3. Measure peaks.as in Steps 1 and 2 under Calculations. 4. Calculate area of each peak as follows: A- hxwx r Where; A area h * peak height w * width at one-half peak height r * recorder range 5. Calculate factors for each component according to the following equation: % F-A Where: F * factor 7. * mol 7. of component in synthetic A - area of component peak calculated in Step 4 above 6. All factors should be normalized such that the factor for ethylene equals 1.000. SAFETY PRECAUTIONS No special precautions need be observed other than those nor mally observed when handling gaseous hydrocarbon samples. ANALYTICAL TIME The average time of analysis using this method should be 0.4 hours. PRECISION OF ANALYSIS AND SIGNIFICANT FIGURES FOR REPORTING RESULTS 957. confidence limits using this method should be / or - 0,57.. Report results to nearest 0,017.. RSV 0014959 METHOD 602.0X6 (GC) Rev. 1 7/20/71 Page 4 of 4 SCOPE This method is designed for samples containing only methane and the C^'s. Samples containing propane, but not propylene, may also be analyzed using this method as propane has a retention time slightly less than acetylene. If "acetylene" appears in a sample normally known not to contain this component, the sample should be analyzed by another method; eg., infrared, to determine if it is acetylene or propane. /jw 7/20/71 RSV 0014960 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL DEPTS. 10, 60 METHOD 602.040 (GC) Rev. 1 7/20/71 Page 1 of 4 High Purity Ethylene ANALYSIS REQUIRED Carbon Dioxide SAMPLE Minimum of liter stainless steel bomb with positive sample pressure. APPARATUS Perkin-Elmer Vapor Fractometer, Model 154B/or equivalent. Gas charging valve with 5 cc sample loop. 1/4" O.D. aluminum or stainless steel tubing. REAGENTS Activated Charcoal (Absorbent-A, used as purchased from Burrell Corp.) Di-2-ethyl hexyl sebacate (Octoil "S" or Narcoil 20) High purity ethylene - C02 free COs PROCEDURE A. Column Preparation 1. Pack 6 feet of 1/4" aluminum or stainless steel tubing with activated charcoal modified with 4 wt.% di-2-ethyl hexyl sebacate. 2. Install the column in the chromatograph. Adjust the temperature to 70C, determine optimum detector current and set at this value, and adjust the pressure such that the C02 peak appears in approximately 5 minutes after charging the sample. Allow the instrument to reach equilibrium at these conditions. RSV 0014961 r METHOD 602.040 (GC) Rev. 7/20/71 Page 2 of 4 PROCEDURE (cont'd) B. Analysis 1. Turn recorder on and set recorder range to 1. Recorder trace should show no drift for five minutes before chromatograph is ready for use. 2. Purge 5 cc gas sample loop with sample to be analyzed, shut off valve from bomb, and enter 5 cc sample into chromatograph. 3. Record all peaks up to and including C02 peak or allow enough time for C02 to appear as determined by retention time from a previous chart run under the same conditions. CALCULATIONS 1. Draw base line for C02 peak only. 2. Use rule with 50 divisions per inch and measure peak height and width at one-half peak height for the C02 peak. Measurements should be made to the nearest onetenth of a division. 3. Calculate ppm of C02 as follows: ppm C02 hxwxrxF Where h * peak height w - width at one-half peak height r =* recorder range F calibration factor for C02, expressed as ppm/unit area PREPARATION OF REAGENT SOLUTIONS None necessary. RSV 0014962 METHOD 602.040 (GC) Rev. 7/20/71 Page 3 of 4 CALIBRATION 1. Prepare at least two synthetics containing C02 in high purity ethylene. These synthetics should be in the range of 10 - 50 ppm C02. Allow to stand overnight to insure thorough mixing. 2. Analyze as in the procedure under Analysis. 3. Measure the C02 peak as in Steps 1 and 2 under Calculations. 4. Calculate area of C02 peak as follows: A*hxwx r Where A - Area h - peak height w - width at one-half peak height r - recorder range 5. Calculate C02 factor according to the following equation: F A Where F * Factor C - Concentration of C02 in synthetic expressed in ppm A * Area of C02 peak calculated in Step 4 above. 6. Calibrations should be checked daily. SAFETY PRECAUTIONS No special precautions need be observed other than those normally observed when handling gaseous hydrocarbon samples. ANALYTICAL TIME The average time of analysis using this method should be 0.2 hour. RSV 0014963 METHOD 602.040 (GC) Rev. 7/20/71 Page 4 of 4 PRECISION OF ANALYSIS AND SIGNIFICANT FIGURES FOR REPORTING RESULTS 95% confidence limits using this method should be / or -2ppm. Report results to nearest ppm. SCOPE This method is designed for trace C02 analysis of high purity ethylene, although it may be used for the determination of C02 in any inert or hydrocarbon gas mixture. If used for analysis of streams containing larger concen trations of C02, it may be desireble to use a smaller sample size. If the sample size Is changed, the factor should be adjusted for the new sample size. Samples containing large amounts of butanes and heavier will eventually "over modify" the carcoal and cause a decrease in the retention time of C02. If this occurs, it may be necessary to replace column. /jw 7/20/71 RSV 0014964 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL DEPTS. 10, 60 METHOD 602.041 REV. 7/20/71 Page 1 of 4 (GC) All gas samples, hydrocarbon and inert samples. ANALYSIS REQUIRED Oxygen, Nitrogen and Carbon Monoxide SAMPLE Minimum of one liter stainless steel bomb with positive sample pressure. APPARATUS Perkln-Elmer Vapor Practometer, Model 154b/ or equivalent. Gas charging valve with 25 cc sample loop. 1/4" O.D. aluminum or stainless steel tubing. REAGENTS 5 Angstrom Molecular Sleve/or 13 Angstrom Molecular Sieve Air - scrubbed with caustic and dried. CO Helium PROCEDURE A. Column Preparation 1. Pack a 2 meter length of 1/4" aluminum or stainless steel tubing with 30 - 60 mesh molecular sieve which has been dried In an oven overnight at 110C. 2. Install the column In the chromatograph. If a 5 Angstrom sieve is used, adjust temperature to 70C; If a 13 Angstrom sieve Is used, adjust temperature to 50C. Determine optimum detector current and set at this value, and adjust the pressure Buch that the oxygen peak appears In one minute after charging the sample. Allow the Instrument to reach equilibrium at these conditions. RSV 0014965 Method 602.041 (GC) Rev. 7/20/71 Page 2 of 4 PROCEDURE (Coat'd) B. Analysis 1. Turn recorder on and set recorder range to 1. Recorder trace should show no drift for five minutes before chromatograph Is ready for use. 2. Purge 25 cc gas sample loop with sample to be analyzed, shut off valve from bomb, and enter 25 cc sample Into chromatograph. 3. Record peaks for oxygen, nitrogen, methane, and carbon monoxide or allow enough time for carbon monoxide to appear as determined by retention time from a previous chart run under the same conditions. CALCULATIONS 1. Draw base lines for all peaks except methane. 2. Use rule with 50 divisions per Inch and measure peak height and width at one-half peak height for all peaks. Measurements should be made to the nearest one-tenth of a division. 3. Calculate concentration of all components, except methane, in ppm as follows: ppm -hxwxrxF Where h -- peak height w - width at one-half peak height r recorder range F - calibration factor for that component expressed as ppm/unit area. PREPARATION OF REAGENT SOLUTIONS None necessary. CALIBRATION 1. Prepare at least two synthetics containing air, which has been caustic-scrubbed and dried, and carbon monoxide In helium. 2.46 mm of air per 100 psla synthetic will be 100 ppm oxygen. Synthetics should be In the range of 25* 100 ppm oxygen and carbon monoxide. Allow to stand over night to Insure thorough mixing. RSV 0014966 Method 602.041 (GC) Rev. 7/20/71 Page 3 of 4 CALIBRATION (Cont'd) 2. Analyze as In the procedure under Analysis. 3. Measure peaks as In Steps 1 and 2 under Calculations. 4. Calculate area of each peak as follows: A-hxwx r Where A Area h - peak height w - width at one-half peak height r recorder range 3. Calculate factors for each component according to the following equation: =_C Where F - Factor C - concentration of component In synthetic expressed In ppm A - area of component peak calculated In Step 4 above. 6. Calibrations should be checked dally. SAFgTY PRECAUTIONS No special precautions need be observed other than those normally observed when handling gaseous hydrocarbon samples. ANALYTICAL TIME The average time of analysis using this method should be 0.3 hour for a 3 Angstrom column and 0.2 hour for a 13 Angstrom column. PRECISION OF ANALYSIS AND SIGNIFICANT FIGURES FOR REPORTINQ RESULTS 95$ confidence limits using this method should be * 4 ppm. Report results to nearest ppm. RSV 0014967 Method 602.041 (GC) Rev. 7/20/71 Page 4 of 4 SCOPE This method 1b designed for high purity ethylene samples; however, It may be used on any Inert or gaseous hydrocarbon mixture. If argon is present In the sample, it will be eluted with oxygen. Periodically, depending on usage, the % column may need to be regenerated. This Is done by purging with nitrogen or helium for 2 hours while the column Is main tained at 500 to 55?F. If sample volume Is changed, all factors should be aaJusted to new sample volume. OL/nv RSV 0014968 MONSANTO COMPANY TEXAS CITY, TEXAS DEFT. 10, 60 METHOD 602.042 Rev. 7/20/71 Page 1 of 5 (GC) MATERIAL High Purity Ethylene ANALYSIS REQUIRED Hydrogen SAMPLE Minimum of one liter stainless steel sample bomb with positive-sample pressure. APPARATUS Loenco, Model 15-B - or equivalent. Gas charging valve with a 25 cc sample loop. 1/4" O.D. aluminum or stainless steel tubing. REAGENTS 13 Angstrom molecular sieve, 20-60 mesh. Nitrogen (to be used as carrier gas) Hydrogen, electrolytic Ethylene, Phillips Research Grade PROCEDURE A. Column Preparation 1. Activate the molecular sieve by drying in an oven at 400 P for 3 hours, cool in a desiccator and store in screw-cap bottles. Pack 12 feet of 1/4" aluminum or stainless steel tubing with the activated sieve. 2. Install the column in the chromatograph. With the in strument at room temperature, determine the optimum detector current and set at this value. Adjust the pressure such that the hydrogen peak appears in approxi mately 1.5 - 2.0 minutes after charging the sample. Allow the instrument to reach equilibrium at these con ditions . RSV 0014969 METHOD 602.042 (GC) Rev. 7/70/71 Page 2 of 5 fi. Analysis 1. Turn on recorder and line out equipment. 2. Purge 25 cc sample loop with sample for 2 to 3 minutes or until all air has been removed. 3. Stop purge and after pressure in sample loop has stabilized/ enter ethylene sample into instrument. 4. The recorder pen will deflect off scale when sample is entered but should return to base-line point after one minute. 5. Record hydrogen peak. CALCULATIONS 1. Read peak height and calculate ppm hydrogen in sample. ppm H2 " Peak height x attenuation x factor PREPARATION OF REAGENT SOLUTIONS None necessary CALIBRATION 1. Prepare standards samples of hydrogen in ethylene in the 1 to 50 ppm range. 2. Analyze these standard samples following the steps under procedure. 3. Read peak heights and calculate calibration factor. p m Concentr" ation of H- Peak height x attenuation SAPSTY PRECAUTIONS No special precautions need be observed other than those normally observed when handling gaseous hydrocarbon samples. RSV 0014970 METHOD 602.C42 (GC) Rev. 7/20/71 Page 3 of 5 ANALYTICAL TIME The average tine of analysis using this method should be 0.2 hour. PRECISION OF ANALYSIS AND SIGNIFICANT FIGURES FOR REPORTING RESULTS 9596 confidence limits using this method should be + or - . 5 /ppm in the 0-50 ppm range. Report results to nearest 1 ppm. SCOPE This method is applicable to any gaseous mixture. Some changes may be desirable as to sample size depending on the concentration of hydrogen in the sample. LYS:ff 10/19/64 RSV 0014971 METHOD 602.042(GC) page 4 of 5 MONSANTO COMPANY TEXAS CITY, TEXAS METHOD 602.042 (O.C.) Page 5 of 5 Mt |-p-----k' ^ J^ m/xmmv /mM* --\* I JiW V/-tY r/ai/* / COA^SA/TfiAT/O*/ * SAUfiltVS 0t/tP4*6Vr RSV 0014973 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.0U3 (C.C.) Rev. 7/20/71 Page 1 of 4 MATERIAL High Purity Ethylene ANALYSIS REQUIRED Propylene and other olefins. SAMPLE Minimum of one liter stainless steel bomb with positivesample pressure. APPARATUS Perkin-Elmer Vapor Fractometer, Model 15^B/br equivalent. Gas charging valve with 1 cc. Bample loop (modified for evacuating the sample loop) n O.D. aluminum or stainless steel tubing. Vacuum pump capable of producing 50 microns vacuum or better, with a free air capacity of at least 21 liters per minute. Mercury manometer. REAGENTS Cellte, 30-80 mesh; a satisfactory source is the Cellte Division, Johns Manville Company, New York. Diethyl Ether, for column preparation. Helium, Hexamethylphosphoramlde, available from Monsanto Chemical Company, Organic Chemicals Division, 600 N. 12th Street, St. Louis, Missouri. Propylene, Phillips Research Grade. RSV 0014974 METHOD 602.043 (G.C.) Rev: 7/21/71 Page 2 f J| PROCEDURE A. Column Preparation 1. Pack 25 feet of t" aluminum or stainless steel tubing with 30-80 mesh Cellte aggregate containing 0.2 g of hexamethylphosphoramide per gram of aggregate and shape column to fit Into*1 2chromatograph. 2. Install the column In the chromatograph and purge with helium (approx. 20 ml/min.) for at least 24 hours before using. 3. With.the instrument at room temperature, determine the optimum detector current and set at this value, and adjust the pressure such that the propylene peak appears in approximately 7 to 8 minutes after charging the sample. Allow the instrument to reach equilibrium at these conditions. B. Analysis 1. Turn recorder .on and set recorder range to 1. Recorder trace should show no drift for five minutes before chromatograph is ready for use. 2. Purge 1 cc gas sample loop with sample to be analyzed, shut off valve from bomb, and enter 1 cc sample at one atmosphere pressure into chromatograph. 3. Record all peaks up to and including propylene on recorder attenuation of 1, or allow enough time for propylene peak to appear as determined by retention time from a previous chart run under the same conditions. q^LCULATIOHS 1. Draw baBe line for propylene peak only. 2. Use rule with 50 divisions per Inch and measure the peak height of the propylene peak. Measurements should be made to nearest one-tenth of a division. RSV 0014975 METHOD 602.0*3 (O.C.) Rev. '7/21/71 rage 3 of 4 CALCULATIONS (cont'd) 3. 'Calculate concentration of propylene as follows: C =D S' Where: C = concentration of propylene in saiaple expressed in mol per cent, D = deflection of propylene peak in sample chromatogram measured in step 2 above. ,S = sensitivity of propylene, expressed as deflection per mole per cent as deter mined from the calibration curve, PREPARATION OP RBAQBKT SOLUTIONS None neoess&ry, .CALIBRATION 1. Prepare a aensltlvlty curve for propylene by adding pure propylene; at 150, 100, 50, and 23 mm of pressure in the 1 cc sample loop* 2. Plot the peak height (scale of.50 divisions per inch) versus pressure and extrapolate.the curve to zero pressure. ' 3. * Calculate the sensitivity in scale divisions (50 divisions per inch) of deflection per mol per cent for a 1 cc sample from the slope of the curve below 20 mm pressure. 4. Before analyzing each set of samples, check the sen sitivity by measuring a secondary standard and make suitable corrections to the calibrations. SAFETY PRECAUTIONS No special precautions need be observed other than those nonoally observed when handling gaseous hydrocarbon samples, ANALYTICAL TIME The average time of analysis using this method should be 0.3 hour. RSV 0014976 METHOD. 602.0^3 (O.C.J Rev. 7721/71 Page 4 of 4 PRECISION OP ANALYSIS AND SIGNIFICANT PIQURSS POR REPORTING RESULTS_____ 95JS confidence limits using this method should bo / or - 0.0003 mol per cent in the 0-0.025 mol per cent range. Report results to nearest .001 mol per cent. SCOPE This method is for the determination of propylene and other olefins in high purity ethylene. It may be used on other gaseouB hydrocarbon mixtures with possible expansion of calibration curves. /jw 7/21/71 RSV 0014977 MONSANTO COMPANY TEXAS CITY, TEXAS DEPTS. 2,3,20, 33,60 METHOD 602.063 (WC) July 21, 1971 Page 1 of 2 MATERIAL NaOH receipts, Circulating Caustic, Waste Caustic ANALYSIS REQUIRED NaOH content SAMPLE SIZE Pint bottle APPARATUS 50 ml Burette Oleum bulbs 300 ml Erlenmeyer flask REAGENTS Methyl red indicator 0,5 N HC1 PROCEDURE Place about 1 gram of sample into a tared oleum bulb. Seal and reweigh bulb. Slide the oleum bulb into a 300 ml Erlenmeyer flask containing about 25 ml of distilled water. Cautiously, break the oleum bulb with a stirring rod which has been flattened on one end. Be sure that oleum bulb stem is also crushed with stirring rod. Add about 25 ml more of distilled water. Add a few drops of Methyl red indicator, swirl and titrate to a red end point with 0.5 N HCl. Analyze receipts (only) in duplicate. Single analysis for other caustic samples. CALCULATIONS ^HCl1 (4-> Sample Weight - % NaOH On caustic receipts also report % Na^O (% NaOH ) (Average of) (1.0195 - % Na 0 ( 76%) (Duplicates) RSV 0014978 METHOD 602.063 (WC) July 21, 1971 Page 2 of 2 PREPARATION OF REAGENTS Refer to solutions manual STANDARDIZATION AND CALIBRATION Refer to solutions manual for standardization of 0.5 N HC1. SAFETY PRECAUTIONS Caustic receipts are-approximately 50% NaOH. Caution should be used to prevent contact with skin, eyes or clothing. If 50% NaOH does come in contact with the body, wash affected part.with copious quantities of water. ANALYTICAL TIME 0.3 Hours PRECISION AND SIGNIFICANT FIGURES Report to the nearest .01%. Duplicate results should agree within 0.5%. Precision is 0.4% at 50% caustic level. SCOPE Method is applicable to any range of-caustic by varying sample.size and normality of HC1. RSV 0014979 MONSANTO COMPANY TEXAS CITY, TEXAS DEPTS. 2,3,10,20, 33,60 METHOD 602.212 (WC) 7/21/71 Page 1 of 2 MATERIAL Specification Acrylonitrile and Product Methanol Muriatic Acid - Caustic Receipts ANALYSIS REQUIRED Appearance SAMPLE Quart Bottle APPARATUS APHA Color Tube REAGENTS None PROCEDURE Observe the sample in a clean dry tube of size large enough to hold about 100 ml of sample. Sample should be clear and free of suspended matter. Report results accordingly. CALCULATIONS None STANDARDIZATION AND/OR CALIBRATION None SAFETY PRECAUTIONS Avoid skin contact with AN, Caustic, HC1, MeOH. Avoid breathing AN and MeOH, HCl, Muriatic Acid and caustic soda vapors. Keep out of eyes. RSV 0014960 METHOD 602.212 (WC) 7/21/71 Page 2 of 2 ANALYTICAL TIME 0.1 hour PRECISION OF ANALYSIS AND SIGNIFICANT FIGURES FOR REPORTING RESULTS Report appearance as clear and free of suspended matter, cloudy or suspended matter present. SCOPE This method is capable of detecting any foreign matter of large enough particle size to be observed visually. REFERENCES Method 20-29-3, MLO, 7-21-51, 10-22-51 /jw 7/21/71 RSV 0014961 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT- 60 METHOD 602.244 Rev. 5/3X/71 Page 1 of 6 MATERIAL Acrylamide ANALYSIS REQUIRED Melting range APPARATUS (a) Bath - JFQ Standard Apparatus Drawing 5 (b) Bath Liquid - Use appropriate liquid as follows: Bath Temperature Liquid 40-85C Water 80-200C Dow Coming No. 550 Silicone Fluid 190-270C Dow Corning No. 550 Silicone Fluid (c) Thermometer - Precision Thermometer and Instrument Company, Philadelphia, Pa., round front precision type thermometer, or equivalent, calibrated against a standard or platinum resistance thermometer, selected as follows: Bath Temperature 40-85*C 80-200 C 190-270 C 40-85C range, 3" Immersion 0.2C division, 12" length 80-200C range, 3" immersion 0.2C division, 18" length 190-270C range, 4" immersion 0.2C division, 20" length RSV 0014982 METHOD 602.244 5/31/71 Page 2 of 6 APPARATUS (cont'd) (d) Magnifier - Surth Number UG-49-D without base. Safety Incorporated, St. Louis, Missouri, type magnifier containing a 2" x 4M lens with a 3" focal length. (e) Melting Point Tubing - Friedrich and Diinmack, Inc. , P.O. Box 230, Millville, New Jersey, 7" length, 1.4-1.6 mm OD purchased with both ends sealed. Score with a chip of carborundum and break off one end just prior to use. Since it is impractical to firepolish the broken end, exercise CARE to prevent lacerations. (f) Continuously Adjustable Transformer, such as No. V-5 Variac, General Radio Co. (g) Variable Speed Stirrer, such as Eastern Industries, Model No. 3, New Haven, Conn. DETERMINATION 1. Reduce a portion of the sample to a very fine powder if necessary, using a mortar arrd"pestle. When specified, dry the sample at the time and temperature designated in che specification for the product. If the determination is to be made on the sample as is, transfer a portion to a clean piece of glassine paper for filling the melting point tube. 2. By tamping the open end in a small mound of sample, charge the tube with sufficient material to form a column in the bottom of the tube from 4.0 to 5.0 mm high when packed down as closely as possible by moderate reverse tapping on a solid surface. The filling of the tube can be aided by carefully scratching the side of the tube with a round file during the process. The remainder of the sample in the mortar or on the glassine paper should be discarded since it may contain slivers of glass. RSV 0014983 METHOD 602.244 5/31/71 Page 3 of 6 DETERMINATION (cont'd) 3. Select the appropriate bath and make certain that it is filled to the proper height. The liquid should be filled so that it is within 1/211 of the top of the bath when at the melting point temperature. Adjust the thermometer to the proper Immersion point, making certain that the thermometer is as close to the center of the bath as possible. 4. Start the sti-rrer and heat the bath rapidly to within approximately 15C of the expected melting point. Regulate the rise with a Variac to 1C per minute + 10 seconds and maintain at this rate throughout the re mainder of the test. 5. Insert the melting point tube exactly 10C below the expected melting point so that the sample portion of the tube is adjacent to the bulb of the thermometer and clearly visible through the bath window. 6. Read the temperature of the melt at the following two points: a. Meniscus Point - When the liquid phase of the sample forms a distinct meniscus at any level within the sample. b. Clear Point (End of Melt) - When the last evidence of solid disappears and the sample is completely liquid.7 * * * 7. Apply the thermometer calibration correction and report to 0.1C the corrected temperatures as the melting point range. DISCUSSION The material must be in a fine powdered state to facilitate proper packing of the melting point tube. Granular or crystalline material will allow air voids, thus affecting the amount of material used. The volume of material is critical since amounts varying from the recommended 4.0-5.0 mm can affect the malting range by 0.2C or more. RSV 0014984 METHOD 602.244 5/31/71 Page 4 of 6 DISCUSSION (cont'd) The position of Che melting point tube and the thermometer are critical. They should be placed adjacent to each other and centered in the bath to minimize variations. It is essential that the proper liquid level be maintained in order to facilitate efficient stirring of the bath. To counteract the greater convection currents in the highest temperature bath, this bath has been made 1" deeper than the other baths. The same liquid level should be maintained, namely 1/2" from the top. Table 1 lists the significant differences in procedure between this method, the USP XVI, and the 3P (1948) methods. TABLE 1 COMPARISON OF THE MONSANTO MELTING POINT METHOD, THE USP XVI, AND THE BP (1948) METHODS ( 1) Method Visual Aid Rate of Rise in Temp., *C per Minute Alteration in Rate of Temp. Rise Immersion Point in *C Below Ex pected Melt Preheating Time From Immersion to Expected Meli in Minutes Monsanto Magnifier r None 10 10 USP XVI None 3*C Change rate to 30 TC per minute at 3* below the expected melt 12 BP (1948) None 3a None 10 3-1/3 RSV 0014985 METHOD 602.244 5/31/71 Page 5 of 6 DISCUSSION (cont'd) Following are the five possible observable points during the transition from solid to liquid with notations of the points taken in each of the above three methods; 1. Sintering Point - The sample shows evidence of shrinking in volume and its appearance is altered. 2. Liquefaction Point - The sample shows pronounced shrinkage in"volume, and the first distinct minute droplet of liquid forms at any level in the sample or on the wall of the capillary. This point closely approximates, or is identical with, the "Beginning of Melting" of the USP XVI method. 3. Flow Point - The sample sorms droplets which readily begin to flow together and droplets adhering to the wall of the capillary begin to spread and flow. Shrinkage of the sample is virtually complete. 4. Meniscus Point - The liquid phase of the sample forms a distince meniscus at any level within the sample. This point is identical with the "Meniscus Point" of this method and the BP (1948). 5. Clear Point (End of Melt) - The point where the last evidence of solid disappears and the sample is com pletely liquid. This point is identical with the "End of Melt" of this method and the USP XVI. SCOPE This method is intended for the determination of the melting point (range) of essentially pure organic com pounds. It involves a capillary tube technique similar to a method proposed by Felker (1) for adoption as a standard procedure by the United States Pharmacopeia. RSV 0014966 METHOD 602.2-^ 5/31/71 Page 6 of 6 PRECISION AND ACCURACY Results by this method, compared to those by the USP XVI and the BP (194.8) methods will differ product for product sir.ce the transition from the solid to liquid phase varies as the complexity of the molecular structure varies. Products such as caffeine and acetophenetidin will respond as follows: 1. The meniscus point will be approximately 0.4C higher than the UXP_ XVI liquefaction point and 0.2C lower than the BP (1948) meniscus point, owing primarily to the different rates of heating. 2. The end of melt will be essentially the same in this method and the USP XVI. The precision of this method is dependent on the purity of the material being tested. Duplicate results on essentially pure material should agree within 0.3eC. SAFETY Mercury is a cumulative poison with a relatively high vapor pressure. In the event than a thermometer is broken, collect the mercury and place in a waste jar under water. REFERENCES Felker, W. S., Drug Standards. 20, 169 (1952). / jw 7/22/71 RSV 0014987 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT 60 METHOD 602.2^5 31. 1971 Page 1 of 2 MATERIAL Acrylamide. ANALYSIS REQUIRED Solution appearance. SCOPE This method is -intended to provide an indication of the completeness of solurim of materials at specified concentrantions in specific solvents. It involves comparison with ar. equivalent solution of an approved standard, or subjective description of the solution when no standard is available. EQUIPMENT a) Clark TurbLdimeter, Cacilcb No, T-11315, The Chemical Rubber Co., Cleveland, Ohio. (Lamp replaced with a 150 watt showcase lamp.) b) Appropriate comparison glassware such as test tubes, Nessler tubes, flasks, or bottles, matched as to volume ar.d tint of glass; thoroughly cleaned, rinsed with distilled water, ar.d dried. c) Sol\er.r as designated in the specification for the product being tested. The solvent must be clear and colorless and should be filtered or distilled if necessary, DETERMINATION Bv Comparison with Standards 1. Read the specification for the product and, using a balance of 0,1 g. sensitivity, weign the designated amount of sample and transfer to the appropriate glass ware. RSV 0014988 METHOD 602-245 May 31, 1971 Page 2 of 2 DETERMINATION (coat'd) 2. Add the specified volume clear, colorless solvent and dissolve the sample by agitation at r^om tempera ture, or at the temperature designated in the speci fication. 3. Compare the color of the sample solution with the prescribed standard for color, referring to Method 38-Dr E if an APHA color is designated, and noting any afcr.ormality in hue. 4. Compare the turbiditv of the sample solution under the turbidimeter in parallel with the prescribed standard, recording the appropriate degree of comparison as: better, slightly better, very slightly better, equivalent very slightly more turbid, slightly mere turbid, or more turbid, and r.ote any difference in particle size, type or opalescence. NOTE: When product minimum standards selected by production departments are designated, solutions of them are prepared in parallel with the sample, ob serving the same precautions. By Description 1. Prepare the specified sample solution as directed in Method 112-A. 2. Describe the color of the solution. 3. Observe the solution u:der the turbidimeter and describe the degree of turbidity, opalescence, particles or sediment. SAFETY Take cognizance of any prent ial hazards in the solvents and samples, such as flammability, corrosiveness, lachrymatory or dermatological properties, or reactivity, and exercise adequate precautions. /jv 7/22/71 RSV 0014969 MONSANTO COMPANY TEXAS CITY. TEXAS DEPT, 60 METHOD 602.246 May 31. 1971 Page 1 of 7 MATERIAL Acrylamide ANALYSIS REQUIRED Mois cure SCOPE This memod is intended as a general directive for the determination of water, titrarable with Karl Fischer reagent, m various organic ar.d inorganic substances. It involves the solubilization or dispersion of a simple of the material to be analyzed in a suitable solvent and the titrimetric determination of the moisture present with Karl Fischer reagent. The end point may be detected colorimetrically in colorless or nearly colorless solutions, or eiectrometrically in colored solutions. EQUIPMENT a) N/100 methanolic iodine - Dilute 10 ml. of N/10 iodine to 100 ml. with methanol. b) Standardized regular and low alcohol Karl Fischer reagents in automatic burettes protected with anhydrous silica gel traps. For details of preparation see Method 1 - Section VII. c) Auto-Aquatrator, Catalog No. S-29742, Precision Scientific Co., Chicago, 111. d) Contno-. laboratory apparatus ard reagents. APPLICATION Solids are measured by weight. Liquids of known gravity may be measured from an appropriate volumetric pipette, multiplying volume by specific gravity to obtain weight. RSV 0014990 METHOD 602.246 .May 31, 1971 Page 2 of 7 Expected Moisture Sample Size 0-0.5% 0. 