Document MoeDkgE3d57JLKwKw2egbZXj

\ ^Chemicals and Plastics India MO. OWICCi DHUN BUtLOHM. 171/1, HOUMT HOAD, r. B. Mk. SMB THOM: MC1I-4 OUMi CHCHCLAtT 5. RAMASWAHY Gnrml Haniar March 8, 1977 & Mr. J.E .Stroope B.F. Goodrich Chemical Company 6100 Oak Tree Boulevard Cleveland Ohio 44131 USA Dear Mr.Stroope: Thank you for your letter of November 11, 1976, which reached me here on February 28, 1977, enclosing copy of the newly issued National Emission Standards for Vinyl Chloride, published by the United States Bavironmental Protective igency. This is certainly of interest to us and I have not received a copy of this from any other source. It is nice of you to have sent this copy on to me, which I am circulating to the senior people in the plant also. With kind regards, Yours sincerely. Cc: Mr.A.L. Hatfield BFG32312 Bovaaber 11, lf74 Mr. S. Iimwm? rhsadt ala and Plasties laila, Ltd. P.O. Bos 2748 Madras 400002, India Deer Mr. laanaaqr: Bhcloead la a copy of tha newly-leaned Vatlonal Badsslon Standards for Vinyl Chloride, published by tha Halted States larlronaaatal Protective Agency. this la seat to you in the mt that yon here net obtained a eopy from aay other aoaree. We know this will be of Interest to yon. Best regards. John B. Streeps Mreetor-Maanfactaring and laginearing Services BFG32313 24548002 PART II: ENVIRONMENTAL PROTECTION AGENCY NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS Standard For Vinyl Ckloride BfG32M4 CQOSt'Sf'Z tuns ANO REGULATIONS te be captured and water usage would be employed CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY iru eia-u and that then would ba no recycling BUUI AMS SMVnOMMSWtSL Iwem af water. Than la no regulation which Mould regain water recycling. Accord EPA' prepared a document entitled the ing to an. the control system utilizing Qecatltatfoe Risk Assessment /or Com- the meet water will not be used gener PART 61--NATIONAL EMISSION STAND immlty Exposure to Vinyl Chloride which ally by the Industry and economic fac ARDS FOR HAZARDOUS AIR POLLUTANTS eetlmetee the risk from vinyl chloride tors win cause plants to recycle much Standard for Vinyl Chloride On December 24. 1171, exposure to population living In the vl- at tbs water. Therefore, according to einity of vinyl chloride-emitting plants SPI the impact of the standard on water before and after implementation of con consumption will be negligible. 112 of the Clean Air Act, aa amended (42 UAC. 1857). the Environmental Protec tion Agency (SPA) added vinyl chloride to the list of hazardous air pollutants (40 FR 59477) and proposed a national trols to meet the standard. There are no The environmental impacts of the dose-response data for the concentra promulgated standard may be summar tion of vinyl chloride found in the am-, ised as follows: The primary environ blent air. Therefore, assessments of risk mental Impacts of the standard are ben at ambient levels of exposure were ex eficial and will consist of vinyl chloride emission standard for it (40 PR 59522). trapolated from dose-response data from emission, reductions of approximately 94 The standard covers plants which manu higher levels of exposure using both a percent at ethylene dichloride-vinyl facture ethylene dlchlortds. vinyl linear model and a log-probit model. chloride plants and 95 percent at poly chloride, and/or polyvinyl chloride. Extrapolations made with each of those vinyl chloride plants. Percentage num XPA decided to regulate vinyl chloride models entailed using different sets of bers for both source categories are based because it has been Implicated as the assumption. Because different assump on an estimated 90 percent reduction in causal agent of angiosarcoma and other tion can bo mado In extrapolating to fugitive emissions and 1974 emission serious disorders, both carcinogenic and low doses, the health risks are reported noncarclnogenlc, in people with occupa in ranges. tional exposure and in animals with ex It was estimated that 4.6 million peo perimental exposure to vinyl chloride. ple live within 5 miles of ethylene dlchoReasonable extrapolations from these ride-vinyl chloride and polyvinyl chlo findings cause conetm that vinyl chlo ride plants and that the average ex ride may cause or contribute to the came posure around these plants before instal or similar disorders at present ambient lation of controls to meet the standard air levels. The purpose of the standard la is 17 parts per billion. The exposure to minimise vinyl chloride emlaalone ' levels for uncontrolled plants were cal The potential secondary environmen tal Impacts of the standard are either Insignificant or will be minimized with out additional action, except for one ad verse