Document xz3Bw38nR6OEoGnbELp1pZOeb

ENVIRONMENTAL PROTECTION AGENCY NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS Standard For Vinyl Chloride NOTICE: The text of the regulation re produced here represents the Federal regulation as of June 1. 1977. Amend ments, additions and corrections occur frequently. Up-to-date information can be obtained from the Environmental Protec tion Agency or from publications such aa the Environment Reporter published by The Bureau of National Affairs, Inc., 1231 25th Street N.W., Washington, O.C. 20037. UCC 026967 HAZARDOUS EMISSIONS S-359 121:0471 Suboart F--National Emission Standard (j) ``Inprocess wastewater" means any for Vtayt Chloride water which, during manufacturing or [41 FR 46559, October 21, 1976] processing, comes into direct contact g 61.60 Applicability. with vinyl chloride or polyvinyl chloride or results from the production or use of (a) This subpart' applies to plants any raw material, intermediate product, which produce? * ' (1) Ethylene dichloride by reaction of oxygen and hydrogen chloride with ethylene, <2) Vinyl chloride by any process, and/or (3) One or more polymers containing any traction of polymerized vinyl chlo ride. <b> This subpart does not apply to equipment used in research and develop ment if the reactor used to polymerize the vinyl chloride processed in the equip ment has a capacity of no more than 0.19 m1 (90 gal). (c) Sections of this subpart other than 61.61; 61.64 (a)(1), (b), (c), and (d); 61.67; 61.68; 61.69; 61.70; and 61.71 do not apply to equipment used in research and development if the reactor used to po lymerize the vinyl chloride processed in the equipment has a capacity of greater than 0.19 m* (50 gal) and no more than 4.07m* (1100gal). [42 FR 29005, June 7, 1977) finished product by-product or waste product containing vinyl chloride or polyvinyl chloride but which has not been discharged to a wastewater treat ment process or discharged untreated as wastewater. <k> "Wastewater treatment process" includes any process which modifies characteristics such as BOD. COD. TSS, and pH, usually for the purpose of meet ing effluent guidelines and standards; it does not include any process the purpose of which is to remove vinyl chloride from water to meet requirements of this subpart. 0) "In vinyl chloride service" means that a piece of equipment contains or contacts either a liquid that is at least 10 percent by weight vinyl chloride or a gas that is at least 10 percent by volume vinyl chloride. (mi "Standard operating procedure" means a formal written procedure offi cially adopted by the plant owner or operator and available on a routine basis to those persons responsible for carrying g 61.61 Definitions. out the procedure. Terms used In this subpart are defined (n> "Run" means the net period of in the Act, in subpart A of this part, or time during which an emission sample Is In tills section as follows: collected. (a) "Ethylene dlchloride plant" in cludes any plant which produces ethyl ene dichloride by reaction of oxygen and hydrogen chloride with ethylene. (b> "Vinyl chloride plant" Includes any plant which produces vinyl chloride by any process* (c) "Polyvinyl chloride plant" Includes any plant where vinyl chloride alone or in combination with other materials is polymerized. (d> "Slip gauge" means a gauge which has a probe that moves through the gas/ liquid interface in a storage or transfer vessel and indicates the level of vinyl chloride in the vessel by the physical state of the material the gauge dls- charges. (e) "Type of resin" means the breed classification of resin referring to the (o> "Ethylene dlchloride purification" includes any part of the process of ethyl ene dlchloride production which follows ethylene dlchloride formation and in which finished ethylene dlchloride is produced. (p) "Vinyl chloride purification" in clude* any part of the process of vinyl chloride production which follow* vinyl chloride formation end in which finished vinyl chloride is produced. (q> "Reactor" Includes any vessel in which vinyl chloride is partially or totally polymerized into polyvinyl chloride. (r* "Reactor opening loee" means the emissions of vinyl chloride occurring when a reactor is vented to the atmos phere for any purpose other than an emergency relief discharge as defined in basic manufacturing procase for produc f 61.65(a). ing that resin, including, but not limited (s> "Stripper" includes any vessel in to. the suspension, dispersion, latex, bulk, which residual vinyl chloride is removed and solution processes. from polyvinyl chloride resin, except (f> "Grade of resin" means the sub bulk resin. In the shiny form by the use division of resin classlfleatian which de of heat and/or vacuum. In the case of scribes it as a unique resin. La, the most bulk resin, stripper Includes any vessel exact description of a resin with lie fur which is used to remove residual vinyl ther subdivision. chloride from polyvinyl chloride resin <g) "Dispersion resin" means s resin immediately following the polymeriza manufactured in such away as to form tion step In the plant process flow. fluid dispersions when dispersed in a (t> "Standard temperature" means a plasticizer or plastldmr/dnuent mix temperature of 20* C'6* F). tures. (u) "Standard pressure1* mesne a (h) "Latex resin" means a resin which pressure of 700 mm of Hg (29.92 to. at is produced by a polymerization process Hg). which initiates from free radical catalyst sites and is sold undried. [42 FR 29005, June 7. 1977) (1) "Bulk resin* 'means a resin which is produced by a polymerisation process 8 61.62 Emission standard for ethylene dlchloride plants. in which no water is used. [42 FR 29005, Juno 7, 1977] (a) Ethylene dlchloride purification: The concentration of vinyl chloride in all' exhaust gases discharged to the at mosphere from any equipment used in ethylene dlchloride purification Is not to exceed 10 ppm. except as provided in 3 61.65(a). This requirement does not apply to equipment that has been opened, is out of operation, and met the require ment in 161.65(b) (6)0) before being opened. (b) Oxychlorination reactor: Except as provided in 161.65(a). emissions of vinyl chloride to the atmosphere from each oxychlorination reactor are not to exceed 0.2 g/kg (0.0002 Ib/lb) of the 100 percent ethylene dichloride product from the oxychlorination process. 