Document DMMXejXR24VezGKpg3EG2Y9MM

UNION CARBIDE CHEMICALS COMPANY VINYL. CHLORIDE MONOMER *nmndatlon ta practice any p a tca ltd (nvantlon wHhaat a Ik iiiM . 1l It o ffe n d te ftly far your coniiiftrarioa, InvttUgaMon and aartfkatton. ta t which w a tta in t Itg a l rttp o n iib ility nor at parmhtlon or rtc- be toVan o i a warranty or reprtienlolioti V IN Y L C H LO R ID E M O N O M E R VINYL CHLORIDE MONOMER CH2= CHCI GENERAL DESCRIPTION Vinyl chloride is a colorlea* gaa at standard temperatwe and preaawa. It has a i* deaired, 50 to 150 ppm. of phenol in generally naed. PHYSICAL PROPERTIES Molecular Weight_______________ ___ Apparent Specific Gravity at 20/20C, A sp. gr. / A L------------------ -------Boiling Point at 760 mm. Hg_............ Ab.p./Ap-------------Vapor Pressure at 20C............. -............................... Coefficient of Expansion at 20C Freezing Point --................ ....... Stpovliuebiviiliintyj iinn Wnaattceir aati 20Cv*........... Solubility of Water in at 20C...... Refractive Index, nD at 20C....... A nD/ At --..... ..--------------------- Heat of Vaporization at 1 atm___ Heat of Polymerization.... ........... Flash Point (open cup) Explosive Limits in Air........ -..... ............................. 62.50 0.9121 0.00186 per C. 13.4C. 63C. 84C. 0.026 CJmm. Hg 2520 mm. Hg 0.00203 -153.8 C. 0.68% by weight 0.09% by weight 1.37 0.00080 0.211 cal./g./C. 153 b.Lu./lb. 272 caL/g. (490 b.Lu./tfa.) <0F. 4 to 22% by volume Pounds per Gal. SHIPPING DATA Net Container Contents Cylinder Labels Required---------------- -------- -----------------------Cylinder Color Scheme Top ... Bottom Red Gas green black PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" UCC 084034 Jnnaary, 1962 F-40540 !M t tftformallon li M l b VINYL CHLORIDE MONOMER SUSPENSION POLYMERIZATION OF VINYL CHORIDE General Coilltlou Reaction Temperature Pressure____________ Agitator Speed______ Monomer Conversion.. 40 to 60 C. 75 to 125 psig 75 to 150 r.p.m. 80 to 95 per cent General Recipes Monomer to Water Ratio_____ __________________ Suspending Agent (either (a) or (b) or both) (a) Colloid (CELLOSIZE WP-09, "Methocell",0 or polyvinyl alcohol)________________________ _______ (b) Surfactant (TERGITOL 4 or 08, sodium lauryl sulfate, or "Aerosol" MA(2) .......... ............................. ......... ...... Catalyst (Benzoyl peroxide or diacetyl peroxide, etc.). Water___ ____________________ _______ ______________ 30/70 to 50/50 .05 to .15% of monomer .05 to .15% of monomer 0.1 to 0,3% of monomer Deionized and Deaerated 0) Dow Chemical Canpwry (2) Americai Cyananid Company Com meats 1. The same general conditions and recipies apply to copolymers with vinyl acetate and other monomers. The mount of comonomer that will react depends on the reactivity rela tive to vinyl chloride. About 25 per cent vinyl acetate is a practical limit. 2. The type and quality of resin produced is markedly affected by changes in conditions and formula ingredients. This can be mini mised by adhering strictly to the same con ditions in each reactant batch. Temperature, agitation, monomer conversion, and ingredi ents must be carefully controlled. S. Resins for different end-uses require varied properties. These changes in properties can be attained by changes in the reaction conditions and formula ingredients. How to make these changes can only be developed through experience with a given production unit. 4. In preparing a suspension resin, add enough suspending agent to prevent coagula tion of the resin during reaction and to control particle size within the desired range, but not enough to stabilize so that recovery of the resin is impeded. This is accomplished by balancing the agitation speed and concentra tions of suspending agent and surfactant. References Vinyl Retina" - Smith (Reinhold PublithingJ mVinyl and Related Polymert" -- Sehildkneeht U.S.P.2,492,087 to Monsanto Chemical Company, 1949 U.S.P.2,492,089 to llontanto Chemical Company, 1949 U.S.P.2,24S,742 to B.F. Goodrich, 1941 Page 2 PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" UCC 084035 VINYL CHLORIDE MONOMER Reactivity of Monomers Relative to Viayl Chloride Vinyl Chloride Methyl Methacrylate Styrene Methacrylonitrile Methyl Vinyl Svlfone Vlnylidene Chloride Acrylonitrile 1.0 20 1$ 15 15 9 5 Methalkyl Chloride Methyl Acrylate Allyl Acetate Allyl Chloride Vinyl Acetate Isopropenyl Acetate Vinyl Ethyl Ether 2.3 2 0.5 0.4 0.3 0.3 0.1 STORAGE AND HANDLING Inhibited vinyl chloride monomer may be stored at normal atmospheric temperatures in steel pressure vessels. Uninhibited monomer may be stored either under refrigeration or at normal atmospheric temperatures in the ab sence of air, sunlight or other catalysts for relatively short periods of time. All tanks, piping, instrument leads, relief valves and equipment in contact with the monomer should be of steel and designed to have a working pressure of at least 138 psi. No copper or copper bearing alloys should be used in the storage facilities in contact with the monomer or its vapors. Cast iron is not recommended for use in flanges or fittings. All liquid inlet lines should enter the bot tom of the tanks or extend to the bottom of the tanks to prevent the accumulation of static charges on filling. In addition all tanks and filling equipment should be grounded. The tanks should be equipped with a com bination of a 138 psi frangible disk and pres sure relief valve. In case excess pressure ruptures the safety disk, the pressure relief valve will prevent the loss of the entire contents of the tank after the excess pressure has been relieved. These tanks are designed for skin temperatures up to approximately 130F. In localities where surface tempera tures may go above this value, the tanks may be cooled with a water spray system. The tanks should not be filled to more than 90% of volume capacity. A blanket of inert gas or vinyl chloride vapor must be maintained in the tank at all times. No air should be allowed to enter the tanks at any time. Relief valve sizes may be determined by using A.S.M.E. Boiler Construction Code VA230 when the valve is designed to relieve all vapor formed without increasing the total pressure by more than 10%. Tanka may be gauged with nitrogen bubbler gauges. Adequate diking and drainage should be provided under the tanks to confine and dis pose of the liquid in case of vessel rupture. A water spray system is recommended as a method of keeping the metal tank cool in case of fire. All outlet lines from storage tanks should contain check valves to prevent contamination of tank contents. Before a tank is put into vinyl chloride monomer service, it should be purged with an inert gas until free of air. Tanks of less than 30,000 gallons capacity are most economically constructed in the form of horizontal cylinders. For detailed information on the storage and handling of vinyl chloride consult Manufac turing Chemists* Chemical Data Sheet SD-S6. This bulletin mentions the following points as being necessary for safe handling. 1. Keep away from heat, sparks and open flame. 2. Provide adequate ventilation. PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" nrC Q84036 u VINYL CHLORIDE MONOMER 3. Ground equipment end containers before discharging to reduce danger of ignition bom static sparks. 4. In discharging do not heat containers above 50C. (122F,). No-beat should be applied to tank cars. 5. All equipment should be of steel and have a designed working pressure of at least 100-150 psi. 6. In the event of accidental leaks, spills, or whenever excessive vapor concentrations may be encountered, only personnel equipped with approved respiratory protection should be permitted in the contaminated area. - 7. Chemical safety goggles should be worn when discharging containers or tank cars or whenever there is a danger of the liquid or saturated vapor coming in contact with the eyes. 8. Waste disposal should bo away from any source of ignition. Dilute phenolic residues before discharging to sewer. In case of fire use carbon dioxide or dry chemical extinguishing equipment. In the event