Document 4Qan9ZDzEo77nVmx8npjaBYZV

4 90 Jlt'J INTER-OFFICE MEMO TENNECO CHEMICALS,INC. To H. Johnson J. P. Sandstedt Subject VCM Analytical Procedures ai Piscataway at Piscataway D-;l December 23, 1980 Cot. to Dr. R. T. Gottesmai: w/o Mr, I. Wakeman The Environmental Protection Agency has proposed to revise its test methods for vinyl chloride. Attached please find copy of this pro posal. As you are aware Tenneco Chemicals currently uses TCI analytical procedures to accomplish these analyses. While I recognize that this proposal probably does not effect our operations, I would appreciate your careful review of the proposal, comparing it with TCI methods and, if necessary, the original EPA methods. The comment period is due to close January 19, 1981. Therefore, I would request your earliest possible consideration of these methods. JPS:ch Att. COLOR!TE 017074 Tuesday November 18, 1980 Part 11 Environmental Protection Agency Kationad Emission Standards for hazardous Air Pottutants COLORITE 017075 7*346 Peduml Rugfoter f Vol 45. No. 224 / Tuesday. November 18,1980 / Proposed Rules ENVIRONMENTAL PROTECTION AGENCY because the revisions are minor and technical. These revisions are issued under the authority of Section 114 of the different column or GC/mass spectroscopy, and has the data available for review by the 40 CFR Part 61 Clean Air Act as amended (42 U.S.C. 7414) Administrator. 4. Apparatus JAP-ERL 1563-11 National Emission Standard* for Hazardous Air Pollutant* agency: Environmental Protection Agency (EPA). action: Proposed rule. SUMMARY: On June 7.1077 (42 FR 29005) the Administrator promulgated amendments to the national emission standards for the hazardous ait pollutant vinyl chloride. The Administrator also promulgated amendment* to Appendix B--Test Methods, of this pari. Since the promulgation of Method 106-- Determination of Vinyl Chloride from Stationary Source* and Method 107. Determination of Vinyl Chloride Content of Inproces* Wastewater Samples and Vinyl Chloride Content of Polyvinyl Ottoride Resin, Slurry. Wet Cake, and Latex Samples, several improvements in the methods have been developedThese revisions incorporate those improvements. Dated. November 10.1060 Douglas Goalie. Administrator 40 CFR Part 61 is amended by revising 4.1 Sampling (see Figure 106-1). The sampling train consists of the folWmi; components: 4.1.1 Probe. Stainless steel. Pyrex glass, or Teflon tubing (as stack Test Methods 106 and 107 of Appendix B temperature permits) equipped with s to read as follows: glass wool plug to remove particulate Appendix B--Teat Methods *** \ matter. 4.1.2 Sample Lines. Teflon. 6.4 mm outside diameter, of sufficient length to Method 106--Determination bf Vinyl connect probe to bag. Use a new unused Chloride From Stationary Sources Introduction 1 piece for each series of bag samples that constitutes an emission test, and discard upon completion of the test. Performance of this method should 4.1.3 Quick Connects. Stainless steel, not be attempted by persons unfamiliar male (2) and female (2|. with ball checks with the operation of a gas (one pair without), located as shown in chromatograph, nor by those who are Figure 106-1. unfamiliar with source sampling, 4.1.4 Tedlar Bags. 50- to 10O-litei because knowledge beyond the scope of capacity, to contain sample. Aluminized this presentation is required. Care must - Mylar bags may be used if the samples be exercised to prevent exposure of are analyzed within 24 hours of sampling personnel to vinyl chloride, a carcinogen. collection- 1. Appicability and Principle, 1.1 Applicability. The method is applicable to the measurement of vinyl OATES: Comment* must be received by chloride in stack gases from ethylene January 19.1981. dichloride, vinyl chloride, and polyvinyl A0ORESSES: Comments should be ubmitted (in duplicate if possible) to: Central Docket Section (A-130). Attention: Docket No. A-00-50, U.S. chloride manufacturing processes. The method does not measure vinyl chloride contained in particulate matter. ( 1.2 Principle. An integrated bag Environmental Protection Agency. 401 M sample of stack gas containing vinyl Street S.W- Washington. DC 20460. chloride (chloroethene) is subjected to KW FURTHER INFORMATION CONTACT; gas chromatographic JGC) analysis Roger Shigehara. Emission Measurement using s Game ionization detector (FID). Brandi (MD-19), US, Environmental 2. Range and Sensitivity. .Protection Agency, Research Triangle ';. This method is designed for the 0.1 to Park, N.C 27711; telephone number(919) ' SO ppm range. However, common GC MI-2237. Instruments are capable of detecting 0.02 UtotEMEMTAItY REFORMATION: These revised procedures differ bom the girevious methods as follows: Method 106--(1) sample hag size can range from 50 to 100 liters rather than the single size hag previously required, and (2) analysis audit and chromatograph with resolution quality assurance requirements are added. These requirements are contained in Appendix ' C 40 CFR Part 61, a* proposed with the National Emission Standard for Benzene Emissions from Maleic Anhydride Plant* (45 PR 26060). Method 107--(1) a head apace vial pre-pressurizer is added to obtain correct head apace gas equilibrium. (2) different chromatograph columns are suggested for analysis, and (3) chromatorgraph resolution quality ppm vinyl chloride. With proper calibration, the upper limit may be. . extended as needed. _.. - 8. Interferences. :'* The chromatographic column* and the corresponding operating parameters herein described normally provide an adequate resolution of vinyl chloride; however, resolution interfere!^** may : r he encountered on some sources- . Therefore, the chromatograph operator -shall select the column and operating ,, parameters best suited to his particular , analysis requirements, subject to the approval of the Administrator. Approval is automatic, provided that the tester - r, produce* confirming dat* through an adequate supplemental analytical technique, such as analysis wiR a ~ .Assurance requirements are added. ^- The Administrator finds that notice And public procedure ts unnecessary M asnUtut* winnawni bjr lb* US.;.~ s EurWon--mt FroUclio* AaRny. '*7 ' ,. w '~ ''MV COLORITE 017076 COLORITE 017077 11 COLORITE 017078 Federal Register / Vol. 45, No. 224 / Tuesday, November 18, 1980 / Proposed Rules 4.1.5Bag Containers. Rigid leakproof The combined columns should be must have been affixed to the cylii),! " containers for sample bags, with operated at 120*C before shipment from the gas covering to protect contents from 4.3.3 Flow Meters (2). Rotameter manufacturer to the buyer. sunlight. type, 100-ml/min capacity, with flow 5.27 Nitrogen. Zero grade, tor 4.1-6 Needle Valve. To adjust sample control Valves. preparation of standard gas mixtures flow rates. 