Document MGMEYp14vmp6ORNeQvj06L2Ly

1-184 (SOM) INTER OFFICE MEMO TENNECO CHEMICALS, INC. To M.W. Williams Vroh h.B. Carr subject Laboratory Methods at Plemington at Burlington [ay H, 1972 Copy to, Two (2) sets of analytical test methods are attached for trans mittal to. the Piscataway and Pasadena R&D locations. These sets include: 1. Manual entitled Tenneco Analytical and Physical Testing Man ual. (This manual includes written procedures from both the Plemington and Burlington Analytical and Physical Testing Laboratories.) .. * ' 2. Test Methods - Burlington ' 2. Test Methods - Flemington Referring to 2. and 2* above, not all of our test procedures are in a written format. These methods are listed in the attached Table I. Should other R&D locations have interest in either our Compound Plant or Resin Plant Quality Control Manual or in the Plemington Analysis and Evaluations Group's physical testing capability, these will be available upon request. Attachments (2). HBC/jt H.B. Carr COXiORITE 014564 TENNECO INTERMEDIATES DIVISION TENNECO CHEMICALS, INC. ANALYTICAL AND PHYSICAL TESTING MANUAL This manual, is made up in two (2) sections: 1. T.A.M. (Tenneco Analytical Method) 2. T.P.M. (Tenneco Physical Test Method) The T.A.M. section will consist of all cjiemical'test methods includ ing methods requiring chemical preparation (e.g., gas chromatography, IR and UV), while the T.P.M. section will contain all methods requir ing physical testing only. The following numbering system will be used: 1-199 200-299 300-399 , 400-499 500-599 600-699 900-999 Raw Materials Testing Homopolymer Testing Copolymer Testing Dispersion Resin Testing Flexible Compound Testing Rigid Compound Testing General Test Methods Both the T.A.M. and T.P.M. sections are made up In this order. The Raw Materials Testing (1-199) numbering system is arranged as fol lows : 1-9 10-19 20-29 30-39 40-49 50-59 60-69 70-79 . 80-89 90-99 100-109 Polymerization Raw Materials Postpolymerization Raw Materials Resins (including modifiers). Processing Aids Plasticizers Stabilizers (including antioxidants, UV) Lubricants Fillers Pigments Dyes Solvents Effluent Plant Raw Materials Numbers 110-199 are reserved for future raw material test methods. COLORXTE 0X4565 The T.A.M. and T.P.M. numbers and individual methods will be is sued by A&E, Flemington. The methods will have the following format: The heading will show T.A.M. or T.P.M. number, issue date and specific use (location of the laboratory the method is to be used). The method text will be broken up into sections start ing with: 1. Application 2. Apparatus 3- Reagents 4. Special Instructions (column prepration, etc.) 5. Conditions (instrument conditions). ' 6. Standardization 7. Procedure 8. Calculation The Divisional Test Method Manuals will be issued to the Manager of Flemington R&d, Supervisor of Quality Control, laboratory super visors and the laboratories. The laboratory manuals will only con tain the copies of test methods applicable to the individual lab oratory location. H.B. Carr, Supervisor Quality Control COLOR!TE 014566 TENNECO CIIEMICAIS, INC. TENNECO PLASTICS DIVISION Appendix No. 1 T.A.M. 900-1 Specific Use: Date Issued: Burlington, Flemington October, 1971 DETERMINATION OF TRACE AMOUNTS OF MERCURY BY FLAMELESS ATOMIC ABSORPTION SPECTROPHOTOMETRY APPLICATION: This is a rapid, accurate and very sensitive method for the " determination of extremely low levels of mercury contaminations down to 1.0 part per billion. The method has been developed to determine the mercury emission levels in the Burlington and Flemington plant effluents. APPARATUS: 1. Perkin Elmer Atomic Absorption Spectrophotometer Model 303, or equivalent, equipped with null meter to read percent absorption. : 2. Hollow-Cathode Mercury Lamp, Perkin Elmer, Catalog No. 303-6044, or equivalent. 