impact. Hydrogen chloride is al ready emitted by process equipment at ethylene dichloride-vinyl chloride plants and by other petrochemical plants in the complexes where ethylene dichloride- from ell known process and fugitive culated baaed on estimated 1974 emis vinyl chloride plants are typically lo emission sources In ethylene dichloride- sion levels. Using the linear dose-re cated. An incinerator used to attain the vinyl chloride and polyvinyl chloride sponse model, EPA found that the standard at an ethylene dichloride-vinyl plants to the level attainable with beet rate of initiation of liver angiosarcoma chloride plant could Increase hydrogen available control technology. This will among people living around uncontrolled chloride emissions by several fold. Typi have the effect of furthering the protec plants is expected to range from less than cally. however, due to the corrosion prob tion of public health by minimizing the health risks to the people living in the vicinity of these plants and to any addi tional people who are exposed aa a result one to ten cases of liver angiosarcoma per year of exposure to vinyl chloride. The log-probit model gave predictions that are 0.1 to 0.01 times this rate. This lems which would otherwise occur both on plant property and in the community, plants use scrubbers to control already existing hydrogen chloride emissions. of new construction. wide range is an Indication of the un Hydrogen chloride emissions resulting Interested parties participated In the certainties in extrapolation to low doses. from control of vinyl chloride emissions rulemaking by sending comments to EPA. Due to the long latency time observed in are expected to be controlled for the The comments have been carefully con cancer cases resulting from vinyl chloride same reason. If even a moderately effi sidered. and where determined by the exposure. Increases initiated by exposure cient scrubber (98 percent control) were Administrator to be appropriate, changes this year .win not be diagnosed until the used to control the hydrogen chloride have been made to the regulation as pro 1990b or latsr. Vinyl chloride is also es emissions resulting from incineration of mulgated. timated to produce an equal number at vinyl chloride emissions, the increase in Sumcsav or tbs Stamms* In ethylene dichloride-vinyl chloride plants, the standard limits vinyl chloride primary cancers at other sites, for a total of somewhere between less than one and twenty cases of cancer per year of ex posure among residents around plants. hydrogen chloride emissions from a typ ical ethylene dlchloride-vinyl chloride plant due to the standard would be re duced to 35 percent. However. EPA plans emissions from the ethylene dicbloride The number of these effects is expected to further evaluate the need to control end vinyl chloride formation end puri to be reduced at least In proportion to the hydrogen chloride emissions, since dif fication processes to 10 ppm. Tor the ox- reduction in the ambient annual average fusion model results indicate that under ychlorination process, vinyl chloride vinyl chloride concentration, which is "worst-case" meteorological conditions, emissions are limited to 02 K/kg of ethyl expected to be 5 percent of the uncon the hydrogen chloride emissions from ene dichloride product. trolled levels after the standard is im the process equipment and the incinera In polyvinyl chloride plants, the stand plemented. tor combined would cause maximum am ard limits vinyl chloride emissions from Changes In the standard since pro bient concentrations of hydrogen chlo equipment preceding end Including the posal do not affect the level of control ride in the vicinity of ethylene dichlo stripper In the plant process How to 10 required. Thus, the environmental im ride-vinyl chloride plants to be in the ppm. Emissions from equipment follow pact of the promulgated standard is, some range or somewhat higher than ing the stripper are to be controlled by with one exception, the same as that existing foreign standards and National stripping dispersion resins to 2000 ppm described in Chapter 6 of Volume X of Academy of Sciences (NAS) guidelines and other resins to 400 ppm. or by using the Standard Support and Environmen for public exposure. equivalent controls. Vinyl chloride emis tal Impact Statement. According to data sions from reactor opening are to be re submitted by the Society of Plastics In Economic Imfact duced to 0.02 g/kg polyvinyl chloride dustry, Inc. iSPI), the Impact on water In accordance with Executive Order product. consumption in the draft environmental 11821 and OMB circular A-107. EPA In both ethylene dlchlorlde-vinyl chloride and polyvinyl chloride plants, relief valve discharges and manual vent ing of gases are prohibited except under emergency conditions. Fugitive emissions Impact statement was overstated. In es timating the Impact on water consump tion. EPA based Its estimates on worst case conditions. That is. EPA assumed that those control systems with the carefully evaluated the economic and inflationary impact of the proposed standard and alternative control levels and certified this in the preamble to the proposed standard. These impacts are nOCBAl UOISTEt, VOL 41, NO. SOS--TMUWOAV, OCTOSm 21. 