4.1.7 Pump. Leak-free, with minimum of 2-liter/min capacity. 4.1.8 Charcoal Tube, To prevent admission of vinyl chloride, and other organics to the atmosphere in the 4.3.4 Gas'Regulators. For required jjas cylinders. 4.3.'5 Thermometer. Accurate to l'C. 1o measure temperature of heated aample loop at time of sample injection. 4.3.6 Barometer. Accurate to 5 mm described in Section 7.1. 57.3 Cylinder Standards (3) mixture standards (50-, 10-, and 5-ppm vinyl chloride in nitrogen cylinders) The tester may use cylinder stands ids k> directly prepare a chromatograph vicinity of samplers. 4.1.9 Flow Meter. For observing sampling flow rate; capable of measuring a flow range from 0.10 to 1.00 liler/min. 4.1.10 Connecting Tubing. Teflon. 6.4-mm outside diameter, to assemble sampling train (Figure 106-1), 4.2 Sample Recovery. Teflon tubing. 6.4-mm outside diameter, to connect bag to gas chromatograph sample loop for sample recovery. Use a new unused piece for each series of bag samples that constitutes an emission test, and discard upon conclusion of analysis of those bags. 4.3 Analysis. The following equipment fa) required: 4.3.1 Gas Chromatograph. With FID, potentiometric strip chart recorder and 1.0- to 5.0-ml heated aampling loop in automatic aample valve. The chromatographic system shall be capable of producing a response to 0.1ppm vinyl chloride that is at least as great as the average noise level. (Response is measured from the average value of the base line to the maximum of the waveform, while standard operating conditions are in use.) 4.37 Chromatographic Columns. Columns as listed below. The analyst may use other columns provided that the precision and accuracy of the analysis of vinyl chloride standards are sot impaired and be has available for review information confirming that there is adequate resolution of the vinyl chloride peak. (Adequate resolution Is defined as an area overlap of not more than 10 percent of the vinyl chloride Hg, to measure atmospheric pressure around gas chromatograph during ample analysis. 4.3.7 Pump. Leak-free, with minimum of 100-ml/min capacity. 4.3.6 Recorder. Strip chart type, optionally equipped with either disc or electronic integrator. 4.3.9 Planimeter. Optional, In place of disc oh electronic integrator on recorder, to measure chromatograph peak areas. 4.4 Calibration. Sections 4.4.2 through 4.4.4 are for the optional procedure in Section 7.1. 4.4.1 Tubing. Teflon. 6.4-mm outside diameter, separate pieces marked for each calibration concentration. 4.47 Tedlar Bags. Sixteen-inchsquare sire, with valve: separate bag marked for each calibration . concentration. 4.4J Syringes. 0.5-ml and 50-iil. gas tight, individually calibrated to dispense gaseous vinyl chloride. 4.4.4 Dry Gas Meter, With Temperature and Pressure Gauges. Singer model DTM-115 with 802 index, or equivalent to meter nitrogen in preparation of standard gas mixtures, calibrated at the flowrate used to prepare standards. 6. Reagents. Use only reagents that are of diromatograph grade. 57 Analysis. The fallowing ore required for analysis. 6.17 Helium or Nitragen-'Zero grade, far chromatographic carrier gas. 6.17 Hydrogen. Zero grade. 6.1.3 Oxygen or Air. Zero grade, as required by the detector. calibration curve as described if Seriio" 777, If the following conditions mu mm (a) The manufacturer certifies the gas composition with an accuracy of 3 percent or better (see Section 57.3,1), (L>) The manufacturer recommends a maximum shelf life over which the gas concentration does not change by greater than 5 percent from the certified value: (c) The manufacture) affixes the date of gas cylinder preparation, certified vinyl chloi ids concentration, and recommended maximum shelf life to the cylinder before shipment to the buyer. 67.3.1 Cylinder Standards Certification. The manufacture; t-l.r.ll certify the concentration of vinyl chloride in nitrogen in each cylinder t>> (a) directly analyzing each cylinder and (b) calibrating his analytical procrdui r on the day of cylinder analysis. To calibrate his analytical procedure, the manufacturer shall use. as a minimum .< three-point calibration curve. It is recommended that the manufacture) maintain (1) a high-concentration calibration standard (between 50 and 100 ppm) to prepare his calibration curve by an appropriate dilution technique and (2) a low-concentration calibration standard (between 5 and 10 ppm) to verily the dilution technique use. If the difference between the apparent concentration read from the calibration curve and the true concentration resigned to the lowconcentration calibration standere exceeds 5 percent of the true concentration, the manufacturer shall determine the source of error and correct it, then repeat the three-point peak by an interfered peak. Calculation 67 Calibration. Use one of the Calibration. of area overlap is explained in following options: either. 67.1 and577. 67.37 Verification of Manufacturer's Appendix C. Supplement A f5i,3. Calibration Standards. Before using n "Determination of Adequate - 47.1 Vinyl Chloride. Pure vinyl standard, the manufacturer shall verify Chromatographic Peak Resolution.*) chloride gas certified by the - each calibration standard (a) by 4J77 Column A. Stainless steel 2D manufacturer to contain a mimimum of comparing It to gat mixtures prepared m by 3.2 mm, containing BO/lOO-mesh BSD percent vinyl chloride, for use in the (with 99 Mol precent vinyl chloride) in Chromasorb 102. preparation of standard gas mixtures in accordance with the procedure 4.3.2.2 Column B. Stainless steel. 2D Section 7.1. If the gas manufacturer described in Section 77 or (b) by having m by 3-2 mm. containing 20 percent GE . maintains a bulk cylinder supply of it analyzed by the National Bureau of SF-96 on 60/80-mesh Chromasorb P BBD-t- percent vinyl chloride, the Standards. The agreement between the AW; or stainless steel ID m by 3-2 mm - certification analysis may have been Initially determined concentration value containing B0/l00-meth Porapak T. performed on this supply rather than on and the verification concentration value Column B is required as a secondary each gas cylinder prepared from this must be within S percent. The column if acetaldehyde la present o . bulk supply. The date of gas cylinder .manufacturer must reverify oil used, column B Is placed after columnA. preparation and the certified analysis calibration standards on a time interval COLORITE 017079 76350 Federal Register / Vol. 45. No. 224 ) Tuesday. November 16. 