5-1.0% 1.0-5.0% 5.0-12.0% 10 + 0.1 g. 5 + O.lg. 2 + O.Olg. 1 + O.Olg. DETERMINATION A-Electrometric 1. Turn the line switch ON. 2. Set the selectcr to "DIRECT ADJUST". 3. Adjust the meter to full scale with the "DIRECT ADJUST" knob. 4. Set the selector to "DIRECT TITRATION". 5. Set the meter Low Set Point (left red needle) to 8 microamperes. (Where the moisture level is 0.057, or less, low set point must be set lower.) 6. Set the meter High Set Point (right red needle) to 15 microamperes. 7. Set the "End Point Hold" to 30 seconds. 8. Fill the K.F. burette. 9. To the titration vessel add a sufficient quantity of the solvent designated on the product specification sheet, to cover the electrode tip. 10. Place the titration vessel under the electrode, swing the support under the vessel and tighten the support until the vessel is snug against the cover. (The system must be air-tight.) Put the cover stopper in place. RSV 0014991 METHOD 602.2^6 May 31. 1971 Page 3 of 7 DETERMINATION (coat'd) 11. Start the stirrer (stir slowly), apply pressure to the cover stopper and evacuate moist air from the system by pulling on the vacuum switch fcr 15 seconds. 12. Depress the "Start" button and allow the unit to titrate to the instrument end point. 13. While the solvent is being titrated, weigh-in a suitable container - an appropriate amount of the sample fcr moisture determination. l*i. When the instrument indicates the end of the solvent titration, turn off the stirrer and remove the cover stopper. 15. Carefully add the sample to the titration vessel. 16. Replace the stopper, turn on the stirrer (stir slowly) and evacuate the system for 15 seconds. 17. Fill the K.F. burette, depress the start button, and while the unit is titrating to the instrument endpoint reweigh the sample container to determine the weight of the sample used. 18. Read the burette and calculate. ml. titre x K.F. factor x 100 X Moisture = sample weight B-Visual 1. Measure about 25 ml. of the solvent designated in the specification for the product (or see Discussion) into a dry 125 ml. Erlemneyer flask. 2. Titre with Karl Fischer reagent to an end point that matches the color of the N/100 methanolic iodine solution, sweeping moisture out of the flask by swirling the solution up the wails of the flask. KSV 0014992 METHOD 602.2^6 May 31, 1971 Page 4 of 7 DETERMINATION (cont'd) 3. Zero the Karl Fischer burette. 4. Add the prescribed weight of sample to the blanked solvent, swirl to dissolve, and immediately titrare to the same endpoint. NOTE: If the material to be analyzed is an insoluble porous solid, disperse finely divided sample in the solvent and allow to stand in a stoppered flask with occasional shaking far periods up to one hour at room temperature before titrating with Karl Fischer reagent. 5. Calculate: ml. titre x K.F. factor x 100 % Moisture - sample weight NOTE: In cases where pre-treatment of the sample is necessary to eliminate interaction of the material to be analyzed and Karl Fischer reagent, a separate solvent or reagent blank may be necessary. The cal culation then becomes: (Sample ml. - Blank ml.) x K.F- factor x 100 % Moisture sample weight PRECISION AND ACCURACY a) Sensitivity, precision, and accuracy depend on several factors, for example, concentration of the Karl Fischer reagent, titration technique, apparatus, quantity of water titrated, and nature of material being analyzed. b) The sensitivity is ab^ut 0.1 mg of water for visual titrations. Less than 0.02 mg can be measured by electrometric titraticr.. RSV 0014993 METHOD 602.246 May 31, 1971 Page 5 of 7 PRECISION AND ACCURACY (cant'd) c) The following is at. example -f the preciSL^n attained in an interlaboratory study on two samples of acetone containing 0.1 percent and 0.4 percent water and two samples of methyl ethyl ketone containing 0.05 percent and 0.17 percent water: Repeatability - Two results (each the average of duplicate determinations) obtained by the same analyst should be "considered suspect if they differ by more chan 0.013 percent., absolute (95 percent confidence level). Duplicate determinations which agree within 0.008 percent are acceptable for averaging. Reproducibility - Two results (each the average of duplicate determinations) obtained by analysts in different laboratories should be considered suspect if they differ by mere than 0.028 percent, absolute (95 percent confidence level). NOTE: The interlaboratory study was carried out by ASTM Committee D-l on Paint, Varnish, Lacquer, and Related Product, Subcommittee V on Solvents, Plastici zers, and Chemical Intermediates. Sevel laboratories participated with a single analyst performing duplicate determinations on each of two days, using two methods cn the four samples described above. The Method cf Test for Water in Lacquer Solvent and Diluents (Fischer Reagent Titration Method) (ASTM Designation: D1364)5 was the subject of the test program being compared with each laboratory's own version of a Karl Fischer method. As neither the means nor the variances of the two sets of data proved significantly different, all of the results were pooled ro give estimates of the repeatability based on 55 degrees of freedom and reproducibility based on 47 degrees of freedom. RSV 0014994 METHOD 602.246 May 31, 1971 Page 6 of 7 DISCUSSION The stoichiometry of the reaction between water and Karl Fischer reagent is as follows: C5H5N.I2 + c5h5n.so2 + c5h5n + H2O so2 2C5H5N.HI + C5H5N( and so2 C5H5< + CH30H 0 H c6h5< so4ch3 Pyridine is used to combine with acidic products, which will cause a reversal in the following reaction: I2 + S02 + 2H20 2HI + H2S04 It has the added advantage of combining with the sulfur dioxide, thereby reducing the vapor pressure of the latter. Most substances are inert to Karl Fischer reagent and may be analyzed without special treatment. However, a number of compounds and classes of compounds react stoichiometrically with one or more of the components of Fischer reagent Included among these are: - Ascorbic Acid, Hydrazine Salts, Substituted Hydrazine Salts, Mercaptans, Alkali Becarbonate Alkali Carbonates, Alkali Sulfites, Alkali Pyrosulfites, Boric Acid and Oxides, Carbonyl Compounds, Cupric Salts, Ferric Salts, Metal Hydroxides, Metal Oxides, Sodium Arsenate, Sodium Arsenite, Sodium Tetraborate, Sodium Thiosulfate, and Stannous Chloride. In general these reactive compounds either may be rendered inert (the use of glacial acetic acid as a solvent elimi nates amine and hydrzaine interference) or may be es timated by an independent method and a stoichiometric correction applied to the water determination. RSV 0014995 METHOD 602.246 May 31, 1971 Page 7 a7 DISCUSSION Although the cyanohydrin technique is the only g5r.eral method for the determination of water in the presence of carbonyl compounds, low alcohol Karl Fischer reagent and/or special solvents may be used to irdiibit interfering side reactions of many ketones and some aldehydes. By greatly reducing the methanol and increasing the pyridine in the regular Fischer solution, the tendency of carbonyls to form acetals and ketals.by reacting with the methanol of the standard reagent Is reduced. Appreciable quantities of lower alcohols ir. the. sample will permit the interfering acetal of ketal reaction even with the use of modified reagent. Details of other method variations are beyond the scope of this method and will be given in the methods of analysis for the specific compounds. In general, methanol may be used as a solvent for the determination of water ir. inert materials. Amines stronger than benzyl amine (KB 2.4 x 10"^) and other basic compounds are preferably treated with or dissolved in an excess of glacLal acetic acid or spent Fischer reagent, which ir* both cases combines with the amines. Some organic acids, formic, acetic, adipic, etc., tend to give slightly high results when methanol is used as a diluent, because of the ease with which they esterify. When equal parts of dry methanol and pyridine are used as a diluent, the inhibiting in fluence of the amine is sufficient to discourage any esterification of the acid at room temperature. SAFETY No unusual hazards are involved in this operation when cognizance of the inflammability and toxicity of the rea gents and solvents is taker.. REFERENCE 1. "Aquametry", Mitchell and Smith, Interscience Publishers, N.Y., 1948. 2. ASTM E203-64, _31 pp. 567-578, 1965. 7/22/71 RSV 0014996 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.247 May 31, 1971 Page 1 of 2 MATERIAL Acrylamide, Sodium lauryl sulfate ANALYSIS REQUIRED Sulfate (as SO^") SCOPE This method is intended for the determination of soluble sulfates in concentrations around 0.17* in essentially water soluble materials. It involves gravimetric deter mination as barium sulfate. EQUIPMENT a) Usual laboratory apparatus and reagents. b) 20 ml. fine porosity Selas filtering crucible, Catalog No. 8-227, Fisher Scientific Co. DETERMINATION 1. Dissolve 10 grams of sample, weighed on a prescription balance, in 100ml. of water in a 600ml. beaker. 2. Neutralize the solution to methyl orange with 10% HC1 and add 4 ml. m excess. NOTE: If the solution is not completely clear at this point, filter by gravity through Whitman 41 paper into a 600 ml. beaker. 3. Dilute the solution to about 400 ml. and heat to boiling. 4. While boiling gently, add 25 ml. and heat to boiling. 5. Cover the beaker with a watch glass and digest the solu tion on a steam bath for one hour, or until the supernatent liquid is clear. RSV 0014997 METHOD 602,247 May 31, 1971 Page 2 of 2 DETERMINATION (cont'd) 6. Filter through an ignited and tared fine porosity Selas crucible, transferring the precipitate quantitatively with a stream of water from a wash bottle, policing the beaker thoroughly, and washing down the inside walls of the crucible* 7. Ignite the crucible in a muffle furnace at 800-900C for 20 minutes, cool in a desiccator for 30 minutes and accurately weigh. 8. Calculate the sulfate content as the specific sulfate designated in the specification for the product: net wt. of ppt. x Factor % Specified Sulfate * sample weight Table of Sulfate Factors Specified Sulfates BaSO/ Factor CaS04 Fe2(S04)3 h2so4 k2so4 MgS04 MnS04 Na2S04 58.3 57.1 42.0 74.7 51.6 64. 7 60.9 PRECISION AND ACCURACY Duplicate determinations should agree to within 0.002%. SAFETY Exercise due care in the use of the high temperature muffle furnace. Handle crucible with long muffle tongs, pre ferably held with an asbestos glove. / jw 7/22/71 RSV 0014998 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.248 May 31, 1971 Page 1 of 2 MATERIAL Ammonia Persulfate ANALYSIS REQUIRED Active Oxygen APPARATUS a) Analytical balance b) 250 ml Erlenmeyer flash c) Titrating burette d) Usual laboratory equipment REAGENTS a) IN H2S04 b) 0.5N ferrous ammonium sulfate solution c) 0.5N KMn04 PROCEDURE The active oxygen content of the persulfates can be con veniently determined by the following method: Weigh approximately 1 gram of the sample to the nearest milligram and dissolve it in 50 ml of approximately 1 normal H2SO4 in an Erlenmeyer flask. Add 40 ml of ferrous ammonium sulfate solution (0.5N). Swirl constantly while adding the iron solution. Let stand for one minute and titrate with 0.5N KMnO/. Run a blank titration on 40 ml of ferrous ammonium sulfate solution, as used above, in 50 ml of the 1 normal H2SO4. RSV 0014999 Page 2 of 2 CALCULATIONS (A-B)C x 0.8 Percent accive oxygen - D (A-B)C x Percent Ammonium Persulfate * D 11.4 A ml KmnO^ solution used for titrating the blank B " ml KnmO^ solution used for titrating sample C Normality of the KmnO^ solution used D Weight of the sample in grams / jw 7/22/71 RSV 0015000 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.249 May 31, 1971 Page 1 of 1 MATERIAL Ferric Ammonium Sulfate Sodium Formaldehyde Sulfoxylate Tetrasodium ethylene diamine tetraacetate ANALYSIS REQUIRED Odor SCOPE This method is intended for the characterization of the odors of materials by olfactory perception. DETERMINATION 1. Remove sufficient material to allow about two inches of head room in the sample bottle above the contents to permit adequate trapping of the odor evolved. 2. If the nature of the sample permits, agitate the con tents of the bottle. 3. Let the bottle stand closed at least 30 minutes before performing the odor evaluation. 4. If unfamiliar with the odor of the product being tested, carefully open a previously approved sample and cautiously smell the air in the neck of the bottle. 5. Describe the sample odor with respect to the specification requirement. / jw 7/22/71 RSV 0015001 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.250 May 31, 1971 Page 1 of 4 MATERIAL Sodium Lauryl Sulfate Tetrasodium ethylene diamine tetraacetate ANALYSIS REQUIRED PH SCOPE This method is intended to be a guide to proper techniques in determining the pH of aqueous solutions by pH meter with the glass electrode. The manufacturer's instruction manual should be consulted for proper operation of the pH meter used. EQUIPMENT 1. pH meter, such as the Leeds and Northrup pH meter 7664 Leeds and Northrup Co., 4901 Stention Avenue, Philadelphia 44, Pa., or the Beckman Model-H2 pH meter, Scientific Instruments Division, Beckman Instruments, Inc., Fullerton, California. 2. Suitable calomel reference electrode. 3. Suitable glass electrode. 4. Brushless stirring motor such as Fultork Labmotor 14-502, Fisher Scientific Co. STANDARDIZATION 1. Ascertain that the meter is connected to the proper line voltage, the electrodes are properly plugged into the proper electrode connections, and that the meter is set for reading pH. RSV 0015002 METHOD 602.250 May 31, 1971 Page 2 of 4 STANDARDIZATION 2. With the meter in a "Zero11 or "Neutral*1 position, remove the water bath in which the electrodes are immersed and check visually to see that they are clean and unbroken and that the salt bridge is filled. Oils, etc. that adhere to the electrodes may be removed with a suitable solvent and the electrodes rinsed with water. 3. Immerse the electrodes in a suitable standard buffer, start the stirrer and check the temperature of the buffer. Adjust the temperature compensator on the meter to this temperature. 4. Switch the meter from "Neutral" to "Read" position and adjust the standardization control so that the meter reads the exact pH of the buffer solution. 5. After two minutes, read the meter again. If it has drifted fron the original setting, adjust the meter to the buffer pH value with fresh buffer solution and once more allow two minutes to check for drift. Con tinue until a stable reading is obtained. 6. Switch the meter from "Read" to "Neutral" position and turn off the stirrer. Remove the buffer solution from the electrodes, rinse them with water, and proceed to measurement of the sample solutions. PH MEASUREMENT 1. After standardization of the meter, rinse the electrodes with a portion of the sample solution and immerse the electrodes in a fresh portion of the sample solution. 2. Turn on the stirrer and allow to stir several minutes; check the sample temperature and adjust the temperature conpensator if necessary. Then switch the meter from "Neutral" to "Readlfposition. 3. Observe the pH reading. Wait two minutes and read again. If the second reading does not vary more than + 0.05 pH units from the first reading, the pH value is acceptable. RSV 0015003 METHOD 602.250 May 31, 1971 Page 3 of 4 pH MEASUREMENT (cont'd) 4. If the second reading varies more than + 0.05 ph units from the first reading, shut off the stirrer, switch the meter to "Neutral11 and repeat steps 2 and 3 with a fresh portion of the sample solution. 5. Continue as in steps 2, 3 and 4 until a reading is obtained that does not vary more than +0.05 pH units within two minutes. 6. Tun off stirrer, switch meter to "Neutral*1 position, remove sample solution from electrodes and clean them with rinses of water or a solvent that will effectively clean them. 7. Leave the electrodes immersed in distilled water. DISCUSSION The meter should be standardized with a buffer, the pH of which is within two pH units of the pH of the sample solution to be measured. Glass electrodes will occasionally lose response, so it is good practice to check the pH reading of a second buffer solution, bracketing the anticipated pH of the sample solution. If the buffers are known to be accurate and the meter does not accurately relate them, then either the meter or the electrode system is not functioning properly and an accurate pH value cannot be obtained. It should be noted that pH meters are often used with nonaqueous systems that remove water from the bridge in the calomel reference cell making a high resistance junction with resultant change in reference potential and instability. The pH response of the glass electrode can also be impaired by dehydration by non-aqueous solutions. The electrodes may be restored by soaking in distilled water. SAFETY Lir.e-operated pH meters should be grounded. RSV 0015004 METHOD 602.250 May 31, 1971 Page 4 of 4 REFERENCES 1. Willard, Merrier, and Dean,, "Instrumental Methods of Analysis", 3rd. ed. , 1958. D. Van Nostrand Co., New York, N.Y. 2. Manov, G. G. , and Acres, S. F. , uThe. pH of Some Standard Buffer Solutions from 0 to 60C, and the Calibration of Glass Electrode pH Meters", ASTM Bulletin No. 137, Dec. 1945. 3. Pharmacopeia of the United States XV, "Potenticmetric Determination of pH", 1. 933. /jw 7/21/71 RSV 0015005 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.251 July 13, 1971 Page 1 of 2 MATERIAL Reac*. Dr Overhead Gases ANALYSIS REQUIRED Vinyl chloride APPARATUS Perkin-Elmer Vapor Fractometer, Model 154B or equivalent Gas charging valve with 5 cc sample loop 1/4" O.D. stainless steel tubing PROCEDURE A. Column Preparation 1. Pack 16 ft of 1/4" stainless tubing with 337 dimethyl sulfolane on 45-60 mesh chromosorb. 2. Install column in the Fractcmeter. Adjust the temperature t.o 30 C and helium flow to 50 ml/min. Determine the optimum detector current and set at this value. Allow instrument to reach equili brium at these conditions. B. Analysis 1. Tun recorder on and set recorder range to 1. Recorder trace should shew no drift for five minutes before Fractometer is ready for use. 2. Purge 5 cc sample loop with sample to be analyzed; shut off valve from sample containers and enter 5cc sample into Fractometer. 3. Record peaks for ethylene and vinyl chloride. RSV 0015006 METHOD 602.251 July 13, 1971 Page 2 of 2 CALCULATIONS 1. Draw base lines for both peaks. 2. Use rale with 50 divisions per inch and measure peak height ar.d width at one-half peak height for all peaks. Measurements should be made to the nearest one-tenth of a division. 3. Calculate areas for both peaks; A-Hxw 4. Calculate mole percent VCM; mol % " Area VCM Area VCM + Area Ethylene /jw 7/22/71 RSV 0015007 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.252 July 13. 19/1 Page 1 of 2 MATERIAL Caustic ANALYSIS REQUIRED Assay APPARATUS a) Hydrometers capable of reading gravity to 0.001 ranging from 1.010 to 1.525. b) Constant temperature both @ 20C. DETERMINATION a) Cool 250 ml of sample to 1-2C below the specified temperature and fill a hydrometer jar to within 2-3 inches of the top. b) Place the specified hydrometer in the liquid and quickly adjust the sample temperature to the specified temp erature. c) Allow the hydrometer to float to rest. d) Read the bottom of the meniscus and record. CALCULATION Convert specific gravity to percent NaOH by following graph. /jw 7/22/71 RSV 0015008 IO * IO TO TH E C E N TIM E TE R 4 6 1 9 1 2 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.253 July 13.. 1971 Page 1 jf2 MATERIAL Acrylamide - Soap Solution ANALYSIS REQUIRED 7* Acrylamide APPARATUS a) Erle'meyer flask.. 250 ml heavy wall, fitted with a 24/40 Standard Taper joint (Ace Glass Co., No. 2671). b) Filling funnel, 50 ml cylindrical, open top with Standard Taper stopcock and 24/40 Standard Taper joint on bottom (Kontes Glass Co., No. K-63I25). In the top of the funnel insert a rubber stopper fitted with a short glass tube for connection to vacuum line. REAGENTS a) 0.1 N KBrO^ - KBr solution (2.79 g potassium bromate and 10 g of potassium bromide per liter) b) 6 N H2S04 c) 207. KI solution d) Std. 0.1 N Na2S203 e) 17* Starch solution PROCEDURE Weigh accurately a sample containing 3-4 g Stream #4 of acrylamide into a 500 ml volumetric flask, dilute to volume with water and mix. Pipet a 25.00 ml aliquot of this solution and 10 ml of bromate-bromide reagent into the 250 ml iodine. Draw 5 ml of 6N sulfuric acid into the flask and seal with water. Allow the solution to stand in the dark for 20 min. and shake frequently. Add 15 ml of potassium iodide solution, mix and then break the vacuum. Titrate the solution immediate ly with standard thiosulfate using starch indicator. Run a blank determination. RSV 0015010 METHOD 602.253 July 13, 1971 Page 2 of 2 CALCULATION (blank titer-sample titer) (N Na2S203) (3.554) % Acrylamide Weight of sample in aliquot /jw 7/22/71 RSV 0015011 * - > -i MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.25^ July 13, 1971 Page 1 of 2 MATERIAL Acrylamide - Soap Solution ANALYSIS REQUIRED X Alkyl Sulfate REAGENTS p-toluidir.e hydrochloride solution 6.8% Formula 30 Alcohol Carbon tetrachloride (reagent grade) Meta-cresol purple indicator (0.17, solution) Phenol red indicator (0.17. solution) 0.1 N NaOH APPARATUS 150 ml beaker 250 ml volumetric falsk 25 ml pipette 500 ml separatory funnel Analytical balance SCOPE This procedure employes the extraction of the organic sulfates by p-toluidine hydrochloride precipitation. PROCEDURE Using an arlytical balance, transfer 25 g on Stream #4 sample to a 150 ml beaker. Dissolve in distilled water and transfer to a 250 ml volumetric flask (a small amount of F-30 Alcohol may be used to dissipate foam) and dilute to 250 ml mark. Mix well and withdraw a 25 ml aliquot portion (equivalent to 0.5 g of sample). RSV 0015012 METHOD 602.254 July 13, 1971 Page 2 cf 2 PROCEDURE (cont'd) Transfer the aliquot portion to a 500 ml separatory funnel. Add 2 drops of phenol red indicator (red-alkaline, yellowacid). If solution is alkaline, adjust to neutral with .1 N HC1. If solution is acid, adjust to neutral with .1 N NaOH. To neutral solution add 30 ml of Formula 30 Alcohol, 30 ml of 6.8% p-toluidine hydrochloride solution and 30 ml of carbon tetrachloride. Shake mixture for three minutes (occasionally releasing gas from separatory funnel). Allow to stand and separate. Cut lower (carbon tetrachloride) layer into 250 ml containing 50 ml of Formula 30 Alcohol and 3 cc H2O adjusted to the alkaline (purple) end-point of meta cresol purple. Add 30 ml carbon tetrachloride to contents of separatory funnel and repeat extraction. Allow to stand and separate and again cut lower layer into same receiving flask. Repeat extraction once more. These combined extractions in the alcohol medium contain all the organic sulfates and are titrated directly with standard 0.1 N NaOH to determine the alkyl sulfate content. The end point is taken as the first change in color from gray to purple that remains for 15 seconds. CALCULATION ml NaOH x N x 300 x 100 Wt. of sample in aliquot x 1000 % Alkyl Sulfate as sodium lauryl sulfate /jw 7/22/71 RSV 0015013 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.255 July 13, 1971 Page 1 of 1 MATERIAL Product Latex B, BH and E Spent THF Solvent ANALYSIS REQUIRED Percent Total Solids APPARATUS Analytical balance capable of weighing to nearest 0.1 mg. Aluminum weighing dish Oven Dessicator 200 mesh sample screen PROCEDURE Screen latex sample through 200 mesh screen. Tare duplicate aluminum weighing dishes to 0.1 mg. Transfer 3-4 g of sampLe to each dish and obtain gross weight to 0.1 mg. Place the dishes in an oven at 130C for 3 hours. Cool dish in a dessicator and weigh to 0.1 mg. Report X solids. If two samples differ by more than 0.37, repeat. CALCULATIONS X Solids * net weight after drying _ net weight before drying x /jw 7/22/71 RSV 0015014 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL Product Latex B, BH and E DEPT. 60 METHOD 602.256 July 13, 1971 Page 1 of 1 ANALYSIS REQUIRED Latex Viscosity APPARATUS Brookfield viscometer. Model LVT with #2 RVT with #2 spindle. 400 ml beaker 200 mesh sample screen (Stainless Steel) spindle or Model PROCEDURE Screen latex sample through 200 mesh screen. Sample temp erature must be 2.5 + 1C. Pour 300 ml sample into a 400 ml beaker. Place a #2 spindle in the Brookfield viscometer model LVT and lower spindle into the sample to the level indicated by the indentation in the spindle shaft. Set the RPM selector at 6 and turn on the viscometer. After the spindle has completed 3 revolutions, depress the clutch and record the viscometer reading. While the clutch is still depressed turn the RPM selector to 60, turn on the viscometer, release the clutch and allow the spindle to complete 10 revolutions. Depress the clutch and record the viscometer reading. CALCULATIONS Convert the readings to centipoise. Reading at 6 RPM x 50 - centipoise (LVT) Reading at 60 RPM x 5 centipoise (LVT) Reading at 100 RPM (RVT) / jw 7/22/71 RSV 0015015 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.257 July 13, 1971 Page 1 of 4 MATERIAL Product Latex B, BH, and E ANALYSIS REQUIRED PH APPARATUS a) pH Meter, such as the Leeds and Ncrthrup pH meter 7664 Leeds and Northrup Co., 4901 Stention Avenue, Philadelphia 44, Pa., or the Beckman Model H2 pH meter. Scientific Instruments Division, Beckman Instruments, Inc., Fuller ton, California. b) Suitable calomel reference electrode. c) Suitable glass electrode. d) Brushless stirring motor such as Fultork Labmotor 14-502, Fisher Scientific Co. STANDARDIZATION a) Ascertain that the meter is connected to the proper line voltage, the electrodes are properly plugged into the proper electrode connections, and that the meter is set for reading pH. b) With the meter in a "Zero" or "Neutral*' position, remove the water bath in which the electrodes are immersed and check visually to see that they are clean and unbroken and that the salt bridge is filled. Oils, etc. that adhere to the electrodes may be removed with a suitable solvent and the electrodes rinsed with water. c) Immerse the electrodes in a suitable standard buffer, start the stirrer and check the temperature of the buffer. Adjust the temperature compensator on the meter to this temperature. RSV 0015016 METHOD 602.257 July 13, 1971 Page 2 of 4 STANDARDIZATION (cont'd) d) Switch the meter from "Neutral" to "Read" positior and adjust the standardization control so that the meter reads the exact pH of the buffer solution. e) After two minutes, read the meter again. If it has drifted from the original setting, adjust the meter ot the buffer pH value with fresh buffer solution and once more allow two minutes to check for drift. Continue until a stable reading is obtained. f) Switch the meter from "Read" to "Neutral" position and turn off the stirrer. Remove the buffer solution from the electrodes, rinse them with water, and proceed to measurement of the sample solutions. pH MEASUREMENT a) Screen the latex sample through a 200 mesh stainless steel screen. After standardization of the meter, rinse the electrodes with a portion of the sample solution and immerse the electrodes in a fresh portion of the sample solution. b) Turn on the stirrer and allow to stir several minutes; check the sample temperature and adjust the temperature compensator if necessary. Then switch the meter from "Neutral" to "Read" position. c) Observe the pH reading. Wait two minutes and read again If the second reading does not vary more than + 0.05 pH units from the first reading, the pH value is acceptable d) If the second reading varies more then + 0.05 pH units from the first reading, shut off the stirrer, switch the meter to "Neutral" and repeat steps b and c with a fresh portion of the sample solution. e) Continue as in steps b, c and d until a reading is obtained that does not vary more than + 0.05 pH units within two minutes. RSV 0015017 METHOD 602.257 July 13, 1971 Page 3 cf 4 pH MEASUREMENT (cont'd) f) Turn off stirrer, switch meter to "Neutral" positio-, remove sample solution from electrodes and clean them with rinses of water or a solvent that will effectively clean them. g) Leave the electrodes immersed in distilled water. SCOPE This method is intended to be a guide to proper techniques in determining the pH of aqueous solutions by pH meter with the glass electrode. The manufacturer's instruction manual should be consulted for proper operation of the pH meter used. DISCUSSION The meter should be standardized with a buffer, the pH of which is within two pH units of the pH of the sample solution' to be measured. Glass electrodes will occasionally lose response, so it is good practice to check the pH reading of a second buffer solution, bracketing the anticipated pH of the sample solution. If the buffers are known to be accurate, and the meter does not accurately relate them, then either the meter or the electrode system is not functioning properly, and an accurate pH value cannot be obtained. It should be noted that pH meters are often used with non-aqueous systems that remove water from the bridge in the calomel reference cell making a high resistance junction with resultant change in reference potential and instability. The pH response of the glass electrode can also be impaired by dehydration by non-aqueous solutions. The electrodes may be restored by soaking in distilled water. SAFETY Line-operated pH meters should be grounded. RSV 0015018 METHOD 602.257 July 13, 1971 Page 4 of 4 REFERENCES a) Willard, Merritt, and Dean, "Instrumental Methods of Analysis", 3rd ed., 1958, D. Van Nostrand Co., New York, N.Y. b) Manov, G. G., and Acree, S. F. , "The pH of Some Standard Buffer Solutions from 0 to 60C, and the Calibration of Glass Electrode pH Meters", ASTM Bulletin No. 137, Dec. 1945. c) Pharmacopeia of the United States XV, "Potentiometric determination of pH", 1. 