1*7* BFG32315 rttonimil to Chapter V of AA a Brittle hearing toe stmtM Iwift and III fnyirf jHtfiMrt, standard on psopoe*d standard tm nHM in lf hr the an* major change to toe eeeoetoto im the Society of tha pact udnk. VA (isttroatod Mat tbto by* laa, Dnr Cheoinl would M four plant domra aa a result sfeftoroefc corporation* ibd tie oi prpfm*nfttf itiodint ofthi imi PHmmfr iM Iter Coptic of idiottM ii ponlili doRBv ma* toe comment letter* received, the publle didates. ona 1ms given notice Vat It no hearing raoerd. and a summary of tha longer produce* poiyvbqri ebtoJde and comment* with KPAh responses an tbs other tom hev* indicated that they available for public inspection and copy do not toteod to doaa aa a rasa* of tbs ing at the KPA Public information M> stewlutfa erence Quit Room 3933 (SPA Library). levels are Tbc economic impact! of toeprooul- 401 U Street SW. Washington. DC. lb expected to change, and gathering the gatsd standard may ba summarised aa foOoms: The total capital'coat tor exist ing plants to mast tba standard la esti mated to be UN minion, of wtitcb fM minion la lor ethylene dlchkuld* vinyl addition, copies of the oommant sum mary and Agency reeponem may be ob tained upon written request from-the PubUe Information center (PM-315), environmental Protection Agency, 401 data would take considerable tone both an the part ef SPA and on the part of toduatry-Btoee toe ptopoee of the standftfd it to mixrimtit fTTlff<Tf, thus not* onrrtnt <Ute vooNI not offset tbe mad- chloride plants and tits mlBlon la tor polyvinyl chloride planta SPA estimates that thaaa plonta will have to spend $70 mfllton per year to maintain the required doji^on IffTtti. Z& ^ ff^|| M Street SW. Washington. D.C. 30460 (specify Standard Sapport end Jtmiroameafof Impact Statement, KmUaitm Standard for Vtafl Chloride. Fohrnu //). ard itself. Tba 1974 emission levels were also used in diffusion modeling to project maximum ambient air concentrations around uncontrolled plants. These maxi mum sir concentrations would probably capital coat for existing Plante to meet the SPA'S ion water effluent gukMtae limitations Is expected to be tto mflMcn and the total annualised operation cost la $17 million. The costs to tbc industry of meeting the OSBA standard cannot be Quantified at this time, but they are ex pected to overlap to some degraa with tba costs to meet SPA's fusltire emission regulations. The costs of mooting the fugitive emission regulation! era included U) Decision to Bat dost chloride m AosordoKf tor peButoat, la general, tha oonmenten did not contest spa's deci sion to Uet vinyl chloride as a hasardous air pollutant However, three cemmentero (two companies and one Pbiteal agency) argued that SPA placed undue emphasis on factors suggesting that vinyl chloride presented a health risk and be lower U197S emission levels were used. This would redue* toe relative Impact ef toe standard Wee that described to toe Standard Sapport end Snvironmentel Impact Statement, but would not ift the basis of toe standard Itself. (3) Approach for Repelettop Vtnri Chloride Coder Section lit. Two ap proaches other than using bast avail able control technology wore suggested by toe commenter* for regulating vinyl to the total costa cited above tor netting Ignored factors suggesting that no sig chloride under section 123. The first was tba promulgated regulation. Broken out nificant risk was involved. Under section to ben polyvinyl chloride product* for separately, tbs capital coat of masting 113, however. SPA could remove vinyl which substitutes are currently aiallahle the fugitive cmMon regulatlobs Is $97 chloride from the list of htearrtous air and to gradually phase out other poly mfllton a*d tba antiuiUmd coat Is $38 pollutants only if information wore peu- vinyl chloride products aa substitutes million. ssnted to SPA that Shows that vinyl are developed. Tba standard la not expected to deter construction of new ethylene dtohtoride- chloride Is dearly not a hssardous air pollutant As discussed more fully in the m the preamble to the proposed stand, ard KPA speolSed 1U reasons tor not set