1060 l Proposed Rules consistent with the shelf life of the cylinder standards sold. 6.2.4 Audit Cylinder Standards (2). Gas mixture standards with concentrations known only to the person supervising the analysis of samples. The audit cylinder standards shall be identically prepared as those in Section 5.2.3 (Vinyl chloride in nitrogen cylinders). The concentrations of the audit cylinders should be: one low- concentration cylinder in the range of 5 of 20 ppm vinyl chloride, and one highconcentration cylinder in the range of 20 to SO ppm. When available, the tester may obtain audit cylinders by contacting: Environmental Protection Agency. Environmental Monitoring ' Systems Laboratory. Quality Assurance Division (MD-77). Research Triangle Park. North Carolina 27711. If audit cylinders are not available at the Enviromental Protection Agency, the tester must secure an alternative source. 6.Procedure. 6.1 Sampling. Assemble the sample train as shown in Figure 106-1. Perform e bag leak check according to Section 7.3.2. |oin the quick connects as Illustrated, and determine that all connections between the bag and'the probe are tight. Place the end of the probe at the centroid of the stack and Start the pump with the needle value adjusted to yield of flow that will Till over 60 percent of bag volume In the specified sample period. After allowing sufficient time to purge the line several times, connect the vacuum line to the bag and evacuate the bag until the rotameter indicates no flow. Then reposition the sample and vacuum lines and begin the actual sampling, keeping the rate proprotional to the slack velocity. At all times, direct the gas exiting the rotameter away from sampling personnel. At the end of the ample period, abut off the pump, disconnect the sample line from the bag. and disconnect the veccuum line from the bag container. Protect the bag container from sunlight. 62 Sample Storage. Keep the sample bags out of direct sunlight. When at all possible, analysis is to be performed within 24 hours, but in no case In axoeas of 72 hours of sample collection. Aluminized Mylar bag samples must be analyzed within 24 hours. 6.3 Sample Recovery. With a new piece of Teflon tubing identified tor that bag. connect a bag Inlet valve to the gas chromatograph sample valve. Switch the valve to receive ges from the bag through the sample loop. Arrange the equipment so the sample gas passes from the sample value to 100-ml/min rotameter with flow control valve followed by a charcoal tube and a 1-In. H.O pressure gauge. The tester may 7.1 Preparation of Vinyl Chloride maintain the aample flow either by a Standard Cat Mixtures. (Optional vacuum pump or container Procedure--delete if cylinder standards pressurization if the collection bag are used.) Assemble the spparatus remains in the rigid container- After shown in Figure 106-2. Evacuate a 16- aample loop purging is ceased, allow the inch-square Tedlar bag that has passed pressure gauge to return to zero before a leak check (described in Section 7.3.2) activating the gas sampling valve. and meter in 5.0 liters of nitrogen. While 6.4 Analysis. Set the column the bag is filling, use the 0.5-ml syringe temperature to 100'C and the detector to inject 250 pi of 99.9-1- percent vinyl temperature to 150*G When optimum chloride gas through the wall of the bag. hydrogen and oxygen flow rates have Upon withdrawing the syringe, been determined, verify and maintain immediately cover the resulting hold these flow rates during all with a piece of adhesive tape. The bag chromatograph operations. Using zero now contains a vinyl chloride helium or nitrogen as the carrier gas. concentration of 50 ppm. In a like establish a flow rate in the range manner use the 50 pi syringe to prepare consistent with the manufacturer's gas mixtures having 10- and 5-ppm vinyl requirements for satisfactory detector chloride concentrations. Place each bag operation. A flow rate of approximately on a smooth surface and alternately 40 ml/min should produce adequate depress opposite aides of the bag 50 separations. Observe the base line times to further mix the gases, these gas periodically and determine that the mixture standards may be used for 10 noise level has stabilized and that base days from the date of preparation, after line drift has ceased Purge the aample which time new gas mixtures must be loop for 30 aeoonds at the rate of 100 ml/ prepared. (Caution: Contamination may min. then activate the aample valve. be a problem when a bag is reused if the Record the injection time (the position of new gas mixture standard is a lower the pen on the chart at the time of concentration than the previous gas sample injection), sample number, mixture standard.) aample loop temperature, column temperature, carrier gas flow rate, chart speed, and attenuator setting. Record the barometric pressure. From the chart, note the peak having the retention time corresponding to vinyl chloride, as determined in Section 7-2.1. Measure the vinyl chloride peak area. A., by use of a disc integrator, electronic integrator, or a planimeter. Measure and record the peak height. H. Record A_ and the retention time.-Repeat the injection at 72 Calibration. 7.2.1 Determination of Vinyl Chloride Retention Time. (This section can be performed simultaneously with Section 72.2.) Establish chromatograph conditions identical with those in Section 6.4 above. Determine proper attenuator position. Flush the sampling ' loop with zero helium or nitrogen and activate the sample valve. Record the injection time, sample loop temperature, least two times or until two consecutive column temperature, carrier gas flow values far the total area of the vinyl rote, chart speed, and attenuator setting. chloride peak do not vary more than 5 Record peaks and detector responses percent Use the average value for these that occur in the absence of vinyl two tofal areas to compute the bqg concentration. , chloride. Maintain conditions with the 'equipment plumbing arranged Compare the ratio of H. to A for the identically to Section 6.3. and flush the vinyl chloride aample with the same sample loop for 30 seconds st the rate of ratio Jbr the standard peak that is 100 ml/min with lone of the vinyl closest in height. If these ratios differ by chloride calibration mixtures. Then more than 10 percent, the vinyl chloride activate the sample valve. Record the peak may not be pure (possibly injection time. Select the peak that acetaldehyde is present) and the corresponds to vinyl chloride. Measure secondary column should be employed the distance on the chart bom the (tee Section 4.9 J 7). injection time to die time at which the 62 Determination of Bag Water peak maximum occurs. This quantity Vapor Content. Measure the amhient divided by the chart speed is defined as temperature and barometric pressure . the retention time. Since other organics near the bog. From a water saturation rosy be present in the sample, positive vapor pressure table, determine and Idantiflcation of the vinyl chloride peak record the water vapor content'of the must be made. bag as decimal figure. (Assume the 7X2 lYeparation of Chromatograph relative humidify to be 400 percent' Calibration Curve. Make a gas unless a teas value la known.) 