of contact with the liquid remove con taminated clothing immediately. For eyes flush immediately with large quantities of water for at least 15 minutes while medical attention is being sought. TOXICOLOGICAL PROPERTIES Practical observations indicate that breath ing vinyl chloride vapors presents the greatest hazard. Because of the high vapor pressure of vinyl chloride, high v^>or concentrations develop rapidly. These vapors have a typical anesthetic effect, first causing dizziness, weakness, mental confusion, and finally loss of consciousness. Removal from exposure brings about rapid recovery with only brief complaints of nausea and headache. High volatility makes prolonged skin con tact with the material improbable. However, contact with saturated clothing may cause skin irritation. There is some suggestion that slcin penetration occurs and that the response given is an anesthetic one. Injury to the eye would be similar to that caused by contact with liquid hand soaps. Eye protection is advisable, and in case of accidental contact wash the eye with clean water for fifteen minutes. SPECIFICATION LIMITS 1. Acidity is Hydrochloric Acid -- 2. Acetylene-------------------------------3. Aldehydes as Acetaldehyde------4. Iron as Fe-------------- -------------5. Phenol (Customer's Preference) inhibited monomer----------------Uninhibited monomer-------------6. Ethylene---------------------------------7. Methyl Chloride------------------------ t. Water-------------------------- S. Nonvolatile matter--------------- --- 10. Color, Pt-Co.--------------------------11, Appearance ............. ..... -....... 5 ppm., max. 2 ppm., max. 4 ppm., max. 0.4 ppm., max. 50 to 150 ppm. 2 ppm., max. 10 ppm., max. 10 ppm., max. 0.03% by wt,, max. 0.01% by wt., max. 20, max. Clear, free of suspended matter. Page 4 PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" UCC 084037 VINYL CHLORIDE MONOMER TEST METHODS 1. ACIDITY a) Solvent mixture Transfer 25 ml. of anhy<kous methanol to a glass-stoppered 500ml. volumetric flask containing approximately 250 ml. of ethylene dichloride and 15 ml. of a 0.1 per cent eolution of thymol blue indicator in methanol. Dilute to the mark with ad ditional ethylene dichloride,, stopper, and mix thoroughly. b) Procedure Introduce 100 ml. of the sol vent mixture into each of two 500-ml. glass-stoppered Erlenmeyer flasks by means of a suitable transfer graduate. c) Chill the solutions to approximately --10C. in a suitable cold bath. d) Neutralize each solution with standard 0.005 N alcoholic potassium hydroxide to an orange end point. e) Reserve one of the flasks as a blank. f) Into the other flask introduce 100 ml. of the chilled sample by means of a suit able chilled transfer graduate. Insert a small piece of paper between the stop per and flask to prevent build-up of pressure and swirl the contents of the flask gently. g) Remove the stopper and, using a 10-ml. buret, titrate with the standard 0.005 N potassium hydroxide to the same color as that of the blank, paragraph e. h) Caluclation A x 1.82 - acidity, ppm, as hydrochloric acid A - ml. of 0.005 normal KOH required for the titration 2. ACETYLENE a) Erlenmeyer flash, 250-ml., specially prepteed Pit with a one-hole rubber stopper. Insert a 3-ineh length of glass tubing into the hole and through the stopper so that approximately one-half of it extends above the top of the stopper. Attach 1.5 ft. of rubber tubing to the glass outlet tube. b) Cos scrubbing bottle Pit a widemouth pint bottle with a two-hole rubber stop per. Into one hole fit a fritted cylinder gas dispersion tube so that it extends to within 1/4 inch of the bottom of the bottle; into the second hole insert a short piece of glass tubing. C) llsovay's solution -- stock solutions Solution "A": Prepare by mixing the following: 200 ml. of 10% cupric nitrate, CuNOa * 3HjO; 80 ml. of 20% ammonium hydroxide, NHeOH (710 ml. of c.p. re agent grade NH4OH to 1000 ml.); 200 ml. of refined isopropanol, 91%; and 580 ml.of distilled water. Solution "B": 15 per cent by weight