vtnyl chloride plants or moat types at comment summary, the commontors did ting a sero emission limit for vinyl new polyvinyl chloride plants. For one not provide conclusive evidence thatvinyl chloride, as fellows: (1) There are bene type of polyvinyl chloride plant (disper chloride Is not a hasardous air pollutant ficial naas of vinyl chloride products for sion proceat) that represents l$ percent which census or contributes to death or which desirable subetltutes are not read of the industry production, the standard serious Ulnees. nor did they conclusively ily available; (3) titers are potentially would significantly deter the construc prove that the health risk factor* ea- adverse health and environmental im tion of smaller plants. phastoed to SPA were insignificant pacts from substitutes which have not It Is estimated that the plies of poly Several other couunenters agreed with been thoroughly studied: (3) there are a vinyl chloride resins wil! rise by approxi mately 7.) percent in order to maintain precontrol profitability and also to re SPA's decision to Ust vinyl chloride as a hasardous air pollutant but argued that SPA had overstated the health problem, number of employee*. particularly in too fabrication industries, who would be come at least temporarily unemployed; cover the total annualised control costs necessitated to the standard at ethylene tha emission levels, and the projected ambient air concentrations around un and (4) control technology Is available which is capable of substantially reduc dichloride-vinyl chlorideplants and poly vinyl chloride plants. This increase is controlled plants. With regard to the al leged overstated health problem, the ing emissions of vinyl chloride into tba atmosphere. estimated to translate Into a maximum commcntere stated, for example, that too KPA agrees that substitutes do exist or consumer mice increase to roods fabri 0A worker SPA discussed as having could be manufactured for most poly cated from polyvinyl chloride resins of been exposed to vinyl chlorido levels tow vinyl chloride usee. However, in general, approximately 3.5 percent Recovery of er than those usually encountered in these substitutes do not have some of the effluent annualized eosts plus mainte polyvinyl chloride production has been more desirable characteristic* of poly nance of precontrol profitability b esti dropped from the National Institute of vinyl chloride, such as nonflammability. mated to add approximately 3 percent to polyvinyl chloride resin prices end remit In an additional maximum consumer price increase of 1 percent Pueuc VutxKtnaem During the public comment period. M comment letter* on the proposed stand ard were received. There were 24 from industry; 3 from environmental groups: IS from Federal. State, and local agen cies; and > from individual citterns. as required by section 113(h) (1) (B) of the Occupational Safety and Health's listing of workers with angiosarcoma. SPA agrees that there are questions concern ing the level at exposure and to some eases tha pathology of these cases not involved directly to polyvinyl chloride and vinyl chloride production. Those un certainties arc stated to the appropriate footnotes of the Scientific and Technical Anmment Report on Vtrt Chlorideend f*o(yi>l*yi Chloride (STAR) when the angiosarcoma ease* are listed. However, to spite of these uncertainties, to view of If vinyl chloride and polyvinyl chloride were banned, other substitute* with these more desirable characteristics would likely bo developed. There Is a risk that these subetltutes would ate have adverse health or environmental efforts. Since control measures ere available which can reduce vinyl chloride emis sions by 90 percent or more, it docs rot seem prudent to reduce emissions tor the remaining percentage and take toe risk ef introducing new untested chemicals into theenvironment. HDCKAl MOISTU, VOL 41, NO. VOWIMUtWAV, OCTOOM It, t*? fOQSPSPZ BFG32316 sisw AMD MQtflAnOMfi Another approash --rti< br Ms, --PM<*> at no mo-- than M| m* <#g v--rtfag will be permitted -- a foet resort cotnracnteiswastoba--tliertanflsHter gal). Reactors in this si-- range cap gen the rsUsf --1-- epene. The saa-- --eh individual smfreion note on --at erally be found In a laboratory, wfasrsas a-- required for versus benefit Several gf M fugitive the larger naoton are typfcaEy pBot _ to tha atmosphere ss a-- sources wart named speettestQy acalc facilities. Eatitflo--from laboratory repaired for rotfordieohargao. u one* far which the eoata of control scale equipment are relatively man, and There a-- several she-- in the nu- were substantially hither than the feane* application of the controls required fey aMdoal