7, Preparation tjfStandardGas chromatographic measurement of each gas mixture standard (described in Mixtum Calibhtiian. and Quality Section 5X3 or 7.1) using conditions Auuranceu - Identical with those listed in Sections 6.3 COLORITE 017080 Federal Register / Vol. 45, No. 224 / Tuesday, November 18, 1980 / Proposed Rules 76351 and 6.4. Flush the sampling loop for 30 seconds at the rate of 100 ml/min with one of the standard mixtures, and CcVl cb Vr(l - vb) q 106-2 1. Applicability and Principle. 1.1 Applicability. This method applies to the measurement of the vinyl activate the sample valve. Record the concentration of vinyl chloride injected (Ct). attenuator setting, chart speed, peak area, sample loop temperature, column temperature, carrier gas flow rate, and retention time. Record the barometric pressure. Calculate Ac the peak area multiplied by the attenuator setting. Repeat until two consecutive Injection areas are within 5 percent, then plot the average of those two values versus Cr When the other standard gas mixtures have been similarly analyzed and plotted, draw a straight line through the points derived by the least squares method. Perform calibration daily, or before and after each set of bag samples, whichever is more frequent 7.3 Quality Assurance. 7.3. Analysis Audit Immediately after the preparation of the calibration curve and prior to the sample analyses, perform the analysis audit described in Appendix C, Supplement B: "Procedure for Field Auditing GC Analysis." 7.3-2 Bag Leak Checks. Checking of bags for leaks is required after bag use and strongly recommended before bag use. After each use, connect a water manometer and pressurize the bag to 510 cm H.O (2-4 in H.O). Allow to stand for 10 min. Any displacement in the water manometer indicates a leak. AIbo, check the rigid container for leaks in this manner. Where: P,=Reference pressure, the laboratory pressure recorded during calibration, mm Hg. T,--Sample loop temperature on the absolute escale at the time of analysis, *K. Pi*= Laboratory pressure at time of analysis, mm Hg. Tr--Reference temperature, the sample loop temperature,recorded during calibration, *K. B^=Volume fraction of water vapor content of the bag sample, as analyzed. 9. References. 1. Brown, D.W., E.W. Loy, and M.H. Stephenson. Vinyl Chloride Monitoring Near the B. F. Goodrich Chemical Company in Louisville, Kentucky. Region IV, US. Environmental Protection Agency, Surveillance and Analysis Division. Athens, GA. June 24, 1974. 2. GD. Clayton and Associates. Evaluation of a Collection and Analytical Procedure for Vinyl Chloride in Air. EPA Contract No. 68-02-1408, Task Order No. 2. EPA Report No. 75VCL-1. December 13,1974. 3. Midwest Research Institute. Standardization of Stationary Source Emission Method for Vinyl Chloride. EPA-600/4-77-026. May 1977. 4. Schell, W. and M.C. Sharp. Collaborative Testing of EPA Method. chloride monomer (VCM) content of inprocess wastewater samples, and the residual vinyl chloride monomer (RVCM] content of polyvinyl chloride (PVC) resins, wet cake, slurry, and latex samples. It cannot be used for polymer in fused forms, such as sheet or cubes This method is not acceptable where methods from Section 304(h) of the Clean Water Act, 33 U.S.C. 1251 et seq (the Federal Water Pollution Control Amendments of 1972 as amended by the Clean Water Act of 1977) are required 1-2 Principle. The basis for this method relates to the vapor equilibrium that is established between RVCM, PVC resin, water, and air in a closed system. The RVCM in a PVC resin will equilibrate rapidly in a closed vessel, 'provided that foe temperature of the PVC resin is maintained above the glass transition temperature of that specific resin. 2. Range andSensitivity. The lower limit of detection of vinyl chloride will vary according to the chromatography used. Values reported include 1 x ltr'mg and 4 X 10'7 mg With proper calibration, foe upper limit may be extended as needed. 3. Interferences. The chromatograph columns and the corresponding operating parameters herein described normally provide an adequate resolution of vinyl chloride; however, resolution Interferences may be encountered on some sources. 'Note.--An stterastive leak check method Is to pressurize the beg to 5-10 an FLO or 2-4 in- FLO and allow H to stand overnight. A deflated bag indicates a leak. 106 (Vinyl Chloride] that will provide for a Standardized Stationary Source Emission Measurement Method. EPA 600/4-78-056. Emission Monitoring and Therefore, foe chromatograph operator shall select foe column and operating parameters best suited to his particular analysis requirements, subject to the For each sample bag in it* rigid 'Support Laboratory. Research Triangle approval of the Administrator. Approve! container, place a rotameter in-line - Park, NC. October 1976. Is automatic provided that the tester .between the bag and the pump inlet . evacuate the bag. Failure of the - rotameter to register zero flow when the bag appears to be empty Indicates a 4eak. 6. Calculations. 6.1 Determine foe sample peak area, Method 167--Determination of Vinyl Qiloride Content of Inprocess Wastewater Samples, and Vinyl Chloride Cootent of Polyvinyl Chloride Rests. Bltnry, Wet Cake, and Latex Sample* produces confirming data through an adequate supplemental analytical technique, such as analysis with a different column or GC/mass spectroscopy, and has the data . available for review by the Administrator. , Ac as follows: ' Introduction1 * lA,aAa AT *4 v.................................. idWherar Ywvrti'-fcyA* Vf_~ ` " . -*T Measured peak bra*. 7-Ar1Attssssttssbctos ** i * '> Performance of fids method should not be attempted by persons unfamiliar * - with foe operation of a chromatograph, nor by gas those who are unfamiliar with source sampling, 'because knowledge beyond foe soope of Vtay! 6hleride Concentrations. . fti* presentation is required. Car* must i From Ike eahbratifu curve described in be exerdsed to prevent exposure T -.'Section 7,2-2, % yahu>oL,C* fo*l * aempttng personnel to Vinyl chloride, a TUninnii.il * ji - i J l S-+! L- - e 4. Precision andReproducibility. An intariaboratory comparison between seven laboratories of three resin samples, each split into three < parts, yielded a standard deviation of: 2.63 percent for a sample with a mean of 2J ppm. 4.16 percent for a sample with a mean of 1X6 ppm. and 629 percent for a aamplt with a mean of 6246 ppm. (. Safety. Do not release vinyl chloride to the ..oorrasponds(fo4u,(ftf-sanpleppak ; >erea. Calculate Ibe cenoentratioo of w.;v * . *4 y;r r 'n- ,i , laboratory atmosphere dbring preparation of standards. Venting or 4 /vt-qvjd' chl-o-ri-d'iet-I,n D"ie h7a*.TC*. a-s,follows: . . ^MmHon stSeds assies or VMtflcsnUuctt ', 4sss ant ooHtUnls esdoi*eBiai< tbs UX purging with VCM/air mixtures must be gsiTrnsisiMilsl PielscUse Assnss. - x.' ' i.