hydroxylamine hydrochloride Solution "C": 1.0 per cent by weight gelatin (Eastman Calfskin) d) Procedure CAUTION! Conduct the reaction part of the procedure under a suitable fume hood. Transfer 110 ml. of Solution "A", 40 ml. of Solution "B", and 10 ml. of Solution *`C" to each of the following containers: the gas scrubbing bottle and a 250-ml. glass-stoppered Erlen meyer flask. e) Reserve the solution in the flask as a blank. f) Chill the specially prepared 250-ml. Erlenmeyer flask, paragraph a, and in troduce 100 ml. of the chilled sample by means of a chilled 100-ml transfer graduate. Hake this trmsfer as quickly as possible. g) Stopper the flask with the stopper that is connected to the inlet tube of the gas scrubbing bottle by means of the rub ber tubing. h) Allow all of the sample to evaporate through the gas scrubbing bottle. PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" UCC 084038 Page VINYL CHLORIDE MONOMER i) Transfer portion of the sample and blank solution* to the respective 20-mm. cells of a Beckman Model B spectrophotometer and determine the absorbance of the sample solution at a wavelength of 540 millimicrons based on a reading of 0 for the blank. For a complete description of the instrument sad its operation refer to Beckman Bulletin 206-B. j) From the previously prepared calibration curve, paragraph m, read the ppm. of acetylene corresponding to the absorbonce of the sample at 540 millimicrons. Duplicate determinations must agree within 1 ppm. k) Calibration curve Prepare a series of acetylene standard* from 1 to 6 ppm., inclnsive, by adding known amounts of acetylene to acetylene-free vinyl chloride. l) Determine the absorbance for each of the synthetics by following the pro cedure given in paragraphs d to i, inclusive. m) Plot a calibration curve of absorbance versus ppm. acetylene using the values obtained in paragraph 1. 3. ALDEHYDES a) Fuchsia reagent Weigh 0.500 g. of Fuchain reagent (rosanilin hydro chloride) in a small weighing dish and transfer to a 1000-ml. volumetric flask containing 490 ml. of distilled water. Add 11 ml. of a satweted (at 25 C.) solution of sulfur dioxide in distilled water. Stopper the flask, mix well, and allow to stand overnight. At the end of this period dilute the contents of the flask to die mark with distilled water. Add approximately one g. of powdered activated carbon and mix until tbe solution is decolorized. Filter the solution by parity to remove the activated carbon. Ihe reagent should be clear and have no more than a trace amount of pink color. b) Standard aldehyde solution Accurately weigh 1.386 g. of acetaldehyde-ammo nia (Eastman Catalogue No. 560-T) in a small weighing dish and transfer to a 100-ml. volumetric flask containing 50 ml. of distilled water. By means of a biuet add 22.7 ml. of standard 1.0 N or 45.4 ml. of 0.5 N sulfuric acid, dilute to tbe mark with distilled water, and mix thoroughly. Allow the solution to stand overnight. Before use, verify the presence of acetaldehyde odor in the solution. This solution should be prepared fresh each time a new cali bration curve is prepared. c) Purity of primary standard Ihe purity of the primary standard should be determined each time a new standard aldehyde solution is prepared. Using a weighing dish, introduce 0.6 to 0.8 g. of the Eastman acetaldehyde-ammonia weighed to the nearest 0.1 mg. into each of two 500-ml. glass-stoppered Erlenmeyer flasks containing 50 ml. of distilled water and swirl to effect solution. Add 50 ml. of distilled water to a third flask and reserve as a blank. Pipet two ml. of 0.04 per cent solution of bromophenol blue indicator in metha nol into each sample and blank flask and carefully neutralize the contents to the indicator with standard 0.5 N aqueous hydrochloric acid. Add ex actly 5.0 ml. of the 0.5 N acid in ex cess. Pipet 50 ml. of 0.5 N aqueous hydroxylamine hydrochloride reagent into each flask and allow the flasks to . stand at room temperature for 60 min utes. Titrate the contents of each flask to a grayish-blue end point with stand ard 