8 61.63 EmiM.in xlundunl' for vinyl chloride plant*. An owner or operator of a vinyl chlo ride plant shall comply with the require ments of this section and | 61.65. (a> Vinyl chloride formation and puri fication: The concentrating of vinyl chloride in all exhaust gases discharged to the atmosphere from any equipment used In vinyl chloride formation and/or purification is not to exceed 10 ppm. ex cept as provided In | 61.65(a). This re quirement does not apply to equipment that has been opened, is out of operation, and met the requirement in I 61.63<b (6) (li before being opened. - S 61.64 EihImhor -landard fur polyvinyl rliloride plants. An owner or operator of a polyvinyl chloride plant shall comply with the re quirements of this section and I 61.65. (a> Reactor: The following require ments apply to reactors: <1> The concentration of vinyl chlo ride in all exhaust gases discharged to the atmosphere from each reactor is not to exceed 10 ppm. except as provided in paragraph ia>(2i of this section and 1 61.65(a). (2) The v*actor opening loss from each reactor is not to exceed 0.03 g vinyl chloride'Kg (0.00002 lb vinyl chloride/ lb > of polyvinyl chloride product, with the product determined on a dry solids basis. This requirement applies to any vessel which is used as a reactor or as both a reactor and a stripper. In the bulk process, the product means the grow product of prepolymerization and poe(polymerization. (3* Manual vent valve discharge: Ex cept for an emergency manual vent valve discharge, there is to be no discharge to the atmosphere from any manual vent valve on a polyvinyl chloride reactor in vinyl chloride service. An emergency manual vent valve discharge means a discharge to the atmosphere which could not have been avoided by taking meas ures to prevent the discharge. Within 10 days of any dlscharg* to the atmosphere from any manual vent valve, the owner or operator of the source from which the discharge occurs shall submit to the Ad ministrator a report In writing contain ing information on the source, nature 8-12-77 Copyright 1977 by The Bureau of Notionol Affairs, Inc, [Sea. 81,64(e)(3l) ucc 026968 121:0472 FEDERAL REGULATIONS and cause ot the discharge, the date and polyvinyl chloride resins, excluding latex (1) Rotating pumps: Vinyl chloride time of the discharge, the approximate resins, with the product determined on a emissions from seals on all rotating total vinyl chloride loss during the dis dry solids basis; pumps in vinyl chloride service are to be charge, the method used for determining (ii) 0.4 g/kg (0.0004 lb/lb) product minimized by Installing sealless pumps, the vinyl chloride loss, the action that from the strippers [or reactor(s) if the pumps with double mechanical seals, or was taken to prevent the discharge, and plant has no stripper(s)] for all other equivalent as provided in 61.66. If measures adopted to prevent future dis polyvinyl chloride resins, including latex double mechanical seals are used, vinyl charges. resins, with the product determined on chloride emission from the seals are to (b> Stripper: The concentration of a dry solids basis. be minimized by maintaining the pres vinyl chloride in all exhaust gases dis charged to the atmosphere from each stripper is not to exceed 10 ppm, except as provided in | 61.65(a). This require ment does not apply to equipment that 61.65 Emu#ion Undard for nliylrnr diillloride, vinyl cliluridr mid poly vinyl chloride plant*. An owner or operator of an ethylene sure between the two seals so that any leak that occurs Is into the pump: by ducting any vinyl chloride between the two seals through a control system from which the concentration of vinyl chlo has been opened. Is out of operation, and dichlortde, vinyl chloride, and/or poly ride in the exhaust gases does not ex met the requirement In | 61.68(b) (6) (1) vinyl chloride plant shall comply with ceed 10 ppm; or equivalent as provided before being opened. the requirements of this section. in 61.66. (c> Mixing, weighing, and holding (a) Relief valve discharge: Except for (ii) Reciprocating pumps: Vinyl chlo containers: The concentration of vinyl chloride in all exhaust gases discharged to the atmosphere from each mixing, weighing, or holding container in vinyl chloride service which precedes the stripper (or the reactor if the plant has no shipper) in the plant process flow is not to exceed 10 ppm, except as provided in i 61.65(a). This requirement does not apply to equipment that has been opened, is out of operation, and met the requirement in 161.68(b) (6) (i) before being opened. (d) Monomer recovery system. The concentration of vinyl chloride in all ex haust gases discharged to the atmos phere from each monomer recovery sys tem is not to exceed 10 ppm, except as provided In 161.65(a). This requirement does not apply to equipment that has been opened. Is out of operation, and met the requirement In I 61.68(b) (6) (i> be fore being opened. (e> Sources following the stripper(s): The following requirements apply to emissions of vinyl chloride to the at mosphere from hie combination of all sources following the stripper(si Cor the reector(s) if the plant hae no stripperis) 1 in the plant process flow in cluding but not limited to, centrifuges, concentrators, blend tanks, filters, dry ers, conveyor air discharges, baggers, an emergency relief discharge, there is to be no discharge to the atmosphere from any relief valve on any equipment in vinyl chloride service. An emergency relief discharge means a discharge which could not have been avoided by taking measures to prevent the discharge. With in io days of any relief valve discharge, the owner or operator of the source from which the relief valve discharge occurs shall submit to the Administrator a re port in writing containing information on the source, nature and cause of the discharge, the date and time of the dis charge, the approximate total vinyl chlo ride loss during the discharge, the meth od used for determining the vinyl chlo ride loss, the action that was taken to prevent the. discharge, and measure* adopted to prevent future discharges. <b) Fugitive emission sources: (1) HUM? Vinyl chloride emlttkmft from and unloading Unea in vinyl chloride service which ere opened to the atmos phere after each loading or unloedlng op eration are to be mlnlretted as follows: [42 FR 29005, June 7, 1977] ti) After each loading or unloading operation and before opening a loading or unloading Una to the atmosphere, the quantity of vinyl chloride in all parts of ride emissions from seals on all recipro cating pumps in vinyl chloride service are to be minimized by installing double outboard seals, or equivalent as provided in 161-66. If double outboard seals are used, vinyl chloride emissions from the seals are to be minimized by maintaining the pressure between the two seals so that any leak that occurs is Into the pump; by ducting any vinyl chloride be tween the two seals through a control system from which the concentration of vinyl chloride in the exhaust gases does not exceed 10 ppm; or equivalent aa provided in 1 01.06. 