3. Absorption Cell, cylindrical, borosilicate glass, 100 mm path, 22 mm O.D., Perkin Elmer, Catalog No. 990-2704, with two ground joints, or equivalent. 4. Nesbitt Absorption Bulb, Corning 1900. 3. Air Pump, Neptune Dyna., Model 2. 6. Gas Washing Bottle, 125 ml with extra-coarse fitted bubbler. Corning 31770 (125 EC), or equivalent. The bottle has a calibration line drawn at 60 ml volume. 7- Tygon Tubing 5mm I.D. for connections. 8. 3-way stopcock with plug of Teflon, Corning 7382, or equivalent'. REAGENTS i 1. Sulphuric Acid (HS04) 1:4 (Caution: * Wear Goggles) Add slowly, with stirring, 200 ml of cone. 96^ reagent grade H2S04 to 800 ml of distilled water. This solution is dispensed from an automatic burette. COLORITE 014567 T.A.M. 5-1 Page 2 2. Potassium permenganate (KMn04) solution, 4$ W/V Weigh 40 grams of reagent grade KMn04 into a. 150 ml tall beaker. Add approximately 70 ml of distilled water and stir for about 20 seconds. Allow the KMn04 crystals to settle, then decant the supernatant liquor into a 1000 ml volumetric flask. Repeat the operations of dis solving and decanting until all the KMn04 has dissolved. Dilute to 1000 ml, mix and store in a brown bottle. ' 3- Hydroxylamine hydrochloride (NHgOH-HCl) solution, 10$ ttf/V Dissolve 20 grams of reagent grade hydroxylamine hydrochloride in 100 ml of distilled water. This reagent is dispensed from a dropping bottle. 4. Stannous Chloride (SnCl2-2Hg0) Solution 10$ W/V Dissolve 20 g. of reagent grade Stannous chloride in 40 ml of warm concentrated hydrochloric acid. When all the stannous chloride has dissolved, add 160 ml of distilled water, mix and store in a 250 ml reagent bottle. 5. Mercury Standard Stock Solution, 1000 ppm Dissolve 1.080 g. of mercuric oxide, HgO, in a. minimum volume of 50$ HC1. Dilute to 1 litter with deionized water. This solution will have 1000 jag/ml mercury or 1000 ppm. 6. Mercury Standard Solution, 100 ppm Transfer by pipette 25 ml of the 1000 ppm mercury stock solution into a 250 ml volumetric flask and dilute to volume with deionized water. Each ml solution is equivalent to 100 Wg Hg. 7- Mercury Standard Solution, 10 ppm Transfer by pipette 25 ml of the 100 ppm mercury standard into a 250 ml volumetric flask and dilute to volume with deionized water. Each ml of solution is equivalent to 10 /ig Hg. 8. Mercury Standard Solution, 1 ppm Transfer by pipette 25 ml of the 10 ppm mercury standard into a 250 ml volumetric flask and dilute to volume with deionized water. Each ml is equivalent to 1 pig Hg. This standard is prepared fresh every time mercury samples are to be run. COLORITE 014568 T.A.M. 5-1 Page 3 PROCEDURE I. Sample Preparation All forms of mercury (i.e. metallic, organic, sulphide, oxide, etc.) in the sample are oxidized with acidic permanganate to mercuric mercury. 1. Mix the sample thoroughly and immediately pipette 50 ml into a 100 ml beaker. 2. Add 1 ml of the 1:4.H2S04 and 1 ml of the 4$ KMn04 from automatic burettes and cover the beaker with a watch glass. 3- Boil for a few seconds, allow to cool and destroy the excess KMn04 by adding a few drops' of 10$ hydroxylamine. . hydrochloride solution until the solution is colorless... 4. Aerate the samples along with standards as described in the aeration procedure. II. Calibration Standards 1. A series of at least three standards are prepared fresh each time the instrument is operated. ... 2. Dilute each standard with deionized water until it is of the same volume as the sample. 3. Add 1 ml of 1:4 H2S04 and 1 ml of 4$ KMn04 from the automatic burettes and cover the beaker with watch glass. 4. Boil the solution for a few seconds, allow to cool and destroy the excess pumanganate by adding a few drops of 10$ hydroxylamine hydroxylamine hydrochloride until the solution is colorless. III. 5. Aerate the standard solutions as described in the aeration procedure. Instrument Conditions The Perkin Elmer 303 apparatus is set-up.using the following condition: Lamp current: Wave length: Slit width: Scale: Noise suppression: 10 MA 2537 A 5 IX 0 UV COLORITE 014569 T.A.M. 5-1 Page 4 IV. Aeration Procedure 1. Connect the apparatus to the Atomic Absorption Spectro photometer using Tygon tubing of 5 mm I.D. and adjust the flow rate of air through the system to give a steady bubbling in the washing bottle. 