0.5 N aqueous sodium hydroxide. Calculation: (A-B)Nx 6.108 . g. acetaldehyde-ammonia - acetaldehyde-ammonia, % by weight A - ml. of N normal NaOH required for the sample. Pags 6 PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" UCC 084039 VINYL CHLORIDE MONOMER B ml. of N normal NaOH required for the blank. d) Procedure Assemble the apparatus as shown in Figure 1. NOTE: All equip ment used in the performance of this test must be cleaned with dichromate cleaning solution, rinsed with watdr, then methanol, and air-dried. The test must be performed under a flame-free fume hood and in an aldehyde-free room. e) Transfer 12 ml. of distilled water to each of six impingers. Insert the impinger tubes and place is beakers of wet ice as shown in Figure 1. Connect the rubber tubing between the impingers in such a manner as to have two aeries of three impingers. f) Using a graduate that has been pre viously chilled with solid carbon dioxide, introduce 100 ml. (100 g.) of the sample into each of two previously chilled 125-ml. flasks. g) Connect the sample flasks to respective series of three impinger tubes. Place a small piece of cork or wood under each flask and allow the sample to evaporate to dryness. h) When the samples have evaporated com pletely, disconnect the rubber tubing, and remove the impinger tubes. Allow the tubes to drain by touching the tips against the insides of the respective impingers. i) Prepare a blank for the reagent by add ing 20 ml. of distilled water to a 25-ml. glass-stoppered graduate. j) Pipet S ml. of the Fuchsia reagent into the blank. Stopper the container, mix thoroughly, and place in a water bath maintained at 25 0.5 C. for 35 1 2 minutes. k) Repeat step j with each sample im pinger, diluting it to 25 ml. with dis tilled water after the addition of Fuch sia reagent. Stopper, mix, and place each container in the water bath, noting its stsrting time, before adding reagent to the next one. This auto matically spaces the starting times approximately 2 minutes apart. l) Remove each container from the bath after 35 2 minutes, and transfer a portion of the solution to one of two matched one-cm. cells. Determine the Figure 1 assembly for aldehyde determination A - 125-ml. flask B~ Cork ring C - Glass tubing D - Rubber stopper G - Midget dust impinger, (Fisher 59, Cetalog No. 9-258A) E - Rubber tubing H - Dust impinger tube, (Fisher 59, Catalog No. 9-258B) F - Beakers for wet ice and large enough to hold two impingers. A minimum of duplicate sets of apparatus are required. PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" UCC 084040 p** 7 VINYL CHLORIDE MONOMER absorbance of each solution at 560 millimicrons using s Beckman Model B spectrophotomer and distilled water as the reference solution. Deduct the ab sorbance due to the blank from each of the sample solutions. ) Calculation A x- 1.222 - acetaldehyde, ppm. g. sample A - total mg. of acetaldehyde. Deter mine from the calibration curve, paragraph q, the mg. of acetalde hyde corresponding to the net ab sorbance due to the solution in each impinger. A the sum of these values. a) Calibration curve Pipet one ml. of the primary standard, paragraph b, into a 100-ml. volumetric flask containing 50 ml. of distilled water. Dilute to the mark with distilled water, stopper, and mix thoroughly. o) Prepare a series of standards by pipet ting 0, 0.5, 1.0, 1.5, 2.0, 3.0, 4.0, and 5.0 ml. of the diluted primary standard into respective 25-ml. glass-stoppered paduatea. These standards contain 0, 0.05, 0.10, 0.15, 0.20, 0.30, 0.40, and 0,50 mg. acetaldehyde, respectively, depending on the purity of the original acetaldehyde-ammonia. p) Dilute the contents of each graduate to the 20-ml. mark with distilled water and determine the absorbance of each standard as described in paragraphs j through 1. Deduct the absorbance of the zero standard from the absorbance of each of the standards to find the net . absorbance of the standards. 