933. /jw 7/22/71 RSV 0015019 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.258 July 13, 1971 Page 1 of 1 MATERIAL Produce Latex B, BHS and E ANALYSIS REQUIRED % Grit APPARATUS 325 mesh stainless steel screen Analytical balance capable of weighing to nearest 0.1 mg Oven Evaporating dish PROCEDURE Take 500 g of latex and filter through a 325 mesh screen. Wash the latex on the screen with a gentle stream of dis tilled or deionized water until no further latex can be washed through. Collect the retained grit by washing onto a weighed evaporating dish. Dry- the grit at 120C and determine the weight. CALCULATIONS % grit - wt- Srit x 100 500 g /jw 7/22/71 RSV 0015020 r- v > MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.259 July 13, 1971 Page 1 of 5 MATERIAL Produce Latex B and E ANALYSIS REQUIRED Surface Tension APPARATUS Fisher tensiomac Shallow sample container 200 mesh stainless steel screen PROCEDURE Screen sample through 200 mesh screen. In making a determination of surface tension, careful preparation of the sample and the Surface Tensicmat must precede the actual manipulation of the instrument. The sample should be placed in a glass beaker or cylindrical vessel with a diameter of at least 45 millimeters. For testing oil samples according to ASIM Method D-971, the glassware should be cleaned according to a definite pro cedure. Any residual oil from the previous sample is removed with petroleum naphtha or benzene followed by several washes with methyl ethyl ketone and water, then the glassware is immersed in a hot cleaning solution of chromic acid. The glassware also Should be rinsed thoroughly with tap water, then with distilled water. It should be drained in an inverted position over a clean cloth, unless it is to be used immediately. The platinum-iridium ring should be cleaned by rinsing it in petroleum naphtha or benzene, then by rinsing in methyl ethyl ketone. The ring should then be heated in the oxidizing portion of a gas flame. RSV 0015021 METHOD 602.259 July 13, 1971 Page 2 of 5 PROCEDURE (coat* d) The preceding instructions apply particularly to preparation for determinations in oil samples. A comparable degree of cleanliness should be maintained for other samples. Since surface tension is dependent upon temperature, con sideration must be given to this factor. For theoretical work, temperatures must be specified; however, 25dC is the temperature mast commonly used. For control work, the operator should use the same temperature for each type of measurement. Since the Surface Tensiomac may be employed as a manual or semi-automatic Instrument, separate procedures are described below for both operating modes. MANUAL DETERMINATIONS Measuring Surface Tension The cleaned platinum-iridium ring should first be attached to the hook at. the end of the lever arm. The arrest mechanism should be holding the arm at this time. The liquid to be measured is transferred to the clean glass vessel and placed on the sample table. The sample table is moved around until it is directly beneath the platinumiridium ring. Raise the sample table until the ring is immersed in the test liquid. The ring should be in the liquid, beneath the surface so that the entire ring will be wetted. About 1/8 inch immersion is generally considered sufficient. The torsion arm is now released and the instrument adjusted to a zero reading. Adjust the knob on the right side of the case until che index and its image are exactly in line with the reference mark on the mirror. Be careful to keep the ring in the liquid during this manipulation, raising or lowering the sample table if necessary by means of the knob adjustment underneath of the table. Now turn the knob beneath the main dial on the front of the case until the vernier reads zero cn che outer scale of the dial. RSV 0015022 METHOD 602.259 July 13, 1971 Page 3 of 5 MANUAL DETERMINATIONS (cont'd) Lower the sample table urttil the rir.g is In the surface of the liquid, while .it the same time adjusting the knob on the right side of the case to keep the index lined up with the reference mark on the mirror. The surface of the liquid will become distended but the index must be kept on the reference. Continue the two simultaneous adjust ments until the distended film at the surface of the liquid breaks. The scale reading at the breaking point of the distended film is the apparent surface tension. This reading is the one obtained after the sample has been adjusted for cross hairs mesh. Make only one repeat determination after this adjustment. Repeat determinations without cleaning the loop will give higher and higher readings due to the latex coating the wire. SEMI-AUTOMATIC DETERMINATIONS The semi-automatic operation of the FISHER Surface Tensiomat is basically similar to the manual mode of operation - the only essential difference being the use of samll electric motor to twist the torsion wire and thus raise or lower the ring in the test solutions. No adjustments or complicated procedures are involved in changing from eigher mode of operation to the other, the use of a switch to activate the semi-automatic feature and a slightly different technique in regard to the level of the surface or interface are the sole differences. The motor is connected to the semi automatic mechanism by means of a clutch which does not interfere with the manual mode. The semi-automatic drive mechanism actuates the torsion arm and consequently the ring; the position of the sample table is not changed or controlled by the drive mechanism. As a consequence, the simultaneous adjustment of torsion arm and sample table is not feasible. Therefore, it is necessary to determine the level of the surface or interface at the instant the film is broken by means of a manual determination and to maintain this level of surface or interface at the instant the film is broken by means of a RSV 0015023 METHOD 602.259 July 13, 1971 Page 4 of 5 SEMI-AUTOMATIC DETERMINATIONS (cont'd) manual determination and to maintain this level of surface or interface for subsequent determinations of similar samples. Provided the subsequent samples are of the same character (approximately the same density and surface or interfacial tension) no appreciable error is introduced by presetting the level of the surface or interface. Since a major advantage of the Surface Tensiomat is its ability to make repetitive determinations on similar samples rapidly, this determination of a level is a simple and worthwhile operation. A practical method for attaining a reproducible level for each sample is to use a sample container with a mark showing the level. More than one sample container can be so marked and used in succession. Also, it is usually practical to introduce reproducible volumes of sample into containers of reasonably uniform size. For example, Petri dishes with identical volumes of sample will produce levels which are for all practical purposes the same. Once the level of the surface has been determined and the approximate reading for the type of sample ascertained, the semi-automatic mode of operation is very simple. The sample is placed on the sample table and the ring immersed in the proper liquid. The knob on the right side of the case is put in the UP position for surface tension measure ments or interfacial tension measurements where the ring is pulled up through the interface, and in the DOWN position for interfacial tension determinations where the ring is forced down through the interface. When the surface or interface film ruptures, the level arm actuates a contact (No. 5 of Figure 1) which in turn actuates a relay and stops the drive motor. The value is then read from the proper scale on the dial. A pilot light on the front of the case indicates when the Surface Tensiomat is running. When the film ruptures, the motor stops and the light goes out. The switch must be returned to the NEUTRAL position and the lever arm returned to the proper position prior to making the next determination. RSV 0015024 METHOD 602.259 July 13, 1971 Page 5 of 5 SEMI-AUTOMATIC DETERMINATIONS (coat'd) Experience has shown that readings obtained using semi automatic operation will be slightly different from those obtained manually. However, with any given set of conditions, these variations can be determined by manual and semi-auto matic experiments, and if necessary, the -variations may then be taken into account by the user. / jw 7/22/71 RSV 0015025 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.260 July 13, 1971 Page 1 of 5 MATERIAL Product Latex B and E ANALYSIS REQUIRED Glass Transition Temperature (Tg) APPARATUS AND MATERIALS duPont 900 Differential Thermal Analyzer or its equivalent Vacuum Pump Liquid nitrogen and reservoir Dry nitrogen gas Bunsen burner TEST SPECIMEN The test specimens are prepared by air drying a film of latex on a glass plate. PROCEDURE A condensed operating procedure is described here. For detailed operating instructions, refer to duPont 900 DTA instruction manual. a) Preparation for the Run 1) Cold junction thermocouples should be at room temp erature. 2) Fill macro sample tube with the sample to depth of 5 mm. Brush the loaded sample tube through a small Bur.sen flame two or three times, and pack the sample tightly by pushing the centering ceramic sleeve to the bottom of the tube. A thermocouple is then placed in the sample so that the junction touches the bottom of the tube. The ceramic sleeve should be positioned over the thermocouple to center it in the macro tube. RSV 0015026 METHOD 602.260 July 13, 1971 Page 2 of 5 PROCEDURE (cont1d) 3) Fill control and reference tubes with quartz powder to depth of 5 mm. Insert thermocouples and center ing sleeves in tubes. 4) Wrap glass wool around thermocouple connections at the receptable in cell assembly in order to shield from drafts during cooling. 5) Place tubes in heating block, bend leads so junctions bottom in tubes, and put cell assembly in place. 6) Place chart paper on recorder. b) Set the Recorder Controls 1) Switch POWER to RECORD (5 minutes warm-up). 2) Set T ZERO SHIFT at +5- 3) Set T SCALE at 10C/in. (Scale on chart: -50C to + 50 C) 4) Turn A T ZERO SHIFT until pen is near top of chart. 5) Set A T SCALE at 0.2C/in. 6) Set BASELINE SLOPE to 0. c) Set Sample Atmosphere Controls 1) Connect nitrogen gas supply to PURGE, liquid nitrogen to COOL and vacuum to VACUUM connections. 2) Open VACUUM and COOL valves fully, this introduces liquid nitrogen into the cell. 3) When pen reaches chart reading of -20C, close COOL valve and adjust the VACUUM gauge to read approxi mately 15. Set GAS FLOW of purge nitrogen at 2 SCFH. RSV 0015027 METHOD 602.260 July 13, 1971 Page 3 of 5 PROCEDURE (cont'd) d) Set Temperature Program Controls 1) Push RESET. 2) Set TEMPERATURE RATE at 20C/min. 3) Turn STARTING TEMPERATURE clockwise until heater voltage indicator reads minimum value. Then turn counterclockwise until voltage indicator just begins to move upscale. e) Start the Run 1) Set PROGRAM MODE at HEAT. 2) Set POWER at RECORD. 3) The thermogram will not be recorded on the chart until the pen reaches on the right hand edge of the paper. The A T SCALE or A T ZERO SHIFT controls may be adjusted at any time during the run to keep strong endotherms or exotherms on the chart paper. Similarly, the BASELINE SLOPE control may be ad justed at any time during the run to make the baseline more nearly horizontal. f) Conclude the Run 1) Turn PROGRAM MODE to HEATER OFF, 2) Turn POWER to STAND BY. 3) After each run the sample tube may be discarded. The sample thermocouple and the centering ceramic sleeve should be cleaned by burning over a small Bunsen flame to burn all organic compounds, they can be reused for twenty or more runs. RSV 0015028 METHOD 602.260 July 13, 1971 Page 4 of5 PROCEDURE (cont'd) g) Definition of Transition Temperature The literature of DTA contains many definitions for the location of significant transition temperatures. This procedure defines the transition temperature as a temperature of extrapolated onset as shown in the figure. Unlike first-order thermodynamic transitions, the glass transitions of amorphous polymers may not exhibit a peak but only show a shift in baseline. Similarly, the Tg is defined as the temperature.of the extrapolated onset in the thermogram. h) Report The report shall include the following: 1) Complete Identification of the material tested. 2) Size of sample tube. 3) Reference material. 4) Heating, rate, C/min. 5) Nitrogen purge rate, SCFH. 6) Temperature scale and shift factor. 7) A T of sensitivity, C/in. RSV 0015029 ^k_ METHOD 602.260 July 13, 1971 Page 5 of 5 SCOPE This method describes a test procedure for the determination of Tg of the polymer using a differential thermal analyzer. SIGNIFICANCE Differential thermal analysis (DTA) is a technique for studying the thermal behavior of materials as they undergo physical and chemical changes during heating or cooling. The glass transition temperature (Tg) of amorphous polymer is only one of many thermal fingerprints of polymer obtainable with DTA. Determination of Tg, which is one of the most important fundamental properties of polymers, by DTA repre sents one of the simplest and fastest methods. / jw 7/23/71 RSV 0015030 7 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.261 July 13, 1971 Page 1 of 4 MATERIAL Product Latex B and E ANALYSIS REQUIRED Intrinsic Viscosity APPARATUS 1. Viscometers: a. Cannon-Ubbelohde Dilution Type, Size 50, uncalibrated b. Cannon-Fenske #50 2. Constant temperature water bath, + 0.05C 3. Volumetric pipettes: 10 ml, 20 ml, 100 ml 4. Aluminum weighing dishes 5. Forced air oven 6. Stopwatch 7. 1 Liter volumetric flask 8. Tetrahydrofuran (THF), Fisher T-397) PROCEDURE 1. Measure the solids content of the latex sample and dilute it to 457. solids. 2. Weigh 2 grams of the 457. solids latex into a 200 ml jar. 3. Add 100 ml of pure THF (Tetrahydrofuran) to the jar, cap tightly, and shake. Heat the sample at 40-50C for 1 hour with intermittent shaking. The solution may still appear hazy. RSV 0015031 V: tZJC'L > METHOD 602.261 July 13, 1971 Page 2 of 4 PROCEDURE (cont'd) 4. Prepare the dilution solvent by adding 10.9 ml H2O to a 1000 ml volumetric flask and making up to the mark with pure THF. 5. Obtain tare weights on two aluminum weighing dishes. Pipette 10 ml of the polymer solution into each dish and dry to constant weight at 40-50C. This will take approximately one hour. Record the weight of residue. 6. Determine the concentration of the polymer solution. Wt. residue x 10 equals the concentration expressed as grams per deciliter. The initial concentration should be just below 1 gm/deciliter. 7. With a small size coarse glass filter adapted to a 10 ml pipette, draw up 10 ml of the dilution solvent and deliver to a viscometer. The viscometer water bath should be maintained at 30C. 8. Record the flux time of the dilution solvent. A viscometer should be chosen which gives a 100-150 sec. flux time for the dilution solvent. Make three deter minations and record the average. 9. Replace the solvent in the viscometer with the polymer solution as in No. 7. Determine the flux time at this concentration. 10a. If a dilution type viscometer is used, simply add 10 ml of the dilution solvent to the polymer solution already in the viscometer and determine the flux time for this solution. Calculate the actual concentration of the solution. b. Make a second dilution by adding 20 ml of dilution solvent to the viscometer after Step 10a. Determine the flux time for this solution and calculate the exact concen tration.11 11. If a dilution type viscometer is not available, the two additional solutions can be made up separately by adding 10 ml and 30 ml of dilution solvent to each of two 10 ml samples of the original polymer solution. RSV 0015032 METHOD 602.261 July 13, 1971 Page 3 of 4 PROCEDURE (cont'd) 12. For each of the three solution concentrations, calculate the reduced viscosity according to the following formula Reduced viscosity i relux time of solution \Flux time of solvent Actual concentration in gm/deciliter 13. Plot the reduced viscosity versus the actual concen tration. The. data should fall on a straight line which is extended to zero concentration. The intrinsic viscosity is given by the value of the reduced viscosity at zero concentration and will gen erally be in the range of 0.6-0.8 deciliters/gm. (See attached Figure.) / jw 7/23/71 RSV 0015033 602.261 Page 4 of 4 RSV 0015034 S o lu tio n C oncentration - g ra m s /d e c ilite r MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.262 July 13, 1971 Page 1 of 5 MATERIAL Product Latex B and E ANALYSIS REQUIRED Particle Size APPARATUS Amberlite XAD-2 resin Analytical balance Tumbler Buchner funnel, monofilament nylon filter cloth Aluminum weighing dish Fisher Tensiomat REAGENTS Sodium lauryl sulfate (sipon WD) PROCEDURE A. Wash Amberlite XAD-2 absorbent with distilled water. Remove excess water from washed Amberlite and store Amberlite in closed jar to keep moist. B. Weigh 150 g of screened (200 mesh) latex (40-507* T.S.) and 300 g wet Amberlite into 16 oz. wide mouth bottle. C. Cap bottle, shake to mix well, and keep mixed by slow tumbling motion for one hour. D. Filter out latex from mixture with Buchner funnel and monofilament nylon filter cloth under suction. E. Determine surface tension of latex. Repeat Steps B-D if surface tension is less than 70 dynes/cm. RSV 0015035 METHOD 602.262 July 13, 1971 Page 2 of 5 PROCEDURE (cont1d) F. Determine total solids of the Amberlite treated latex stock: Weigh out 1-2 g of stock in aluminum dish. Add enough water to thin out latex and barely cover dish bottom. Dry in oven at 120eC to constant weight (approx. 1 hour). Calculate 7. T. S. from dry weight. G. Prepare two latex samples in 4 oz. bottles with following compositions: Sample 1: 60 g Amberlite treated latex stock 11 g 107, SLS (Sipon WD) 39 g Distilled water 110 g latex with 17* SLS Sample 2: 60 g Amberlite treated latex stock 50 g Distilled water 110 g latex without SLS Shake to mix well. H. Mix Samples 1 and 2 in 1 oz. bottles at various proportions as shown in Column I of Table I. Shake to mix well. The corresponding SLS concentration of each sample is shown in Column II of Table I. I. Determine surface tension of the 11 samples. A hypo thetical set of surface tension values is given in Column III of Table I for illustrative purposes. J. Plot surface tension vs. SLS concentration of sample in semi-log graph paper as shown in Fig. I. The resulting graph will typically show a break which separates the two rather distinct portions of the graph, i.e., the initial portion where the surface tension decreases rapidly with increasing SLS concentration, and the latter portion where surface tension practically remains at a constant low value. RSV 0015036 METHOD 602.262 July 13, 1971 Page 3 of 5 PROCEDURE (cont'd) K. Compute the particle size using the following equation: % T.S. of latex stock x (60/110) Particle size (X) * 0.24 Titration end point in g SLS g latex L. When particle size is much larger than 1000 X or much A,smaller than 500 the titration end point will move too close to the low or high end of the covered SLS concentration range, making a precise determination of the end point difficult. -g-SLS When the end point is too low (<0.002 g latex), repeat the determination using the same procedure except change the canposition of Sample I of Step G as follows: 60.0 g Amberlite treated latex stock 5.5 g 10% SLS 44.5 g Distilled water______ 100.0 g latex with 0.5% SLS and correct the computed particle size of Step K by a factor of 2. R SLS When the end point is too high (>0.008 g latex), repeat determination. Change composition of Sample I of Step G to: 60 g Amberlite treated latex stock 22 g 10% SLS 28 g Distilled water 110 g latex with 2% SLS and then correct particle size computed in Step K by a factor of 0.5. RSV 0015037 Table I METHOD 602.262 July 13, 1971 Page 4 of 5 I gr Sample 1 gr Sample ii 0/20 2/18 4/14 6/14 8/12 10/10 12/8 14/6 16/4 18/2 20/0 II gr SLS gr latex 0 0.001 0.002 0.003 0.004 0.005 0.006 0.0m 07 0.008 0.009 0.010 III Surface tension 71-5 64,8 56.7 49.6 43.5 38.2 34.5 33.3 33.1 33.1 33-0 / Hypothetical set of values for Illustrative / jw 7/23/71 RSV 0015038 , y -*r*>L > METHOD 602.262 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.263 July 17, 1971 Page 1 of 3 MATERIAL Product Latex B and E ANALYSIS REQUIRED Instron tests for tensile stress, elongation, and 100% modulus. APPARATUS Instron Tester Glass Plate and Razor PROCEDURE 1. Draw down a wet film of screened (200 mesh) latex using an 9-9 mil bar. 2. Slowly air dry the film. If drying proceeds too fast, the film will crack and craze excessively. Drying can be slowed down by placing a flat box over the wet film immediately after it is drawn down. Drying will take 2-3 hours. 3. Remove the film from the glass plate and place it onto a Teflon covered plate. If the film adheres too tightly to the glass plate, it may be necessary to slightly moisten it to remove it. Also, it is usually better to cut small sections of film with a razor and remove these from the glass plate rather than trying to remove the entire film intact. 4. Allow the film to air dry completely, then cure in a hot air circulating oven for 5 minutes at 150C. 5. Accurately cut the cured film into pieces 1/2" x 2" for testing. Use a sharp razor for cutting the test pieces and avoid any edge defects. Also avoid using sections of the cured film with obvious defects, such as air bubbles or inclusions of foreign particles. If a specimen cutting die is available as described in A5TM D882-GIT, it can be used.6 6. Determine the thickness of each test strip, using any con venient calipering device which can measure and read out to 0.05 mil. RSV 0015040 Procedure (cont'd) METHOD 602*263 7/17/71 Page 2 of 3 7. Reinforce the ends of each test specimen, using Scotch tape. This allows more secure clamping of the specimen and helps to minimize slippage in the jaws. One-half inch of each end should be taped. Taged_ 1/2" 1" Taped 1/2" 8. Place the specimen in the Instron with a jaw span set at 1" and strain the specimen at a rate of l"/min. until it fails. 9. Discard samples which show slippage in the jaws or within the taped ends. Also discard the results if an obvious defect develops upon straining. 10. The output curve will look something like this: a Nominal tensile stress at break = (psi) Load at break (A) (Sample width in inches) x (Initial thickness in inches) b. % Elongation at break * Extension in inches at break (B) Initial sample length (1") x 100 RSV 0015041 METHOD 602.263 7/17/71 Page 3 of 3 Calculations (cont'd) c. Initial tensile modulus (psi) - from line C Nominal tensile stress at break (A)____________ Extension E in inches/initial span (1" ) d. Secant modulus at 100% extension * (psi) - from line D Load at elongation of 1" (F) (Sample width in inches) x (Initial thickness in inches) sff 7/19/71 RSV 0015042 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.264 July 17, 1971 Page 1 of 3 MATERIAL Product Latex B and E ANALYSIS REQUIRED % Acrylamide APPARATUS Kjeldahl apparatus 2000 ml beaker Laboratory agitator for 2000 ml beaker Buchner funnel Vacuum source Vacuum desiccator REAGENTS Isopropanol PROCEDURE Twenty ml latex are slowly added to a stirred beaker containing 1200 ml isopropanol. The coagulated latex and isopropanol are then stirred for 5 minutes. The polymer is filtered out using -wo isopropanol rinses. The vacuum to the filter is released before the polymer packs into the filter paper. The polymer is shredded up and stirred in 1500 ml of H2O for 2 hours. It is then filtered using five 300 ml portions of H2O as rinses. The polymer is dried in a vacuum desiccator for 24 hours at room temperature or until completely drv. Total nitrogen in the dry polymer is obtained by the standard Kjeldahl method. Total nitrogen is assumed to be present as acrylamide. Therefore, % acrylamide (%N) The total acrylamide put into the latex based on solids content may be calculated. % Acryl (% Acryl. in Soln) (100)j +0 RSV 0015043 NITROGEN DETERMINATION - KJELDAHL METHOD 602.264 7/17/71 Page 2 of 3 EQUIPMENT 1. Kjeldahl digestion rack - gas fired. 2. Kjeldahl digestion flask - 100 ml capacity. 3. Distillation unit - JFQ Plant standard apparatus drawing 2. 4. Kjeldahl digestion catalyst - thoroughly mix 150 g. of po tassium sulfate anhydrous arrf 10 g. of yellow mercuric oxide powder. 5. Bromcresol green methyl red mixed indicator solution - mix 50 ml of bromcresol green solution (0.1% in 95% ethanol) and 10 ml of methyl red solution (0.1% in 95% ethanol). 6. Zinc metal, 20 mesh. 7. Phenolphthalein solution - 1.0% in Formula 30 alcohol. 8. Boric acid solution - 4% in distilled water. 9. Sodium thiosulfate - 44% aqueous solution. 10. Sodium hydroxide - 50% aqueous solution. 11. Volhard absorbers - JFQ Plant standard apparatus drawing 22. 12. Usual laboratory reagents and equipment. DETERMINATION 1. Accurately weigh 0.20 to 0.25 g. of sample into a 100 ml Kjeldahl flask, add 15 g. of the digestion catalyst and 20 ml of concentrated sulfuric acid and swirl to mix. carry through a blank digestion omitting the sample. 2. Add several glass beads or boiling chips and place the flask in a 110C oven for over night charring. 3. Remove the sample from the oven and digest slowly, gradually increasing the heat until the mixture boils briskly. Continue to heat until the mixture becomes clear. 4. Continue the digestion for an additional hour. RSV 0015044 Nitrogen Determination (cont'd) METHOD 602.264 7/17/71 Page 3 of 3 5. Cool to room temperature and cautiously add approximately 75 ml of distilled water with mixing. 6. Transfer quantitatively with the aid of distilled water to a 500 ml round bottom flask containing 10 g. of zinc metal. Add several drops of phenolphthalein solution and attach the flask to the distillation assembly. Carry through the blank in a similar manner. 7. Add sufficient 4% boric acid solution to a Volhard absorber so that the bottom overflow exit is completely covered and add 4-5 drops of the mixed indicator. 8. Attach the absorber tightly to the condenser exit. 9. Add to the round bottom flask, via the distillation side arm, sufficient 50% sodium hydroxide to make the sample alkaline to phenolphthalein. Add 5 ml of 44% sodium thiosulfate in the same manner. 10. Make sure all connections are tight, apply heat to the flask and distill approximately 100 ml of distillate into the Volhard absorber. 11. At the end of the distillation, disconnect the Volhard absorber and titrate its contents with standardized N/10 HC1 solution. 12. Calculate: (ml titer for blank-ml titer for sample) x 0.14% sample weight % Nitrogen sff 7/19/71 RSV 0015045 r MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.266 July 17, 1971 Page 1 of 1 MATERIAL Product Latex B and E ANALYSIS REQUIRED Film Clarity APPARATUS Glass plate Drawdown bar PROCEDURE 1. Draw down a latex film from screened latex (200 mesh) on a clean glass plate, using an 6 mil applicator bar. The exact thickness of the film is not critical. 2. Allow the wet film to slowly dry at room temperature. The film should be about 3 mils thick. If the film is too thick, it will show excessive crazing upon drying. 3. Observe the film and note the following points: a. Continuity of the film formed. b. Presence of grit. c. Presence of incompatible deposits in the film. d. Excessive roughness or graininess in the film. e. Clarity and color of the film. :ff 7/19/71 RSV 0015046 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.26? July 17, 1971 Page 1 of 6 MATERIAL Product Latex BH ANALYSIS REQUIRED I.G.T. Test APPARATUS Brookfield LVT or RVT viscometer Holder for wire wound coating rods Analytical balance Supply of paper and board substrates Paper cutter I.G.T. Printability Tester, consisting of: Printmaker equipped with pendulum and one inking disc ink distributing apparatus with a set of two polymethane rollers. I.G.T. Spring Drive Device to increase speed to the 0-650 ft/min range. Four double width inking discs (20 mm), aluminum I.G.T. ink pipette Extra mouthpiece for I.G.T. ink pipette Set of two glue-glycerine composition rollers 10 sets of 6-paper packings 25 mm wide for I.G.T. Tester Mylar film - 1 mil thick (Herculene or Stabiline Drawing film from Keuffel and Esser). Solvent for clean-up. 2-5 gal cans of Varn Wash V-120 from Vain Products Co., Flushing, N.Y. Two, 1/2# tubes of #4, #5, #6 black tack graded inks from Interchemical Corp., I.P.I. Printing Ink Division, 4168 Meramec, St. Louis, Mo. 63105 Three, 50# bags of Lustra Coating Day from Freeport Kadin Co., 405 Lexington Ave., N.Y., N.Y 10017. A binocular microscope with a 15-20X magnification. One - Series 2000 standard Premier laboratory Dispersator, 1/2 HP single phase, universal type motor, powerstat, com plete with stand and mounting bracket, B/H 2053 equipped with l-l/2h Hi-Vis head and stub shaft assembly, with shaft 3/4" dia. x 11" long constructed of 316 stainless steel. Order from Premier Mill Corp., 224 Fifth Ave., New York, N.Y. Pyrex radiant panel heater, cat. no. 604001, 250 volts, 3500 watts. Corning Glass Works, Corning, N.Y. RSV 0015047 Apparatus (cont'd) METHOD 602.267 7/17/71 Page 2 of 6 One - ATC percentage input timer, type 304B-07-B-C-XX, 230 volts, 60 cycle, 20 amp.. Automatic Timing & Controls, Inc., King of Prussia, Pa. 19406. 3 each of the following wire wound drawdown coating rods: #8, #10, #12, R.D. Specialties Co., P.0. Box 6, Webster, N.Y. 14580. One - #162D case for surface mounting of type 304 ATC0TR0L manual set percentage timer, general purpose sheet steel (Order with #15 above) PROCEDURE FOR MEASURING PIGMENT BINDING STRENGTH OF LATEX - IGT PICK STRENGTH The procedure can be broken down into four parts: 1) preparation of the coating formulation, 2) coating and drying of the substrate, 3) printing of the samples on the tester, 4) determination of end-point. 