* COLOR!TE 017081 IVS52 pji f Vol 45, No. 224 / Tuesday. November IB. 1880 / Proposed Rules held to a minimum When they an required, the vapor must be routed to outside air. Vinyl Qiloride, eves at low ppm level*, must sever be vented Iseide toe laboratory. After viala have been analyzed, the gae must be vented prior to removal of toe vial from the instrument turntable. Vials must be vented through a hypodermic needle connected to an activated charcoal tube to prevent release of vinyl chloride into the laboratory atmosphere. The charcoal must be replaced prior to vinyl chloride breakthrough. 6. Apparatvi. 6.1 Sampling. The following equipment is required: 0.1.1 Glass Bottles. 80-ml (2-oz) capacity, with wsx-lined screw on tope, for PVC samples. 0,1.2 Glass Vials. 50-mi capacity Hypo-vials, sealed with Teflon faced Tuf-Bond discs, for water samples. 6.1.3Adhesive Tape. To prevent loosening of bottle tops- 6.2 Sample Recovery. The following equipment is required: 6-2.1 Glass Vials. With seals and caps. Perkin-Elmer Corporation No. 105011& or equivalent The seals must be made hum butyl rubber. Silicone rubber seals are not acceptable. 6X2 Analytical Balance. Capable of weighing to to 00001 gram. 6^-3 Vial Sealer. Perkin-Elmer No. 10&0106 or equivalent 6J Analysis. The following equipment is required: 6X1 Gas Chromatogreph. PerkinElmer Corporaticm Model F-40, F-42. or F-4S Head-Space Analyzer, or equivalent Equipped with backflush accessory. &12 -Cbromatograhk: Columns. Stainless steel 1 tn by J-2 mm and 2 m by 8.2 mm. both containing 60/SD-mesh Porapak Q. The analyst may use other columns provided tost to* precision and accuracy ot toe analysis of vinyl chloride standards are not impaired and he has available tot review information confirming that there is adequate resolution of toe vinyl chloride peak. (Adequate resolution is defined as an area overlap of not more than 10 percent of the vinyl ckloride peek by an Inierferent peak. Calculation of area overlap la explained in Appendix C. Supplement A: Determination of Adequate Chromatographic Peek Resolution.*'} Two 1A3 m columns, each containing 1 percent Caibowax 1S00 on Caibopak B. have been suggested for sample* containing acetaldehyde. UJ Thermometer. 0 to 100"C, accurate to to 0.1*C, Perkin-Elmer No. 105-01OB, or equivalent ... . gj.A Sample Tray Thermostat System. Perkin-Elmer No. 1060103. or equivalent. 0.3.5 Septa. Sandwich type, for automatic coring. 13 mm. Perkin-Elmer No. 105-1006. or equivalent 6.3.6 Intergrator-Recorder. Hewlett- Packard Model 3308QA. or equivalent. 6-3.7 Filter Drier Aeeembly (3). Parking-Elmer No. 2230117, or equivalent 6.3-8 Soap Film Flowmeter. Hewlett Packard No. 0101-0113, or equivalent 0X9 Roguetots. For required gat cylinders. 0X10 Headspace Vie] Pre- Pressurizer. Nitrogen pressurized hypodermic needle inside protective shield. (Blueprint available from Test Support Section. Emission Measurement Branch. Office of Air Quality Planning and Standards, Environmental Protection Agency, Mail Drop 19. Research Triangle Park, N.G 27711.) 7, Reagent*. Dae only reagents that are of chromatograph grade. 7.1 Analysis. The following items are required for analysis: 7.1.1 Hydrogen. Zero grade. 7XX Nitrogen. Zero grade. 7XJ Air. Zero grade. 72 Calibration. The following items are required for calibration: 7X1 Cylinder Standards (4). Gas mixture standards (50-, S00-, 2008- and 4000-ppm vinyl chloride in nitrogen cylinders). The teeter may use cylinder standards to directly prepare a chromatograph calibration curve as described in Section 0X tf the following conditions are met (a) The manufacturer certifies the gas composition with an accuracy of to3 percent or better (see Section 7X1.1). (b) The manufacturer recommend* a maximum shelf life over which the gas concentration does not change by greater than 5 percent from the certified value, (c) The manufacturer affixes the date of gas cylinder preparation, certified vinyl chloride concentration, end recommended maximum shelf life to toe cylinder before shipment to the buyer, 7X1.1 Cylinder Standards Certification. The manufacturer shall certify the concentration of vinyl chloride in nitrogen in each cylinder by (a) directly analyzing each cylinder and (b) calibrating his analytical procedure on toe day of cylinder analysis. To calibrate his analytical procedure, toe manufacturer shall use. as a minimum, a three-point calibration curve. It is recommended that the manufacturer maintain (1) a high-concentration calibration standard (between 4000 and 6000 ppm) to prepare his calibration curve by an appropriate dilution j technique and (2) e low-concentration i calibration standard (between so and S00 ppm) to verify toe dilution technique need. If the difference between the apparent concentration read from the calibration curve and the true concentration assigned to the low- concentration calibration standard exceeds 5 percent of the true concentration, toe manufacturer shall determine the source of error and correct It, then repeat toe three-point calibration. 7X1.2 Verification of Manufacturer' i Calibration Standards. Before using, the manufacturer shall verify each calibration standard by (a) comparing it to gas mixtures prepared (with 99 Mol percent vinyl chloride) in accordance with the procedure described in Section 7.1 of Method 106 or by (b) having it analyzed by the National Bureau of Standards. The agreement between the initially determined concentration value end toe verification concentration value most be within 5 percent The manufacturer must reverify all calibration standards on a time interval consistent with the shelf life of the cylinder standard* sold. X Procedure. 6.1 Sampling. 0.1.1 PVC Sampling. Allow toe ream or slurry to flow from s tap on the laid; or silo until the tap line has been well purged. Extend and fill a 00-ml-sample bottle under toe tap, and immediately tighten a cap on toe bottle. Wrap adhesive tape around the cap and bottic to prevent toe cap from loosening. Plow an identifying label on each bottle, and record toe data, time, and sample location both on the bottle* end in a log book. 6.12 Water Sampling. Prior to use. the fiO-ml viols (without the discs) must be capped with aluminum foil and muffled at 400* C for at last 1 hour to destroy or remove any organic matter tost could interfere with analysis. At toe sampling location fill the vials bubble- free to overflowing so that e convex meniscus forms at the top. The excess water is displaced as the sealing disc is carefully placed, with the Teflon aide down, on the opening of the vial. Place toe aluminum seal over tire disc and the neck of tiie vial, and crimp Into place. Affix an Identifying label on the bottle, ami recced the date, time, and sample location both on the vials and in a log bock. AH sample* must be kept refrigerated until analyzed. 