1 ul) Rotating compressor: Vinyl chloride emissions from seal* an all ro tating compressors in vinyl chloride service are to be minimized by Installing compressors with double mechanical seals, or equivalent as provided in I 61.66. If double mechanical seals are used, vinyl chloride emissions from the seals are to be minimized by maintaining the pres sure between the two seals $0 that any leak that occurs is Into the compressor; by ducting any vinyl chloride between the two seals through a control system from which the concentration of vinyl chloride in the exhaust gases does not exceed 10 ppm; or equivalent as provided in 1 01.66. storage containers, and lnprocess waste- each loading or unloading line that are <iv) Reciprocating compressors: Vinyl water : to be opened to the atmosphere is to be chloride emissions from seals on all re (1) In polyvinyl chloride plants using reduced so that the parts combined con ciprocating compressors in vinyl chloride stripping technology to control vinyl tain no greater than 0.0038 (0.13 ft*) service are to be minimized by installing chloride emissions, the weighted average of vinyl chloride, at standard tempera double outboard seals, or equivalent aa residual vinyl chloride concentration In ture and pressure; and provided in ! 61.66. If double outboard all grades of polyvinyl chloride resin (ii) Any vinyl chloride removed from seals are used, vinyl chloride emissions processed through the stripping opera a loading or unloading line In accord from the seals are to be minimised by tion on each calendar day, measured ance with paragraph (b) (1) (1) of this maintaining the pressure between the immediately after the stripping opera tion is completed, may not exceed: (1) 2000 ppm for polyvinyl chloride dispersion reslne, excluding latex resins; (ii) 400 ppm for all other polyvinyl chloride resins, including latex rains, averaged separately for each type of ra in; or section is to be ducted through a control system from which the concentration of vinyl chloride in the exhaust gases does not exceed 10 ppm. or equivalent as pro vided in 161.66. (2) Slip gauges: During loading or un loading operations, the vinyl chloride emissions from each slip gauge in vinyl two seals so that any leak that occurs Is into the compressor; by ducting any vinyl chloride between the two seals through a control system from which the concentration of vinyl chloride In the exhaust gases does not exceed 10 ppm; or equivalent as provided in 1 61.66. (v) Agitator: Vinyl chloride emissions (2) In polyvinyl chloride plants con chloride service are to be minimised by from seals on all agitators in vinyl chlo trolling vinyl chloride with ducting any vinyl chloride discharged ride service are to be minimized by in technology other than stripping or in from the slip gauge through a control stalling agitators with double mechani addition to stripping. --of vinyl system from which the concentration of cal seals, or equivalent as provided in chloride to the atmosphere may not vinyl chloride in the exhaust gases does * 61.66. If double mechanical seals are exceed: not exceed 10 ppm. or equivalent as pro used, vinyl chloride emissions from the (i>2 g/kg (0.003 lb/lb> product from vided in 161.66. seals are to be minimized by maintaining the stripper(s) [or reactor(s) if the (3) Leakage from sump, compressor, the pressure between the two seals so plant haa no strlpper(s) 1 for dispersion and agitator seals: that any leak that occurs is into the agl- Environment Reporter [See. 61.66(bl(3(.)J ucc 026969 HAZARDOUS EMISSIONS S-3S9 121:0473 tated vessel; by ducting any vinyl chlo ride between the two seals through a control system from which the concen tration of vinyl chloride in the exhaust gases does not exceed 10 ppm; or equiva lent as provided In f 61.00. i4) Leakage from relief valves: Vinyl chloride emissions due to leakage from each relief valve on equipment in vinyl chloride service are to be minimized by installing a rupture disk between the equipment and the relief valve, by con necting the relief valve discharge to a process line or recovery system, or equiv alent as provided in 1 61.60. <5> Manual venting of gases: Except as provided in 5 81.84(a) (3 >, all gases which are manually vented from equip ment in vinyl ehloride service are to' be ducted through a control system from which tlie concentration of vinyl chloride In the exhaust gases does not exceed 10 ppm; or equivalent as provided in J 61.68. (6) Opening of equipment: Vinyl chloride emissions from opening of equipment (including loading or unload ing lines that are not opened to the at mosphere after each loading or unload ing operation) are to be minimised as follows; (1) Before opening any equipment for any reason, the quantity of vinyl ehlo ride is to be reduced so that the equip ment contains no more than 3.0 percent by volume vinyl chloride or 0.0950 m1 (35 gal) of vinyl chloride, whichever is larger, at standard temperature and pressure; and til) Any vinyl chloride removed from the equipment in accordance with para graph U>) <6) (i) of this section is to be ducted through a control system from which the concentration of vinyl chlo ride in the exhaust gases does not exceed 10 ppm, or equivalent as provided in 5 61.00. >7) Samples: Unused portions of sam ples containing at least io percent by weight vinyl chloride are to be returned to the process, and sampling techniques are to be such that sample containers in vinyl chloride service are purged into a closed process system. <8> Leak detection and elimination: Vinyl chloride emissions due to leaks from equipment in vinyl chloride service are to be minimised by instituting and implementing a formal leak detection and elimination program. The owner or operator shall submit a description of the program to the Administrator for approval. The program Is to be sub mitted within 40 days at the effective date of these regulations, unless a waiver of compliance la granted under |01.11. If a waiver of compliance Is granted, the program is to be submitted on a date scheduled by the Administrator. Ap proval of a program will be granted by the Administrator provided he finds: < i) It includes a reliable and accurate vinyl chloride monitoring system for de tection of major leaks and Identification of the general area of the plant where a leak is located. A vinyl chloride monitor ing system means a device which obtains air samples from one or more points on (vi) It contains a definition of leak a continuous sequential basis and ana which is acceptable when compared with lyzes the samples with gas chromatog the background concentrations of vinyl raphy or, if the owner or operator as chloride In the areas of the plant to be sumes that all hydrocarbons measured monitored by the vinyl chloride monitor are vinyl chloride, with infrared spectro ing system. Measurements of background photometry flame ion detection, or an concentrations of vinyl chloride in the equivalent or alternative method. areas of the plant to be monitored by the < it > It Includes a reliable and accurate vinyl chloride monitoring system are to portable hydrocarbon detector to be used be included with the description of the routinely to find small leaks and to pin program. The