4 IRON a) Standard inn eolation Dissolve 0.2809 g. of ferrous ammonium sulfate, Fe(NH^)2(S04)2 * 6H2O, in 50ml. of dis tilled water contained in a 1000ml. glass-stoppered volumetric flask. Slow ly and with constant switling add 10 ml. of concentrated c.p. nitric acid and heat to boiling. Cool and dilute to the mark with distilled water. A 1.0-ml. aliquot of this dilution is equivalent to 0.4 ppm, iron, as Fe, when using a 100-ml. sample. b) Sodium acetate, 2 molar Dissolve 164 0.01 g. of c.p. sodium acetate in 1000 ml. of distilled water. c) Alcokol-umter eolation Measure 25 ml. of S.D.2-B alcohol into a 100-ml. glass- stoppered graduate containing 30 ml. of distilled water. Stopper and mix thoroughly. d) Procedure Transfer 25 ml. of the alco hol-water solution to a 250-ml. glass- stoppered Erlenmeyer flask. e) Into the flask introduce 100 ml. of the chilled sample by means of a suitable chilled transfer graduate. f) Gently swirl the contents of the flask, remove the stopper, and allow the vinyl chloride to evaporate under a fume hood. Swirl the flask to remove the last trace of vinyl chloride. g) Filter the remaining alcoholic solution through a Gooch crucible fitted to a 250-ml. filtering flask and connected to a suitable vacuum system. h) Quantitatively transfer the filtrate to one of two, 100-ml. glass-stoppered volumetric flasks, rinsing the filtering flask with five 5-ml. portions of dis tilled water. i) To the second volumetric flask add 25 ml. of the alcohol-water solution and introduce 1.0 ml. of the standard iron solution by means of a suitable meas uring pipet. Reserve as a blank. j) To each flask add 2 drops of concen trated c.p. hydrochloric acid and 2 drops of 0.1 per cent bromo-phenol blue indicator in ethanol. k) Add the 2 molar sodium acetate solution dropwise to each flask until each solu tion turns a faint blue. l) To each flask add 4.0 ml. of 10 per cent hydroxylamine hydrochloride solution in water and 10.0 ml. of 0.12 per cent solution of o-phenanthroline in water. PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" UCC 084041 VINYL CHLORIDE MONOMER tn) Dilute each solution to the mark with distilled water, stopper the flasks, and mix each thoroughly. n) Allow the solutions to stand at room temperature for at least 20 minutes. o) Transfer the sample and blank solutions to respective 100-ml. matched tail-form Nesaler tubes. p) Compare the colors of the sample and blank solutions visually in transmitted light. If the color of the sample is more reddish-orange than that of the blank, the iron content of the sample is in excess of 0.4 ppm., as Fe. 5. PHENOL a) Weigh 25 g. of the sample, chilled in a solid carbon dioxide-acetone mixture, to the nearest 0.1 g., into a chilled 100-ml. glass-stoppered volumetric flask. b) Place the flask in room temperature water and allow the' vinyl chloride to evapo- , rate under a fume hood. Do not agitate until nearly dry and then do so to drive off any remaining vinyl chloride. c) Allow the flask to warm to room tempera ture and dilute to the mark with metha nol, specification 1-6A1-1.1 or equiv alent. Stopper the flask and mix thoroughly. d) Introduce 20 ml. of this dilution into a second 100-ml. glass-stoppered volu metric flask by means of a suitable transfer pipet and dilute to the mark with additional methanol. Stopper and mix thoroughly. e) Determine the ultraviolet absorbance on a portion of this dilution using a Beck man Model DU spectrophotometer, a wavelength near 271 millimicrons, and 1.00-cm. silica cells. f) Prepare a series of synthetic samples containing from 5 to 30 ppm. phenol in anhydrous methanol and determine the absorbance of each as described in paragraph e using methanol as a blank. g) Plot the absorbance of the synthetic samples against their respective con centrations. h) Using the absorbance value obtained, pamgtph e, determine the phenol con tent of the sample by reading from the calibration curve, paragraph g, and cal culating as.follows: i) Calculation C x 20 phenol, ppm., in original sample C ppm. phenol obtained from curve, paragraph g j) Note: Nonvolatile aromatics, i.e., hydroquinone and diphenylamine, will inter fere with this determination. 