1. preparation of the Coating Formulation The coating formulation is a simple mixture of latex plus coating clay diluted to a total solids content of 60%. The amount of latex used is such as to give a mixture of 18 parts dry latex solids per 100 parts dry clay solids. A 70% solids clay slip is prepared as follows: a. Add 1.5 grams tetrasodium pyrophosphate (TSPP) to 215 grains of deionized or distilled water and stir until the TSPP is dissolved. b. Place the solution under the Premier Dispersator and slowly add in 500 grams of Lustra Coating Clay. It will be necessary to increase the speed of the agitator as the clay is being added. c. After all the clay has been added, disperse at the highest speed possible for 10 minutes. d. Determine the solids content of the clay slurry. To make up the coating formulation, add 286 grams of the clay slurry (equal to 200 grams of oven dry clay) to a 250 ml beaker. Add latex to the beaker to give the equiva lent of 36 grams of oven dry latex. RSV 0015048 Procedure (cont'd) METHOD 602.267 7/17/71 Page 3 of 6 The amount of latex to table: % Solids of Latex add can be found from Grams of Latex to To Clay Slurry the Add following 45 80.0 46 78.3 47 76.7 48 75.0 49 73.5 50 72.0 After the latex has been added, add water to make the solids content of the total coating formulation equal to 60%. The amount of water needed will depend on the solids content of the latex, assuming that the clay slurry has been made up properly at 70% solids. The following table can be used as a guide for the water addition: ; of Latex Grams of Water to Add To Formulation 45 27.0 46 20.7 47 30.3 48 32.0 49 33.5 50 35.0 The coating mixture should be stirred for 10 minutes to insure proper mixing of all components. Filter the coat ing through a conical 200 mesh stainless steel screen to remove any aggregates of dried material ar.d to remove excess entrained air. The viscosity of the coating formulation should be measured with a Brookfield viscometer. Model RVT, using a #2 spindle at 10 RPM, room temperature in the 250 ml beaker. 2. coating and Drying of the Substrate The substrate to be used is a bleached solid sulfate board (15 point Fold-Brite White Tag Bleached Board from Riegel paper Corp., Riegelwood, N.C.). The coating is applied to the "wire" side of the sheet. The wire side of the sheet can be discerned by the faint screen-like markings on the RSV 0015049 Procedure (cont'd) METHOD 602.267 7/17/71 Page 4 of 6 sheet when viewed with glancing light. it is important that the proper side be coated since each side may give different results A dry coat weight of 10-12#/3300 ft.^ is-applied using the appropriate wire wound rod. This is equivalent to a dry coat weight of .00957-.01148 gm./in.2. The uncoated base sheets are supplied cut to 12" x 15" with the- grain direction in the long dimension. The base sheet should be weighed and the base sheet weight calculated as follows: grams 12" x 15" = base sheet weight in gm./in. 2 Immediately after the coating is applied, the sheet is dried in the infrared oven for one minute at a temperature of 120C. If the sheet is not properly dried, the results may be too low. After drying, the sheet is allowed to come to equilibrium in a constant temperature and humidity room and trimmed to a size of 10" x 11". it is important to keep track of the grain direction. A good convention to follow is to keep the long dimension the grain direction. Weigh the coated sheet and calculate the weight per unit area: weight of coated sheet in grams 10" x 11" Coated sheet 2 wt. in gm/in. The coat weight is the difference between the coated sheet weight and base sheet weight. 3. Printing of the Samples The samples to be tested should be allowed to equilibrate to constant temperature and humidity. Control of both room temperature and humidity is very important in obtaining reproducible results. T.A.P.P.I. standard conditions of 73F. and 50% relative humidity are recommended if at all RSV 0015050 Procedure (cont'd) METHOD 602.26? 7/17/71 Page 5 of 6 possible to achieve with tolerable temperature variations of 3.5F and relative humidity variations cf 2%. The samples should be cut as strips one inch wide by ten inches long? in this case with the grain direction being the short dimension. Avoid touching the coated surface or in any other way contaminating the coated surface. The tester should be set up and inked with 2 ml of #5 ink according to the instructions supplied with the tester. The B scale spring drive is used to give a velocity range of from 0 to 630 fpm. A loading of 70 kg. should be used on the printing nip to insure good contact of inked roll and coated sample. At least two strips from each sample should be printed. In addition, a control latex should be run with each set of samples to insure reproducibility of results from one day to the next. After every four strips, the ink supply on the distribution system should be replenished with 0.16 ml of ink. The glue-glycerine roll should be used as the top roll of the ink distribution device. After two hours the ink distribu tion system should be cleaned up and a fresh supply of ink used. 4. Determination of the End-Point The test is designed to measure the tack stresses on the surface of the sheet which cause rupture of the coating film. These stresses are a function of the ink viscosity and the speed of printing, in the I.G.T. test the ink viscosity is kept constant by the use of a special tack graded ink. The strip which is printed is accelerated through the printing nip so that the speed of the sample through the nip is a logarith mic function of distance along the nip. The end point measured is that speed which just causes rupture of the coating film. In order to define this point the sample is removed from the tester and examined under a low power microscope. Starting with the lowest speed end (the clamped end) draw the sample under the microscope and look for areas RSV 0015051 Procedure (cont'd) METHOD 602,267 7/17/71 Page 6 cf 6 where the coating has been torn away. These will shew up as distinct white spots against the black ink printed surface* Do not confuse white spots caused by the ink not covering the surface with picked areas. A little practice will be needed to tell the difference between a non-inked area and a pick. As the strip is scanned, the severity of picking should in crease. The end point is marked as the point at which picking appears to increase in severity. Occasionally, a few isolated will be observed- on the early part of the sample. These should be ignored if the picking does not increase in severity with distance. There is a considerable judgment factor in volved in consistently calling the end point so it is often advisable to have only one person perform the test. The end point is marked on the strip and converted to a speed reading (f.p.m.) using the scale supplied with the instrument. s ff 7/20/71 RSV 0015052 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL DEPT. 60 METHOD 602.269 July 17, 19 M Page 1 cf 2 Aqueous Charge ANALYSIS PP-OTTTRFD SLS Concentration APPARATUS 100 ml, 200 ml volumetric 20 ml pipet 125 ml separatory funnel 50 ml pipet Cotton Beckman Spectrophotometer flasks REAGENTS Methylene Blue Solution Chloroform PROCEDURE Accurately weigh 1 g sample into a 200 ml volumetric flask. Dissolve in distilled water and make up to volume. Pipette 20 ml into a 125 ml separatory funnel. Add 30 ml of distilled water and 25 ml of methylene blue solution. Mix well by swirling. Extract with 15 ml CHCln, then 25 ml CHCI3 collecting the fractions in a 100 ml volumetric flask. NOTE; Filter the fractions through a cotton plug that has been previously wetted with CHCI3. Bring to volume with CHCI3. Read at 652 mfi on the Beckman vs. CHCI3 for blank. Settings Required; Phototube in Load Resistor #3 Slit width 0.04 to 0.1 Tungsten lamp RSV 0015053 / METHOD 6C2.263 7/17/71 Fags 2 of 2 CALCULATIONS % SLS (A652)(0.38) Sample Weight SCOPE This method is for small concentrations of S.L.S. (40.5%) in process streams such as the initial aqueous charge, it involves complexing the SLS with methylene blue? extraction with CHCI3, and subsequent U.V. reading at 652 mu DISCUSSION 1. Samples should be read within 90 min. 2. Sample size may ha^'e to be varied with stream charge variations. 3. Methylene blue, N.F. - Matheson, Coleman and Bell. Methylene 3lue Solution - dissolve 0.1 g methylene blue, N.F. contained in a 100 ml volumetric flask in distilled water and dilute to 100 ml. Transfer 30 ml cf this solution to a 1 liter volumetric flask, containing 500 mi of distilled water, 6.8 ml of concentrated sulfuric acid, and 50 g of sodium sulfate anhydrous, A.R. grade. Shake until solution is com plete and dilute to volume with distilled water. : ff 7/20/71 RSV 0015054 .J MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL Vinyl Chloride ANALYSIS REQUIRED Determination of Iron in Vinyl Chloride SAMPLE 100 ml glass pressure sample bomb APPARATUS Beckman Spectrophotometer Dry Ice Chest Two, 250 ml Erlenmeyer Flasks 100 ml Graduated Cylinder 10 ml Graduated Cylinder 100 ml Volumetric Flask DEPT. 60 METHOD 602.289-A (WC) July 17, 1971 Page 1 of 4 REAGENTS -10% Aqueous solution of Hydroxylamine hydrochloride -2 molor solution of C.P. sodium acetate (164 + 0.01 g in 1 liter of distilled water) -0.1% solution of brom phenol blue (0.1 g dissolved in 100 ml of 50% ethyl alcohol) -0.12% aqueous solution of o-phenanthroline -Alcohol water solution (25 parts 2B alcohol and 30 parts water) -Concentrated C.P. HC1 PROCEDURE Place 25 ml of the alcohol-water solution in a 250 ml erlen meyer flask. From the sample bomb, previously cooled for two hours in the dry ice chest, measure out 100 ml of vinyl chloride into a chilled graduated cylinder. Add the vinyl chloride to the 250 ml erlenmeyer flask and allow to evaporate. Then swirl the flask to remove the last trace of vinyl chloride. A vented hood is needed for the above evaporation. RSV 0015055 t METHOD 602.289-A (WC) July 17, 1971 Page 2 of 4 Procedure (cont'd) Quantitatively transfer the residue to a 100 ml volumetric flask. Acidify the solution in the volumetric flask by adding two drops of concentrated hydrochloric acid. Add two drops of brora phenol blue to the flask and then add the 2 molar sodium acetate solution dropwise until the solution turns a faint blue. Next, add four ml of 10% hydroxylamine hydrochloride solution, and then 10-ml of 0.12% o-phenathrcline. Dilute to the mark with distilled water; mix well, and allow the solution to stand for at least 20 minutes. With the Beckman spectrophotometer measure the light trans mission at 510 mu, with visible light. CALCULATIONS Refer to the attached graph and report the iron concentration to the nearest 0.05 ppm. PREPARATION OF REAGENTS 10% aqueous hydroxylamine HCl - dissolve 100 g of the salt in 900 ml of distilled water. Be sure water is iron free. Store in P.E. bottle. 2 molar sodium acetate - dissolve 164 gms of C.P. salt in one liter of distilled water. Mix. Store in clean bottle. .1% solution of brom phenol blue - dissolve .1 gm of the in dicator in 50 ml of EtOH. Dilute to 100 ml with distilled water. .12% of o-phenanthroline - dissolve .12 gms of o-phenanthroline in 100 ml distilled water. Alcohol water solution - Mix 455 ml of 2B alcohol and distilled water up to one liter.1000 1000 ppm Fe Standard - dissolve .1000 gms of C.P. iron wire in 10 ml of 20% HCl (iron free). Cool and dilute to 100 ml with distilled water. Mix. Keep for stock reagent. 10 ppm Standard - dilute 1 ml of 1000 ppm standard to 100 ml with demineralized water. Mix. Keeps only one or two days. RSV 0015056 f METHOD 602.289-A (WC) July 17, 1971 Page 3 of 4 STANDARDIZATION AND/OR CALIBRATION To five 100 ml volume flasks add 0, 3, 5, 7. and 10 ml of the 10 ppm standard. These correspond to 0, 30, 50, 70 and 100 pgms of Fe, Follow the procedure outlined above from paragraph three on. Determine absorbance in 20 mm cells against the zero standard above at 510 mp. Plot the absorbances so obtained against the corresponding pgxns of Fe. Draw in the best average line. Use this as a working curve or calculate a factor . f from it such that f x absorbance pgms Fe. SAFETY Handle VCM with caution. Keep vapors away from sparks and flames. Guard against cold burns, handle with gloves. Use normal pre cautions with chemicals, glassware, and electrical apparatus. ANALYTICAL TIME 1/2 hour PRECISION OF RESULTS & SIGNIFICANT FIGURES TO REPORT 95% confidence limits are .1 ppm at a level of 1 ppm or 10% of the level found. Report results to nearest .05 ppm. SCOPE VCM sample is evaporated leaving any iron in a non-freezing . mixture of water and alcohol. The iron is reduced to valence two and reacted with 1,10 phenanthroline to a red product analytical to iron at 510 rap. These are known interferences. RPfffPPMCFrS Plastics Division Control Lab. procedure 112-70-3. Texas City C.L. Method 22-18-10, G.L. 4/22/54. iff 7/20/71 RSV 0015057 METHOD 602.289-A (WC) July 17, 1971 Page 4 of 4 IRON IN VCM CALIBRATION CURVE Wave Lengths 510 mu Cell Length: 20 mm Standard: Blank (with reagents) ppm Fe 0-0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Optical Density 0-0.05 0.05-0.09 0.090-0.112 0.112-0.150 0.150-0.19 0.19-0.23 0.23-0.27 0.27-0.31 0.31-0.34 0.34-0.40 RSV 0015058 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.331 (G.C.) July 17, 1971 Page 1 of 3 MATERIAL Product ethylene ANALYSIS REQUIRED Methanol SAMPLE 200 ml stainless steel flow thru bomb APPARATUS Gas chromatograph equipped as follows: 1. Hydrogen flame ionization detector which should have a sensitivity of approximately 1 coulomb per mole for a hydrocarbon. 2. Amplifier and recorder with sensitivity sufficient to yield a full scale response to 1 x 10-11 amps of ion current and a noise level equivalent to less than 1 x 10-13 aarps. 3. Gas sampling valve with a 5CC sample loop. 4. Temperature controller for operation at 80C. 5. Column consisting of 20 feet of l/8 inch O.D. aluminum tubing packed with 30-60 mesh red chromosorb coated with 2056 EAC-l-R- 296 polyester (available from Cambridge Industries Co., Inc., Cambridge, Mass.) Methylene chloride is the solvent used in coating the chromosorb with the polyester. REAGENTS 1. Ethylene - Pure grade from Phillips Petroleum Co. 2. Methanol - Reagent grade 3. Hydrogen - Electrolytic grade 4. Helium - Commercial 5. Air - Free of water, organic compounds and particulate matter. RSV 0015059 METHOD 602.331 July 17, 1971 Page 2 of 3 PROCEDURE 1. Install the column In the instrument and adjust oven temperature to 80C and helium carrier flow to 45 cc per minute. 2. Adjust the hydrogen and air flow to the detector for maximum signal-to-noise ratio. Vary hydrogen flow first then air. 3. Allow instrument to "line tut" at these conditions as indicated by a stable baseline on the recorder for five minutes or more using maxinum sensitivity on the amplifier. 4. Using the gas sample valve, introduce 5cc of sample into the instrument. 5. Record the chromatogram. Methanol is eluted in approximately 7 minutes. CALCULATIONS 1. Measure the area of the methanol peak. 2. Calculate percent methanol as follows: Peak area x attenuation x calibration factor * % MeOH CALIBRATION 1. Prepare synthetic mixtures of methanol ir. ethylene to cover concentration range cf interest. The importance of using clean bombs for preparation of synthetic mix tures cannot be over emphasized. 2. Analyze the synthetic mixtures according to the above procedure. 3. Calculate the calibration factor. SAFETY PRECAUTIONS Normal safety precautions on handling hydrocarbon gases should be observed. ANALYTICAL TIME Average time required for this analysis is 0.25 hours. RSV 0015060 t r METHOD 602.331 July 17, 1971 Page 3 of* 3 PRECISION OF ANALYSIS The precision of this method 1st 5 ppm in the range of 5 to 50 ppm methanol In ethylene. SCOPE This Is a gas chromatographic procedure for the determination of methanol in the concentration range of 1-500 ppm in ethylene. The minimum detection limit is approximately 5 ppm of methanol. C4's and up to ec's will not interfer with this analysis. Heating bomb above ambient temperature before injecting a sample into the chromatograph was found unnecessary. REFERENCES 1. Research Method TC - 1180 (GC) 2. Research Notebook HC No. 1, pp. 24-33. 7/20/71 RSV 0015061 MONSANTO COMPANY TEXAS CITY, TEXAS METHOD 602.343 (l\\C.) August 29, 1961 Page 1 of 3 MATERIAL Vinyl Chloride Monomer ANALYSIS REQUIRED Acidity as HC1 SAMPLE SIZE Glass Bomb APPARATUS 500 ml Iodine Flasks 5 ml Micro Burette .01 ml Graduations Mettler Balance REAGENTS 0.1# Thymol Blue in Methanol C.P. Methanol Ethylene Dichloride (Neutral) Methanolic Caustic (.003 N) Solvent Mixture Prepared from above. PROCEDURE 1. Add 100 ml solvent mixture to each of two 500 ml iodine flasks. To the ''blank" flask add 60 ml of neutral EDC. 2. Neutralize both flasks to an orange-yellow end point with .003 N MeOH-NaOH. Bring "sample" flask and "blank" flask to the same color. Check the color by looking down through the liquid from the top. Stopper flasks. 3. Place flasks in dry ice chest for 2-3 minutes. Remove and match colors again. Adjust, if necessary, with MeOH-NaOH to the same color again. RSV 0015062 METHOD 602.343 (V.'.C. August 29, 1961 Page 2 of 3 PROCEDtfRF. (Continued) 4. Attach bomb to 1/3'1 SS coil in cooling bath (-35C). place sample flask under outlet of tubing. Open valve on bomb and drain VCM into sample flask. Tubing should be under the surface of the liquid. When cample stops bubbling, close valve and remove bomb. Purge a small amount of nitrogen through the SS tubing. 5. Remove flask, swirl to mix, and titrate to end point of the blank by matching the colors. Note volume of MeOHNaOH used. NOTE: Obtain sample weight by weighing bomb on Mettler balance before and after entering sample into titration flask. CALCULATION ppm HC1 = V MeOH - NaOH x N MeOH-NaOH x 36,500 Sampl^' Weight PREPARATION OF REAGENTS Titration solvent: 920 ml neutral EDO, 30 ml 0.1# thymol blue and 50 ml CP. Methanol per liter of solution. Neutral EDC: Refer to Solutions Manual. .003 MeOH-NaOH: Refer to Solutions Manual. 0.1# Thymol Blue in Methanol: Refer to Solutions Manual. STANDARDIZATION AND CALIBRATION: Refer to Solutions Manual for standardization of .03 MeOHNaOH. This in turn is diluted 1:10 with methanol for .003 N MeOH-NaOH. SAFETY PRECAUTIONS When disposing of material in sample flask, be sure that all VCM has been evaporated from the solution before the EDC is put in solvent drain. ANALYTICAL TIME 0.3 Hours. RSV 0015063 METHOD 602.343 (V.'.C. ) August 29j i9kl Page 3 of 3 PRECISION AMD SIGNIFICANT FIGURES + 0.1 ijpjr. at 1 pp*R level. Report to the nearest 0.1 ppm. SC0PE This is a non-aqueous acid-base titration capable of detecting about 10 micrograms of HC1. REFEREI'CE Research Notebook #2271, pp. 1^87^6-53- /jw 7/29/71 RSV 0015064 MONSANTO COMPANY TEXAS Cl TV,. TLXAS MATERIAL Produce vinyl chloride and 22E11 ANALYSTS REQUIRED Determination of aldehydes SAMPLE SIZE Quart thermos bottle APPARATUS Beckman Model "3" Spectrophotometer 100 ml volumetric flask Coca-cola bottle and cap Bottle'opener Ice pick 250 ir.l Erlenmeyer flask 100 ml graduated cylinder 25 ml graduated cylinder 1 ml pipette Triple beam balance REAGENTS Alpha - methyl indole solution Ammonium hydroxide (SH OH*. !cp cone.) 4 Acetaldehyde {CH^CKO) DEPT. 60 METHOD 602.344 May 1-1, 1264 Page 1 of 5 RSV 0015065 METHOD 602. 344 May 14, 1964 Prigs 2 of 5 (WC) PROCEDURE Select a clean, dry Coca-cola bottle free from large ' scratches. Pipette 1.0 ml of concentrated NH^OH into the bottle and add 10 ml H^O. Pour 100 ml of vinyT chloride into a 100 ml graduate which harj been cooled in dry ice for at least 15 minutes. Transfer to the Coca-cola bottle and cap the bottle immediately. Shake the sealed bottle vigorously and place in the cabinet for one hour (CAUTION! Wear face shield while handling vinyl chloride). Puncture the cap with an ice pick and then remove cap. Allow the vinyl chloride to evaporate in the hood. When all of the vinyl chloride has evaporated, wash the contents of the bottle into a 100 ml volumetric flask with several portions of distilled water. The volume of distilled water shall not exceed 50 ml. Add 20 ml of OC- methylindole solution to the washings.- Shake to mix thoroughly and allow the solution to stand for 10 minutes. Dilute to 100 ml with distilled water and again shake thoroughly. Read the optical density of this solution on the Beckman "B" Spectrophotometer at 550 mu using 20 mm cells and distilled water as the blank. If the turbidity exceeds the range of the chart, repeat the analysis using a smaller volume of vinyl chloride. CALCULATIONS The results are read directly from the chart to the nearest part per million. Duplicate determinations should check within 2 ppm. See chart on last page of procedure. RSV 0015066 METHOD 602.344 (WC) May 14, 1964 Page 3 of 5 PREPARATION OF SOLUTIONS Prepare fresh solutions daily by adding 60 ml con centrated CP iici to 30 ml of distilled water in a 250 ml Erlenmeyer flask. Then dissolve in this 0.15 + 0.05 grams of alpha methyl indole. STANDARDIZATION AND/OR CALIBRATIONS Chill a 5 ml Mohr pipette graduated in 0.1 ml increments to a temperature of 0C by placing in an ice chest. Wrap pipette with a paper towel to avoid moisture contamination. After ten minutes, remove and pipette 5 ml of technical grade acetaldehyde. Introduce 1.25 ml of this chilled acetaldehyde into a 1000 ml chilled volumetric flask containing distilled water. Make up to volume with distilled water and shake thoroughly. The contents of this flask contains 1000 ppm acetaldehyde. Call this Solution A. 10 millileters 'of A diluted to 1 liter water * 10 ppm AcH 5 millileters of A diluted to 1 liter water = 5 ppm AcH 1 millileter of solution A diluted to 1 liter = 1 ppm AcH Intermediate parts are obtained by diluting various parts of A to 1 liter. These aliquot portions are then run in a similar manner to that of the sample and the various scale readings recorded. Duplicate determinations should be run for a check. These scale readings will relate to the concentration of the acetaldehyde present. SAFETY PRECAUTIONS When depressurizing the VCM in the Coca-cola bottle, be sure that the ice pick is removed slowly and the bottle is kept in a safety cage and wearer has on a face shield. RSV 0015067 MEVilOT) 602.344 (wc) May 14, 1964 Fage 4 of 5 ANALYTICAT- V'JME 0.2 hour PRECIS!OK OF ANALYSTS AND SIGNIFICANT FIGURES FOR REFORTINO Report to nearest 1-ppm; duplicate determinations should check each other I 1 ppm at 1 ppm level. SCOPE Alpha methyl indole reacts with aldehydes to form a turbidity. A measure (spectrophotometer) of turbidity determines the amount of aldehydes present. /jw 7/29/71 RSV 0015068 METHOD 602.344 May 14, 1964 Pago 5 of 5 (WC) ACETA.LDEUYPE TW SPECIFICATION VCM 20 mm Cells Becking HBM Spectrophotometer Optical Density 00.028 - 0.027 0.082 O.O83. - O.I36 0.137 - 0.190 0.191 0.246 - 0.245 0.299 0.300 - 0.354 0.355 - 0.409 0.410 0.464 - 0.463 0.518 0.519 - 0.572 ppm AcH 0 1 2 3 4 5 6 '7 8 9 10 RSV 0015069 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL Acrylamide Ferric Ammonium Sulfate Sodium Formaldehyde Sulfoxylate Tetrasodium Ethylene diamine Tetraacetate DEPT. 60 METHOD 602.431 May 23, 1971 Faqe 1 of 1 ANALYSIS REQUIRED Appearance of Solids SAMPLE SIZE 8-ounce bottle APPARATUS None REAGENTS None PROCEDURE 1. If the material consists of free flowing relatively stable non-hazardous particles, spread a small amount on a white card. Otherwise observe in the sample container. 2. Describe the color of the sample. 3. Describe the physical size, form, and uniformity of particles such as powder, crystals, flakes, briquettes, lumps, fused mass, etc., with respect to the specification requirement. 4. Note the presence of any discolored areas or particles and/or the presence of extraneous materials. SCOPE This method is intended to provide a general physical description of solid materials. : ff 7/20/71 RSV 0015070 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL DEPT. 60 METHOD 602.432 May 23, 1971 Page 1 of 1 Sodium Lauryl Sulfate Tetrahydrofuran ANALYSIS REQUIRED Appearance of Liquids SAMPLE SI2E 8-ounce bottle APPARATUS Source of strong oblique illumination shaded from the observer's eye, such as Turbidimeter, Clark, Catalog No. T11315, The Chemical Rubber Co., Cleveland, Ohio. REAGENTS None PROCEDURE 1. Rinse the outside of the sample container, a clear glass bottle, with methanol and water, wipe it with a towel and place it on a white card or opal glass background. 2. Describe the color of the sample. 3. Describe the clarity with respect to haze, sediment, globules or layers of immiscible liquids or other insolubles. 4. Swirl the sample, avoiding the introduction of air bubbles, and observe under the Clark Turbidimeter, describing any turbidity, opalescence, or sediment. 5. Describe the fluidity with respect to the specification re quirement . SCOPE This method is intended to provide general physical description of liquid materials when viewed under a constant set of conditions, and to define any visibly apparent contamination. sff 7/20/71 RSV 0015071 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL Acrylamide DEPT. 60 METHOD 602.413 May 23, 1971 Page 1 of 2 ANALYSIS REQUIRED Assay SAMPLE SIZE 8-ounce bottle APPARATUS 1. Erlenmeyer flask, 250 ml heavy wall, fitted with a 24/40 Standard Taper joint (Ace Glass Co., No. 2671). 2. Filling funnel, 50 ml cylindrical, open top with Standard Taper stop-cock and 24/40 Standard Taper joint on bottom (Kontes Glass CoJ, No. K-63125). In the top of the funnel insert a rubber stopper fitted with a short glass tube for connection to vacuum line. REAGENTS 1. 0.1 N KBr03 - KBr solution (2.79 g. potassium bromate and 10 g. of potassium bromide per liter). 2. 6 N H2S04 3. 20% KI solution 4. Std. 0.1 N Na2S203 5. 1% starch solution PROCEDURE Weigh accurately a sample containing 1.0 - 1.5 g. of acrylamide into a 500 ml volumetric flask, dilute to volume with water and mix. Pipet a 25.00 ml aliquot of this solution and 25.00 ml of bromate-bromide reagent into the 250 ml Erlenmeyer flask. Attach the filling funnel and rubber stopper, evacuate the flask, then close the stopcock and remove the stopper. Draw 5 ml of 6N sul furic acid into the flask while preserving the vacuum. Allow the solution to stand in the dark for twenty minutes and shake fre quently. Add 15 ml of potassium iodide solution, mix and then break the vacuum. Titrate the solution immediately with standard thiosulfate using starch indicator. Run a blank determination. RSV 0015072 METHOD 602.433 May 23, 1971 Page 2 of 2 CALCULATION % Acrylamide = (blank titer~5amole titer)(N ya^S^O-x (2.534; Weight of sample in aiiq-aGt SCOPE Acrylamide may be determined by bromination of the double bond. This method, which is used in the laboratories of the American Cyanamid Company, is applicable to solids and solutions. sff 7/20/71 RSV 0015073 MONSANTO COMPANY TEXAS CITY, TEXAS DEFT. 60 METHOD 602.434 May 23, 1971 Page 1 of 4 MATERIAL Sodium Formaldehyde Sulfoxylate ANALYSIS REQUIRED Ash SAMPLE SIZE 8-ounce bottle APPARATUS a. Porcelain wide form crucible, such as Coors No. 2, Catalog No. 7-955, Fisher Scientific Company. b. Platinum dish, 25 ml. American Platinum Works c. Burner, such as Catalog No. 3-902, Fisher Scientific Company. d. Nichrome Triangles, such as Catalog No. 15-260, Fisher Scien tific Company. e. Nichrome Triangles with Fused Silica Tubes, such as Catalog No. 15-280, Fisher Scientific Company. f. Desiccator, such as Catalog No. 8-631, Fisher Scientific Co. g. Desiccant, such as anhydrous 4-mesh calcium chloride. h. Furnace - muffle, such as Catalog No. 10-526, Fisher Scientific Co. REAGENTS Sulfuric Acid, T.S., Diluted - Cautiously add 57 ml of sulfuric acid (95-98%) to sufficient water to make 1000 ml. PROCEDURE NOTE: This procedure specifies a platinum crucible for general applicability. A porcelain crucible may be used if pre vious experience with the product being ashed indicates no attack on porcelain. RSV 0015074 Procedure (cont'd) METHOD 602.434 May 23, 1971 Page 2 of 4 1. Sand polish and mold the platinum crucible. 2. Heat the crucible on a silica sleeved Nichrome triangle for 5-10 minutes being careful net to allow the blue reducing flame of the burner to come in contact with the crucible. 3. Allow the crucible to pre-cool for 10 minutes on the silica covered triangle, place in a desiccator for 30 minutes if using platinum or 1 hour if using porcelain, and weigh accurately. 4. Add 2.00 0.01 "grams of sample and 10 ml of diluted sulfuric acid T.S. to the crucible. 5. Place the crucible on a porcelain top hot plate and heat gently until the sample is dry and thoroughly charred, then continue heating until the sample has been volatilized or nearly all the carbon has been oxidized. 6. Allow the crucible to cool and then carefully moisten the residue with 0.1 ml of H2S04 7. Heat as in Step 5 until the remainder of the sample and any excess sulfuric acid have been volatilized. 8. Finish the ignition in a muffle adjusted to 800 25C. 9. Pre-cool the crucible for 10 minutes on a silica covered tri angle, cool in a desiccator for 30 minutes if using platinum or 1 hour if using procelain, and weigh accurately. .10 Calculate: % Ash net weight of residue x 100 sample weight DISCUSSION To obtain constant weight of the porcelain crucible within a rea sonable time, it is imperative that it be pre-cooled on a porcelain or aluminum block for 10-15 minutes prior to placing in a desiccator and then further cooled in the desiccator for one hour. Eliminination of the pre-cooling step necessitates a three hour or more cooling cycle in the desiccator. One hour cooling periods without the pre-cooling period could incur errors of 5-10 milligrams, depending on the size and number of crucibles and the size of the desiccator. The initial combustion should be made with as low a temperature as possible. Only when the carbon has fully disappeared from t>e RSV 0015075 J Discussion (cont'd) METHOD 602.434 May 23, 1971 Page 3 of 4 sides of the crucible should it be placed in a muffle furnace. A further consideration to be kept in mind is that if the flame is allowed to envelop the crucible fully, the atmosphere within the crucible is not air but largely a mixture of nitrogen and the products of combustion, of which water vapor is an important one. The chief effect of the water vapor is to raise the temperature necessary for complete dehydration. This is the reason long ig nition periods are often required for the conversion of a metal salt to the oxide, whereas under proper conditions the conversion could be made in minutes. Once the carbon is completely removed from the wall of the crucible, it is only a matter of expedience as to whether the muffle or the Meker burner is used to burn the carbonaceous matter from the residue (Ref. 1). If the residue after ignition contains sodium or potassium car bonate, it may fuse and occlude carbon, making complete removal of the latter difficult. Increasing the sample weight only in creases the tendency toward false higher answer. Results will always be low in the presence of easily reducible oxides of volatile metals. Due to the fluffiness of some ash residues, extreme care must always be exercised to prevent loss by air currents. PRECISION The following criteria should be used for judging the acdeptability of results (95% confidence): a. Repeatability. Duplicate results by the same operator should be considered suspect if they differ by more than the following amount - 0.0 to 0.15 Ash, %j 0.003 Repeatability. b. Reproducibility. The results submitted by each of two labora tories should be considered suspect if the two results differ by more than the following amount - 0.0 to 0.15 Ash, %; 0.005 Reproducibility. SAFETY Handle hot crucibles with tongs. Operate in a fume hood, and behind a safety shied, if there is any possibility of the material having explosive tendencies. RSV 0015076 Safety (cont'd) METHOD 602.434 May 23, 1971 Page 4 of 4 Make sure the ground glass flange of the desiccator is greased to prevent sticking. REFERENCES 1. "Applied Inorganic Analysis", Hillebrand, Lundell, Bright, and Hoffman, John Wiley & Sons, London, 1953. 