definition of leek for a point the major leaks indicated by the given plant may vary among the differ vinyl chloride monitoring system. A ent areas within the plant and is also to portable hydrocarbon detector means a change over time as background con device which measures hydrocarbons centrations In the plant are reduced. with a sensitivity of at least 10 ppm (9) Inprocess wastewater; Vinyl chlo and is of such design and size that it can ride emissions to the atmosphere from be used to measure emissions from local Inprocess wastewater are to be reduced ized points. as follows: (ill) It provides for an acceptable cali (1) The concentration of vinyl chlo bration and maintenance schedule for ride in each inprocess wastewater stream the vinyl chloride monitoring system and containing greater than 10 ppm vinyl portable hydrocarbon detector. For the chloride measured - immediately as It vinyl chloride monitoring system, a daily span check is to be conducted with a concentration of vinyl chloride equal to the concentration defined as a leak ac leaves a piece of equipment and before being mixed with any other inproesas wastewater stream Is to be reduced to no more than 10 ppm by weight before being mixed with any other Inproesas wastewa cording to paragraph (b) (8) (vi) of this ter stream which contains 1cm than 10 section. The calibration- is to be done ppm vinyl chloride; before belns exposed wi(A)el)fecillbratioa gaa mixture pre to the atmosphere, before being dis charged to a wastewater treatment proc pared from the gasee specified in sectlona ess; or before being discharged untreated 5.3.1 and 5.3.3 of Test Method 100 end as a wastewater. This paragraph does in accordance with section 7.1 of Test apply to water which is umd to displace Method 100. or vinyl chloride from equipment beforslt (B) A calibration gee cylinder stand is opened to the atmosphere In accord ard containing the appropriate concen ance with 161.64(a)(2) or paragraph tration of vinyl chloride. The gas com (b) (0) of this section, but does not apply position of the calibration gas cylinder to water which is used to wash out equip standard it to have been certified by the ment after the equipment has already manufacturer. The manufacturer must been opened to the atmosphere in ac have recommended a maximum shelf life cordance with 1 61.64(a) (2) or para for each cylinder so that the concentra graph (b) (6) of this section. tion does not change greater than 8 (U> Any vinyl chloride removed from percent bom the certified talus. Hie date the inprocess wastewater In accordance of gas cylinder preparation, certified with paragraph (b> (9) (1) of this section vinyl chloride concentration and recom is to be ducted through a control system mended maximum ahelf life mutt have from which the concentration of vinyl been affixed to the cylinder before Ship chloride in the exhaust gases does not ment flrom the manufacturer to the exceed 10 ppm. or equivalent as provided buyer. If a gee chromatograph is used sa in I 61.66. the vinyl chloride monitoring system. (c) The requirements in paragraphs these gas mixtures may be directly used (bXl), (b)(2). (b)(0), (b)(0), (b)(7) to prepare a chromatograph calibration curve as described In section 7.3 of Teet Method 106. The requirements in sec and (b) (8) of this section are to be In corporated Into a standard operating procedure, snr made-available upon re quest for inspection by the Administra tion 53.3.1 and 5.3.3 3 of Teat Method tor. TIM standard operating procedure ]g 100 for certification of cylinder stand to include provisions for measuring the ards and for establishment and verifica vinyl chloride In equipment M.79 mf tion of calibration standard! are to be 1,250 gal lit volume foe which an ends' followed, (42 FR 29005, June 7, 1977) tion Unfit la premribed lit 101.08(b) <6> (i) price to openhig the equipment and using Teet Method ISO. a portable hydro <lv) The location and number of points carbon detector, or an equivalent or al to be monitored and the fraquanny of ternative method. The method at meas monitoring provided for in the program urement is to meet the requirements in are acceptable when they ere compered 1 81.07(g) (5) (i) (A) or (g)((0>(l)(B>. with the number of pieces of equipment in vinyl chloride servioe and the aim and (41 FR 53017, December 3. 1976) physical layout of the Plant. | 61.66 Equivalent equipment sad pro (v) it contains an acceptable plan of cedures. action to be taken what a leak la de Upon written application from an own tected. er or operator, the Administrator may 8-12-77 Copyright 0 1977 by The Bureau at National Attain, Inc. (See. 61.06) ucc 026970 121:0474 FEDERAL REGULATIONS approve um of equipment or procedures which have been demonstrated to his satisfaction to ha equivalent In terms of reducing vinyl chloride emissions to the atmosphere to those prescribed for com pliance with a specific paragraph of this subpart. For an existing source, any re quest for using an equivalent method as the initial measure of control is to be submitted to the Administrator within 30 days of the effective date. For a new source, any request for using an equiva lent method is to be submitted to the Administrator with the application for approval of construction or modification required by { 01.07. end equivalent or alternative methods do not agree, the result* obtained by the reference method prevail, and the Ad ministrator may notify the owner or operator that approval of the method previously considered to be equivalent or alternative 1s withdrawn. (1) Test Method 106 is to be used to determine the vinyl chloride emissions from any source for which an emission limit is prescribed In || 01.02(a) or (b) I 01.63(a), or || 61.64(a) (1), <b>, (c>, or <d). or from any control system to which reactor emissions are required to be ducted In I 01.64(a) (2) or to which fugi tive emissions are required to be ducted in 1161.63(b)(1) (11), (b)(2), (b)(9). (b>(6)(il),or (b)(9)(U). c,, [Ct (2.60)010-*) [100] when: fax-kg vinyl chloride/100 kg prod uct. Ct--The concentration of vinyl chlo ride as measured by Test Method 106. 2.60--Density of vinyl chloride at one atmosphere and 20* C in kg/m*. 0--Volumetric flow rate in m*/hr as determined by Reference Method 2 of Appendix A to Part 60 of this chapter. 