2. Allow the system to stabilize with the three way stopcock in the bypass position with an empty gas washing bottle connected to the apparatus. 4. 3. Wash the sample or standard into the gas washing bottle and make up the 60 ml mark on the bottle with distilled water. 4. Add 2 ml of 10$ SnCl2*2H0 and immediately connect the^ bottle with the aeration system and notice the mercury, absorption on the null meter. 5. Record the peak of highest abosrption on the null meter. 6. After the sample is completed air is passed through the line to bleed all traces of mercury out; i.e., until a zero reading is observed on the null meter. CALCULATION 1. Convert the results of absorption obtained into absorbance from the tables provided with the instrument. 2. A standard curve is plotted from the values of standard solutions absorbance against concentrations. 3. The samples absorbance figures are read off the curve to find the corresponding mercury concentrations. Written By: Y. B. Hanna Issued By: H. B. Carr, Manager Quality Control COLORITE 0X4570 TABLE I FLEMINGTON AND BURLINGTON TEST METHODS TEST METHODS - FLEMINGTON A. Analytical Testing 1. Instrumental Gas chromatography procedure for the identification of plasticizers and plasticizer mixtures Preparation of IR samples suitable for analysis by cast films, nujol mulls, KBr pellets and liquids Atomic absorption methods for the determination of the following elements: aluminum, barium, calcium, cadmium, copper, iron, magnesium, lead, antimony, sili con, tin, titanium and zinc 2. Wet Chemical Analyses Separation scheme for vinyl compounds Chlorine analysis, Schoniger oxygen flask method Elemental tests for the presence of chlorine, sulfur, phosphorus and nitrogen Extraction procedures for the separa tion of soaps from vinyl resins Ashing and wet methods for the prepa ration of solutions suitable for atomic absorption analysis Reference Developed It ft ft rt ft n M TEST METHODS - BURLINGTON A. Analytical Testing 1. Instrumental * a. Wet Instrumental Analyses Peroxides in VCM (limited to high peroxide level) ! Trace oxygen in VCM Phenol in RVCM-VAcM Bound vinyl acetate in Copolymer Identification of raw materials by, IR TAM 1-4 TAM 1-5 TAM 1-7 TAM 500-1 IR Library COLORITE 0X4571 2 Wet Instrumental Analysis (cont* d.) Reference pH of latex QC TM 2-14 pH of plasticizers Developed Iron in water Hach Colorimeter Copper in water o-Phosphate in water Phenol in water Nitrogen,, ammonia in water Dissolved oxygen (DO) in water COD BOD b. Gas Chromatographic Analyses Light end impurities in VCM Heavy end impurities in VCM Acetylene in VCM VAcM and TCE in VCM Residual lauryl alcohol in polymer Residual tridecanol in polymer Residual octadecene-1 In polymer TAM 1-1 TAM 1-2 TAM 1-8 QC TM 4-104 TAM 2-1 Developed I! It Residual VAcM in Copolymer tv DOP in Plastisol paste or compound Plasticizer in compound Phenol in RVCM-VAcM Impurities in VAcm Residual VCM in latex (Total and Surface) VCM/propylene ratio % Impurities in plasticizers (DOP, DIDP, DTDP, NODP, TIOTM, DOA, HB-40, DNODP) .2 Wet Chemical Analyses Fatty alcohol sulfate in sodium lauryl sulfate TAM 3-1 Fatty alcohol sulfate in latex, filter vat effluent, dried Plastisol, Ef fluent Plant water TAM 3-2 Assay and A(0) of 223M TAM 4-1 COLORITE 0X4572 5 Wet Chemical Analyses (contJd.) Assay and A(0) of lauroyl peroxide Assay of ammonium persulfate Acidity of various raw materials Alkalinity of various raw materials Peroxides in compressor solids Assay of sulfuric acid Reference QC TM 3-51 USP Modified QC TM 3-15 TAM 100-11 COLORITE 014573