2. 1963 Book of ASTM Standards, part 17, page 195. 3. Food Chemicals Codex I. 4. USP XVIII. SCOPE This method is intended for the determination of Ash contents of less than 1.0% in pharmaceuticals, oils, etc. The scope is simi lar to that of the ASTM D-482-63 method for "Ash From Petroleum Products." The method does not necessarily give a true measure of the metallo-organic compounds or the inorganic compounds present because of possible losses by vaporization or reduction of the metal compounds present. : ff 7/20/71 BSV 0015077 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL Ammonium Persulfate DEPT. 60 METHOD 602.435 May 23, 1971 Page 1 of 1 ANALYSIS REQUIRED Assay SAMPLE SIZE 8-ounce bottle APPARATUS a. Analytical balance b. 250 cc glass stoppered flask c. Titrating burets d. Usual laboratory equipment REAGENTS a. Standard Acid Ferrous Sulfate solution (0.2 N) b. 0.1 N potassium permanganate PROCEDURE Add 0.5 gm of sample, accurately weighed, to 25.0 ml of Standard Acid Ferrous Sulfate solution (about 0.2 N) in a glass-stoppered flask. Stopper the flask, allow it to stand for 1 hour with frequent shaking and titrate the excess ferrous sulfate with C.l N potassium permanganate. Titrate 25.0 ml of the Standard Acid Ferrous Sulfate solution with 0.1 N potassium permanganate. From the volume of 0.1 N permanganate required, subtract the volume of 0.1 N permanganate required in the titration of the sample solu tion. Each ml of the difference, consumed by the sample, is equivalent to 0.01141 gm of (NH4) 2S28' :ff 7/20/71 RSV 0015078 - *'**?* MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL DEPT. 60 METHOD 602.436 May 23, 1971 Page 1 of 1 Ferric Ammonium Sulfate ANALYSIS REQUIRED Assay SAMPLE SIZE 8-ounce bottle APPARATUS a. Analytical balance b. 250 cc glass stoppered flask c. Titrating burets d. Usual laboratory equipment REAGENTS a. 0.1 N hydrochloric acid b. 0.1 N potassium iodide c. 0.1 N sodium thiosulfate d. Starch indicator PROCEDURE Dissolve about 1.5 gm of sample, accurately weighed, in 50 ml of water in a glass-stoppered flask. Add 3 ml of hydrochloric acid and 3 gm of potassium iodide and let stand for 30 minutes in the dark. Dilute with 100 ml of water and titrate the liberated iodine with 0.1 N sodium thiosulfate adding starch indicator solu tion toward the end of the titration. Correct for a blank. Each ml of 0.1 N sodium thiosulfate consumed is equivalent to 0.04822 gm of FeNH4(S04)2*12H20. :ff 7/20/71 RSV 0015079 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL DEPT. 60 METHOD 602.437 May 23, 1971 Page 1 of 1 Sodium Formaldehyde Sulfoxylate ANALYSIS REQUIRED Assay SAMPLE SIZE 8-ounce bottle APPARATUS a. Analytical balance b. 1000 ml glass flask; 250 ml glass flask c. Titrating buret d. Usual laboratory equipment REAGENTS a. 0.10 N iodine b. 10% formaldehyde solution c. Starch indicator PROCEDURE Weigh out 10 grams of SODIUM FORMALDEHYDE SULFOXYLATE, dissolve in 150 cc of warm water, add distilled water to make a total volume of 500 cc. Take a 4 cc aliquot in 100 cc distilled water and titrate with 10 N Iodine (adding first 5 cc of 10% Formaldehyde solution) and Starch Indicator. CALCULATIONS cc ,10N Iodine x .00385 x 100 Wt. of sample is 0.08 grams = % Sodium Formaldehyde Sulfoxylate : ff 7/20/71 RSV 0015080 MONSANTO COMPANY TEXAS CITY, TEXAS MATERIAL DEPT. 60 METHOD 602.438 May 23, 1971 Page 1 of 2 Sodium Lauryl Sulfate ANALYSIS REQUIRED Assay SAMPLE SIZE 8-ounce bottle APPARATUS 150 ml beaker 250 ml volumetric flask 25 ml pipet 500 ml separatory funnel Analytical balance REAGENTS p-toluidine hydrochloride solution, 6.8% 3-A Alcohol, Form #30 Carbon Tetrachloride (reagent grade) Meta-cresol purple indicator (0.1% solution) Phenol red indicator (0.1% solution) 0.1 N NaOH PROCEDURE Using an analytical balance, transfer 5.00 grams of SIPON WD to a 150 ml beaker. Dissolve in distilled water and transfer to a 250 ml volumetric flask (a small amount of 3-A Alcohol may be used to dissipate foam) and dilute to 250 ml mark. Mix well and withdraw a 25 ml aliquot portion (equivalent to 0.5 grams of sample). Transfer the aliquot portion to a 500 ml separatory funnel. Add 2 drops of phenol red indicator (red-alkaline, yellow-acid). If solution is alkaline, adjust to neutral with .IN HCl. If solution is acid, adjust to neutral with .IN NaOH. To neutral solution add 30 ml of 3-A Alcohol, 30 ml of 6.9% p-toluidine hydrochloride solution and 30 ml of carbon tetrachloride. Shake mixture for RSV 0015081 J METHOD 602.438 May 23, 1971 Page 2 of 2 Procedure (cont* d) three minutes (occasionally releasing gas from separatory funnel). Allow to stand and separate. Cut lower (carbon tetrachloride) layer into 250 ml wide-mouth Erlenmeyer flask, containing 50 ml of 3-A Alcohol and 3 cc H20 adjusted to the alkaline (purple) end-point of meta cresol purple. Add 30 ml carbon tetrachloride to contents of separatory funnel and repeat extraction. Allow to stand and separate and again cut lower layer into same receiving flask. Repeat extraction once more. These combined extractions in the alcohol medium contain all the organic sulfates and are titrated directly with standard 0.1N NaOH to determine the alkyl sulfate content. The end-point is taken as the first change in color from gray to purple that remains for 15 seconds. CALCULATION ml NaOH x N x 300 x 100 - % Alkyl Sulfate as sodium lauryl sulfate Wt. of sample in the aliquot x 1000 SCOPE This procedure employs the extraction of the organic sulfates by p-toluidine hydrochloride precipitation. sff 7/20/71 RSV 0015082 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.439 May 23, 1971 Page 1 of 2 MATERIAL Tetrasodium Ethylenediamine Tetraacetate ANALYSIS REQUIRED Chelation value SAMPLE SIZE 8 ounce bottle APPARATUS a. Analytical balance b. 250 ml Erlenmeyer flask c. Titrating burette e. Usual laboratory equipment REAGENTS a) Ammonium oxalate, saturated solution. Dissolve approximately 60 grams of ACS reagent grade (calciul- free) ammonium oxalate (NH4)2C2^4 H2O in a liter of water and allow to cool to room temperature. b) Calcium chloride, standard solution. Dissolve 0.5 molar of primary standard calcium car bonate (Mallincrodt No. 4071) in 300 ml of distilled water by slowly adding 86 ml of concentrated hydro chloric acid to completely dissolve the calcium carbonate. Heat to boiling to remove carbon dioxide and completely dissolve the sample. Cool to room temperature and dilute this solution to exactly one liter. One ml of this solution contains the equivalent of 50 mg of calcium carbonate. c) Ammonium hydroxide, 1:1 solution. Add one volume of concentrated ammonium hydroxide to one volume of distilled water. RSV 0015083 i >. >_ f- METHOD 602.439 May 23, 1971 Page 2 of 2 PROCEDURE Weigh, to the nearest milligram, a 10 gram sample of chelating agent into a clean 250 ml Erlenmeyer flask, and add 85 ml of distilled water and 5 ml of saturated ammonium oxalate solution. Titrate the sample to the first faint permanent turbidity with standard calcium chloride. The pH of the solution should be checked by using pH paper after the endpoint has been reached; if the pH is below 11, a dilute solution of ammonium hydroxide should be added to raise the pH above 11." After the pH has been adjusted, the titration should be completed. CALCULATION ml CaCl2 solution x 50 gms of sample mg CaC03 per gm of chelating agent SCOPE The total chelation value is determined by titrating with a solution of calcium salt in the presence of oxalate ion as an indicator at a pH of 11 or slightly higher. The pH is important because the chelating ability decreases when the pH of the solution drops below 11 and consequently low results are obtained. /jw 7/23/71 RSV 0015084 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT, 60 METHOD 602.440 May 23, 1971 Page 1 of 2 MATERIAL Ferric Ammonium Sulfate, Sodium Lauryl Sulfate ANALYSIS REQUIRED Chlorides SAMPLE SIZE 8 ounce bottle APPARATUS a) Usual laboratory apparatus b) Potentiometer sensitive to potential changes of 5 mv. or less, coupled to the system: Ag::Solution::2M MgS04:Hg2S04:Hg REAGENTS a) 107. H2S04 b) Methyl orange indicator c) 0.01 N AgN03 PROCEDURE 1. Dissolve 5 grams of sample, weighed on a prescription balance, in 40 ml of water in a 150 ml beaker. 2. Slowly neutralize to methyl orange with 107. HjSO^ and add 0.5 ml in excess. 3. Cool the solution to 0-5C in an ice bath and stir mechanically under the silver electrode system. NOTE: If a precipitate forms, as with some organic salts, add just sufficient acetone to redissolve. RSV 0015085 METHOD 602.440 May 23, 1971 Page 2 of 2 PROCEDURE (cont'd) 4. Titrate fairly rapidly with N/100 AgNO^ until the potential begins to decrease markedly with small incre ments of titrant. 5. Continue the titration in. 0.1 increments, recording the potential after each, then underscore the total volume of titrant at the point corresponding to the largest potential change per increment of titrant. 6. Calculate the chloride concent as the specific chloride designated in the specification for the product: 7. Specified chloride t^tre x Factor sample weight Table of Chloride Factors Specified Chloride Factor for N/100 AgNO^ Cl* CaCl2 HC1 MgCl2 MnCl2 NaCl NH4CI PRECISION AND ACCURACY 0.0355 0.0555 0.0365 0.0476 0.0629 0.0585 0.0535 Duplicate determinations should agree to within 0.027.. SAFETY No unusual hazards are involved in this operation. SCOPE This method is intended for the determination of 0.01 to 0.57. ionizable chloride in water soluble materials. It involves a potentiometric titration with silver nitrate solution. 7/23/71 RSV 0015086 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT, 60 METHOD 602.441 May 23, 1971 Page 1 of 2 MATERIAL Sodium Lauryl Sulfate ANALYSIS REQUIRED Cloud point Determination SAMPLE SIZE 8 ounce bottle APPARATUS a) ASTM cloud and pour point kerosene cooling baths adjusted to 30F, 0F and -30F with dry ice. b) Test jars, gaskets and ASTM Cloud and Pour Point thermometers. c) Usual laboratory equipment. REAGENTS None PROCEDURE 1. Bring the fluid to be tested to a temperature at least 25F above the specification cloud point in the bath adjusted to the next lower temperature. 2. If moisture is present, remove by filtration thru dry filter paper until the fluid is perfectly clear. The temperature at which the filtration is made must be at least 25F above the cloud point.3 3. Fill a test jar to a point slightly above the mark with a portion of the sample. RSV 0015087 METHOD 602.441 May 23, 1971 Page 2 of 2 PROCEDURE (cont'd) 4. Close the jar tightly wish a stopper carrying a cloud and pour point test thermometer in a vertical position in the center of the jar, with the bulb touching the bottom of the jar. 5. Adjust a gasket around the jar one inch from the bottom and place in the jacket of the bath adjusted to the first temperature below the temperature of the sample. 6. As the temperature falls at each reading that is a multiple of 2, remove the test jar from the jacket, quickly without disturbing the sample, observe against a good light for the appearance of a cloudy haze, and replace the jar in the bath within 3 seconds. 7. If the sample does not develop a cloud when it has cooled to within 20F of the bath temperature, place the jar in the next lower bath and continue observing at 2F intfe8 rvals. 8. Record as the cloud point the temperature at which the first distinct cloudiness or haze appears in the bottom of the test jar. SAFETY Kerosene is a flammable liquid. Avoid open flames or ex cessive heat. Take cognizance of any dermatological, lachrymatory, or corrosive properties of samples and avoid skin contact and inhalation of vapors. SCOPE This method is intended for the determination of the cloud point of fluids which are transparent in layers l-l/2tf in thickness. It has the same general scope as ASTM D97-57 as applied to the determination of cloud points in petroleum products. /jw 7/23/71 RSV 0015088 MONSANTO COMFANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.442 May 24, 1971 Page 1 of 5 MATERIAL Tetrahydrofuran Tetrasodium ethylenediamine tetraacetate ANALYSIS REQUIRED Color of Liquids, Melts, and Solutions (APHA) APPARATUS AND REAGENTS a) Marched short form Nessler tubes of 50 ml capacity and tall form Nessler tubes of 100 ml capacity. b) 0.05 M Periodic Acid - Dissolve 11.4 g. of HIO^ * 2^0 in water and dilute to 1000 ml. c) Color Standards - Prepare APHA 500 standard by dissolving 1.0 g of cobaltous chloride (C0CI2* 6H2O) and 1.245 g of potassium chloroplatinate (l^PtClg) in water, adding 100 ml of cone. HC1, and diluting to 1000 ml with water. NOTE: The absorbance of the 500 platinum-cobalt stock solution must fall within the limits given bfelow. The measurements shall be made in a cell having a 10 mm light path using a Beckman Model B Spectrophotometer at a sensitivity setting of one, or in another spec trophotometer having equivalent resolution and sen sitivity. Reagent water in a matched cell shall be used as the reference solution. Wavelength, mu Absorbance 430 455 480 510 0.110 to 0.120 0.130 to 0.145 0.105 to 0.120 0.055 to 0.065 RSV 0015089 METHOD 602.442 May 24, 1971 Page 2 of 5 APPARATUS AND REAGENTS (cont'd) From a burette add the amount of APHA 500 standard indicated in the following table to the respective tube, add 0.5 ml of 0.05 M periodic acid and dilute to the mark with double distilled water. If the marks on a series of tubes very in depth, a final adjustment of all standards to the depth of the shortest should be na de. All tubes should be kept covered when not in use and wrapped in black paper so that no Tight enters from the side. AMA No. s 6 7 8 9 10 11 12 13 14 IS 16 18 20 2S 30 35 40 45 50 60 70 80 90 100 125 150 175 200 250 300 350 400 450 Short (SO ml.) Tubes ------- SMFPT300----------- -- .. 00 1.0 ml. .. .. .1. 5 ml. -. 2.0 ml. 2.S ml. 3. 0 ml. 3. 5 ml. 4. 0 ml. 4.5 ml. 5. 0 ml. 6.0 ml. 7.0 ml. 8. 0 ml. 9.0 ml. 10.0 ml. 12. 5 ml. 15.0 ml. 17.5 ml. 20.0 ml. 25.0 ml. 30.0 ml. . 35.0 mL 40.0 ml. 45.0 mL Tall (100 ml.) Tubes ----- XKTT5B0---------- 1.0 ml. 1.2 ml. 1.4 ml. 1.6 ml. 1.8 ml. 2. 0 ml. 2.2 ml. 2.4 ml. 2.6 ml. 2.8 ml. 3.0 ml. 3.2 ml. 3.6 ml. 4.0 ml. S. 0 ml. 6.0 ml. 7.0 ml. 8.0 ml. 9.0 ml. 10.0 ml. 12.0 ml. 14.0 ml. 16.0 ml. 18. 0 ml. 20. 0 ml. RSV 0015090 ii METHOD 602.442 May 24, 1971 Page 3 of 5 PROCEDURE 1. Fill a (black paper-wrapped) Nessler Cube, usir.g a 50 ml low form cube for off-white fluids or a 100 ml Call form tube for wacer-white fluids, to the depth of the standards with a portion of the sample, melt, or specified solution. NOTE: If the sample has any visible turbidity, filter it. (Note this on the analysis ticket). 2. Compare with the APHA standards viewing vertically against a white glass plate. 3. Record the number of the APHA standard which most nearly matches the sample, making a note cf any ab normality in tint of clarity of the sample. In the event the color lies midway between two standards, report the darker of the two. SAFETY Take cognizance of any potential hazards in the material being tested, such as the temperature melts, corrosiveness, lachrymatory of dermatological properties, and exercise appropriate precautions. PRECISION Results should not differ from the mean by more than the following amounts: Reproducibility Platinum-Cobalt Repeatability Different Color______________ One Operator & Apparatus Operators & Apparatus Under No. 50 No's. 50 to 100 Over No. 100 2.5 5 10 5 10 15 RSV 0015091 > METHOD 602.442 May 24, 1971 Page 4 of 5 DISCUSSION The function of the periodic acid is to stabilize the colors of the standards. It will r.ot, however, protect against contamination. Hence, care must be exercised against splashing samples into the standards. In any event, the standards should be renewed monthly, unless obvious dis crepancies dictate more frequent renewal. The chart on page four shows some comparisons of color in tensities as designated in various systems. In the com parison of color intensities of the ASTM D-1500 and the NPA systems, the asterisk (*) indicates the colors are not matched but they are close approximations. See also, references 3, 4. SCOPE This method is intended for the estimation of the color of liquids in terms of platinum-cobalt (Hazer.) standards * established by the American Public Health Association (ref. It involves visual comparisons of the sanple with prepared standards in matched Nessler tubes. 1). REFERENCES 1. "Standards Methods for the Examination of Water, Sewage, and Industrial Wastes", American Public Health Associa tion, Inc., New York, 1955. 2. 1968 ASTM Standards, part 20, pages 555 and 817. 3. Federal Standard Stock Catalog, Section IV, Part 5, TT-P-14lb. Method 458.1. 4. Quality Assurance Register Directory/Handbook and Specifications Catalog, Hitchcock Publishing Company, Hitchcock Building, Wheator., Illinois 60187. /jw 7/26/71 RSV 0015092 COLOR OF LIQUIDS, MELTS, AND SOLUTIONS (APHA) METHOD 602.442 Page 5 of 5 COLOR IN TE N S ITY COMPARISONS II H IJ5 h r *f M- M . H*0tSTu- s Ol aa 5* g JC "as " ,,I = * s ;=_= s aa a, =r.,:,ss::.,.e,o.Nn. 8 : 8S: is ssssssa:aia: : s aN <imM > l e6 d dd d dddddd d d dd --` a : a : ;ogeS!sss!8!-::I 512i ?* i i SI ! I !n S!S' !SR 8,ssa as sss s ss d d d d d d 2 d 2 d 2 - I --* 2 ~ n nw tfce A" r w ChM NnMH i|>i > < !2 !!2** I.IT ;;* JP -- *s ***> ** do -- -- -- - - - n ' S j TM B n I i ^ V * * p.' " t""*J , ,i l*i .i <*l i Io*i t no i i tn*On inAO i <noIWn ! Im i 2222 2 j j j ; ; 2 " 2 M J '**' j * j f-n o_Hn* , g^"-2*3aRS^^St33^SS8S5SSgS 2 J j^""*** ssrssaas-sgs-sssa-SRasssxaaRSR-;-;;*!; RSV 0015093 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.443 May 31, 1971 Page 1 of 2 MATERIAL Te trahydro furan ANALYSIS REQUIRED Distilling range APPARATUS a. 100 ml Engler flask b. + 50C to +70C, grade AA, 76 mm immersion thermometer graduated in 0.1C c. Asbestos ring with 1 1/4 inch diameter d. 100 ml graduated cylinder e. 9/16" O.D. No. 20GA seamless brass tubing 2 feed long for condenser f. Bunsen burner, ring stand and steam bath g. Usually laboratory equipment h. Apparatus setup pictured in Figure 1 Flgura 1 1OILIH0 APPARATUS RSV 0015094 MONSANTO COMPANY METHOD 602.443 May 31, 1971 Page 2 of 2 PROCEDURE AND CALCULATION Prior co conducting the boiling range test, use Method 602.-46 to check the THF sample for THF-peroxide. If more than trace amounts of peroxide are present, add a few caustic pellets to the distillation flask to be used in the deter mination and proceed with the following test.* Measure a 100 ml sample of THF at approximately 20C, into a standard 100 ml Engler flask. Insert a +50C to +70C, grade AA, 716 mm immersion thermometer graduated in 0.1C. (Wm. Hiergesell 6-Sons Catalog No. 6536) into the neck of the Engler flask so that the top of the-mercury in the ex pansion bulb is level with the inside of the bottom of the flask vapor outlet tube. Support the flask by an asbestos ring or a "Trjansite"^ plate having a 1 1/4 inch diameter hole and assemble the distillation apparatus as shown in Figure 1. Place a 100 ml graduated cylinder at the outlet of the condenser tube with the tube extending at least one inch into, but not below the 100 ml mark of, the cylinder. Cover the top of the graduated cylinder closely with blotting paper cut to fit the condenser tube tightly. Heat the concents of the flask over an enclosed steam bath, taking care that the water in the steam bath is actively boiling before the flask is placed in position. Place a "Transite11 board guard on all sides around the legs of the steam bath except that facing away from the condenser assembly. Record as the initial boiling point the temperature at which the first drop of condensate falls from the end of the condenser tube. Adjust the receiving graduate so that the end of the condenser tube touches the side of the cylinder and continue distilling. Maintain the rate of distillation between 3 ml and 5 ml per minute and record the temperature at which 95 ml has been collected, halt the distillation. Record the barometric pressure and room temperature at the time of distillation and correct the recorded boiling range temp eratures to 760 mm of mercury according to the following formula temperature correction (C) "(760 - barometric reading reduced to 0C) x 0.041 * Based on ASTM D 1078-58 test method. RSV 0015095 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602. *44 May 31, 1971 Page 1 of 1 MATERIAL T e t rahydr ofurar. ANALYSIS REQUIRED Specific Gravity APPARATUS Westphal balance PROCEDURE Determine the specific gravity at 20C by means of a Westphal balance which has been standardized with distilled water at 4C. /jw 7/26/71 RSV 0015096 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.445 May 31, 1971 Page 1 of 1 MATERIAL Tetrahydrofuran ANALYSIS REQUIRED Moisture APPARATUS Usual laboratory- equipment including 100 ml titrating buret. REAGENTS Anhydrous methanol Karl Fisched reagent PROCEDURE AND CALCULATIONS Titrate 50 ml of anhydrous methanol to a permanent deep-red color with Karl Fischer reagent. Add a 10 ml sample of tetrahydrofuran and titrate immediately to the same endpoint with Karl Fischer reagent, using an "Aquameter" or the visual endpoint. Calculate percent moisture by use cf the following equation. X moisture -(ml reagent) (water equivalent) x 100 (specific gravity) x 10 /jv 7/26/71 RSV 0015097 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.446 May 31, 1971 Page 1 of 2 MATERIAL Tetrahydrofuran ANALYSIS REQUIRED Peroxide APPARATUS a. 2 x 250 ml Erlenmeyer flasks and stoppers b. 25 ml graduated cylinders c. Titrating buret and equipment REAGENTS a. 1:4 concentrated sulfuric acid to water b. 10% potassium iodide solution c. 0.02 N sodium thiosulfate PROCEDURE AND CALCULATION Unstabilized tetrahydrofuran upon exposure to air may slowly form THF hydroperoxide, also designated as THF-peroxide. A simple, accurate analysis for THF-peroxide may be made as follows: 1. Place 100 ml of distilled water in each of two Erlenmeyer flasks 2. To each flask add 25 ml of a 1:4 mixture of concentrated sulfuric acid and water, and then add 25 ml of a 10% potassium iodide solution. 3. Add a 25 ml sample of tetrahydrofuran to one flask, stopper both flasks, shake, and place in the dark for 15 - 20 minutes. 4. Titrate the contents of each flask with 0.02 N sodium thiosulfate until the solutions become colorless. RSV 0015098 METHOD 602.446 May 31 1971 Page 2 of 2 PROCEDURE AND CALCULATION 5. Calculate the THF-perjxi.de content of the THF sample by by use of the following formula: % THF peroxide - (ml this in sample - ml thio in blank) N of thio x 0.23 /jw 7/26/71 RSV 0015099 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.447 May 31, 1971 Page 1 of 3 MATERIAL Tetrahydrofuran ANALYSIS REQUIRED Carbonyl and hydroxyl canpounds APPARATUS a. Vapor fractometer equipped with one millivolt recorder b. 6 ft column filled with 157* carbowax 1500 on 80-100 meah chromosorb W 1 c. 60 ml serum bottle d. 0.05 ml Hamilton syringe fitted with Chaney adapter e. Usual laboratory equipment REAGENTS a. Helium b. Acetone c. Isopropyl alcohol d. n-propyl alcohol e. n-butyl alcohol PROCEDURE AND CALCULATIONS The amounts of acetone, laoproply alcohol, n-propyl alcohol, and n-butyl alcohol in tetrahydrofuran may be determined by gas chromatography, using a 6-ft column filled with 15Z `'Carbowax" 1500^ on 80-100 meah "Chromosorb" W. Apparatus suitable for this determination includes a vapor "Fractometer" (equipped with a 1-millivolt recorder)^ or an equivalent gas chromatograph. The column may be purchased as a complete unit (Perkin-Elmer type "K" column or equivalent) or pre pared in accordance with instructions outlined below. To prepare the column, dissolve 3.5 g of "Carbowax11 1500 in 75 ml of methylene chloride and mix wL th 20 g of 80-100 mesh "Chromosorb" W to make a slurry. Evaporate the methy lene chloride on a steam plate with occasional stirring to obtain the dried adsorbent. Fill a 6 ft (1/4U o.d.) RSV 0015100 METHOD 602.447 May 31, 1971 Page 2 of 3 PROCEDURE AND CALCULATIONS (cont'd) thin-walled tube of stainless steel with the dried adsorbent, tapping the tube continually while filling to insure uniform packing. Plug the ends of the tube with glass wool and insert into the "Fractaneter", bending the tube as required to fit. Prepare a standard sample by adding 50 ml of THF known to contain only minute quantities of other components to a tared serum bottle (60 ml) fitted with a rubber stopper. Into the THF standard, measure 0.01 ml acetone, 0.01 ml isopropyl alcohol, 0.01 ml n-propyl alcohol, and 0.02 ml n-butyl alcohol. Calculate the percentage by weight of each constituent added to the THF standard. Before operating the "Fractometer", adjust the detector to 8.0 volts and sensitivity 1, and allow the "Fractometer" to attain a temperature of 73C. Apply a helium gas pressure of 15 psi at a flowmeter reading of 5.5 (70 ml/min of helium), and inject 0.01 ml of the THF standard into the "Fractometer" by means of a Hamilton syringe (0.05 ml) fitted with a Chaney adapter. As the carrier gas passes through the "Fractometer", the components of the sample appear at the detector after various lengths of time according to their partition coefficients. The times of elution of the components in the sample are plotted automa tically against recorder response on the recorder chart (Figure 2). Deflections in recorder response are indicated on the chart as peaks characteristic of each component. flaw* 9 j, TYfICAi CMSOMATOG&APH >02 THF RSV 0015101 METHOD 602.447 May 31, 1971 Page 3 of 3 PROCEDURE AND CALCULATIONS (cont'd) Repeat the chromatographic procedure, injecting a 0.01 ml sample of the original THF into the "Fractometer". Measure the heights of the acetone, isopropyl alcohol, n-propyl alcohbl, and n-butyl alcohol peaks and compare with the THF standard. Calculate the percentage by weight of each component in the standard in accordance with the following equation: % added x peak height (std) % in std - peak height (std) - peak height (sample) Chromatograph the samples of THF to be analyzed under the conditions specified above, and measure the peak heights corresponding to each component. Calculate the percentage by weight of component in the unknown by means of the following equation: % (std) x peak height (sample) % in sample - peak height (std) / jw 7/26/71 RSV 0015102 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 METHOD 602.448 May 31, 1971 Page 1 of 6 MATERIAL Tetrasodium ethylene diemi"-*/ tetraacetate ANALYSIS REQUIRED Heavy metals (Pb) APPARATUS A. Matched 100 ml low fcrm Nessler tubes. B. pHydrion test papers, 3.0 t: 5.5 (Micro Essential Laboratory) or glass electrode pH indicator. REAGENTS A. 6% acetic acid B. Saturated hydrogen sulfide water C. Concentrated ammonium hydroxide D. 107. hydrochloric acid E. Redistilled acetone F. Lead stock solution (100 mg/1) - Dissolve exactly 0.1598 gram of lead nitrate in 100 ml of water containing 1 ml of cone, nitric acid and dilute to 1 liter in a volu metric flask. G. Standard lead solution (10 mg/1) - Accurately pipette 10.00 ml of the 100 mg/1 stock solution into a 100 ml volumetric flask and dilute to volume with water. Prepare fresh daily. J. 0.1% p-Nitropher.ol indicator solution DETERMINATION 1. Ascertain into which the following classifications the product being tested falls and treat as indicated: a. Soluble Products: Weigh 2.0 grams (see note on page 2) into a 100 ml Nessler tube and treat as directed in the table. RSV 0015103 METHOD 602.448 May 31. 1971 Page 2 g 6 DETERMINATION (cont'd) If the product under test is not listed but is soluble in water or acetone, dissolve in 25 ml of acetone or water; if acid or basic adjust to pH 3.5 with NH4OH of 107. HCl, or if neutral add 4 ml of 67. HOAc and dilute to 50 ml with the alternate solvent to obtain an approximate 50% aqueous-acetone solution. (Some products may tend to separate on dilution. This difficulty can sometimes be overcome by a judicious selection of acetone-water ratio, taking care to duplicate this ratio in preparation of the standard (Step 4). Alternately, the product may be treated as described below under b3 c, d or e. ) NOTE: With strong buffers such as the glycerophosphates, start with 1.0 gram of sample and 50 ml of water, omit acetone from both sample and standard (Step 4) and adjust to pH 3.5 by glass electrode. Product Dissolve In Add Dilute to 50 ml with Aspirin 25 ml acetone Aminoacetic Acid (Glycine) 25 ml water Amobarbital 25 ml acetone Benzoic Acid 25 ml acetone Caffeine 20 ml hot H2O Caffeine Citrate 25 ml water Calcium Carbonate 20 ml 107. HCl Calcium Chloride 20 ml water Calcium Cyclamate 25 ml water Calcium Saccharin 25 ml water Chloramphenicol 25 ml acetone Chlorothenyl- 25 ml water pyramine Citrate (Chlo- rothen Citrate) water water 4.0 ml 6% HOAc water water 4.0' ml 6% HOAc 0.5 ml NH4OH acetone water water acetone acetone NH4OH to pH 3.5 acetone 4.0 ml 67. HOAc acetone 107. HCl to pH 3.5 acetone 107. HCl to pH 3.5 4.0 ml 67. HOAc 1.0 ml 107. HCl acetone water acetone RSV 0015104 Product Dissolve In Maleic Anhydride Phenacetin Saccharin Insoluble 25 ml water 25 ml acetone 25 ml acetone Salicylamide Salicylic Acid 25 ml acetone 25 ml acetone Sodium Acetate 20 ml water Sodium Benzoate 25 ml water Sodium Carbonate 15 ml water Sodium Cyclamate 25 ml water Sodium Saccharin 25 ml water Sodium Salicylate 25 ml water Sodium Seco- barbital 25 ml water Sulfanilamide 25 ml acetone Sulfathiazole 25 ml acetone Sulfuric Acid 25 ml water Thenylpyramine Fumarate (methyl- pyrilene Fu marate) 25 ml water Thenylpyramine Hydrochloride (Methapyrilene HCl) 25 ml water Urea 25 ml water METHOD 602.448 May 31, 1971 Page 3 of 6 Add Dilute to 50 ml with NH-OH tj pH 3.5 4.5 ml 6% HOAc acet one water 0.8 ml NH4OH 4.0 ml 6% HOAc 1.0 ml NH4OH 4.25 ml 10% HCl 3.5 ml 10% HCl 10.0 ml 10% HCl 10% HCl to pH 3. 