10~*= Conversion factor for ppm. Production rate (kg/hr). [42 FR 29009, June 7, 1977) 3 61.67 Emission tesla. (a) Unless a waiver of emission testing is obtained under 9 61.13, the owner, or operator of a source to which this sub part applies shall test emissions from the source, (1> Within SO days of the effective date in the case of an existing source or a new source which has an Initial startup date preceding the effective date, or (2) Within 90 days of startup In the case of a new source. Initial startup of which occurs after the effective date. (b> The owner or operator shall pro vide the Administrator at least 30 days prior notice of an emission test to afford the Administrator the opportunity to have an observer present during the test. (c> Any emission test is to be con ducted while the equipment being tested Is operating at the maximum production rate at which the equipment will be op erated and under other relevant condi tions as may be specified by the Adminis trator based on representative perform ance of the source. (d> [Reserved] (e) When at all possible, each sample Is to be analysed within 24 hours, but in no case in excess of 73 hours of sample collection. Vinyl chloride emissions are to be determined within 30 days after the emission test The owner or operator (i) For each run, one sample Is to be collected. The sampling site is to be at least two stack or duct diameters down stream and one half diameter upstream from any flow disturbance such as a bend, expansion, contraction, or visible flame. For a rectangular cross section an equivalent diameter is to be determined from the following equation: equivalent ditundfr^i (length) (width) lengths width " The sampling point in the duct is to be at the centroid of the cross section. The sample is to be extracted at a rate proportional to the gas velocity at the sampling point. The sample Is to be taken over a minimum of one hour, and Is to contain a minimum volume of 90 liters corrected to standard conditions. (II) Each emission test la to consist of three runs. For the purpoee of determin ing emissions, the average of recults of all runs is to apply. The average is to be computed on a time weighted basis. (III) For gas streams containing more than 10 percent oxygen the concentra tion of vinyl chloride as determined by Test Method 106 Is to be corrected to 10 percent oxygen (dry basis) for determi nation of emissions by using the follow ing equation: 2) Test Method 107 is to be used4 determine the concentration of vii. s chloride In each lnprocess wastewater stream for which an emission limit is prescribed in 9 61.69(b) (9) (1). (3) Where a stripping operation is used to attain the emission limit In { 61.64(e), emissions are to be determined using Test Method 107 as follows: (l> The number of strippers and sam ples and the types and grades of resin to be sampled are to be determined by the Administrator for each Individual plant at the time of the test based on the plant's operation. (11) Each sample is to be taken imme diately following the stripping operation. (ill) The corresponding quantity of material processed by each stripper is to be determined on a dry solids basis and by a method submitted to and approved by the Administrator. (lv) At the prior request of the Ad ministrator, the owner or operator shall provide duplicates of the samples re quired In paragraph (g)(3)(i> of this section. (4) Where control technology other than or in addition to a stripping opera tion Is used to attain the emission limit in 161.64(e), emissions are to be deter mined a* follows: hu report the determinations to the Administrator by a registered,letter dis r -r 1Q. tdwww-tt 20.9-percent 0, patched before the close of the next busi ness day following the determination. where: The concentration of vinyl [42 FR 29000, June 7. 1977] chloride in the exhaust game, corrected (f) The owner or operator shall retain at the plant and make available, upon request for inspection by the Adminis trator. for a minimum of 3 yearn reoorde of laiaatow teat results and other data needed to determine emission# (g) Uniem otherwise specified, the to 10-percent oxygen. C--The concentration of vinyl* chloride as measured by Test Method 106. 20.9Percent oxygen in the ambient air at standard conditions. 10.0m Percent oxygen in the ambient air at standard conditions, minus the 10.0-percent oxygen to which the owner or operator shall use test Test correction is being made. Methods In Appsndlx B to this pert for Percent Oj-- Percent oxygen in the each teat ae required by paragraphs exhaust gas as measured by Refer (g)(1). <g)<3>, (e)(3), (g)(4), and ence Method 3 in Appendix A of (g) (9) of this section, unless an equiva Part 60 of this chapter. (1) Test Method 106 Is to .be used to determine atmospheric emissions from all of the process equipment simultane ously. The requirements of paragraph (g) (1) of this section are to be met. (U) Test Method 107 Is to be used to determine the concentration of vinyl chloride In each inprocess wastewater stream subject to the emission limit pre scribed In f 01.64(e). The mass of vinyl chloride in kg/100 kg product In each in process wastewater stream is to be de termined by using the following equa tion: m Ihfw: CYs ICj R IQ-1 [100] "Z lent method or an alternative method has been approved by the Administrator. If the Administrator finds reasonable grounds to dispute the results obtained by an equivalent or alternative method, he may require the use of e reference method. If the results of the reference (Iv) For those emission sources where the emission limit Is prescribed In terms of mas* rather than concentration, mass emissions in kg/100 kg product are to be determined by using the following equa tion: Cst -k* \in>l fhlurkli* 109 kf product. Cc-Um uiMMtoulrtdton oI vinyl chloride us mt by Teat Method 107. Rtewotef (low rate (it 1/hr, determined lit :nvordiinco with ft method which hue been submitted to ul approved by tlM Administrator. IQr* >Conversion factor lor rank Z* Production nta (ki/nr), determined In nn'ord* tuitv with ft method which hoo town suhmitU-d and approved by the Administrator. Environment Reportor [See. 61,67(41Oil! ucc 026971 HAZARDOUS EMISSIONS S-359 121:0475 (5) The reactor opening loss for which an emission limit is prescribed in { 61.64 (a) (2) is to be determined. The number of reactors for which the determination is to be made is to be specified by the Administrator for each individual plant at the time of the determination based on the plant's operation. For a reactor that is also used as a stripper, the deter mination may be made immediately fol lowing the stripping operation. (i) Except as provided in paragraph ig.H&xui of this section, the reactor i pernng loss is to be determined using the following equation: W (2.60) (10-*) (Cb) ` " YZ C~kg vi iiy 1 chloride Fillissions/kg product. H'w* ("opacity oftb rntcLor in m*. Density of vinyl chloridt at on* atmosphere and 20 Cinkfto*. 