82 Sample Recovery. Semples must be run within 24 hours. 8X1 Resin Sample*. The weight of tire resin used must be between M end 42 grams. An exam weight must be i4*v Ikhm*#**'kMM* COLORITE 017082 Federal Register / Vol. 46, No. 224 / Tuesday, November 18, I860 / Proposed Rules 76353 obtained (0.0001 g] for each sample. In operation. Porapak oolumns must be the case of suspension resins, a purged for 1 hour at 230*C Do not volumetric cup can be prepared for connect the exit end of the column to the holding the required amount of sample. detector while conditioning. Hydrogen When the cup is used, open the sample and air to the detector must be turned bottle, and add the cup volume of resin off while the column Is disconnected. to the tared sample vial (fared, including 83.1.1 Flow Rate Adjustments. septum and aluminum cap). Obtain the Adjust flow rates as follows: exact sample weight add two drops of a. Nitrogen Carrier Gas. Set regulator distilled water, and immediately seal the on cylinder to read 50 pelg. Set regulator vial. Report this value on the data sheet: on chromatograph to produce a flow it is required for calculation of RVCM. In ' rate of SOlO oc/mln. Accurately measures the case of dispersion resins, the cup the flow rate at the exit end of the cannot be used. Weigh the sample in an column using the soap film flowmeter aluminum dish, transfer the sample to end e stopwatch, with the oven and the tared vial, and accurately weigh It in column at the analysis temperature. the vial. After pre-pressurization of the samples, condition them for a minimum After the instrument program advances to the *TT (backflush) mode, adjust the of 1 hour in the 90* C bath. Do not nitrogen pressure regulator to exactly exceed 5 hours. balance the nitrogen flow rate et the Note.--Some aluminum vial caps have a center section that must be removed prior to placing into sample tray. If the cap is not removed, the Injection needle will be damaged. detector as was obtained in the "A" mode. b. Vial Pre-Pressurizer Nitrogen. After the nitrogen carrier is set, eolye the following equation and adjust the 833 Suspension Resin Slurry and Wet Cake Samples. Decant the water pressure on the vial pre-pressurizer accordingly. from a wet cake sample, and turn the sample bottle upside down onto a paper towel. Wait for the water to drain, place approximately 03 to 4.0 grams of the , wet cake sample in a tared vial (fared, including setum and aluminum cap) and seal immediately. Then determine the sample weight (0.0001 g). All samples must be pre-pressurized and then conditioned for 1 hour at 90* C. A *1 '.1 " 7.50 - Ip k P* sample of wet cake is used to determine TS (total solids). This is required for calculating the RVCM. 8.2.3 Dispersion Resin Slurry and Geon Latex Samples. The materials should not be filtered. Sample must be thoroughly mixed. Using a tared vial (tared, including septum and aluminium cap) add approximately 8 drop* (0.25 to 035 g) of slurry or latex using Whew: - medicine dropper. This should be done immediately after mixing. Seal dm vial as soon as possible. Determine sample weight (00001 g). After pre- Tj--Ambient temperature, *K. Ti--Conditioning bath temperature. *K. Pi--Gas chromatograph absolute dosing pressure (analysis mode), k Pa. pressurization, condition the vial for 1 P,,, --Water vapor pressure @ 90*C hour at 90*C in the analyzer bath. (5258 mm Hg). Determine the TS on the slurry sample P---Water vapor pressure @ 22*C (198 (Section 833.). - 8.2.4 fnprooess Wastewater Semples. Using a tared vial (tend, including septum end aluminum cap) quickly add approximately 1 cc of water mm Hg). 230--mm Hg per k Pa. 10 k Pa--Factor to adjust the pre- pressurized pressure to sligntly less than the dosing pressure. using a medicine dropper. Seal the vial Because of gauge errors, the apparatus as soon as possible. Determine temple may avar-presmrize the viaL If the vial weight (03001 g). Pre-praeemtee the pressure is ml or higher then the dosing vial, and then condition for 2 hove at pressure, an audible doable injection 90*C far the analyser bath, rj will occur.If the vial pressure is too low, 83 Analysis - tt," ' errors will occur on resin samples 83.1 Preparation of Equipment. . because of inadequate tims for _ Install the chrdmatogrephic column end headspace gas equilibrium. This condition overnight at 180*C. teths first comhtiac can be avoided by running several standard gas samples at various pressures around the calculated preserve, and then selecting the highest pressure that does not produce a double injection. All samples and standards must be pressurized for 60 seconds using the vial pre-pressurizer. The vial is then placed into die 90*C conditioning bath and tested for leakage by placing a drop of water on the septum at the needle hole. c. Burner Air Supply. Set regulatory on cylinder to read 50 psig. Set regulator on chromatograph to supply air to burner at a rate between 250 and 300 cc/min. Check with bubble flowmeter. d. Hydrogen Supply. Set regulator on cylinder to read 30 psig. Set regulator on chromatograph to supply approximately 35 5 cc/min. Optimize hydrogen flow to yield the moat eensitive detector response without extinguishing the flame. Check flow with bubble meter and record this flow. 83.13 Temperature Adjustments. Set temperatures as follows: a. Oven (chromatograph column), 140*C. b. Doaing Line. 170*C c. Injection Block. 170`C. d. Sample Chamber. Water Temperature. 90*C l.*0C 8.13 Ignition of Flame Ionization Detector. Ignite the detector according to the manufacturer's instructions. 8.3.1.4 Amplifier Balance. Balance die amplifier according to the manufacturer's instructions. 833 Programming the Chromatograph. Program the chromatograph es follows: a. 1-Dosing or Injection Time. The normal setting is 2 seconds. h. A-Analyris Time. The normal setting is approximately 70 percent of the VCM retention time. When the analysis timer terminates, the programmer Initiates backflushing of the first column. c. B-Backflushlng Time. The normal setting is double the analysis time. d. W-Stabihxation Time. The normal setting Is 03 minute to 13 minute. a. X-Number of Analyses Per Semple. The nomal setting is 1. 