5 0.25 ml 10% HCl water water water acetone acetone acetone acetone acetone 1.0 ml 10% HCl acetone 2.5 10% HCl 4.0 ml 6% HOAc 4.0 ml 67, HOAc NH4OH to pH 3.5 acetone water water acetone 4.0 ml 6% HOAc acetone 4.0 ml 6% HOAc 4.0 ml 6% HOAc acetone acetone b. Insoluble Powders - (such as Acramer, Phtnalyl Sulfathiazole, Succinyl Sulfathiazole, Theobromine) Moisten 2.0 grams with 10 ml cf 10% HCl in a 100 ml beaker, hold on the steam bath for 5 minutes, cool to about 20C, let stand until the superr.atent liquid is clear, filter by vacuum and wash the residue with a small amount of water. To the filtrate add 1 drop of 0.1% p-nitrophenol, titrate to a faint yellow endpoint with NH,OH, add 4.0 ml of 6% HOAc and 25 ml of acetone, and dilute to 50 ml with water. RSV 0015105 _ V: ~>ro^ 7' METHOD 602.448 May 31: 1971 Page 4 of 6 c. Oils (such as Metrvl SalLcylate): Extract 2.0 grams with 10 ml of 10% HC1 in a 60 ml separatorv funnel and filter rhe aqueous layer through a small circle of wet filter paper. To the extract add 1 drop of 0.17* p-nitrophenol, titrate to a faint yellow endpoint with NHOH, add 4.0 ml of 6% HOAc and 25 ml of acetone^ and dilute to 50 ml with water. d. Colored Products (such as MHA or Kalcolor Acid): Moisten 2.0 grams with 4 ml sufluric acid in a 250 ml beaker. Hold the beaker with tongs and swirl until any initial reaction subsides. With constant swirling, heat to boiling over a moderate flame to carbonize. Remove the flame and add 30% hydrogen peroxide ((Superoxol) DROP-WISE from a 15 ml pipette, allowing the reaction to subside somewhat between drops. When there is noticeable diminution in the vigor of the reaction upon addition of hydrogen peroxide, heat cautiously to fumes, remove the heat and resume addition of hydrogen peroxide, cool the beaker in ice, add 10 ml of water and 1 drop 0.17. p^nitrophenol. Neutralize t.o a faint yellow endpoint with ammonium hydroxide, add 4 ml of 6% acetic acid and dilute to 50 ml with water. e. Volatile Products (such as Acetic Anhydride): Weigh 2.0 grams into a clean evaporating dish and take to dryness on the steam bath. Dissolve the residue in 4 ml of 67. acetic acid, add 25 ml acetone and dilute to 50 ml with water. 2. Add (an additional) 25 ml of acetone to the prepared solution.3 3. Verify the pH by a spot test on pHydrion paper, adjusting to 3.5 with NH^OH or 10% HC1 if necessary. RSV 0015106 _r METHOD 602.448 May 31, 1971 Page 5 of 6 DETERMINATION (coat'd) 4. Prepare a standard by pipetting exactly 1.00 ml of 10 mg/1 standard lead solution for each 5 ppm of the heavy metals specification, into a second Nessler tube containing 20 ml of water, 4 ml of 670 acetic acid, and the same quantity of acetone as is in the sample solu tion. (NOTE: if a 1.00 gram sample was taken, use 0.5 ml of standard lead solution for each 5 ppm of the heavy metals specification). 5. Dilute the standard and sample solutions to 75-80 ml with water. 6. Add 20 ml of saturated hydrogen sulfide water to the standard and to the sample solution, dilute both solutions to 100 ml with water, mix well and note the time. 7. Exactly 10 minutes after mixing the solutions compare longitudinally over a white, well lighted background.8 8. Record the sample as containing less, equal to, or more than the ppm of heavy metals represented by the com parison standard, depending on whether the sample solution is lighter, equivalent to, or darker than the standard solution. SAFETY Prepare hydrogen sulfide water in an efficient fume hood and avoid inhalation during use. Conduct wet digestions (Determination, step 1, part d) in an efficient fume hood and behind a safety shield. DISCUSSION This method is essentially equivalent to the USP limit test, with no provision for compensating for inherent sample color. It is not directly applicable to ferric and manganese glycerophosphates owing to complex precipitation and oxida tion of the sulfides. RSV 0015107 METHOD 602.448 May 31, 1971 Page 6 of 6 DISCUSSION (cont'd) Although some indication is retained for most metals of the copper and arsenic groups, the method is most sensitive to lead. Thus, for example, the absorptivity of an equivalent amount of copper sulfide is about half that for lead. Since the test is intended primarily for the detection of toxic metals, the inclusion of iron is avoided by conducting the test in. acetate solution below pH 5. Glassware used in this test should be rinsed with concen trated hydrochloric acid and distilled water before use. Even reagent grade acetone should be redistilled. Oxidizing agents, such as traces of chlorine in the diluent water used, will cause the precipitation of elemental sulfur and invalidate the results. REFERENCES 1. Stewarjt, F. N. and Strode, C. W. , J. Am. Pharm. Assoc. , Sci. Ed., 41, 242 (1952) 2. U.S.P. SVII. SCOPE This method is intended for the detection of apparent heavy metal contamination beyond a designated amount in fine chemicals. It involves formation of the sulfides at pH 3.5 and visual comparison with a standard. /jw 7/26/71 RSV 0015108 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT- 60 METHOD 602.449 May 31. 1971 Page 1 of 4 MATERIAL Acrylamide Sodium Lauryl Sulfate ANALYSIS REQUIRED Iron APPARATUS a. Usual laboratory apparatus and reagents including matched 50 ml short form Nessler tubes. b. Colorimeter such as the Bausch and Lomb Spectronic 20, with matched 1" test tube cells. REAGENTS a. 15% Ammonium Thiocyanate - Dissplve 75 g of ammonium thiocyanate A.R. in water and dilute to 500 ml'. b. 100 mg/1 Iron - Clean primary standard iron wire with emery paper and cleansing tissue, holding with tweezers. Accurately weigh 0.1000 g into a 1000 ml volumetric flask, add 10 ml HC1. heat o- a steam bath until dis solved, add 1.0 g. ammonium persulfate, and dilute to volume with distilled water at room temperature. c. 5 mg/1 Iron - Pipette 25 ml of 100 mg/1 iron into a 500 ml volumetric flask and dilute to volume with water. d. Acetone, A.R. Grade CALIBRATION 1. Pipette 09 5, 10, 20, 25, and 30 ml aliquots of 5 mg/1 iron solution into separate 50 ml glass stoppered cylin ders, add 2 ml .of cone. HC1 and dilute each solution to about 35 ml with distilled water. (After treatment and dilution t.z volume, these solutions will represent con centrations of 0, 0.5, 1.0, 1.5, 2.0, 2.5, and 3.0 mg/1.) RSV 0015109 t METHOD 602.449 May 31, 1971 Page 2 of 4 CALIBRATION (coat'd) 2. To each soluti.cn add 0.03 g of ammonium persulfate. 5.0 ml of 157 ammonium tniccyarate, and 5 ml of acerone; then dilute to volume with water and mix well. 3. Using 1" test tube cells in the Spectror.ic 2}0 colorimeter and a wavelength setting of 475. immediately measure the absorbance of the 1.5 mg/1 solution against the 0, 0.5, and 1.0 mg/1 solutions; measure the absorbances of the 2.0, 2.5, and 3.0 mg/1 solutions against the 1.5 mg/1 solution. 4. Plot the absorbances against concentrations on coordinate paper to obtain a "V" shaped curve with the apex at 1.5 mg/1 Divide (1.5 - respective solution concentration) by the absorbances of the first three solutions, divide (respec tive solution concentration - 1.5) by the absorbances of the last three solutions, and average the results as calibration constant K. NOTE: For JFQ Lab Spectronic 20 Colorimeter, Serial No. RD 8233, calibration of 12-2-55, K - 4.7. DETERMINATION A-1 - Spectrophotometricallv 1. Prepare 35 ml of clear, colorless, oxidized extract or solution of the sample or ash containing the equivalent of 2 ml of free cone. HC1 in a 50 ml glass stoppered cylinder, as directed for the product being tested. NOTE: The optimum sample size in grams is between 25 and 125 divided by the expected iron content, in ppm. 2. Add 0.5 g of ammonium persulfate, 5.0 ml of 157, ammonium thiocyanate, and 5 ml acetone; then dilute to 50 ml with water and mix well.3 3. Concurrently prepare a separate mixture of 15.0 ml of 5 mg/1 iron solution, 2 ml of cone. HC1, 0.05g of ammonium persulfate, 5.0 ml of 157* ammonium thiocyanate, and 5 ml acetone; then dilute to 50 ml with water and mix well. RSV 0015110 DETERMINATION METHOD 602.449 May 31, 1971 Page 3 of 4 4. Immediately measure the absorbance of the darker of the two solutions against the lighter solution in the Spectronic 20 colorimeter, using 1" test tube cells and a wavelength setting of 475. 5. Calculate: 50 (1.5 KA) ppm Fe - sample wt. in solution (% - ppm/-10,000) where: K * the calibration constant, which has a positive value when the sample solution is darkest and a negative value when the 1.5 mg standard solution is darkest. and A - the absorbance found A-2 - Visually 1. Prepare 35 ml of clear, colorless oxidized extract or solution of the sample or ash containing the equivalent of 2 ml of free cone. HC1 in a 50 ml Nessler tube, as directed for the product being tested. 2. Add 0.05 g of ammonium persulfate and 5.0 ml of 157ammonium thiocyanate, and 5 ml of acetone. 3. To a blank of 35 ml of water and 2 ml of cone. HC1 in a second Nessler tube add 0.05 g of ammonium persulfate, 5.0 ml of 157- ammonium thiocyanate and 5 ml of acetone. 4. Using a Mohr pipette, titrate the blank with 5 mg/1 iron solution, observing the tubes transversely over a white background, until the color of the blank matches that of the sample. RSV 0015111 METHOD 602.449 May 31, 1971 Page 4 of 4 DETERMINATION (cont'd) 5. Calculate: ml iron solution x 5 ppm Fe sample wt. in solution (% - ppm/10,000) DISCUSSION In condentrations between approximately 0.1 and 100 ppm of iron in various materials the precision and accuracy of this method may vary from 5 to 10% of the amount present in the absence of interferences. Fluoride, pyrophosphate and oxalate interfere, as may colored ions, metals such as mercury or 2inc which react with thiocyanate, or substances present in sufficient amount to exhibit color before the addition of thiocyanate. High salt concentration may inhibit color formation, and strong light may cause fading. The color is not stable for more than 30 minutes. SCOPE This method is intended for the determination of small amounts of iron in aqueous solutions of soluble colorless materials, ashes or extracts. It involves formation of the ferric thiocyanate complex and colorimateic estimation of the concentration. SAFETY With proper regard to observance of handling instructions on bottles of ammonium persulfate, no unusual hazards are in volved in this operation. REFERENCE Snell and Snell, "Colorimetric Methods of Analysis", Vol. II, D. Van Nostrand Company, Inc., New York, 1954. /jw 7/26/71 RSV 0015112 MONSANTO COMPANY TEXAS CITY, TEXAS DEPT. 60 I'lETHOD 602.626 April 20, 1002 Pa^e 1 of 7 r.. MATTAIaL Vinyl Cnior-i'it (VC IT) ANALYSE H^avy-enu Iinpuritlec: MV A Ethyl Chloride 2-CPY Vinylidene Chloride (1, 1-DCY) t-1,2-DCY CB SAMPLE Liquid Sample in VCM Bomb APPARATUS .* 2 P. E. Model 15^-C Vapor Fractorneter equipped with gas inlet valve, or equivalent, valved for multi-column operation (See attached drawing.) Hydrogen Flame Ionization Detector - capable of detecting 2 x 10"1 moles of chlorinated compounds. Meeco Vaporizing Valve, Type IS, or equivalent, for flashing liquid VCM into gas sample loop of chromatograph. Flow-meter for determining rate of purge on sample loop. Recorder - L. & N. Speedomax Type G, or equivalent, with 1 second pen and 5 mv full-scale deflection. Recorder should be modified to switch to either the thermistor detector or the flame detector. RSV 0015113 r* ' - 1^102602.626 (C-.C. ) April 26, 1262 Pago 2 of 7 REAGENTS AND SUrFLIES Aluminum Tubing - 3/1C inch C.D. Helium - 2 regulated supplies. Chromosorb - red, 30/60 mesh. Narcoil 40 - dinor.yl phth&lats fi'om No.clonal Research Corp. Hydrogen - electrolytic grade. Air - well-filtered, clean supply. * Ethyl chloride - commercial grade. 2-Chloropropene - Columbia Organic Chemical Co., purified by gas chromatography. 2-Chloro-l,3-butadiene - Monomer-Polymer, Inc., purified by gas chromatography. 1,1-Dichloroethylene - Monomer-Folymer, Inc., purified by gas chromatography. Vinylacetylene - E. I. DuPont Co., purified by gas chromatography. Vinyl. Chloride - Free of, or very low concentration of, impurities. Acetone - for column packing preparation. PROCEDURE A. Column Preparation 1. Mix 15 grams of Narcoil 40 with approximately 100 ml of acetone. 2. Pour mixture over 85 grams of 30/60 mesh chromosorb and add more acetone if necessary to make a slurry. 3* Mix continuously while evaporating the acetone. If available, use rotary-film evaporator with baffled flask for mixing. Apply heat from hot air gun and vacuum to flask to aid in evaporation. RSV 0015114 602.626 (o.C. ; April 26. 1$62 Pace 3 of 7 FROCTDURE (cor.t'd) fins ana length of fraction, :c ! i. v.` joir.iwd , x t.-'i.-creen to remove ;i; o-'.. I u-_t length find one 35-foot 16- Anti- with the 30/60 me oh 5. Install tiio cchjr,!i*H in the instrument as shown on the attached drawing. 6. Adjust the"two helium pressures and restrictob valve to give the follc-wing flcv-s: a. Column I: 75 ml/minute. b. Column II (with restrictor in flow path): 85 ml/min c. Columns I & II (in backflush position): 85 ml/min. 7. Adjust temperature to 50 C. and allow instrument and columns to reach equilibrium. 8. Light the hydrogen burner and adjust the hydrogen and air flows so as to yield maximum signal-to-noise ratio when MVA passes through it.' 9. Turn on amplifier and recorder and set for maximum sensitivity. The instrument should show no drift for at least five minutes before it is ready for use. B. Analysis 1. Purge the 3 cc sample loop for at least one minute with sample flashed through the Meco Vaporizing Valve, then inject the sample into, the flowing carrier stream with the columns in Position A and the recorder turned to the thermal conductivity detector. The attenuator switch of the detector should be set on an attenuation of 2. The valve between the thermal detector and the flame detector should be in the v:nt position to prevent VCM from going to the flame detector.2 2. Allow the sample le flow in Column I as shown in Position A for approximately three minutes (valve should be switched when recorder pen reaches 50# of full scale coming down on VCM peak). This allows the components lighter than VCM and most of the VCM to be vented from Column I. RSV 0015115 ME??:'*'.' 602.626 (0. C.) Apr.ll 26, 1902 Page 4 of 7 FROCraXJRE (r. or.r,' c ) 3. Ju.rt br:fyyi\ eluted from Column I, switch the vaiv-; 13. Th.ir> allows everything behind the 10:! uti.k to bo bacl:flushed onto Column II v/liere they i-i-e" separated end then flow to the detector. Sn.-.-.ltd.};/- ! bachf luf'hj r.g r.nd prior to the back- flushed VCh being eluted from Column II, switch the recorder to the flame detector and the valve between the thermal detector and the flame detector to the position r,uch that the flov.' is through the flame detector, b, Record all peaks eluted from Column II. A typical chromatogram is attached. CALCULATIONS The concentration of each component is calculated as follows: 1. Measure the peak height and width at one-half the peak height using a scale of 50 divisions to 1 inch. 2. Calculate the area of each peak according to the following equation: area = peak height x peak width at one-half peak height x attenuation 3. Calculate the concentration of each component as follows: Concentration{/p^pm;>. = oeak area x factor PREPARATION OF REAGENT SOLUTIONS None necessary. CALIBRATION 1. Prepare synthetics of KVA, ethyl chloride, 2-CPY, 1,1-DCY. trans-1,2-DCY, and CB in VCM to cover the concentration range of lntrest. At least two synthetics should be pre pared in each concentration range. Synthetics should be prepared in clean, stainless steel borab3 of any convenient size. The pressure should be sufficient to permit extended use of the mixtures. The blending system used must be completely free of leaks arid all kinds of foreign materials. RSV 0015116 *) s C 1. (, X <. w u A UU r\ uu C._Z3 ?n l Z*3 U\z i < 0 53 l > > .1 V < Ct J .1, I.J Ol . ls> -.i ^? ii c> i <: O O -s P <> Col_ S l'i ^ t.'r 602.626 April 26, Vj.A Pace: 6 o." : ; RSV 0015118 VZiC'j 6n2.626 ( :.C. ) /.prxl 26, IG`~2 Pace 7 Q-r' 7 RSV 0015119 MONSANTO COMPANY TEXAS CITY, TEXAS ;_>_- f DEPT. 60 METHOD 602.628 (G.C.} June 18, 1902 Pace 1 of 7 MATERIAL Vinyl Chloride (VCM). ANALYSIS Light-end Impurities: ^1 _ 4 Hydrocarbons Methyl Chloride SAMPLE Liquid sample In VCM bomb. APPARATUS Gas chromatograph equipped with valve(s) for multi-column operation and two regulated helium supplies. (See Note) Hydrogen flame ionization detector, Barber-Colman Model A-^504 or equivalent; sensitivity should be approximately one coulomb per mole. Amplifier and Recorder: Over-all sensitivity should be suffi cient to yield full-scale deflection for 1 x 10"^ amp with a noise level of less than 1 x 10 "^3 amp. Barber-Colman Electrometer for above flame detector is recommended. Integrator: Perkin-Elmer Printing Integrator, or equivalent. Tubing: 3/l6" O.D. Aluminum. Pressure Regulators. Two for helium, one for hydrogen, and one for air. Meeco Vaporizing Vnlve, Type IS, or equivalent, for flashing liquid VCM into gr.c sample loop of chromatograph. REAGENTS N Helium - Two regulated supplies. Chromosorb - red, 30/60 mesh. Trioctyl Phosphate: Union Carbide Chemical Company. RSV 0015120 METHOD 602.628 (G.C.) June 13, 1\)02 Page 2 of 7 REAGENTS (cont'd) Tributyl Phosphate; Fisher Scientific. Ci - Cii Hydrocarbons: Phillips Research Grade. Methyl Chloride: The Matheson Company. Vinyl Chloride Monomer: Free of, or very low concentration of, impurities. Hydrogen: Electrolytic Grade. Air: Purified source, such as cylinder breathing air. Acetone: For column packing preparation. PROCEDURE A. Column and Instrument Preparation 1. Prepare two columns as follows: a. Column I: 20 feet of 155$ w/w Trioctyl Phosphate on 30/60 mesh red chromosorb packed in 3/16" O.D. tubing. b. Column II: ^5 feet of 15# w/w Tributyl Phosphate on 30/60 mesh red chromosorb packed in 3/16" O.D. tubing. 2. Install the columns in the gas chromatograph as shown in Position A and adjust the helium pressure on Column I to give a flow of 100 cc/minute. When the valve is switched to Position B, the flow through Columns I and II should be 100 cc/minute. The columns are operated at room temperature. 3. Light the hydrogen burner and adjust the hydrogen and air flows so as to yield maximum signal-to-nolse ratio when a C3 or C4 hydrocarbon passes through it. 4. Turn on amplifier and recorder and set at maximum sensitivity. The instrument should show no drift for at least five minutes before it Is ready for use. 5. Prepare the integrator for use. RSV 0015121 r^TKOP 602.628 (U. C. ) June lS, 1962 Pago 3 of 7 PROCEDURE (cont'd) b. Analysis The analysis of light-ends may be made using the following procedure: 1. Line-out instrument in Position B, then switch to . Position A for entering sample. 2. Purge the 5 cc sample loop for at least one minute with sample flashed through the Meeco Vaporizing Valve, then inject the sample into the flowing carrier stream with the columns in Position A. 3. Fifteen (15) seconds after entering the sample, switch the valve to diagram Position B. .This allows the entire sample to be backflushed onto Column II where the components are separated and then flow to the detector. Using the integrator, record areas for all peaks eluted ahead of VCM. 4. When VCM begins to be eluted, switch the valve to diagram Position A. This allows the VCM to be ventfed Instead of passing through the detector. CALCULATIONS The concentration of each light-end component is calculated as follows: ppm - attenuation x peak area x factor PREPARATION OF REAGENT SOLUTIONS None necessary. CALIBRATION 1. Prepare synthetics of the light-end impurities, hydro carbons and methyl chloride, in VCM to cover the concen tration range of interest. At least two synthetics should be prepared. Synthetics should be prepared in clean stainless steel bombs of any convenient size. The^ * pressure should be sufficient to permit extended use of the mixtures. The blending system must be clean and completely free of leaks. RSV 0015122 METHOD 602.628 (G. C\ ) June l3, 1962 Page ^ of 7 CALIBRAVION (coni'*d) 2. Ansl.y:vf synthetic mixtures as described under the Procedure for Analysis. 3. Calculate factors for each of the light-end impurities according to the following equation: factor = concentration of component in synthetic integrated area x attenuation SAFETY PRECITATIONS VCM is a toxic, volatile, and highly flammable material and should be treated as such. Sample used to purge sample loop should be vented outside of building. ANALYTICAL TIME The average analytical time for this analysis should be 0.5 hour. PRECISION OF ANALYSIS AND SIGNIFICANT FIGURES FOR REPORTING RESULTS 9556 confidence' limits using this method is 4. 10# of the amount present. Report results to nearest 0.1 ppm. SCOPE This method is designed for light-end Impurities in VCM; however, it may be used for the analysis of light-end impurities in volatile pure grade hydrocarbons as long as the impurities are hydrocarbons in the C^ - range. REFERENCE Monsanto Research Notebook - No. 2330, pp. 15^660-15^665. NOTE: Valving recommended for this procedure is as follows: a. Backflushlng and column switching may be done with a Wall 8-Port Valve purchased from Tycam Engineering and Manufacturing Co., Inc., Houston, Texas. A drawing (may be a rough sketch) should be furnished to indicate number and location of channels in teflon slide. RSV 0015123 r-r^noD 602.628 (g.c. ) Juno 15, .1:. :<2 race 5 o 7 KPT(cont'd) b. A double- t-Port Circle Seal Valve? is&y be? used for the control of air to the air actuator of the Wall Valve as well as M-zitching the flow of the second helium supply when backflushinc. (See attached drawing.) /jw 7/29/71 RSV 0015124 ;____ - <2 <r* ^* v- ^ !: O *> i 5; 8 3 11 -sM i-.:c* t u -a ^ $ S g * S l 4 g j j tl s METHOD 602.628 Juu;': lS , J Z>`ti Psye 6 of 7 (G.C.) K1f c; :r C (j l . > o A4* r <u Po* itioa; f ,. RSV 0015125 {'>^;.?:;h:;: r^te'^! !ir:/r t^;;:: ^r'-v v'-^i-;1' : i`*'-^'': i^:^i:::7 ::: ; ,! i fti .'I:! iLp ILN rFf.-s1!^' i:.r^ !- ? T- i f`*-r"-'- -*1 ' fSi.' fi'l : .f''^L:-:r.ii ':f *f, i"_ ;*;[[};.'' .' J i . I ! NiiliU.: < i . ? ' * ^ ^ i > * r. . _ri _ . _ ,, > 602.628 Page 7 of 7 n-i ,,n RSV 0015126 !l!iaii MOi-SAMTG COMPAQ/ TEXAS CITY, TEXAS DYP'j . 60 lirTiTiOD 602.639 Kay 23, 13C4 Pac,o 1 cl 3 (vv) MATERIAL Product vinyl chloride monomer ANALYSIS REQUIRED Phenol SAMPLE SIZE Quart thermos jug APPARATUS 250 ml Erlenmeyer flask 50 ml beaker 2 ml pipette 100 ml graduate Beckman Model "B" Spectrophotometer 50 mm absorption cells (matched pair) REAGENTS Millons reagent - Prepare in well ventilated hood. PROCEDURE Evaporate 100 mis of sample in a 250 ml Erlenmeyer flask. When sample is completely evaporated, add 25 ml distilled HjO. Pipette 2 ml of Millon3 Reagent into flask. Boil for 1 minute on hot plate. Prepare a blank in the same manner, omit the sample. When solution has cooled, filter end read sample against blank on Beckman Model "B". Use 59 mm cells sensitivity of 3, and wavelength of 440 mu. RSV 0015127 METHOD 602.639 (WC) May 28, 1964 Page 2 of 3 CALCULATIONS Multiply O.D. by 10 to obtain ppm phenol. Report to nearest 0.1 ppm. Note: Use of sensitivity of 3 is not normal for our procedures. Use setting of 3 to adjust instrument on blank. This will allow the use of much smaller slit and will give some improvement in reproducibility of results. PREPARATION OF REAGENT SOLUTIONS To 100 grams of fuming nitric acid, add 100 grams of mercury. Allow sufficient time for mercury to react and go completly in solution. Add 20 mis of distilled H^O while stirring mixture. Place in a glass stoppered container. STANDARDIZATION AND/OR CALIBRATIONS See Solutions Manual. SAFETY PRECAUTIONS Handle mercury with care, avoid breathing vapors and dust spilled mercury with sulfur. Mercury reacts vigorously with nitric acid liberating large quantities of toxic NO^. Perform the preparation of this reagent in the hood with good ventilation. ANALYTICAL TIME .2 hour RSV 0015128 KUTWOD 602.639 (l.'C) I-jay 28, 1964 Psyt: 3 Of 3 PRECISION AMD SIGPTr.W.NT FT.C;U~~.3 95"o confidence limit - 1 ppu r. t 5 op,.; level. Report to nearest 1 ppm level. SCOPE Mercuric nitrate reacts v/ith the phenol in the sample to produce a color cample::. /jw 7/29/71 RSV 0015129 MONSANTO CHEMICAL COMPANY ORGANIC DIVISION TEXAS CITY, TEXAS DEPT. 33 , 60 METHOD 602.657 :W.C. February 4, 1964 Page 1 of 4 MATERIAL Caustic receipts ANALYSIS REQUIRED Iron SAMPLE 1 pint APPARATUS Beckman "B" spectrophotometer 50 mm matched cells 5 ml pipettes 100 ml volumetric flasks Analytical balances Fhydrion paper 4.0-6.0 range Small weighing bottle REAGENTS AND SOLUTIONS 1. 0.15% 1, 10 - phenanthroline (aqueous) 2. 10% hydroxylamine hydrogenchloride (aqueous * 3. Iron standard lOO^gm/ml (aqueous) RSV 0015130 METHOD 602.657 (W.C.) February 4, 1964 Page 2 of 4 4. A. R. grade ammonium hydroxide 5. 5N NaOH 6. .5N HC1 7. 1-1 HC1 solution (iron free) PROCEDURE 1. Fill a small weighing bottle with sample and weigh. 2. Place 2 gm of sample (40-50 drops) in a 100 ml beaker and dilute with 10-15 ml of water. Reweigh weighing bottle to obtain sample weight. 3. Add 10 ml of 1-1 HC1 to the beaker and boil down until approximately 5 ml remains. 4. Pipette 5 ml of 10% NHjOH . HC1 and 5 ml of .15% 0-phenanthroline to the beaker. Then pipette 4 ml of concentrated NK4.OH into the mixture. 5. Adjust the pH to 6-7 using phydrion paper with .5N HCl or .5N NaOH.6 7 6. Transfer contents of the beaker to a 100 ml volumetric, rinsing the beaker several times to insure removal of all the son pie. Adjust the volume with distilled water and mix. 7. Prepare a reagent blank. 6. Wait 20 minutes and then determine the absorbance of the sample at 510 wavelength in a 50 mm cells against a reagent blank. Obtain net absorbance. CALCULATIONS PPM Fe - abs. X 526 Weight of sample X 5 The 5 in the calculation denotes the cell length in CM. RSV 0015131 METHOD 602.657 ^W.C-' February 4, 1964 Page 3 of 4 PREPARATION OF REAGENTS 1. 0.15% 1, 10 phenanthroline - dissolve ,75-^grn of reagent grade material in 5 ml of glacial acetic acid. Dilute to 500 ml with distilled water. 2. 10% hydroxylamine HC1 - dissolve 50 -^gms of AR grade material in 500 ml of distilled water. 3. Iron standard 100 gra/ml - weigh 1000 gms of standard iron wire Dissolve in 10 ml HC1, dilute to 1 liter- 4. Iron standard 20 -"^gm/ml - dilute 20 ml of the standard 100-^gm/ml to 100 ml iron free distilled water. 5 Iron standard 5-^gm/ml - dilute 5 ml of the 100 -"^gm/ml standard to 100 ml with iron free distilled water. STANDARDIZATION AMD/OR C*T.TttPATTOMS Pipette 5, 10, 15, and 20 ml of the 5^<gm/ml standard to each, of 4-100 ml volumetric flasks. These will contain 25, 50, 75 and 100 of iron. Similarly pipette 10, 15, 20 and 25 ml of the 20 ^^gm/ml standard to each of 4-100 volumetric flasks. These will continue 200, 300, 400 and 500 -^gm of Fe.' Prepare a reagent blank. Analyze following the method in the procedure. Plot the absorbances found against the corresponding -^gm Fe. Draw in the best straight line through the points obtained. Re check any points that are over 10% from the line value. From this line, find the->*gm of Fe corresponding to unit absor bance. The factor 526 -**gm Fe/unit absorbance was determined by reading the absorbance at 500 .^gm from the curve and dividing 500 by the unit absorbance at this point (.95 abi.) PRECISION AND SIGNIFICANT FIGURES 95% confidence limits are - 0.1 PPM at a level of 1.05 PPM. Re port results to two significant figures. RSV 0015132 Ji METHOD 602.657 (WC) February 1964 Page 4 of 4 ANALYTICAL TIME 0.5 hours SAFETY Use normal precautions in handling laboratory chemicals, glassware and electrical equipment. Strong caustic can cause severe burns if spilled on the skin. If such a spill does occur, wash with large amounts of water and report to first aid. SCOPE Iron is reduced to the divalent state with hydroxylamine at a pH 4 to 7. Fe(II) forms a red complex with 1.10 orthophenthroline. -This red color is analytical W.R.T. iron. REFERENCES J.F.Q. General Method 70-F /jw 7/26/71 rSV 0015133 MONSANTO CHEMICAL COMPANY ORGANIC DIVISION TEXAS CITY, TEXAS DEPT. 33,60 METHOD 602.658 February 4, 1964 Page 1 of 3 MATERIAL Caustic Receipts ANALYSIS REQUIRED Sodium hydroxide and sodium carbonate SAMPLE 1 pint bottle APPARATUS 50 ml acid burette Small weighing bottle with dropper attached 250 ml Erlenmeyer flaBk Analytical balance REAGENTS 0.5.N standard HC1 Distilled Water Phenolphthalein Indicator Methyl Orange Indicator PROCEDURE 1. Fill a small weighing bottle with the sample and weigh. This sample bottle can be used for all subsequent analyses of the caustic.2 2. Place approximately 50 ml of distilled water in a 250 ml Erlenmeyer flask and add 2 gms of sample from the weighing bottle (approx. 40-50 drops). Reweigh to obtain the weight of sample. RSV 0015134 METHOD 602.658 February 4, 1964 Page 2 of 3 3. Add 2-3 drops of phenolphthalein Indicator and titrate with 0.5 N HC1 until the solution is Just colorless. Record this volume of HC1 as V^. 