1)-< Convonion factor for ppm. O-ppm by volume vinyl chloride as determined by Teat Method 100 or a portable hydrocarbon detector which measure* hydrocarbons with a Aeneltivlty of at leant 10 pun. 1'- NujuIht of belches since the reactor was last opened to the atmosphere. ^Averucc ki of polyvinyl chloride produced per Paten in the number ofbatches ainct; the reactor was last opened to the atmoapbara. i A) if Method lOtf- is used to deter mine the concentration of vinyl chloride <Cb>, the sample is to be withdrawn at a constant rate with a probe of sufficient length to reach the vessel bottom from the manhole. Samples are to be taken for 5 minutes within 6 inches of the ves sel bottom. S minutes near the vessel center, and S minutes near the vessel top. *B> If a portable hydrocarbon detec tor is used to determine the concentra tion of vinyl chloride (Cb). a probe of sufficient length to reach the vessel bot tom from the manhole is to be used to make the measurements. One measure ment will be made within 6 inches of the vessel bottom, one near the vessel center and one near the vessel top. Measure ments are to be made at each location until the reading is stabilized. All hydro carbons measured are to be assumed to be vinyl chloride. tC> The production rate of polyvinyl chloride <Z) is to be determined by a method submitted to and approved by the Administrator. (ii) A calculation based on the number of evacuations, the vacuum involved, and the volume of gas in the reactor is hereby approved by the Administrator as an al ternative method for determining reac tor opening loss for poetpolymerlzation reactors in the manufacture of bulk resins. 61.64 EmikiMm nwwiuwlngt i a) A vinyl chloride monitoring sys tem is to be used to monitor on e con tinuous basis the emissions from the sources for which emission limits are pre scribed in $ 61.62(a) and (b>, 1 61.63(a), and i 61.64(a)(1), (b), (c), and (d).and for any control system to which reactor emissions ate requited to be ducted fat 61.64(a) (2) ot to which fugitive emiuioas are requited to be ducted in 61.65 (b) (1) (U), and (b) (2), (b) (5), (b) (6) (ii), and (b) (9) (ii). [41 FR 53017, December 3, 1976] b) The vinyl chloride monitoring sys tems) used to meet the requirement in paragraph <a; of this section is to be a device which obtains air sampels from one or more points on a continuous sequential basis and analyzes the samples with gas chromotography or, if the owner or operator assumes that all hydrocar bons measured are vinyl chloride, with infrared spectrophotometry, flame ion detection, or an equivalent or alterna tive method. The vinyl chloride monitor ing system used to meet the requirements in { 61.66(b) ((i) may be used to meet the requirements of this section. (c) A daily span check la to be con ducted for each vinyle chloride monitor ing system used. For all of the emission sources listed in paragraph (a> of this section, except the one for which an emis sion limit is prescribed in | 61.62(b), the daily span check is to be conducted with a concentration ot vinyl chloride equal to 10 ppm. For the emission source for which an emission limit is prescribed in 3 61.62(b). the daily span check is to-be conducted with a concentration of vinyl chloride which is determined to be equivslent to the emission limit for thst source based on the emission test requited by 61.67. The calibration is to be done with either [41 FR 53017, December 3,1976] (1) A calibration gaa mixture pre pared from the gasee specified in sections 3.2.1 and 5.2.2 of Test Method 106 and in accordance with section 7.1 ot Test Method 106, or |42 FR 29005, June 7, 1977] (2) A calibration gas cylinder stand ard containing the appropriate concen tration of vinyl chloride. The gee com position of the calibration gee cylinder standard is to have been certified by the manufacturer. The manufacturer must have recommended a "sdimim shelf life for each cylinder so that the concen tration doee not change greater than 5 percent from the certified value. The date of gas cylinder preparation, certified vinyl chloride concentration end recom mended maximum shelf life must have been affixed to the cylinder before ship ment front the manufacturer to the buyer. If a gee chromatograph is used as the vinyl chloride monitoring system, these gas mixtures may be directly used to prepare a chromatograph calibration curve as described in section 7.3 of Test Method 106. The requirements In sec tions S.2.3.1 and 5.2.3.2 of Test Method 106 far certification of cylinder stand ards end for establishment and verifica tion of calibration standards are to be followed. [42 FR 29005, June 7, 1977] 61.69 Initial report. (a) An owner or operator of any source to which thle subpart applies shall submit a statement in writing notifying the Administrator that the equipment and procedural specifications in 55 61.65 (b)(1), <b)i2), (b)(3). (b)(4), (b)(3), <bH6), (b)(7), and (b)(8) are being implemented. (b)(1) In the case of an existing source or a new source which has an initial startup date preceding the effec tive date, the statement is to be submit ted within 90 days of the effective date, unless a waiver of compliance is granted under j 01.11, along with the informa tion required under $ 61.10. If a waiver of compliance ie granted, the statement is to be submitted on a date scheduled by the Administrator. (2) In the case of a new source which did not have an initial startup date pre ceding the effective date, the statement is to be submitted within 90 days of the initial startup date. (c> The statement is to contain the following information: (1) A list of the equipment installed for compliance, (2) A description ot the physical and functional characteristics of each piece of equipment. (3) A description of the methods which have been incorporated into the standard operating procedures for meas uring or calculating the emissions for which emission limits are prescribed in 1161.65 (b> (D(i> and (b)(6)(i>, (4) A statement that each piece of equipment is installed and that each piece of equipment and each procedure is being used. 61.70 Semiannual report. (a) The owner or operator of any source to which this subpart applies shall submit to the Administrator on Septem ber 15 and March IS Of each year a report in writing containing the information required by this section. The first semi annual report is to be submitted follow ing the first full 6 month reporting period after the initial report ie submitted. [41 FR 53017, December 3,1976] (b) (1) In thecase of an existing source or a new aouroe which has an Initial startup date preceding the effective data the first report Is te be submitted within ISO days of the effective data unless a waiver of compliance b granted uate 161.11. It a waiver at compliance is granted, the first report is to be sub mitted an a date scheduled by the Ad ministrator. (3) m the case ot a new source which did not have an initial startup data pre ceding the effective date, the tint report is to be submitted within 190 days of the initial startup data (o) Uhlam otherwise specified, the owner or operator shall use the Test Methods in Appendix B to this part to conduct "(--testa as required by paragraphs (e)(2) and (e)(3) of this section, unless an equivalent or an alter native method has bowl approved by the Administrator. If the Administrator finds reasonable granule to dispute the 8-12-77 Copyn ght 1977 by The Bureou