t****iitf*^ limit* in the aramii. flu. A1though SPA did detonate a the standard would be expansl-- and im gated standard. Except Mr the standard benefit ratio for the control* practical. EPA also decided to exempt re for reactor opening toss, the-- changes for a number of eataion point*. SPA search and development facilities con simply Involve conventan to the Interna doe* not believe cuch a ratio 1* *n appro taining reactors greater than 0.19 m* (50 tional System at Units Off). There was priate basis on which to set a standard, gal) and no more than 4.07 m* (1100 gal) an srror invohrsd in the original calcula flection ill cf the Clean Air AetprosMaa in capacity from all parts of the standard tion u--d to derive the standard tor reac for the development of standarda baaad except the 10 ppm limit for re--tors, tor opehlng. Correcting this error dou on best control technology (conafetering strippers, monomer recovery systems, and bles the allowable emissions. Zt Is em costs). Even under asetion 111. however, mixing, weighing and holding containers. phasised that the change in this stand standard* are not based on a fine bal EPA decided not to require the-- facili ard is a correction, and not a change in ancing of cosU versus benefits, instead, ties to meet other parts at the Stamford the intent for the degree at control re cost* are considered in tarns of the af- because of the technical prohlsms in quired. fordabilitr of the control technology re volved in doing so. For ex*mule, the The propoeed standard required the quired to achieve a given emission level standard for reactor opening is baaed in installation of a rupture disc beneath and the economic impact of passible part on reducing tbs frequency of open each relief valve to prevent leakage from standards on the industry in ques ing the reactor. Research and develop the relief valve. A provision has been tion. Unlike section 111. section 113 does ment reactors ha-- to be opened after added to the promulgated standard so not explicitly provide for consideration every batch for thorough cleaning. Ate . that a rupture disc is not required if of costs, so it would dearly be inappro stripping technology is developed Indi the relief valve is tied into a process line priate to consider casts to a greater ex vidually for each resin in research and or recovery system. In this case, any tent under section 113 then would be development equipment. Therefore, at leakage from the relief valve would be done under section 111. As dlscnmed in tainment of the stripping limitations in contained. the preamble to the proposed standard the research and development equipment The regulation for obtaining vinyl for vinyl chloride, SPA believes coats would not always be possible. Tbs 4.07 chloride samples has been changed to an may bo considered under section 113, but only to a very limited extent; 1a. to assure that the costs of control technol ogy are not grossly disproportionate tp the amount of emission reduction m* <1100 gal) figure was selected -- an upper cut-off point because there are no commercial re--tors smaller than this. (4) Emission limits. The only major Change in the emission limits between operating procedure. The proposed standard stated that there were to be no emissions from taking the samples. Several eommenters pointed out that the nee of the word "no" would make this achieved, in comparison with other emission points, the costs of controlling the fugitive emission sources mentioned by the commenters are relatively small compared, with the amount of emission reduction achieved. Several eommenters recommended adding to the regulation a provision for excess emissions during startup, shut down. and malfunction. EPA considered proposal and promulgation is the addi tion of a provision for emergency manual venting of vinyl chloride from re--tors to the atmosphere. The proposed stand ard prohibited all manual venting to the atmosphere. In the preamble to the pro posed standard, EPA invited inter--ted persons to comment on whether permit ting manual venting to the atmosphere could result In overall lower emissions. regulation impractical to enforce. There fore, the promulgated standard specifies the operating procadure which EPA orig inally intended to be used to control this source. This revision Is only a chance in wording and doss not represent a change In the level of the standard. The regulation for taking samples has ate been revised to apply only to sam ples containing at least 10 percent by this comment, and deekfod that this addition is not necessary for the vinyl chloride standard. 