4. Refill HC1 burette to zero. Add 2-3 drops of methyl orange indicator to the titration flask and titrate with 0,5 HC1 until the solution is red orange. Record this volume of HC1 as V2. CALCULATIONS (V1 - V2) (IW 4- Weight of Sample NaOH (2y2) (NHC1) 5.3 Weight of Sample % NagCO^ PREPARATION OF REAGENTS Prepare indicator solutions and normal acid solution outlined in Reagent Manual. STANDARDIZATION AND/OR CALIBRATIONS Standardize HC1 solution according to Reagent Manual. SAFETY Use care in handling strong caustic solutions, as caustic can cause severe burns if spilled on the skin. If a spill should occur, flush the area with large amounts of water and report to first aid. Use normal precautions with chemicals, glassware, and electrical equipment. ANALYTICAL TIME 0.5 hours RSV 0015135 METHOD 602.658 February 4, 1964 Page 3 of 3 PRECISION OF ANALYSIS AND SIGNIFICANT FIGURES No precision has been determines, but duplicate analysis should agree within 0.5#. SCOPE In titrating to the phenolphthalein end point, the following two reactions occur: NaOH + HC1-------* NaCl + H^O N^CQ3+ HCl----- >NaHC03 + NaCl The subsequent titration to the methyl orange end point completes the.titration of the NaHCO- by the following reaction. ^ Na HCO^ + HCl------ NaCl + COg + H2O REFERENCE Method 22-10-1,' Revised 3/17/53 GK/mlw RSV 0015136 MONSANTO CHEMICAL COMPANY ORGANIC DIVISION TEXAS CITY, TEXAS DEPT. 33 ,60 METHOD 602.659 February 4, 1964 Page 1 of 2 MATERIAL Caustic Receipts ANALYSIS Chlorides SAMPLE 1 pint APPARATUS Small weighing bottles 250 ml beaker 50 ml burette pH meter Magnetic stirrer with stirrer bar Silver electrode Hg-HgSO^ - KgSO^ electrode REAGENTS Concentrated nitric acid 0.1.N silver nitrate solution PROCEDURE 1. Weigh 2 gmB of sample (40-50 drops) and place in a 250 ml beaker. Add 50 ml of distilled water and 5 ml of concentrated nitric acid. 2. Place on magnetic stirrer and immerse the electrodes in the solution. 3. While solution is being agitated, titrate with 0.1 AgNO^ to the first break, which will be about 100 MV. RSV 0015137 ../ > 1 t METHOD 602.659 February 4, 1964 Page 2 of 2 CALCULATIONS (Volume of AgNO^) (Normality) (3.55) % Cl" Weight of Sample PREPARATION OF REAGENTS Prepare 0.1 AgNOj according to Reagents Manual STANDARD AND/OR CALIBRATIONS Standard AgNO^ by procedure In Reagents Manual SAFETY Handle all chemicals, glassware, and electrical equipment with normal precautions. Caustic can cause severe bums to the skin. Handle with caution and If a spill should occur, wash the area with large amounts of water and report to first aid. ANALYTICAL TIME 0.5 hours PRECISION OF ANALYSIS AND SIGNIFICANT FIGURES No precision has been determined, but should be accurate to .0156. Report 2 significant figures. SCOPE Chlorides in an acid solution precipitate as AgCl. An excess of chlorides in AgNO-a causes a sharp change in potential, which is taken as the end point of the titration. REFERENCES Method 20-29-50, Rev. 7/27/58 (Modified) GK/mlw RSV 0015138 MONSANTO CHEMICAL COMPANY ORGANIC DIVISION TEXAS CITY, TEXAS DEPT. 33.60 METHOD 602.660 (W.C.) February 4, 1964 Page 1 of 4 MATERIAL Cauatlc Receipts ANALYSIS REQUIRED Sulfates SAMPLE 1 pint APPARATUS 100 ml beaker Small weighing bottle 50 ml stoppered graduated cylinders Pyrex hydrosol 'filter holders. Cat. #XX1002500 Millipore Filter Corp., Bedford, Massachusetts Millipore filter discs., 25 mm dia. type AA 0.8-^ Scoop, glass. Cat. #1H-12. Laboratory Equipment Company St. Joseph, Michigan Beckman Model B 50 mm cells (matched) REAGENTS 1. Barium chloride 20-30 mesh parr turbidimetric grade, J. T. Baker Chemical Company. 2. Dispersing reagent 3. Concentrated HC1 4. Phenolphthalein indicator RSV 0015139 METHOD 602.660 (W.C.) February 4, 1964 Page 2 of 4 PROCEDURE 1. Weigh 2 gms of sample (40-50 drops from a weighing bottle) into a 100 ml beaker. Add 10 ml of distilled water and 1-2 drops of phenolphthalein indicator to the beaker. Carry a reagent blank along with the sample. 2. Drop-wiee, add concentrated HC1 until the solution is Just colorless, then filter the sample through a milllpore filter type AA7 Wash the beaker several times with 5 ml portions of distilled water, passing the wash water through the filter after each washing. Transfer the contents of the filter flask to a 50 ml stoppered graduate cylinder, again washing the filter flask several times with 5 ml portions of distilled water. 3. Add 5 ml of dispersing reagent to the graduate and dilute to 50 ml with distilled water. Mix well. Then add 1 scoop (0.3 gm) of BAClg and shake for 1 minute. Allow the graduate to stand for five minutes, and then transfer to a 50 mm cell and read against the blank at 420 m.^*on the Beckman "B." CALCULATIONS From the attached calibration chart, determine the amount of SOjj present. ><gra of SO. _____________= PPM SOh Sample weight PREPARATION OF REAGENTS 1. Dispersing reagent - Mix 25 ml concentrated HC1, 75 ml of deeminac water, 300 ml Cp glycerine, and 600 ml of 95* ethanol. STANDARDIZATION AND/OR CALIBRATION 1. Measure .148 gm of AR Na2S04 (Sodium sulfate) into a liter volumetric flask and dilute to a liter. This gives a 100-^gm/ml of SO^ solution. RSV 0016140 METHOD 602.660 (W.C.) February 4, 1964 Page 3 of 4 2. Pipette 10, 30, 50, 70 ml of the 100^gm/ml standard solution Into a 100 ml volumetric flask and dilute to volume. This cive a 10* 30* 50, 70 >*gm/ml solution. 3. Use 1 ml of each solution and carry through the standard procedure for S0ji determination. Plot the absorbance for each sample against the "sn SOh present.. Draw a straight line connecting these values for an absorbance versus ^gm chart. SAFETY Use normal laboratory safety precautions In handling chemicals, glassware and electrical equipment. Caustic can cause a severe burn If spilled on the skin. If a spill should occur, wash with large amounts of water and report to first aid. ANALYTICAL TIME 0.5 hours PRECISION OF ANALYSIS AND SIGNIFICANT FIQURES Report to the nearest PPM SO,.. 95^ confidence limits are 5PPM at a 50 PPM level. * SCOPE The SO. present reacts with Ba to produce a tubldlty, which Is readies absorbance on the Beckman "B." REFERENCES Method 602.503 (W.C.) (Modified) RSV 0015141 Mlcrograma of SO^, versus absorbance on Beckman Model "B" spectrophotometer at 420 millimicrons with a 50 mm cell. Absorbance .002 .003 .004 .005 .007 .009 .010 .012 .013 .014 .015 .017 .019 .020 .021 .022 .023 .024 .026 .027 .028 .030 .031 .032 .034 .035 .036 .038 .040 .042 .043 .044 .045 -^gm SC^ 3 6 9 12 15 18 21 24 27 30 33 36 39 42 45 48 51 54 57 60 63 66 69 T2 75 78 81 84 87 90 93 96 99 Absorbance .049 .054 .059 .062 .068 .075 .080 .085 .090 .095 " .101 .106 .110 .115 .120 .125 .130 .135 .140 .146 .155 .160 .166 .172 .180 .186 .194 .199 .209 .219 .230 .240 .251 METHOD 602.660 (W.C.) February 4. 1964 Page 4 of 4 ^gm SO4 102 117 126 135 144 153 162 171 180 189 198 207 216 225 234 243 252 261 270 279 288 297 306 315 324 333 342 351 366 381 s 426 GK/mlw BSV 0015142 RSV 0015143 } TANK CALIBRATION TABLE TANK NUMBER: 60N2 TANK NAME: Caustic-Finished Latex Mix Tank TANK CONTENTS: Caustic & Hydrolyzed Latex METHOD OF GAUGING : LI 214 TANK DIMENSIONS: 4' OD x 6* 6" TYPE: Vertical HEADS: Bottom Flat; Top Dished EQUIPPED WITH: An agitator TRANSMITTER RANGE : 82.5 inches H2O SP. GR. : 1.145 GALLONS/INCH: 7.83 Instrument Readina(%) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 Gallons 47 53 58 64 70 75 81 86 92 98 103 109 115 120 126 132 137 143 149 154 160 165 171 177 182 188 194 199 205 211 216 222 228 233 239 244 250 ZJl 5 .6 N/ Instrument Reading (%) 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 60-001.00 Page 1 of 2 MMS/ff Rev. 2/25/72 Gallons 2 56 261 267 273 278 284 290 295 301 307 312 318 323 329 335 340 346 3 52 357 363 369 374 380 386 391 397 402 408 414 419 425 431 436 442 448 453 459 A Z-A 5 .6 >f RSV 0015144 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME: 60N2 Caustic-Finished Latex Mix Tank TANK CONTENTS: Caustic & Hydrolyzed Latex METHOD OF GAUGING : LI 214 TANK DIMENSIONS: 4* OD x 6' 6" TYPE: Vertical HEADS: Bottom Flat; Top Dished EQUIPPED WITH: An agitator TRANSMITTER RANGE : 82.5 inches H2O SP.GR.: 1.145 GALLONS /INCH : 7.83 Instrument Reading(%) 74 75 76 77 78 79 80 61 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 - Gallons 464 470 476 481 487 493 498 504 510 515 521 527 532 538 543 549 555 560 566 572 577 583 589 594 600 605 611 A 5 .6 vN/f Instrument Reading (%) 60-801.00 Page 2 of 2 MMS/ff Rev. 2/25/72 Gallons A J RSV 0015145 TANK CALIBRATION TABLE TANK NUMBER: 60S1-1 & 2 TANK NAME: Blowdown Separat< 31 #1 & #2 TANK CONTENTS: Latex METHOD OF GAUGING: LI 201-1&2 TANK DIMENSIONS: 11' dia. x 15* S. TYPE: Vertical HEADS: Flanged & Dished EQPT. WITH: Impingement Plat TRANSMITTER RANGE: 16.5 to 80.5 incl 1 s H2O SP. GR. : 1-10 GALLONS/INCH: 5` Instrument ' Readinaf%) Gallons 00 37.5-Top of Dish 807 36 824 39 858 40 892 41 927 42 961 43 996 44 1030 45 1064 46 1099 47 1133 48 1168 49 1202 50 1236 51 1271 52 1305 53 1340 54 1374 55 1408 56 1443 57 1477 58 1512 59 1546 60 1580 61 1615 62 1650 63 1684 64 1718 65 1752 66 1787 67 1821 68 1856 A 807 17 34 4 \f Instrument Readina 69 70 71 72 73 74 75 76 77 78 79 80 . 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 60-801.00 Page 1 of 1 MMS/ff Rev. 2/25/72 Gallons 1890 1924 1959 1993 2028 2062 2096 2131 2165 2200 2234 2268 2303 2337 2372 2406 2440 2475 2509 2544 2578 2612 2647 2681 2716 2750 2784 2819 2853 2888 2922 2956 A 34 .4 I ! 1 RSV 0015146 TANK CALIBRATION TABLE 60-801.00 TANK NUMBER: TANK NAME: TANK CONTENTS: 60S2 THF Recovery Column Still Pot THF/toter/Latex Solids Page 1 of j MMS /ff Rev. 2/16/72 METHOD OF GAUGING: LIC 305 TANK DIMENSIONS: 6'4" I.D. X 7'8" SS TYPE: Vertical HEADS: Bottom double w/one inverted? Top F&D SOFT. WITH: Steam jacket and Agitator TRANSMITTER TYPE: Displacer SP. GR.: 1.0 GALLONS/INCH: 17.6 Instrument Reading 1%) 0 2 4 6 8 10 12 14 16 18 20 Gallons 88 113 138 164 169 215 240 265 291 316 342 A -- 25 .4 Instrument Readina(^fe) 52 54 56 58 60 62 64 66 68 70 72 Gallons 748 773 799 824 850 875 900 926 951 977 1002 A 25 4 22 367 74 1027 24 392 26 418 28 443 30 469 32 494 76 1053 78 1078 80 1104 82 1129 84 1154 34 519 36 545 38 570 40 596 86 1180 88 1205 90 1231 92 1256 42 621 44 646 46 672 48 SO 697 723 r 94 96 98 100 1281 1307 1332 13 58 \ RSV 0015147 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQPT. WITH: 60S3 THF Separator THF LIC 304 30" OD x 39" Vertical Flanged and Dished - 60-801.00 Page 1 of 2 JSM/ff 7/4/71 rument inqiXl. 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 Gallons 21.7 22.2 22.6 23.0 23.4 23.9 24.3 24.7 25.2 25.6 26.0 26.4 26.9 27.3 27.7 26.1 28.6 29.0 29.5 29.9 30.3 30.8 31.2 31.6 32.0 32.5 32.9 33.3 33.8 34.2 34.6 35.0 35.5 35.9 36.3 J 43 f Instrument Readinq 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons 36.8 37.2 37.6 38.1 36.5 38.9 49.4 39.8 40.2 40.6 41.1 41.5 41.9 42.4 42.8 43.2 43.6 44.1 44.5 44.9 45.4 45.6 46.2 46.7 47.1 47.5 47.9 46.4 48.8 49.2 49.7 50.1 50.5 51.0 51.4 _A_ .43 RSV 0015148 TANK CALIBRATION TABLE 60-801.00 TANK NUMBER: 60S3 Instrument Reading 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 Gallons 51.8 52.3 52.7 53.1 53.5 54.0 54.4 54.8 55.3 55.7 56.1 56.6 57.0 57.4 57.8 58.3 L .43 \y|r (continued) Page 2 of 2 JSM/ff 7/4/71 Instrument Reading 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons 58.7 59.1 59.6 60.0 60.4 60.9 61.3 61.7 62.1 62.6 63.0 63.4 63.9 64.3 64.7 a 13 'jt RSV 0015149 TANK CALIBRATION TA3LE 60-801.00 TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: TRANSMITTER RANGE: SP. GR. : .919 60T1-1 & 2 Vinyl Chloride Storage Vinyl Chloride LI 111-16.2 10' dia x 40' Horizontal Elliptical 98 Inches H2O Page 1 of ^ MMS/ff Rev. 2/25/72 Instrument Reading (%) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18* 19 20 21 22 23 24 25 26 27 26 29 30 31 32 33, `34 Gallons 453 572 712 857 1011 1171 1336 1506 1686 1876 2071 2271 2476 2686 2901 3122 3345 3572 3801 4034 4274 4517 4763 5012 5263 5520 5780 6042 6306 6573 6840 7113 7387 7662 7938 A 124 135 145 154 160 165 170 180 190 195 200 205 210 215 221 223 227 229 233 240 243 246 149 254 257 260 262 264 267 267 273 274 275 276 Instrument Readinq(%) 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons 8218 8499 8782 9066 93 53 9640 9928 10216 10504 10793 11083 11373 11663 11954 12245 12 540 12833 13124 13414 13704 13994 14285 14576 14867 15157 15447 15735 16021 16305 16587 16867 17147 17426 17704 17979 A 280 281 283 264 287 287 288 2 88 288 289 290 290 290 291 291 295 291 291 290 290 291 291 291 291 290 290 288 286 284 282 280 280 279 278 275 RSV 0015150 TANK CALIBRATION TABLE 60-801.00 TANK NUMBER: 60T1 -1 & 2 instrument Readingf%) 70 71 72 73 74 75 76 77 76 79 80 81 82 83 84 85 Gallons 18254 18527 1879B 19067 19334 19598 19858 20114 20368 20618 20866 21110 213 50 21586 21818 22046 A 275 273 271 269 267 264 260 256 254 250 248 244 240 236 232 228 (continued) Page 2_ of 2_ MMS/ff Rev. 2/25/72 Instrument Reading(%) 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons 22270 22490 22706 22918 23126 23326 23520 23708 23890 24065 24235 24397 24551 24698 24837 A1 224 220 216 212 208 200 194 188 182 175 170 162 154 147 139 RSV 0015151 TANK CALIBRATION TABLE TANK NO.: 60T2-1&2 TANK NAME: THF Storage Tank 1 & 2 TANK CONTENTS: Tetrahydrofuran METHOD OF GAUGING: LI 301-1&2 TANK DIMENSIONS: 94.8" O.D. x 30' TYPE: Horizontal Cylindrical HEADS: ASME Flanged & Dished TRANSMITTER RANGE: 75 inches H20 SPECIFIC GRAVITY: 0.89 Str. Side 60-801.00 Page 1 of 2 MMS/ff 6/21/72 Instrument ReadinQ(%) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 6/26/72 Gallons 495 570 647 720 802 898 987 1078 1161 1266 1363 1462 1564 1668 1773 1880 1989 2099 2210 2322 2436 2552 2669 2787 2906 3026 3147 3269 3393 3518 3643 3769 3895 4022 4149 4276 4404 - A 0 75 77 80 82 86 89 91 93 95 97 99 102 104 105 107 109 110 111 112 114 116 117 118 119 120 121 122 124 125 12 5 126 126 127 127 127 128 Instrument Readina 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 Gallons 4533 4662 4792 4922 5053 5184 5315 5447 5579 5711 5843 5975 6107 6239 6370 6500 6629 6757 6885 7013 7141 7269 7396 7523 7649 7774 7898 7921 8193 8264 8384 8503 8621 8737 8852 8966 9079 A 129 129 13 0 130 131 131 131 132 132 132 132 132 132 132 131 130 129 128 128 128 128 128 127 127 126 125 124 123 122 121 120 119 118 116 115 114 113 RSV 0015152 TANK NO.j TANK CALIBRATION TABLE 60T2-1&2 60-801.00 Page 2 of 2 MMS/ff 6/21/72 Instrument Reading(%) 74 75 76 77 78 79 80 81 82 63 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons 9191 9300 9408 9515 9620 9723 9824 9924 10022 10119 10215 10300 10390 10475 10557 10636 10711 10783 10853 10921 10987 11050 11107 11158 11200 11233 11258 6/26/72 1 Instrument Reading (%) 112 109 108 107 105 103 101 100 96 97 96 95 90 85 82 79 75 72 70 68 66 63 57 51 42 33 25 30 feet Gallons 94.8 inches RSV 0015153 TANK CALIBRATION TABLE 60--801.00 TANK NUMBER: 60T3 TANK NAME: si Storage Tank TANK CONTENTS: Sodium Lauryl Sulfate METHOD OF GAUGING: LI 102 TANK DIMENSIONS: 12' OD x 15' SS TYPE: Vertical HEADS: Top - Conical; Bottom EQPT. WITH; Side-mounted agitator TRANSMITTER RANGE: 175 inches H20 SP. GR. : 1.031 GALLONS /INCH: 70.46 Instrument Reading(%) Gallons J 0 846 119 1 965 2 1085 3 1205 4 1325 5 1444 6 1564 7 1684 8 1804 9 1924 10 2043 11 2163 12 2283 13 2403 14 2523 15 2642 16 2762 17 2882 18 3002 19 3121 20 3234 21 3354 22 3474 23 3594 24 3713 25 3833 26 3953 27 4073 28 4192 29 4312 30 443 2 31 4552 32 4672 33 34 4791 4911 Nf Page 1 of ^1 MMS /ff Rev. 2/25/72 - Flat and heating coil Instrument Reading(%) 35 36 38 40 42 44 46 48 50 52 54 56 58 60 62 64 66 68 70 72 74 76 78 80 82 84 86 88 90 92 94 96 98 100 Gallons 5031 5151 5390 5630 5869 6109 6348 6588 6828 7067 7307 7546 7779 8018 8258 8498 8737 8977 9216 9456 9695 9935 10174 10414 10654 10893 11133 11372 11541 11851 12091 12324 12563 12803 J 119 119 239 f RSV 0015154 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS; TYPE: HEADS: EQPT. WITH: 60TS Ammonia Make-up Tank NH4OH (22.2%) LG 121 4" dia x 6' SS Horizontal Flanged & Dished Cooling Coil 60-801.00 Page 1^ of _1 J3M/ff 7/4/71 Height O' 0" 1 2 3 4 5 6 7 8 9 10 11 1' 0" 1 2 3 4 5 6 7 8 9 10 11 Gallons 45 57 69 82 95 110 125 140 155 170 185 200 216 232 249 267 285 303 322 341 359 377 393 409 A 12 12 12 13 13 15 15 15 15 15 15 15 16 16 17 18 18 19 19 19 16 16 16 16 Heioht 2' 0" 1 2 3 4 5 6 7 8 9 10 11 3' 0H 1 2 3 4 5 6 Gallons 425 441 457 472 487 502 517 532 546 559 572 584 596 607 616 624 631 637 641 A 16 16 15 15 15 15 15 14 13 13 12 12 11 9 8 7 6 6 4 RSV 0015155 -J TANK CALIBRATION TABLE TANK CHAMBER: TANK NAME; TANK CONTENTS ? METHOD OF GAUGING; TANK DIMENSIONS- TYPE: HEADS: EQPT. WITH: 60T6 20% Caustic Storage Tank 20% Sodium Hydroxide LG 210 6' 6" OD X 15' Horizontal Flanged & Dished 60-801.00 Fage 1 of 1 JSM/ff 7/4/71 Height O' 0" 1 2 3 4 5 6 7 8 9 10 11 1* 0" 1 2 3 4 5 6 7 8 9 10 11 2* 0" 1 2 3 4 5 6 7 8 9 10 11 Gallons 135 170 207 246 266 330 378 426 476 526 577 629 683 739 796 855 914 974 1037 1101 1165 1220 1293 1358 1423 1488 1553 1618 1683 1749 1815 1666 1957 2029 2101 2172 5 35 37 39 40 44 48 48 50 50 51 52 54 56 57 59 59 60 63 64 64 64 64 65 65 65 65 65 65 66 66 71 71 72 72 71 71 Heiaht 3' 0" 1 2 3 4 5 6 7 8 9 10 11 4' 0" 1 2 3 4 5 6 7 8 9 10 11 5' 0" 1 2 3 4 5 6 Gallons 2243 2309 2375 2440 2505 2570 2635 2700 2765 2829 2893 2957 3021 3084 3144 3203 3262 3319 3375 3429 3481 3532 3582 3632 3680 3728 3772 3812 3851 3888 3923 A. 66 66 65 65 65 65 65 65 64 64 64 64 63 60 59 59 57 56 54 52 51 50 50 48 48 44 40 39 37 35 RSV 0015156 i TANK CALIBRATION TABLE TANK NUMBER: 60T7 TANK NAME: Condensate Storage Tank TANK CONTENTS: Condensate METHOD OF GAUGING: LIC 101 TANK DIMENSIONS: 12' ID x 19'11" SS TYPE t Vertical HEADS s Top - Conical; Bottom - Flat TRANSMITTER RANGEt 154 inches H^O SP. GR.s 1.00 GALLONS/INCHES: 70.5 60-801.00 Page 1 of 1 MMS /ff Rev. 2/25/72 Instrument Reading 1%) 0 5 io 15 20 25 30 35 40 45 50 Gallons 846 1388 1956 2473 3016 3558 4101 4643 5186 5728 6271 A 543 Instrument Reading(%) 55 60 65 70 75 80 85 90 95 100 Gallons 6814 7356 7899 8441 8984 9526 10069 10611 11154 11696 A 543 RSV 0015157 TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS* TYPE: HEADS: EQPT. WITH: tank calibration table 60T8 Aqueous Make^Tank Aqueous Solution None 90" 0D x 8* 6" SS Vertical Flanged & Dished An agitator 60-801.00 Page 1 of _1 JSM/ff 7/4/71 Liquid Level % or Inches 0 5 10 15 20 25 30 35 40 45 50 Gallons 256 396 536 676 ei6 956 1096 1236 1376 1516 1656 A 140 Liquid Level % or Inches 55 60 65 70 75 80 85 90 95 100 Gallons 1796 1936 2076 2216 2356 2496 2636 2776 2916 3056 A 140 RSV 0015158 tank calibration table 60-801.00 TANK NUMBER: 60T9 TANK NAME; Aqueous Storage Tank TANK CONTENTS: Aqueous Mix METHOD OF GAUGING: LI 110 TANK DIMENSIONS: 11' dia. x 15' SS TYPE: HEADS: Vertical Top - Conical; Bottom - Flat EQPT. WITH; Internal Coils TRANSMITTER RANGE: 157 inches H20 SP. GR. i 1,00-___ GALLONS/INCH:___ 59.2 instrument ReadingGallons a Instrument Readingf%) 0 710 52 2 894 184 54 4 1083 56 6 1267 58 8 1456 60 10 1640 62 12 1823 64 14 2013 66 16 2196 68 18 2386 20 2569 70 72 22 2753 74 24 2942 76 26 3126 78 28 3309 80 30 3499 82 32 3682 84 34 3872 86 36 4055 88 38 4245 90 40 4428 92 42 4612 94 44 4801 96 46 4985 98 48 5174 \f 50 5358 100 Page 1 of ^1 ms/ff Rev. 2/25/72 Gallons 5541 5731 5914 6104 6287 6471 6661 6844 7033 7217 7400 7589 7773 7962 8146 8329 8519 8702 8892 9075 9259 9448 9632 9821 10005 A 184 / RSV 0015159 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME; TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQPT. WITH: 60T10 APS Make-Up Tank APS Solution None 4* 6" OD x 5* 3" Vertical Flanged and Dished An agitator and Heating Coils 60-801.00 Page 1 of 1 JSM/ff 7/4/71 Liquid Level % 0 5 10 15 20 25 30 35 40 45 50 Gallons 55 86 117 148 179 210 241 272 303 334 365 A 31 31 31 31 31 31 31 31 31 31 31 Liquid Level % 55 60 65 70 75 80 85 90 95 100 Gallons 396 427 458 489 520 551 582 613 644 675 A 31 31 31 31 31 31 31 31 31 31 RSV 0015160 jr TANK CAL IH PAT ION TABLE TANK NUMBER: TANK NAMES TANK CONTENTS: METHOD OF GAUGING; TANK DZMENSIONSs TYPE: HEADS: 60T11 APS Feed Tank APS solution LG 118 36*' OD X 3'0" Vertical Flanged & Dished 60-801.00 Fage 1. of ^ JSM/ff 7/4/71 LG Height rt. In. 00 1 2 3 4 5 6 7 8 9 10 11 10 1 2 3 4 5 6 7 8 9 10 11 Gallons 34 39 43 47 52 56 61 65 69 74 78 83 87 91 96 100 105 109 113 118 122 127 131 135 A. 4.4 V 1 1 i LG Height p-fr. Tn. 20 1 2 3 4 5 6 7 8 9 10 11 30 Gallons 140 144 149 153 157 162 166 171 175 179 184 188 193 A_ 4.4 RSV 0015161 I TANK CALIBRATION TABLE ; TANK NVMRER* TANK NAME; TANK COCITENTSMETHCE OF GAUGING: TANK DIMENSIONSTYPEr HEADS: EOPT. WITH: 60T12 SFS Maxe-Up Tank SFS Solution None 42" OD x 4` 0" SS Vertical Flanged 6 Dished Agitator and Heating Coils 60-801.00 Paae 1 JSM/ff 7/4 '*71 Liquid Laved % 0 5 10 IS 20 25 30 35 40 45 50 GaIlona 26 40 55 69 84 98 112 127 -141 156 170 . n 14.4 \1f/ }' Liquid Level .% Gallons : 55 1 i 60 184 199 65 213 70 226 75 242 80 256 85 271 90 285 95 300 100 314 k A 14.4 >1 RSV 0015162 tank calibration table TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS' TYPE: HEADS: 60T13 SFS Feed Tank STS Solution LG 114 36" OD x 3'0" Vertical Flanged & Dished 60-801,00 Page 1 of 1 JSM/ff 7/4/71 LG Height Ft. In. 00 1 2 3 4 5 6 7 8 9 10 11 10 1 2 3 4 5 6 7 8 9 10 11 Gallons 34 39 43 47 52 56 61 65 69 74 78 63 87 91 96 100 105 109 113 118 122 127 131 13 5 A 4.4 LG Height Ft. In. 20 1 2 3 4 5 6 7 8 9 10 11 30 Gallons 140 144 149 153 157 162 166 171 17 5 179 184 168 193 A 4.4 V RSV 0015163 J TANK CALIBRATION TABLE TANK NUMBER: TANK NAME; TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQFT. WITH: 60T14 Acrylamide Make-Up Tank Acrylamide/SLS solution None 60** x 63" Vertical Flanged & Dished Agitator and Heating Coil 60-801.00 Page 1_ of ^ JSM/ff 7/4/71 Liquid Level % 0 5 10 15 20 25 30 35 40 45 50 Gallons 131 213 295 377 459 541 623 705 787 869 951 A 82 Liquid Level % 55 60 65 70 75 80 85 90 95 100 Gallons 1033 1115 1197 1279 1361 1443 1525 1607 1689 1771 _A 82 RSV 0015164 TANK CALIBRATION TABLE 60-801.00 TANK NUMBER: 60T15 Page 1 of 1 TANK NAME: Acrylamide Feed Tank MMS /ff TANK CONTENTS: Acrylamide/SLS Solution Rev. 2/25/72 METHOD OF GAUGING: LI 122 TANK DIMENSIONS: 5* ID x 6' 2" TYPE: Vertical HEADS: 5' radius EQPT. WITH: External jacket (not used) TRANSMITTER TYPE: Displacer SP. GR*: 1.04 GALLONS/INCH: 12.24 Instrument Reading {%) Gallons jt____________ Instrument Readina(%) Gallons 07 2 15 8 50 428 52 446 4 28 13 54 464 6 42 14 56 481 8 59 17 58 499 10 76 18 60 577 12 93 14 111 62 534 64 552 16 129 66 569 18 147 20 164 22 181 24 200 68 588 70 605 72 622 74 640 26 217 28 235 76 657 78 676 30 252 32 269 80 693 82 710 34 288 36 305 38 323 40 340 42 357 44 376 46 392 48 411 f 50 428 84 86 88 90 92 94 96 98 100 728 746 764 781 798 816 834 852 869 j 18 \Nf RSV 0015165 TANK CALIBRATION TABLE 60-601.00 TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQPT. WITH: 60T16-1 & 2. 60T17 Page 1 of 2 Hydrolyzer #1 & 2, Filter FD. TK AKS/ff Product Latex Rev. 2/11/72 LI 203-1&2 (0-110" WC) 7.5' dia. x 8'9" Vertical Flanged & Dished Agitator and Heating Coils (#1 only) Instrument ReadingGallons 0 411 1 438 2 466 3 493 4 520 5 548 6 575 7 602 8 629 9 657 10 684 11 711 12 739 13 766 14 793 15 821 16 848 17 875 18 902 19 930 20 957 21 984 22 1012 23 1040 24 1066 25 1094 26 1121 27 1148 28 1175 29 1203 30 1230 31 1257 32 1285 33 1312 34 1339 _ 27.3 f Instrument Readina(%) 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 se 59 60 61 62 63 64 65 66 67 68 69 Gallons 1367 1394 1421 1448 1476 1503 1530 1558 1585 1612 1640 1667 1694 1721 1749 1776 1803 1831 1858 1885 1913 1940 1967 1994 2022 2049 2076 2104 2131 2158 2186 2213 2240 2267 2295 _ 27.3 \LI RSV 0015166 60-801.00 TANK CALIBRATION TABLE TANK NUMBER: 60T16- 1 & 2.60T17 (continued) Page 2 of ^ AKS/ff Rev. 2/11/72 Instrument Reading(%) 70 71 72 73 74 75 76 77 78 79 80 81 62 83 84 85 Gallons 2322 2349 2377 2404 2431 2459 2486 . 2513 2540 2568 2595 2622 2650 2677 2704 2732 A 27 .3 \yr/ Instrument Reading(%) 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons 2759 2786 2813 2841 2866 2895 2923 2950 2977 3005 3032 3059 3086 3114 3141 A A 27.3 RSV 0015167 TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE; HEADS: EQPT. WITH: TANK CALIBRAT:ON TABLE 60T18 Latex Receiver Filtered Latex LIC 206 (0-50" WC) 3'6" OD x 4` 3" Vertical Flanged and Dished 60-801.00 Page 1 of 2 AKS/ff Rev. 2/11/72 Instrument ReadinafK^ 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 Gallons 62.0 64.7 67.4 70.1 72.8 75.5 78.2 80.9 83.6 86.3 89.0 91.7 94.4 97.1 99.8 102.5 105.2 107.9 110.6 113.3 116.0 118.7 121.4 124.1 126.8 129.5 132.2 134.9 137.6 140.3 143.0 145.7 148.4 151.1 153.8 J 2 ,7 ' Instrument Re&dino(%) 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons 156.5 159.2 161.9 164.6 167.3 170.0 172.7 175.4 178.1 180.8 183.5 186.2 188.9 191.6 194.3 197.0 199.7 202.4 205.1 207.8 210.5 213.2 215.9 218.6 221.3 224.0 226.7 229.4 232.1 234.8 237.5 240.2 242.9 245.6 248.3 A 2 .7 V RSV 0015168 TANK CALIBRATION TABLE 60-001.00 TANK NUMBERr 60T18 Instrument Re*dinaf%) 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 Gallons 251.0 253.7 256.4 259.1 261.8 264.5 267.2' 269.9 272.6 275.3 278.0 280.7 283.4 286.1 288.8 291.5 A 2.7 w V (continued) Page 2 of 2 AKS /ff Rev. 2/11/72 Instrument Readina(%) Gallons . A 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 294.2 296.9 299.6 302.3 305.0 307.7 310.4 313.1 315.8 318.5 321.2 323.9 326.6 329.3 332.0 2.7 V RSV 0015169 TANK NUMBER: TANK NAME; TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS* TYPE: HEADS: EQPT. WITH: taw calibration table 60T19 Latex B Storag e Tank Latex B LI 208 (0-366. 5" WC) 13' dia. x 28' SS vertical Top - Conical; Bottom - Flat An eductor 60-801.00 Pag e 1 of 2 AKS /ff Rev . 2/14/72 Instrument Readina{%) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 Gallons 910 1183 1456 1729 2002 2275 2548 2821 3094 3367 3640 3913 4186 4459 4732 5005 5278 5551 5824 6097 6370 6643 6916 7189 7462 7735 8008 8281 8554 8827 9100 9373 9646 9919 10192 J 273 'If Instrument Reading (96) 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 6S 66 67 68 69 Gallons 10465 10738 non 11284 11557 11830 12103 12376 12649 12922 13195 13468 13741 14014 14287 14560 14833 15106 15379 15652 15925 16198 16471 16744. 17017 17290 17563 17836 18109 18382 16655 18928 19201 19474 19747 A 273 1f RSV 0015170 TANK CALIBRATION TABLE 60-801.00 TANK NUMBER 60T19 Instrument Readme (%) 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 Gallons 20020 20293 20566 20839 21112 21385 21658 21931 22204 22477 22750 23023 23296 23569 23842 24115 A 273 V f/ (continued) Page 2 of 2 AKS /ff Rev. 2/14/72 Instrument Reading(%) 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons 24388 24661 24934 25207 25480 25753 26026 26299 26572 26845 27118 27391 27664 27937 28210 A 273 Ni RSV 0015171 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME: ' TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQPT. WITH: 60T20 Latex BH Storage Tank Latex BH Product LI 207 (0-218.5" WC) 17' ID x 18* Vertical Bottom Flat? Top Conical An Agitator 60-801.00 Page 1 of 2 RTH /1 Rev. 1/25/72 Instrument Readlna 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 Gallons 707 987 1266 1545 1824 2103 2382 2661 2940 3219 3498 3777 4056 4335 4614 4893 5172 5451 5730 6009 6288 6567 6846 712 5 7404 7683 7962 8341 8520 8799 9078 9357 9636 9915 10194 a 279 f Instrument Readino 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons 10473 10752 11031 11310 11589 11B68 12147 12426 12705 12984 13263 13 542 13821 14100 14379 14658 14937 15216 15495 15774 16053 16332 16611 16890 17169 17448 17727 18006 18285 18564 18843 19122 19401 19680 19959 A 279 f RSV 0015172 TANK CALIBRATION TABLE 60-801.00 TANK NUMBER: 60T20 Instrument Readina 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 Gallons 20238 20517 20796 21075 213 54 21633 21912 ' 22191 22470 22749 23028 23307 23586 23865 24144 24423 A 279 - Ni (continued) Page 2_ of 2_ RTH/ff Rev. 1/25/72 Instrument Readina(%) 86 87 86 89 90 91 92 93 94 95 96 97 98 99 100 Gallons 24702 24981 25260 25539 25818 26097 26376 26655 26934 27213 27492 27771 28050 28329 28608 iQ_ 279 \ ft RSV 0015173 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQFT. WITH: 60T21 Misc. Product Storage Latex Product LI 209 (0-323. 