of Notional Affairs, Inc. [See. 61-70(c)I ucc 026972 121:0476 FEDERAL REGULATIONS result* obtained by equivalent or al (Ill) The quantity of material proc (A) The vinyl chloride content found ternative method, he may require the use essed by the stripper Is to be determined in all the samplee required In paragraphs of a reference method. If the result* of on a dry solids basis and by a method (c> (2) (1) and (c> (2) (11) of this section, the reference and equivalent or alterna submitted to and approved by the Ad identified by the realn type and grade tive methods do not scree, the results ministrator. and the time and date of the sample, and obtained by the reference method pre vail, and the Administrator may notify (iv) At the prior request of the Ad (B) The corresponding quantity of the owner at operator that approval of ministrator. the owner or operator shall polyvinyl chloride resin processed by the the method previously considered to be provide duplicates of the samples, re strlpper(s), identified by the resin type equivalent or alternative is withdrawn. quired In paragraphs (c) (2) (1) and (c) and grade and the time and date it (1) The owner or operator shall in (2> (11) of this section. represents. clude in the report a record of any emis sions which averaged over any hour period (commencing on the hour) are in excess of the emission limits pre (v) The report to the Administrator by the owner or operator is to include the vinyl chloride content found in each scribed in || 61.62(a) or <b>, I 61.63(a), sample required by paragraphs (e)(2) or II 61.64(a) (1), (b), (c), or (d), or for (1) and (c> (2) (11) of this section, aver (3) The owner or operator shall in clude In the report a record of the emis sions from each reactor opening for which an emission limit Is prescribed in 161.64(a) (2). gmi--wi- are to be deter any control system to which reactor aged separately for each type of resin, mined in accordance with 161.67(g) (S>, emissions are required to be ducted In 161.64(a) (2) or to which fugitive emis sions are required to be ducted in 161.66 (b> (1) (11), (b> (2>. (b> (8). (b> (6) (U), or (b> ((11). The emission* are to be meas ured in accordance with I 61.68. over each calendar day and weighted according to the quantity at each grade of resin processed by the stripper(s) that calendar day, according to the fol lowing equation: except that emission! for each reactor are to be determined. For a reactor that Is also used as a stripper, the determination may be made immediately following the stripping operation. (2) In polyvinyl chloride plants for which a stripping operation is used to attain the -mH-TM level prescribed in ^-lPe.Afe, _PoIMet+PatAfat+ 161.64(e). the owner or operator shall Ati----------------------- --- - <3r( +Po.Mo,, include In the report a record of the vinyl chloride content In the polyvinyl chloride resin. Test Method 107 Is to bo when: 161.71 Reeardfcaapia used to determine vinyl chloride content as follows: (1) If batch stripping Is used, one rep resentative sample of polyvinyl chloride resin Is to be taken from' each batch of each grade of resin immediately follow ing the completion of the stripping op eration, and identified by resin type and grade and the date and time the batch is completed. The corresponding quan tity of material processed In each strip per batch Is to be recorded and Identi fied by resin type and grade and the date and time the batch Is completed. [42 FR 29006. June 7, 1977] (il> If continuous stripping Is used, one representative TMTMpi* of polyvinyl chloride resin Is to be taken for each grade of resin processed or at intervals of 6 hours for each grade of rseln which la being pioccned, whicheverIs more fre A--24-hour average concentration of type T, resin in ppm (dry weight basis). Q--Total production at type T, resin over the 24-hour period, in kg. 7\*Type of resin: *'*1,2 ... si where m is total number of resin types produced during the 34-hour period. iVf--Concentration of vinyl chloride in one sample of grade O, resin, in ppm. P-- Production of grade G resin represented by the sample, in kg. 0,-- Grads of resin; e.g., 0^ Ot, and Gi n-Total number of grades of resin produced during the 24-hour period. [42 FR 29066, June 7, 1977] (a) Tha owner or operator of any souroe to which this subpart.applies shall retain tha following Information at tha source and make It available for inspec tion by the Administrator for er mini mum of two years: (1) A record at the leaks detected by the vinyl chloride monitoring system, as required by 161.65(b) (8), including the concentrations of vinyl chloride as manured, analysed, and recorded by the vinyl chloride detector, the location of each measurement and the date and ap proximate time of each measurement. (2) A record of the leaks detected dur ing routine monitoring with tha portable hydrocarbon detector and tha action taken to repair tha leaks, as required by 161.68(b) (8). Including a brief state ment explaining the location and causa of each leak detected with tha portable hydrocarbon detector, the data and time of the leak, and any action taken to quent. The sample is to be taken as the iUmlnitf tbit ink* realn flows out of the tripper and ldm- (42 FR 29006, June 7, 1977] tifled by resin type and grade and tbs (vi> The owner or operator shall re (3) A record at emission date and time the ""t1* was talma. tain at tha source and make available in accordance with 161.66. The corresponding quantity of material for invention by tha Administrator for processed by each stripper over the time a minimum of 2 years records of all data period renr--ted by the sample during needed to furnish the Information re the eight hoar period, is to be recorded quired by paragraph (c> (2) (v> of this and Identified hr resin type and grads section: Tha records are to contain tha (42 FR 29068, June 7, 1977) (4) A dally operating recant for < polyvinyl chloride reactor. Including preeraree and temperature* and tha date and time it following information: [42 FR 29096, June 7, 1977} Environment Reporter [See. 61,71(e)(411 ucc 026973 hazardous emissions S-359 121:0497 U>m 100 iTmminunii or Vnm. 0SLOMM nOH 8T*TtD*JJIT fiOOSCTO (41 FR 465S9, October 21, 1976] Performance of this method should not bo attempted by pemona unfamiliar with the operation of a gaa chromatograph, nor bp thoee who are unfamiliar with source sempUng. ae there are many detail* that are beyond the eoope of thta presentation. Care must be ezerelaed to pretent ezpoaure of ---rM"t peraonnel to tinyl chloride, a ear* clnogon. 1. Principle and Applicability. 1.1 An Integrated bag aample of ataeh gaa containing tiny! chloride (chletoathene) la eublaeted to chromatographio analyala, ostng a flame Ionnation deteeter. [42 FR 29005, June 7, 1977) 1.3 The method la applicable to the mere momentof tinyl chloride in meek gaeee from ethylene dichlorldo, tinyl chloride and polytinyl chloride manufacturing pamwt sxeept where the tinyl chloride ie contained In particulate matter. 