833 Preparation of Sample Turntable. Before placing any sample into turntable, be certain that the center section of the aluminum cap has been removed. All samples and standards must be pressurized for 60 seconds by using the vial pre-pressurizer. The numbered sample vials should be placed in the corresponding numbered positions in the turntable. Insert samples in the following order: Positions 1 end 2--Old 2000-ppm standards Corconditioning. These ere COLOR!TE 017083 76354 Federal Register / Voi. S, No. 824 / Tuetday, November 18, 1980 / Proposed Rules necessary only after the analyser has necessary to minimise mixing air with Draw a straight line through the po. not been used for 24 boor* or longer. the standard in the vial Each vial Is to derived by the least squares method Petition* 3--50-ppm standard, freshly be purged with standard for BO seconds, 10. Calculations. preparedPositions 4--500-ppm standard, freshly prepared. during which time the filling tube is 10.1 Response Factor. If the gradually slid to the top of the vial. -After calibration curve described in sector, the BO seconds, the tube U removed with 92 passes through zero, a response Position 5--2000-ppm standard, freshly prepared. Position 6--tOOO~ppm standard, freshly prepared. Position 7--Sample No. 7 (This i* the first sample of the day. but ia given as 7 to be consistent with the turntable and the integrator printout.) After all samples have been postponed, insert the second set of SO-, 500,2000, and 4000ppm standards. Samples, including standards, must be conditioned in the bath of 90*C for 1 hour (not to exceed 5 hours). 8.3.4 Start Chromatograph Program. When all samples, including standards, have been conditioned at 0O C for 1 hour, start the analysis program according to the manufacturer's the septum, simultaneously sealing the trial. Practice will be necessary to develop good technique. Rubber gloves should be worn during the above operations. The sealed vial must then be pressurized for 80 seconds using the vial pre-pressurizer. Test the vial for leakage by placing a drop of water on the septum at the needle hole. 8.2 Preparation of Chromatograph Calibration Curve. Prepare two 50-, 500-, 2000-, and 4000- ppm standard sample*. Run the calibration samples in exactly the same manner a* regular samples. Plot A. the integrator area counts for each standard ample, versus C* the concentration of vinyl chloride in each standard sample. factor, R* may be used to compute vin; chloride concentrations. To compute a response factor, divide any particular t by the corresponding C*. R,=A*/C, Eq. 107-1 If the calibration curve does not pass, through zero, the calibration curve must be employed to calculate each sample concentration unless the error introduced by using e particular R, is known. 102 Residual VinylChloride Monomer Concentration. (Ctk) or Vinyl Chloride Monomer Concentration. Calculate C*, in ppm or mg/kg as follows: instructions. These instructions must be carefully followed when starting and stopping a program to prevent damage S'. to the dosing assembly. rvc Eq. 107-2 8.3.5 Determination of Total Solids (TS). For wet cake, slurry, resin solution, and PVC latex samples, determine TS for each sample by accurately weighing approximately 3 to 4 grama of sample in an aluminum pan before and after placing in a draft oven (105 to 110*C). Samples must be dried to constant weight After first weighing, return the Where: A*=Chromatograph area counts of vinyl chloride for the sample. P, Ambient atmospheric pressure, mm Hg. R<= Response factor in area counts per T5a>Total solids expressed as a decimal -fraction. T* Equilibrium temperature, "K K_*=Henry's Law Constant for VCM in water @ BO'C pxitr'g/g/mm Hg). pan to the oven for a short period of time, and then reweigh to verify complete dryness. TS is then calculated as the final sample weight divided by initial sample weight 9. Calibration. Calibration ia to be performed each 8hour period when the Instrument ia used. Each day, prior to funning samples, the column Should be conditioned by running two 2000-ppm ppm VCM. Ti=Ambient laboratory temperature, "K. M,-= Molecular weight of VCM (82.5 g/ mole). V,=Volume of the vapor phase, cm*. 4l<*Gos constant (82380 cm* - mm Hg/ mole *K). m-=Sample weight, g. K,--Henry's Lew Constant for VCM in PVC @ arc (2xur.*c/g/mm Hg). Assuming the following conditions are met, these values can be substituted into equation 107-2: P.*=7S0 mm Hg. V,--Vial volume--sample volume (Fisher vials ere 22j0 cm* and PerkinElmer vials era ZL8 an*). T,=23`C orfrW'K. T.=90*Carl83'iC standards from the previous day. 9.1 PreparationofStandards. Calibration standards are prepared as follows: Mace two drops of distilled 7*0 m -JEW i + *'.tSjtlC"`(n)(KJh7.U10',(I-T5)O3! water (with the use of an eyedropper) in the sample vial, then fill the vial with the VCM/nitrogen standard, rapidly seat the septum, and teal with the Results calculated using these * r -ACS--Division ofPolymer Chemistry, -equations reproseat canoentratian based itolymer Preprints 15 [Zf. 1B7,1974. aluminum cap. Use a %-in. stainless ' ` on the total temple. To obtain results - Borens, A. K. *lhe Diffusion of vteel tine from the cylinder to the vial. - boed on dry PVC nontenf, divide by TS. Viuyl Chloride in Nyvinyl Chloride," Do not use rubber or tygon tubing. The -11. tUferenoes. ----- ' -ACS--Division of Polymer Chemistry. sample ha* from the cylinder must be - 7 1. Residual Vinyl Chloride Monomer Polymer Pceprints 15(21203,HJ74. purged (into a property vented hood) for Content of Polyvinyl Chloride Raatua, ~ 4, Serene, A. R. L B. Crider, G J. several minutes prior to fill tha vials. Latex, Wet Cake, Shay end Water Tranenek and ). M. Whitney, "Analysis After purging, reduce the flow tats to -V Samples, B. P. Goodridb Chemical Group -for Vinyl Chloride to PVC Powders by -oo to 1000 cc/ratn. Piace and of tubing Standard Tset ProeadareN*. 