9" WC) 13' ID x 25* Vertical Top - Conical; Bottom - Flat An agitator 60-801.00 Page 1 of 2 AKS/ff Rev. 2/14/72 Instrument Reading(%) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 IS 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 Gallons 703 944 1186 1427 1668 1910 2151 2392 2633 2875 3116 3357 3599 3840 4081 4323 4564 4805 5046 5288 5529 5770 6012 62 53 6494 6736 6977 7218 7459 7701 7942 8183 8425 8666 8907 a 241.3 y Instrument Reading 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons 9149 9390 9631 9872 10114 103 55 10596 10638 11079 11320 11562 11803 12044 12285 12527 12768 13009 13251 13492 13733 13975 14216 14457 14698 14940 15181 15422 15664 15905 16146 16388 16629 16870 17111 17353 A 241.3 RSV 0015174 TANK CALIBRATION TABLE 60*801.00 TANK NUMBERS 60T21 Instrument Read i na ( 70 71 72 73 74 75 76 77 78 79 80 81 62 83 64 85 Gallons 17594 17835 18077 18318 18559 18801 19042 19283 19524 19766 20007 20248 20490 20731 20972 21214 J 241.3 - T (continued) Page 2 of 2 AKS /ff Rev. 2/14/72 Instrument Readina(%) 66 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons 21455 21692 21937 22179 22420 22661 22903 23144 23385 23627 23868 24109 243 50 24592 24833 a 241.3 \'Ifi RSV 0015175 TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TAHC DIMENSIONS: TYPE: HEADS: EQUIPPED WITH: TANK CALIBRATION TABLE 60T22 Waste Latex & Vent Tank Off- Spec* Latex LT 123 (0 -304 WC) 9' 0" ID X 27* ss Vertical 8`6" Radius Impingement P 1<ate Page 1, of 2 AKS/ff Rev. 2/11/72 Instrument Readinaftt) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 2i 22 23 24 25 26 27 28 29 30 31 32 33 34 Gallons H*iO - 795 916 1036 1157 1277 1398 1518 1639 1759 1880 2000 2121 2241 2362 2482 2603 2723 2844 2964 3085 3205 3326 3446 3567 3687 3808 3928 4049 4169 4290 4410 4531 4651 47TT 4892 A oal/% 120.5 N/ Instrument Readincf%l 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons H-fO 5013 5133 52 54 5374 5495 5615 5736 5856 5977 6097 6218 6338 6459 6579 6700 6820 6941 7061 7182 7302 7423 7543 7664 7784 7905 8025 8146 6266 8387 8507 8628 8748 8869 8989 9110 Agal/* 120.5 \f RSV 0015176 TANK NUMBER: tank calibration table 60T22 (continued) Page 2_ of 2_ AKS/ff Rev. 2/11/72 Instrument Reading (%) 70 71 72 73 74 75 76 77 78 79 80 81 62 83 84 85 Gallons H-jO 9230 9351 9471 9592 9712 9833 9953 10074 10194 10315 10435 10556 10676 10797 10917 11038 Aaal/* 120.5 f Instrument Reading (%) 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons H'tO 11158 11279 11399 11520 11640 11761 11881 12002 12122 12243 12363 12484 12604 12725 12845 Aaal/% 120.5 i/ RSV 0015177 tank calibration table TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: BEADS: EQPT. WITH: 60T24 Haste Tank Water/lAtax Solids LI 303 (0-100**WC) B* 6" dia. X 8*8** SS Vertical 8*6** Radius 60-801.00 Page 1 of 2 AKS/ff Rev. 2/14/72 Instrument Reading f*) 0 1 2 3 4 5 6 7 B 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 Gallons* H?0 460 495 531 566 602 637 672 708 743 779 814 849 885 920 956 991 1026 1062 1097 1133 1168 1203 1239 1274 1310 1345 1380 1416 1451 Zl 35.4 29 1487 30 1522 31 1557 32 1593 33 1628 34 1664 1 Instrument Reading f%) 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons H-pO 1699 1734 1770 1805 1841 1876 1911 1947 1962 2018 2053 2088 2124 2159 2195 2230 2265 2301 2336 2372 2407 2442 2478 2513 2549 2584 2619 2655 2690 2726 2761 2796 2832 2867 2903 A. 35 4 \/ ___J RSV 0015178 TANK CALIBRATION TABLE 60-801.00 TANK NUMBER: 60T24 instrument Readme {%) 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 Gallons 2938 2973 3009 3044 3080 3115 3150 3186 3221 3257 3292 3327 3363 3398 3434 3469 A 35.4 (continued) Paae 2 of 2 AKS/ff Rev. 2/14/72 Instrument Readino(%) 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons H-,0 3504 3540 3575 3611 3646 3681 3717 3752 3788 3823 3858 3894 3929 3965 4000 . A 35.4 RSV 0015179 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQPT. WITH: 60T25 Seal Pot Filtered Water LG 403 4* dia. x 10* SS Horizontal 4* Radius - 60-801.00 Page 1. of ,1 JSM/ff 7/4/71 Height Ft. In. 00 2 4 6 8 10 Gallons 37 69 106 147 191 236 1 0 284 2 336 4 388 6 442 8 496 10 550 AA 32 37 41 44 45 48 52 52 54 54 54 54 ft Height In. 20 2 4 6 8 10 Gallons 604 656 708 756 804 845 3 0 886 AA 52 52 48 45 44 41 RSV 0015180 TAW CALIBRATION TABLE TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQFT. WITH: 60T26 Chilled water Tank Chilled Condensate LI 501 < 0-114" WC) 10' dia. X 40* Horizontal Elliptical 60-801.00 Fage 1_ of 2, JSM/ff 7/4/71 Instrument ReadinaGallons 0 448 1 581 2 725 3 877 4 1037 5 1206 6 1385 7 1574 8 1770 9 1971 10 2177 11 2395 12 2617 13 2844 14 3075 15 3310 16 3552 17 3796 18 4045 19 4301 20 4565 21 4835 22 5108 23 5382 24 5658 25 5935 26 6215 27 6496 28 6781 29 7067 30 7363 31 7660 32 7960 33 8262 34 8566 A 133 144 152 160 169 179 189 196 201 206 218 222 227 231 235 242 244 249 256 264 270 273 274 276 277 280 281 285 286 296 297 300 302 304 305 Instrument Re&dina 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons 8671 9176 9482 9790 10098 10407 10718 11031 11347 11663 11979 12295 12611 12928 13245 13561 13877 14193 14507 14819 15131 15442 15751 16060 16368 16674 16976 17276 17575 17873 18169 18463 18751 19036 19318 A. 305 306 308 308 309 311 313 316 316 316 316 316 317 317 316 316 316 314 312 312 311 309 309 308 306 302 300 299 298 296 294 288 285 282 280 RSV 0015181 TANK CALIBRATION TABLE 60-001.00 TANK NUMBER: 60T26 Instrument Readino <%) 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 Gallons 19598 19875 20149 20421 20690 20956 21219* 21476 21728 21975 22216 22452 22682 22906 23125 23337 _A_ 277 274 272 269 266 263 257 252 247 241 236 230 224 219 212 205 (continued) Paqe 2 of 2 JSM/ff 7/4/71 Instrument Readina(%) 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons 23542 23740 23933 24118 24296 24463 24619 24765 24902 25032 25159 25259 25348 25421 25460 _A_ 198 193 185 178 167 156 146 137 130 127 100 89 73 39 RSV 0015182 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQFT. WITH: 60T36 Catch Tank Filtered Water None 8' I.D. x 14* O' Horizontal Dished Heads - 60-801.00 Page 1 of 2 JSM/ff 7/4/71 Height Ft. In. 00 1 2 3 4 5 6 7 e 9 10 11 10 1 2 3 4 5 6 7 8 9 10 11 20 1 2 3 4 5 6 7 8 9 10 11 Gallons 16 32 49 76 108 139 177 216 255 299 343 391 441 491 544 597 651 706 767 628 891 954 1017 1082 1147 1214 1282 1351 1420 1490 1561 1633 1705 1778 1851 A 16 17 29 30 31 38 39 39 44 44 48 50 50 53 53 54 . 55 61 61 63 63 63 65 65 67 68 69 69 70 71 72 72 73 73 74 Height Ft. In . 30 1 2 3 4 5 6 7 8 9 10 11 40 1 2 3 4 5 6 7 8 9 10 11 50 1 2 3 4 5 6 7 8 9 10 11 Gallons 1925 1999 2073 2148 2223 2298 2374 2450 2527 2604 2682 2760 2838 2916 2994 3072 3149 3226 3302 3378 3453 3528 3603 3677 3751 3825 3898 3971 4043 4115 4186 4256 4325 4394 4462 4529 A 74 74 75 75 75 76 76 77 77 78 78 78 78 78 78 77 77 76 76 75 75 75 74 74 74 73 73 72 .72 71 70 69 69 68 67 65 RSV 0015183 TANK CALIBRATION TABLE 60-901.00 TANK NUMBER: 60T36 Height Ft. In. 60 1 2 3 4 5 6 7 8 9 10 11 Gallons 4594 4659 4722 4785 4848 4909 4970 5025 5079 5132 5185 5235 * 65 63 63 63 61 61 55 54 53 53 50 50 (continued) Page 2 of 2 JSM/ff 7/4/71 Height Ft. In. 70 1 2 3 4 5 6 7 8 9 10 11 80 Gallons 5285 5333 5377 5421 5460 5499 5537 5568 5598 5627 5644 5660 5676 * *1 48 44 44 39 39 38 31 30 29 17 16 16 RSV 0015184 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD 05 GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQPT. WITH: SOT 3 8 Chemlime Storage Tank Chemlime LI 402 12' OD x 14* 0" Vertical Top - Conical; Bottom - Plat Agitator and Internal Coils 60-801.00 Page 1 of 2 JSM/ff 7/4/71 Instrument ReadingGallons 0 846 1 956 2 1066 3 1176 4 1286 5 1396 6 1506 ? 1616 6 1726 9 1836 10 1946 11 2056 12 2166 13 2276 14 2386 15 2496 16 2606 17 2716 18 2826 19 2936 20 3046 21 3156 22 3266 23 3376 24 3466 25 3596 26 3706 27 3816 28 3926 29 4036 30 4146 31 4256 32 4366 33 4476 34 4586 a 110 f Instrument Reading (%) 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons 4696 4806 4916 5026 5136 5246 5356 5466 5576 5686 5796 5906 6016 6126 6236 6346 6456 6566 6676 6786 6896 7006 7116 7225 7335 7445 7555 7665 7775 7885 7995 8105 8215 8325 8435 A 110 11 RSV 0015185 TANK CALIBRATION TABLE 60-801.00 TANK NUMBER: 60T38 Instrument Readinaf*) 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 Gallons 8545 6655 8765 8875 8985 9095 9205 ` 9315 9425 9535 9645 9755 9865 9975 10085 10195 L 110 - \ ft (continued) Page 2 of 2 JSM/ff 7/4/71 instrument Reading (?} 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 Gallons 10305 10415 10525 10635 10745 10855 10965 11075 11185 11295 11405 11515 11625 11735 11845 a 110 > RSV 0015186 TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQPT. WITH: TAKK CALIBRATION TABLE 60T40 Latex E Storage Tank Latex E Product LI 216 (0-230.2"WC) 20' 0- ID x 18' Vertical Bottom - Flat? Top - Conical An Eductor 60-801.00 Page 1 of 2 AKS/ff Rev. 1/25/72 Instrument Reading f%l Gallons 0 2153 1 2559 2 2965 3 3371 4 3777 5 4183 6 4588 7 4994 8 5400 9 5806 10 6212 11 6618 12 7024 13 7430 14 7836 15 6242 16 8647 17 9053 18 9459 19 9865 20 10271 21 10677 22 11083 23 11489 24 11895 25 12301 26 12706 27 13112 28 13 518 29 13924 30 14330 31 14736 32 15142 33 15548 ________ u______ 15548 a 405.9 \f 11 Instrument Re&dinci f*) 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 S3 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons A 16360 16765 17171 17577 17983 405 .9 18389 18795 19201 19607 20013 20419 20824 21230 21636 22042 22448 22854 23260 23666 24072 24478 24883 25289 25695 26101 26507 26913 27319 27725 28131 28537 28942 29348 29754 29754 u\ f , RSV 0015187 mCC IHM Monsanto FtO** iNAMi ft LOCATION) 0* Texas City, Texas____________________ cc SuMCT Additional Material for Dept, (a) __ Operating Manual/Specification Manual -7h&L,- 9,L TO Please insert the attached material into its correct location in your Department(s) Operating Manual/Specification Manual, Copy No. Freida Fredericks Standards Section The attached material is COMPANY-CONFIDENTIAL ANY MATERIAL THAT IS BEING SUPERSEDED BY THE ATTACHED SHOULD BE DESTROYED OR RETURNED TO THE STANDARDS SECTION RSV 0015188 TANK CALIBRATION TABLE TANK NUMBER: TANK NAME: TANK CONTENTS: METHOD OF GAUGING: TANK DIMENSIONS: TYPE: HEADS: EQPT. WITH: 60T41 LATEX STORAGE TANK LATEX PRODUCT (Sp.Gr. 1.11) LI (0-360" W. C.) 16' 0" OD x 30' VERTICAL BOTTOM-FLAT? TOP-CONICAL BAFFLES FOR FUTURE AGITATOR 60-801.00 Page .1 of 2_ JSM/ff 9/7/73 Instrument Reading (%) 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 Gallons 1. 467 1. 872 2,277 2, 682 3, 087 3,492 3, 897 4,302 4, 706 5. Ill 5, 516 5, 921 6, 326 6,731 7,136 7, 540 7. 946 8,351 8. 756 9. 161 9, 566 9,970 10,375 10, 780 11, 185 11,590 11,995 12,400 12,805 13,210 13.615 14,020 14, 425 14, 830 15.234 A 404.9 \f Instrument Readina{%) 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 Gallons 15.639 16,044 25, 357 16, 854 17,259 17,664 18,069 18,474 18.879 19,284 19,689 20. 094 20,498 20, 903 21, 308 21,714 22.118 22,523 22,928 23,333 23,738 24,143 24,548 24,953 25, 357 25, 762 26,167 26.572 26,977 27, 382 27,787 28,192 22,597 29,002 29,407 A 404. 9 Y RSV 0015189 TANK NUMBER: TANK CALIBRATION TABLE 60T41 (continued) Instrument Readme(%) 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 Gallons 29, 812 30, 217 30. 621 31,026 31,431 31,836 32.241 32,646 33,051 33,459 33,861 34, 266 34,671 35, 676 35, 481 35,885 A 404.9 N Instrument Readinq(%) 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 60-801.00 Page 2_ of 2 JSM/ff 9/7/73 Gallons 36,290 36. 695 37. 100 37,505 '37, 910 38,315 38,920 39, 125 39. 530 39.935 40, 340 40. 745 41, 149 41, 554 41,959 A 404.9 N/ RSV 0015190 MONSANTO COMPANY MONSANTO INDUSTRIAL CHEMICALS DIVISION TEXAS CITY PLANT STANDARD MANUFACTURING PROCESS FOR ETHYLENE VINYL CHLORIDE (Dept, 60) Prepared by: M. E. Gibbs R. T. Hammann G- A. Hart M. M. Siegel A. Shadensack J. Morgan CL* Approved by: J. L. Raassmmuusssen Manufacturing Superintendent R. W, Flint Guest Superintendent M- E. Gibbs Research Group Leader Copy / of JL 0 Issued: J, R. Savage] Manufacturing Manager OCT 1 1372 CONFIDENTIAL INFORMATION This process is the property of Monsanto Company and the recipient is responsible for its safekeeping. It contains confidential information of Monsanto Company which must not be reproduced, revealed to unauthorized persons or sent outside the Company without proper authorization. Either retain in a secure file or return to Standards Department. RSV 0015191 COPY NO. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17-20 DISTRIBUTION DISTRIBUTION TO: Technical Information Center St. Louis Research Technical Information Center St. Louis Research Vital Records Center General Offices Business Group Research Manager Specialty Products Group Administration Business Group Research Group Leader Specialty Products Group Administration Manufacturing Manager Specialty Products Group Administration General Superintendent MICC Manufacturing, Texas City Manufacturing Superintendent Texas City Manufacturing Supervisor Texas City Manufacturing Foreman Texas City Process Technology Supe rintendent MICC Manufacturing, Texas City Central Files, Texas City Library, Texas City Safety Review Committee Safety Review Committee Safety Review Committee Extra RSV 0015192 10. 11. 12. 13. 14. 15. 16. 17-20 DISTRIBUTION DISTRIBUTION TO: Date: Technical Information Center - St. Louis Research Technical Information Center - St. Louis Research Vital Record Center - General Offices - St. Louis W. R. Richard - St. Louis M. E. Gibbs - St. Louis J. R. Savage - St. Lotus R. W. Flint - Texas City J. L. Rasmussen - Texas City R. T. Hamm arm - Texas City G. A. Hart - Texas City W. L. Smull - Texas City Central Files - Texas City Library - Texas City J. F. Quinn - St. Louis M. A. Terpstra - St. Louis R. W. Radue - St. Louis Extra Copies CONFIDENTIAL RSV 0015193 TABLE OF CONTENTS TITLE PAGE DISTRIBUTION TABLE OF CONTENTS PHE-SECTION* SECTION I - AMENDMENTS SYNOPSIS OF PROCESS SECTION II - FLOW SHEETS A. Makeup System, Raw Material Storage B. Autoclave Feed System C- Autoclave System D. Blowdown, Hydrolysis and Filter Feed E. Filtration and Product Storage F. THF Storage and Recovery G. Vent System and Incineration H. Chilled Water and Hot Water Systems SECTION III - PROCESS IN DETAIL A. Raw Materials B. Solution Makeup C. Autoclave D. Hydrolysis E. Filtration F. Storage and Packout RSV 0015194 Table of Contents (cont'd) SECTION IV - COMMENTS ON PROCESS A. Raw Materials and Feed Makeup 1. Acrylamide Solution 2. Ammonium Persulfate Solution 3. Aqueous Solution 4. Sodium Formaldehyde Sulfoxylate Sol'n. 5. Sodium Lauryl Sulfate B. Polymerization 1. Catalyst 2. Polymerization Reaction a. Pressure b. Temperature c. Heat Generation and Removal d. Initial Batch Charging e. Reaction Start f. Rate and Timing of Acrylamide Addition g. Catalyst Addition Rates h. Total Amount of VCM Addition 3. Blowdown 4. Agitation C. Hydrolysis 1. Temperature 2. Caustic Concentration 3. Amount of Caustic 4. Percent Total Solids D. Screening and Latex Transfer 1. Temperature 2. Pressure 3. Grit Content 4. Latex Transfer RSV 0015195 Table of Contents (cont'd) SECTION IV - COMMENTS ON PROCESS (cont'd) E. Auxiliary Systems 1. Incinerator 2. Chilled Water 3. Reactor Sequencer 4. Ethylene 5. Solvent System SECTION V PROCESS CONTROL PROCEDURES A. Introduction B. Safety and Housekeeping C. Quality D. Yields and Rates E. Performance - Key Variables RSV 0015196 APPENDIX A MATERIAL BALANCES APPENDIX 1. Material Balance for Latex B Production 2. Material Balance for Latex BH Production 3. Material Balance for Latex E Production _> SPECIFICATIONS. FINISHED GOODS AND RAW MATERIALS 1. Raw Mate'rials a. Acrylamide b. Ammonia c. Ammonium Persulfate d. Butylated Hydroxy Toluene e. Ethylene f. Ferric Ammonium Sulfate g. Methanol h. Mono Methyl Ether Hydroquinone i. Sodium Formaldehyde Sulfoxylate j. Caustic k. Sodium Lauryl Sulfate 1* Tetrasodium Ethylenediamine Tetraacetate m. Tetrahydr ofuran n. Vinyl Chloride 2. Finished Product a. Latex B b. Latex BH c. Latex E APPENDIX C PHYSICAL CONSTANTS APPENDIX D PACKAGING AND SHIPPING APPENDIX E SAFETY DATA 1. Rules and Precautions a. Personnel b.. Equipment c. Operating Practices II. Toxicity RSV 0015197 APPENDIX F - ENVIRONMENTAL CONTROL AND WASTE DISCHARGE I. Incinerator Operation II. Comments on Incineration IH. Water Emissions tv. Emission Summary for Latexes B & BH V. Emission Summary for Latex E APPENDIX G - EQUIPMENT LIST APPENDIX H - UTILITY SUMMARY APPENDIX I - PERSONNEL APPENDIX J - TIME CYCLES APPENDIX K - QUALITY CONSIDERATIONS APPENDIX L - FORM FOR TENTATIVE AMENDMENT TO THE STANDARD MANUFACTURING PROCESS RSV 0015198 M 10 Monsanto r iCC *' J G. A. Danner - Texas City March 12, 1974 S.'MC EVC Tentative Amendment B **?--C* TO Ethylene Vinyl Chloride SMP Holders I Attached is a copy of Amendment B to the Ethylene Vinyl Chloride SMP. Please add this to your copy of the SMP. / jp Attach. G. A. Danner t RSV 0015199 Date: January 24, 1974 Tentative Amendment No. B STANDARD MANUFACTURING PROCESS FOR ETHYLENE VINYL CHLORIDE Product Code No. `s 840. 61, 840.62, 840.63, 840.64 ISSUANCE OF CURRENT PROCESS DOCUMENT1972 TITLE OF AMENDMENT: Autoclave Heatup for Hydrolyzing EVC-BH PRESENT PRACTICE: At the end of the reaction period when producing EVC-BH, the batch is heated from 55 to 60C by the use of steam on the autoclave coils 60 that the product in the hydrolyzer will be greater than 45C. SUGGESTED CHANGE: When the VCM addition is 90% complete, the steam valve on the autoclave will be manually blocked in and the temperature con troller will be increased from 55 to 60C letting the heat of reaction increase the temp. Due to a period of low VCM addition because of pressure control on the autoclave, the reaction cycle will be increased from 4 1/3 to 4 2/3 hours per batch, JUSTIFICATION FOR CHANGE: There is some indication that heating the latex using steam on the coils may have contributed to fouling of the autoclave coils. This suggested approach will allow the department to make hydrolyzed EVC-BH without using steam on the autoclave coils. SAFETY: No new property or personnel hazards will be introduced by the proposed change. All temperature and pressure shutdown devices will continue to be in service. QUALITY: No quality problems are expected from this change. RSV 0015200 Tentative Amendment No. B 2. EXTENT OF DEMONSTRATION: Permission is requested to run for three months. If successful this amendment will become part of the Standard Manufacturing Process. APPROVED BY: /U0M<^ - R. W. Flint Originated by: *> >a.-R. T. Hammann Endorsed by: 3. _________ J. L. Rasmussen Supt., Mfg. M. E. Gibbs Research Group Leader W. R. Richard Research Manager J. R. Savage Mfg. Manager mm RSV 0015201 Monsanto .)WM^4ioc*nowi______ J. S. Morgan - Texas City_________________ February 23, 1973 cc ***ci EVC Tentative Amendment A IffWNCI TO #Ethylene Vinyl Chloride SMP Holders 2- Amendment A to the Ethylene Vinyl Chloride SMP was successfully demonstrated_in October and November, 1972. Attached is a copy of the amendment to be included in your SMP. /jp Attach. RSV 0015202 Tentative Amendment A to the Ethylene Vinyl Chloride Tentative Process DATE: March 20, 1972 TENTATIVE AMENDMENT: A TENTATIVE PROCESS REPORT FOR PRODUCTION OF POLVIN PIGMENT BINDER. MONSAT AND MONFLEX January 7, 1970. Report No. P-1556. TITLE: Eliminate Second Water Wash PRESENT PRACTICE: The EVC reactors are washed with 55C steam condensate twice after batch blowdown to remove any residual latex and grit particles that will foul the cooling coils. Every fifteenth reaction batch also includes a solvent (tetrahydrofuran - THF) wash between the first and second condensate washes to dissolve any coagulated latex that has built up on the cooling coils. The wash cycle consists of the following steps: 1. Fill reactor (2,150 gallons) with condensate (or THF) - 20 min. 2. Agitate reactor contents - 15 min. 3. Pump out reactor contents to sewer (or THF storage) - 10 min. TOTAL - 45 min. PROPOSED CHANGE: This amendment proposes the elimination of the second condensate wash - retaining the first condensate wash on each batch and the THF wash every 15 batches. Each THF wash will be followed by a second condensate wash to remove residual THF from the reactor. JUSTIFICATION The primary justification for eliminating the second water wash is the reduction of 2,150 gallons H20/batch (15.9 M gallons/day at standard production rate) to the sewer. This represents a RSV 0015203 Tentative Amendment A to the Ethylene Vinyl Chloride Tentative Process -2- JUSTIFICATION (cont'd.) raw material savings of $5 M/year and $16 M in proposed secondary waste treating capital. These figures are for standard product rate - 23.7 M lbs./yr. (January, 1972 Monthly Report - M. E. Gibbs). The wash elimination will result in an individual batch cycle reduction of 45 minutes (8 1/2%). No savings due to increased unit capacity can be claimed at this time. The first water wash contains approximately 20 lbs. fl,100 ppm) of dissolved polymer so-lids and approximately l/2 lb. of grit. The color of this stream is chalky white. The second water wash contains approximately 2 lbs. (110 ppm) polymer solids and has been observed to be clear with some grit (settleable) present. Each wash is pumped to the sewer which flows through the Primary Waste Treatment Area (startup 6/1/72) and the proposed secondary treatment facility and eventually to Galveston Bay. Any latex left in the reactor prior to batch start will result in the production of some larger than normal particle sizes. The 2 lbs. of latex from the second wash will be left in the reactor prior to the next batch start. The amount of latex remaining, however, is slight and will probably not noticeably affect latex particle size. BACKGROUND The low solids content of the second water wash has been observed on every batch since the unit startup in November, 1971. The Tentative Process gives approximately 100 ppm as the solids concentration of the second wash. It has been observed the amount of solids in the washes can be reduced by optimizing the 2 low pressure (100 psig) reactor blowdowns. SAFETY Safety will not be affected. QUALITY Product quality will be monitored through regular analysis throughout the demonstration. The solids content of the first wash will also be monitored to determine if the solids concentration increases. Reactor heat transfer data will be taken to assure that the THF wash frequency is not increased to greater than 1/15 ba due to coil fouling. Particle size will be obtained every fifth batch during the demonstration. RSV 0015204 Tentative Amendment A to the Ethylene Vinyl Chloride Tentative Process -3- EXTENT OF DEMONSTRATION Permission is requested to run for one month - in order to get at least 15 batches on one reactor * with the second water wash eliminated. If in this period no "off-spec" product is produced and the THF wash frequency-is not increased to greater than 1/15 batches (U overall should remain > 100 BTU/hr. ft.2F at max. heat load), the Tentative Amendment will be considered permanent. Originated by; Endorsed by; R. T. Hammann Approved by; L. Smull j L. Rasmussen /R. W. Flint Y?t Qj E. Gibbs ac( /w. R. Richard Safety Review Committee nltS. Quinn Terpstra Savage / jp 4/7/72 RSV 0015205 M 10 ACC *KW Monsanto m*i*iocAfo.1, j. S. Morgan - Texas City February 20, 1973 EVC Tentative Amendment A uftuKCf , Plant Demonstration TO : Ethylene Vinyl Chloride SMP Holders Tentative Amendment A was successfully demonstrated October 28 November 8, 1972. Objective was to eliminate the second auto clave water wash from the normal batch cycle. The results are shown below. Objectives and Results For Plant Demonstration Performance Criteria Objective Results THF Wash Frequency Heat Transfer Coefficient (BTU/hr. F2 F) Product Particle Size (A) Off-Spec Product Produced (lbs.) Condensate Savings @ 23.7 M lbs./yr. ($/yr.) Secondary Treatment Capital Savings ($) Batch Cycle Reduction (%) 13 >100 650-900 0 5M 16 M 8.5 15 >178 685-327 0 5M 16 H 8.5 A tabulation of the complete test results is attached. Conclusions The second water wash can be eliminated from the batch cycle without effecting product quality or the frequency of the washes. The $5 M/yr. condensate savings (at 23.7 M lbs./yr.) and the 8 1/2% reduction in batch cycle time will be achieved. This amendment does not include: 1, Elimination of the two water washes during the THF wash sequence. 2. New products with significantly different heat transfer require ments and fouling characteristics as compared to Latex B cr E. Disposition of Tentative Amendment D The amendment is accepted. No modifications will be required to permanently implement the new procedure. The sequencer currently RSV 0015206 EVC Tentative Amendment A 2- - halts after the first water wash and must be manually advanced to the subsequent step* Under Amendment A the sequencer is advanced to Step 25 and held until the next batch is started. /jP Attach. J. S. Morgan RSV 0015207 Date 10/28/72 10/29/72 10/29/72 10/30/72 10/30/72 10/31/72 10/31/72 11/1/72 11/2/72 11/3/72 11/4/72 11/5/72 11/6/72 11/7/72 11/8/72 Batch Number 223 225 227 229 230 233 235 237 239 241 243 246 248 250 252 Heat Trans. Coefficient* 238 236 211 -205 213 206 185 188 182 196 192 181 169 182 178 2 * Assuming Coil Area = 468 ft. H20 Flow = 340 GPM Particle Size 795 827 822 685 Since THF Wash 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 JSM/jp 2/20/73 RSV 0015208 RSV 0015209 SYNOPSIS OF PROCESS RSV 0015210 I. SYNOPSIS OF PROCESS 1-1 TheJEVC department located at the Texas City plant was designed to produce 19 M pounds of EVC latex (weight on basis of dry polymer) per year via a Monsanto developed batch process. Three different latices are made, de noted as Latex B, Latex BH and Latex E. Capacity for Latex B and Latex E has been demonstrated at 22-23 M pounds per year. Capacity of BH is as yet not defined but is somewhat lower at present. The basic raw materials include the three monomers: vinyl chloride, ethylene, acrylamide, and a surfacant, sodium lauryl sulfate. Ethylene is obtained via pipeline from the Polymers and Petrochemical Division facilities at both the Texas City and Chocolate Bayou plants. Vinyl chloride is shipped by rail car from Dow. Sodium lauryl sulfate is received in bulk and acryla mide in 50 pound bags. The manufacture of EVC latex is centered in the polymerization step and accomplished in 2150 gallon, 2500 psi, stainless steel reactors. The reactors are equipped with high intensity agitation and internal coils which provide the ability to remove high heat loads. The reaction is a semi-batch type whereby initial charges of aqueous solution, vinyl chloride and ethylene are made batchwise and continuous charges of vinyl chloride and other aque ous streams are made on a programmed basis during ensuing reaction. Two basic reactions occur simultaneously: one, the redox catalyst reaction in cluding reduction of ferric to ferrous ion by sulfoxylate and the coupling oxidation reaction regenerating ferric ion and decomposing persulfate ion to a free radical;and two, the subsequent free radical emulsion polymerization forming molecular weight chains of about 35, 000 from the vinyl chloride, ethylene and acrylamide monomers. Molecular weight data and simplified equations follow: Persulfate Redox Catalyst System Reduction HSO* + Fe Sulfoxylate +X Oxidation Polymerization Reaction Initiation SOT7 + H2C = - S04H2C - CH* Cl fcl RSV 0015211 1-2 Chain Growth ? S04H2C-H' + m(H2C = CH) + n(H2C = CH2) + p(H2C * CHC - NH2) - ci ii Vinyl Chloride ethylene acrylamide [S04H3C-CH-CHz-CH2-CH2-CH-CH2-CH-CH2-CH-CH2-] Cl il Cl , O NH2 Chain to mol. wt of 35, 000 The reaction is carried out at 55C and 1750 - 1850 psi. Vinyl chloride is added to maintain constant pressure, as a pressure fall is associated with reaction of less dense monomers to more dense polymer. Surfactant addition maintains appropriate charge distribution on polymer particle surface to pre vent coagulation. Acrylamide is added directly in proporation to degree of reaction. Two catalyst streams generate necessary free radicals. When reaction mass reaches a solids content of about 50%, reaction is terminated and blowdown to atmospheric pressure during which a gas/liquid phase separation occurs. The unreacted monomers are vented to an incineration system and the residual liquid latex is sent forward for further processing. Primary difference in Latex B and Latex E is polymer composition which is determined during polymerization by feed rates and compositions. B type latices contain about 76% VCM, 21% ethylene and 3% acrylamide. E type latices contain more ethylene (29%) and less vinyl chloride (68%). No by product, as such is made but some solid coagulum must be filtered out of the liquid latex before storage as final product. This is accomplished by a special type of vibrating filter screen. Latex BH is produced by a further chemical processing step. B latex is hydrolyzed with caustic already diluted by previously hydrolyzed latex such that the caustic concentration is not too severe for virgin latex. High caustic concentrations can result in undesirable amounts of coagulation. The amide group contributed to the polymer of acrylamide is partially converted to carboxyl and imide as follows: [-CH2-CH-CH2-] + OH' [-ch2-ch-ch2-] + NH3 A o nh2 oo Amide _ Carboxyl [-CH2-CH - CH2-CH -ch2} OH -CH2-CH-CH2-CH-CH2-] + nh3 d^&H, H2N . O NH Imide c Hydrolysis is a relatively slow reaction requiring temperature, time and agitation to reach completion in a satisfactory batch cycle. RSV 0015212 1-3 Following filtration, the latex is stored in bulk storage tanks. Loadout of the product is made from the storage facilities into tankcar, tank trucks, or into 55 gallon fibre drums. A tetrahydrofuran solvent system is provided to solvent wash reactors at a given frequency (currently after every 15 batches). Between solvent washes heat transfer coefficients decrease due to a solid film deposition on the cool ing coils. When the coefficients reach a minimum value, solvent washing is instituted. A solvent recovery system is also provided to remove water and polymer solids from spent solvent. The recovery system consists primarily of a 26 foot packed, distillation tower. EVC yields of major component's are as follows: Materials Theory Usage____________ Lbs / Cwt B Lbs/Cwt E V CM 72.4 65. 2 Ethylene 21.0 28. 0 Acrylamide 3. 15 2. 62 Sodium Lauryl Sulfate 7.29 7. 11 Design _____________Usage Lbs/Cwt B Lbs/Cwt E 82.7 79. 5 36, 1 42.8 3. 58 3.07 8. 35 8. 06 RSV 0015213 1 2 4 . 14 1-4 Li ft *4 o3 -a 4> 41 O 2 co r- in o in fi (NJ oo ro ro iOn < oo ro rJ rO 0tj0- ro *4 , i>--n<*i Tj 00 0m0 O' rr Oin ro --. 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FLOW SHEETS RSV 0015216 -tJ* --- 11*1 RSV 0015217 SIS A lO d iU H ' IWOOMOIfl *-t> A l .'y3V fO WOH RSV 0015220 RSV 0015222 3J (D 8-n < o _o. cn wfO WMftiW^yt^w^n^ttawy.' - 25 .L PROCESS IN DETAIL RSV 0015225 III. PROCESS IN DETAIL RSV 0015226 in. PROCESS IN DETAIL HI-1 A. RAW MATERIALS SECTION The following raw materials are used in theproduction of EVC Latexes: 1. Vinyl Chloride Monomer (VCM) a. Product: b. Received: c. Storage: B, BH, E Received from Dow in 20, OOC gallon tank cars Stored in two (2) 24, 000 gallon, horizontal, carbon steel storage tanks under 90 psig pressure Ethyl ene a. Product: b. Received: c. Storage: B, BH, E Received from a plant header at 350 psig Stored in two (2) - 372 cubic foot bottles under 3, 000 psig of pressure Acrylamide a. Product: b. Received: c. Storage: B, BH, E Received from American Cyanamid in 50 lb bags The bags of acrylamide are stored in a solids storage shed until ready for use. 4. Sodium Lauryl Sulfate (SL.S) a. Product: b. Received: c. Storage: B, BH, E Received from Proctor and Gamble in 4,500 gal. trucks Stored in a 12, 000 gallon, 304 SS storage tank. 5. Ammonium Persulfate (APS) a. Product: b. Received: c. Storage: B, BH, E Received from FMC Corp. in 250 lb fibre drums. The drums of APS are stored in a solids storage shed until ready for use. RSV 0015227 in-2 A. RAW MATERIALS SECTION (cont'd) 6. Ferric Ammonium Sulfate (FAS) a. Product: b. Received: _S- Storage: B, BH, E Received from Mallinc.krodt in 25 lb fibre drums The drums of FAS are stored in a solids storage shed until ready for use. 7. Sodium formaldehyde Sulfoxalate (SFS) a. Product: ' B, BH, E b. Received: Received from Rohm and Haas in 325 lb. fibre drums. c. Storage: The drums of SFS are stored in a solids storage shed until ready for use. .8 Tetrasodium Ethvlenediamine Tetraacetate (EDTA) a. Product: b. Received: c. Storage: B, BH, E Received from Dow in 100 lb fibre drums The drums of EDTA are stored in a solids storage shed until ready for use. 9. Ammonia a. Product: b. Received: c. Storage: 10. Caustic B, BH, E Received from a plant header at 50 psig Stored as a solution with water at 22.2%. a. Product: BH b. Received: Received from a ^ 25% plant header. c. Storage: Stored at 20% concen. in a 4, 000 gallon, horizontal, C. S. storage tank. .11 Tetrahydrofuran (THF) a. Product: b. Received: c. Storage: B, BH. E Received from DuPont in 500 lb drums and 6, 000 gallon tank trucks Stored in two (2) 11,200 gallon, horizontal storage tanks. RSV 0015228