3. Benge and fionstttvity. The lower Umtt of detection will vary ac cording to the chromatograph mad. Velum reported Include 1 X-10-* mg and 4 x id1* mg. 1 Mention of trad# on apectfle prod uct! does not constitute endorsement by the Environmental Protection Agency. 3. Inttr/trtneat. Acetaldehyde, which can occur in come tinyl chloride courser, will in terfere with the tinyl chloride peek from the Chromaeorb 103 * column. See aaettona 43.3 and 6.4. If reeolutlon of the tinyl chloride peek la still not satisfactory for a particular cample, then chromatograph pa- rametora can be further altered with prior approval of tho Administrator. If alteration of the chromatograph pawn*ten fall* to resolre th* tinyl ehlorldo peak, than sup plemental confirmation of the tinyl chloride peak through an absolute analytical tech nique. such a* masa spectroscopy. must he performed. [42 FR 29009, June 7, 1977] 4. Apparatus. 4.1 Sampling (Figure 104-1). 4.1.1 Probe--Stainless steel, pyrez glass, or Teflon tubing according to stack temper ature. seek equipped with a glass wool plug to remove particulate matter. 4.13 Sample Una--Teflon, 0.4 mm outside diameter, of nMud length to connect probe to beg. A now unused piece la employed for each series of bag sampler that constitutes lAMlMOBtNi 443 MMe (3) and female (3) stainless steel quick-connects, with ball checks (one pair without) located aa shown in Figure 100-1. [42 FR 29009, June 7, 1977) 4.1.4 Tsdlar bags, loo liter capacity--To contain -~p Teflon bags are not accept able. Alumlniaed Mylar bags may ha used, provided that the samples are analysed within 34 hours of collection. 4.13 Rigid leakproof containers for 4.1.4, with covering to protect contents from sun light. 4.1.0 Needle valve--To adjust sample flow rata. 4.1.7 Pump--Leak-free. Minimum capac ity 3 Uters par minute. 4.13 Charcoal tube--TO prevent admis sion of vinyl chloride to atmosphere in vicin ity of samptera. 4.13 Flow mater--For observing sample flow rate: oapaMe of measuring a flow range from 0.10 to 130 liter per minute. 4.1.10 Cbanocfiny tubrny. Teflon. 0.4 mm outside diameter to assemble sample train (Flguie 1QO-1). [42 FR 29009, June 7, 1977] 4.1.11 Pitot tube--Typo S (or equivalent), attached to the probe so that the sampling flow rata can be regulated proportional to tho stack gae velocity. 43 Sample recovery. 43.1. Tubing--Teflon, g.4 mm outside diameter, to oonnect beg to gaa chromato graph sample loop. A new unused piece la employed fee each series of hag samples that constitutes an teat, and la to he dis carded upon conclusion of analysis of thoee baga. 43 Analysis. 4.3.1 Oaa chromatograph--With flame v-anim dstsotor. potentlometrte atrip chert recorder and 13 to 83 ml heated sam pling loop In automatic sample valve. 433 Chromatographic column, stainless steel, 3 mx33 man containing 80/100 mcah Chromaeorb 103. A secondary column of OB SF-M. aopcrosnt on 80/80 mseb aw chrome- sorb F.stalnlero steal, 3 mx3J mm or Pore- pek T, 80/100 msah, eteinlcm steel, l mxSJ mm' la required if geetaldshyde la present. If need. > secondary oolumn is plaosd attar the CbroumaorU ios column. The combined columns should then be operamd at iso* C. [42 FR 29009, June 7, 1977] 433 Plow mstam (3)--Rotameter type, 0 to 100 ml/min capacity, with flow control VllVMi 43.4 Oaa regulators Poe required gas cylinders. 4.3 3 Thermometer--Accurate to one de gree centigrade, to measure temperature of heated sample loop at time of sample injec tion. 'l * Barometer--Accurals to 6 mm Hg, to measure atmospheric pressure around gas cn.'omi.onreph during sample analyala. t.3,7 Pump--Leak-free. Minimum capac ity 100 ml/min. 4.4 Calibration. 4.4.1 Tubing--Teflon, 8.4 mm outside diameter, separate pieces marked for each calibration concentration. 4.43 Tcdlar bags--BUtean-inch square slae, separate bag marked for each calibra tion concentration. 4.4.8 Syringe 0.8 ml, gas tight. 4.4.4 Syringe--30*1, gaa tight. 4.43 Plow meter--Rotameter typo, 0 to 1000 ml/min range accurate to 1*. to meter nitrogen in preparation of standard gM nlztuftiv 4.4.8 Stop watch--Of known accuracy, to time gaa flow in prepetition of standard gaa mixtures. S. Reagents, it is necessary that all rea gents be of chromatographic grad*. 5.1 Analysis. 9.1.1 Helium gas or nitrogen gaa--Zero grad*, fee chromatographic carrier gaa. 3.13 Hydrogen gae Zero grade 3.13 Oxygen gaa, or Air, aa required by the detector--Zero grade. 83 Calibration, Uee one of the following options: either 83.1 end 833, CC 833. 83.1 Vinyl chloride: 8834- percent. Pure vinyl chloride gae certified by tho manufao- tvtrcr to oontaln * minimum of 803, percent vinyl chloride fee use in the preparation of standard gae mlxtune in Section 7.1. If the -- gaa manufacturer maintains a bulk cyllndge supply of 993+ percent vinyl chloride, the certification analysts may have baas pa*, formed on this supply rather than on each gaa cylinder prepared from this bulk supply. Hie date of gaa cylinder pceperatiea and the certified analysis must have been affixed to th* cylinder before shipment from the gee manufacturer to tho buyer. 833 IWnym pas. zero grade, for prepe- ntktt of oteDdiM no mirhir-- 833 cylinder iMndsrde (3). Oaa min. tuzo standards (80, 10, and 0 ppm vinyl chloride in nitrogen cylinders) for which th* gae oomposmon has bean ocrtlflsd by the manufacturer. The manufacturer must here recommended a maximum shelf Ufa for each cylinder so that the concentration doss not change greater than ns percent from the certified value. The date of gaa cylindsr prep aration. certified vinyl ehlorldo concentre tion Astf neammodid thiMf lift mom have been affixed to the cylinder before shipment from the gee manufacturer to tho buyer. Thsee gas mixture standards may be directly used to propose e chromatograph oalffitmUon curve ae described in section 73. 833.1 cylinder standards ctrtt/loatum. The concentration of vinyl chloride in nitro gen In seen cylinder must have been certified by the manufacturer by a direct analysis of each cylinder using an analytical procedure that the manufacturer had oaUbtated on tte day at cylindsr analyala. Tha calibration of the analytical procedure shall, aa a minimum, have utilised e three point calibration curve. It la recoinmended that the manufacturer maintain two calibration standards and uae theca standards In the following way: (1) a high concentration stasidaid (between SO and 10O ppm) for preparation at a oallbratMt curve by an appropriate dilution technique; (S) a low oonmntnum standard (balesen Sand 10 ppm) for vsnllcaMon of the dilution used. 0333 htsMUtemt and wthdiM of saiibrefioa standard*. Tho concentration at each calibration standard must have bean established by tha manufacturer using 8-12-77 Copyright 1977 by The Bureau of National Affairs, Inc. [Appendix B) ucc 026974