18054L ' fieed-4Speoe GosGuwnatagraphy," to into vial (near bottom). Position a -S. F. Goodrich Tedmieo! CenterrAvtm ' be publlsned. septran on top of the vial, pressing M ' ' Vke,Ghio, OctubmAMfi*-' '-^ 7^ - * U- V *' - -- ' against the W-in. filling tubs to mtntmbca L Barone. A. R, "The BifbsUntf `rC: -the size of the vent opening. This is ^ VtnylChloride inWdyviqylCMaikte.' >' COLORXTE 01*7084 90 2184 nter-office memo TENNECO CHEMICALS, INC. To From Subject Mr. J,, P. Sandstedt Dr. R. T. Gottesman A i Piscataway At Saddle Brook EPA Proposal -- Vinyl Chloride Air Pollution Tests Da :t c December 15, 1980 EPA has proposed to revise its test methods for vinyl chloride under NESHAPS (45 FR76346). The notice is reported to indicate that several improvements have been developed in the test methods since their adoption in 1977 and the Agency proposes to incorporate these improvements in these revisions. Comments are due by January 19, 1981. X would suggest your careful review of this proposal including consultation, if necessary, with the Analytical Department. If these proposed revisions constitute a problem to us, we should plan to offer comments by the January 19 date. Please advise. RTG:jmd R. T. Gottesman U* , tv ^ , U(_ . tr COLORITE 017085 r CURRENT REPORT The controversy over Love Canal was the "biggest trouble we've gotten into this year, on scientific grounds," she told the panel. "It has been a very unfortunate thing for the agen cy that we're constantly measured for that flaky chromosome study." Wellford said "it's pretty clear now" that the Center for Disease Control, not EPA, will be doing health effects work related to Love Canal. There is "some concern," she added, that the work may be transferred to the Department of Health and Human Resources. David M. Rosenbaum, deputy assistant administrator for radiation programs, told the advisory board that it's very dif ficult to get highly qualified people to bid on competitive con tracts. "Getting the best people has nothing to do with the federal contract procedure," he said. "Very often the very best peo ple in a field won't bid at all... The system's just not set up to get the best." Rosenbaum stated that environmental impact statements generated by EPA are often "terribly written, with made-up numbers." EISs are often done "on the basis of, if they're very thick and dull, no one will ever read them," Rosenbaum said, which he called "a form of middle class subsidy." Rosenbaum said he does not contract out for EISs or policy statements. It is worth it to have the work done in-house, he said, because at least he knows "what the numbers mean." Air Pollution EPA PROPOSES TO REVISE TESTS FOR VINYL CHLORIDE AIR POLLUTANTS The Environmental Protection Agency Nov, 18 proposed to revise its test methods for vinyl chloride under its national emission standards for hazardous air pollutants (45 FR 76346). In its announcement, EPA said that several improvements have been developed in the test methods since they were adopted in 1977. The proposed revisions would incorporate the improvements, the agency stated. Comments on the proposal should be submitted in duplicate by Jan. 19, 1981, to the Central Docket Section (A-130), Attention: Docket No. A-80-50, EPA, 401 M St. S.W., Washington, D.C. 20460. For further information, contact Roger Shigehara, Emis sion Measurement Branch (MD-19), EPA, Research Triangle Park, N.C. 27711, (919) 541-2237. Hazardous Waste EPA TELLS OIL COMPANY TO ELIMINATE LAKE ERIE HAZARDOUS DISCHARGE THREAT CLEVELAND -- (By a BNA Staff Correspondent) -- The Environmental Protection Agency Oct. 28 told the Stevenson Oil k Chemical Corporation to take immediate measures to eliminate the threat of oil and hazardous discharges into Lake Erie. EPA Region V Administrator John McGuire said that numerous inspections at the suburban Cleveland facility have determined a "substantial threat of discharge of oil and hazardous substances" into the lake. Runoff from the two-acre site flows into a swampy area which then can flow into Lake Erie through a drainge system, he explained. Two actions have been requested by EPA to eliminate the discharge threat. They include removal of waste material drums to an approved hazardous waste disposal site, and consultation with a contractor to remove a black, oily sub stance from the swampy area at the rear of the site. 1123 This action was taken under Section 311 provisions of the Clean Water Act, which prohibits oil or hazardous substance discharges into navigable waterways. Should Stevenson be unable or unwilling to take discharge threat elimination measures, McGuire said EPA may take further action in volving federal authority and funding. In that case, the owner or operator could become liable for the costs of federal remedial actions, he said. Stevenson has a week to respond to EPA's request before further action will be considered. Enforcement WASTE DISPOSAL FIRM, EMPLOYEES INDICTED FOR MAIL FRAUD, CONSPIRACY A Newark, N.J., federal grand jury Nov. 5 indicted three individuals and four companies on various mall fraud and conspiracy charges connected with their alleged failure to fulfill contracts for the proper disposal of hazardous wastes. The indictments charged that the defendants agreed to accept waste from chemical companies and promised to dis pose of the waste in accordance with requirements set by the New Jersey Department of Environmental Protection, but that they never performed the services even though payment was made. Michael Colleton, Ridgewood, N.J., the principal operating officer of the Chemical Control Corp., was charg ed in the indictments with multiple counts of mall fraud. Colleton allegedly induced payments for services never per formed, using the mail to further the scheme. He could fact a sentence of 50 years and a fine of 810,000 if found guilty. John Albert and Eugene Conlon, both of North Brunswick, N.J., were charged by the grand jury with mail fraud and conspiracy in connection with an allegedly similar scheme. According to the indictments, the two men accepted payments for transporting hazardous wastes for disposal by the Chemical Control Corp., but instead stored drums of waste at a different site and in an unlawful manner. If found guilty, the two would be subject to sentences of up to 60 years imprisonment and fines of 121,000. The corporate defendants are the Chemical Control Corp., and its parent corporation, the Northeast Pollution Control Corp., Elizabeth, N.J., the Jersey Sanitation Co. Inc. , East Brunswick, N.J., and A to Z Chemical Resource Recovery Inc., New Brunswick, N.J. The grand jury Nov. 12, also indicted for mail fraud William Carracino, Union, N.J., the previous owner of Chemical Control. Carracino could face a sentence of 35 years imprisonment and a J7000 fine if found guilty. Publications EPA RELEASES QUARTERLY BIBLIOGRAPHY OF DOCUMENTS PUBLISHED BY AGENCY OFFICES A quarterly abstract bulletin of Environmental Protection Agency publications is available from the agency's Center for Environmental Research Information. The bulletin lists EPA publications by National Technical Information Service number and price, title, subject, and sponsoring EPA office. The bulletin also includes an abstract of each publication and a list of key descriptive and identifying words. The bulletin includes EPA publications issued from July through September 1980. It is available from the center, Cin cinnati, Ohio 45268. 11-28-80 Copyright 1980 by The Bureau of National Affairs, Inc. 0148 7973/80/S00 60 COLORITE 017086