6. ETHYLENE AND METHYL CHLORIDE a) Sample handling and special precautions All samples must be taken from a liquid sampling point into evacuated cylinders to prevent fractionation and loss of the more volatile components. Fill the cylinder to approximately 90 per cent of capacity, and drain off 10 per cent from the liquid phase to pre vent possible rupture of the cylinder. Equip the gas handling system of the gas chromato^aph with a conven tional vacuum system as described in 58C-9C1-V6.3. b) Instrument parameters Instrument -- Beckman GC 2A Gas Chromatograph or equivalent Recorder -- Brown, M mv., with integrator from Disc Instruments, Inc. Column -- 25-ft, 1/4-inch O.D. tubing packed with 25 per cent hexadecane on 60 to 80 mesh Chromosorb W Column temperature -- room tempera ture (25 C.) Eluting gas -- helium Pressure -- 35 poig Flow (measured at outlet at room tem perature)-- 100 c.c, per minute. Filament current -- 300 ma Sample volume -- 10 c.c. (gas) Total elution time -- 20 minutes PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" UCC 084042 Page VINYL CHLORIDE MONOMER e) Report the concentrations of the various components as part* per million on a peak area basis. 7. WATER ) Transfer 50 ml. of anhydrous methanol to each of two dry 250-ml. glass-stop' pered Erlenmeyer flasks. b) Titrate the contents of each flask with SO2-I2 reagent to the same light red dish-brown color. Chill the solution to approximately --10C. in a suitable cold bath. c) Reserve one of the flasks as a blank. d) Into the second flask introduce 50 ml. (50 g.) of the chilled sample by means of a suitable chilled transfer graduate. e) Titrate immediately with the SO2-I2 re agent until the color matches that of the blank. f) Calculation *"50 " w*ter * by weight A ml. of SO2-I2 required for the sam ple P * factor, g. of water equivalent to 100 ml. of reagent S. NONVOLATILE MATTER a) Heat a 125-ml. platinum evaporating dish to constant weight at 105 to 110C., cool in a desiccator, and weigh to the nearest 0.1 mg. b) Introduce 100 ml. of the chilled sample measured from a chilled graduate. c) Evaporate the sample to dryness at room temperature under a fume hood. d) Place the dish in an oven maintained at 105 to 110C. for 30 minutes or until constant weight is attained, o) Cool the dish in a desiccator and weigh to the nearest 0.1 mg. The difference in weight is the g, residue., f) Calculation g. residue - nonvolatile matter, X by weight 9. COLOR a) Chill one of two matched tail-form Nessler tabes. Add 100 ml. of the chilled sample to the chilled tube. b) Fill the second tube to the mark with the platinum-cobalt standard representing tbe maximum limit permitted by the specification. c) Compare the colors of the sample and v the standard by viewing vertically down through the tubes against a white background. d) Tbe color of the sample should not be darker than that of tbe standard. Re serve tbe sample for visual examina tion in Section 10. 10. APPEARANCE a) Examine tbe tail-form Nessler tube con taining sample, naed in Section 9, for the presence of haze-producing poly mer and/or suspended matter. Pngs 10 CELLOSIZE and TERGITOL are trade marks of Union Carbide Corporation. PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" XJCC 084041 J VINYL CHLORIDE MONOMER SOLUBILITY OF VINYL CHLORIDE IN WATER AT VARIOUS TEMPERATURES SOLUBILITY OF WATER IN VINYL CHLORIDE AT VARIOUS TEMPERATURES AT SATURATION PRESSURE WATER .PER CENT BY WEIGHT TEMPERATURE ,*C. PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" ucc 084044 Pg ll VINYL CHLORIDE MONOMER YAPOR PRESSURE OF VINYL CHLORIDE AT VARIOUS TEMPERATURES 10.000 9.000 8.000 7.000 6.0000 5.000 4.000 3.000 2.000 PRESSURE 1,000 900 800 700 600 500 Zz X (0 400 300 200 100 -60 -50 -40 -30 -20 -10 O 10 20 40 60 80 100 120 PRIVILEGED AND "CONFIDENTIAL MATERIAL SUBJECT TO PROTECTIVE ORDER" Mated in UiLA. TEMPERATURE, C UNION CARBIDE CHEMICALS COMPANY DIVISION or UNION CAMIDE COWOftATION 270 Puk Avomio, Now York 17, N. Y. UCC 084045 F-40S40