8tartup and shutdown There are several methods available for preventing relief discharge* from re--- tors, one of which is manual venting at weight vinyl chloride. This is consistent with the other parts at the standard which apply to equipment "In vinyl of the process has essentially no effect part of the re--tor contents tor purposes chloride service." "in vinyl chloride serv on emissions to the atmosphere for poly vinyl chloride production, and technology exists to avoid excess emissions during of cooling and reduction in pressure within the reactor. The higher the tem perature and pressure within the reac ice" distinguishes between situations where vinyl chloride is clearly involved and situations when vinyl chloride is a startup and shutdown at ethylene di- tor, the greater the amount of vinyl minor component or contaminant, and chlorideviayl chloride plants. We do not believe plants should be allowed to emit chloride which has to be removed to bring the reactor under control. Manual as defined in promulgated |91.6Ki> means that a piece of equipment con excess emissions during malfunctions, venting can be done at a lower pressure tains or ccmt--ts either a liquid that is and therefore are requiring them to shut down immediately. (3) Selection of source categories, m than the pressure required to open the relief,valve. For this reason manual vent ing can result in lower emissions than at least 10 percent by weight vinyl chlo ride or a gas that is at least 10 percent by volume vinyl chloride. the preamble to the proposed standard would occur by allowing the reactor to The propoeed standard required a vinyl EPA recognized that some small research and development facilities may exist discharge through the relief valve. Fur thermore. a manual vent valve is under chloride monitoring system for continu ously measuring vinyl chloride levels both where the emissions of vinyl chloride are insignificant and covering these facilities the control of an operator and can be dosed. A relief valve may become dogged within the plant (for leak detection) and within stacks. The proposed standard did under the standard would be and inappropriate. However, unnecessary EPA did not with "would resin and be loss of not do--. The result all the re--tor contents. have sufficient information available to dearly define which facilities should be The contents of a re--tor can be man ually vented to a gasholder or other hold excluded from the standard, and ing vessel. However, in some cases, such encouraged interested parties to submit as during severe weather conditions, sev such information during the comment eral re--tors may be out of control at period. Based on the information sub one time. There would be Insufficient mitted. EPA decided to exempt poly holding capacity under the-- conditions vinyl chloride reactors and as-dated to manually vent the contents of all the not outline required specifications for the monitoring system, except that it was to analyse the samples with gas chromatog raphy. or if all hydrocarbons were as sumed to be vinyl chloride, with infrared spectrophotometry, flame ion detection, or equivalent It required that each plant submit a description of its monitoring system to EPA. so that EPA could deter mine whether it was acceptable or not Comments were received indicating a equipment tram applicability of oil parts reactors to a gasholder. Therefore, when need for EPA to specify some criteria for of the standard if the reactors are used all other measures to prevent relief valve Judging the acceptability of monitoring in research and development and have a discharges have been exhausted, manual systems. The accuracy of U monltor- FfDCIAl MOISTtS, VOL 41, NO. MS--IHUtSMV. OCTOSM 31, 1*7* BFG32317 frtroffl m s I f f B to h t e r i 1 1 KUIES AND MIOVUTIOIIt taw witen would bo rvlatsd to tho fre (gHSHtt). and ei.tote) (Si to so thot quency of calibration. Thsnfon. B>A mtoaunuMBt of the vinyl chloride lev* etocro wqusoted tout they be mude km boo In M1* promulgated stud* to the resins k to be mads immediately jU^BteMMmthMkto id muimuli for U ftogaenco of after stripping k completed rather than calibration and procedures to bo carried as tha reata k baton transferred oat at tK. oat tai Um calibration o< toe SMnitoring the stripper. Thk allows a plant to cany k sufficient evidence to twitesto toot instruments oat operations to a stripper after strip them resins am more difficult to strip The portable hydrocarbon detector re ping has been computed bat befort it is than other rarias. With regard to mak quired by Um propooed standard was * transferred out of tho stripper. Thk k ing too stripping levels tor dispersion qulred to hove o semittvtty of 6 ppm. consistent with the original Intent of the resins teas stringent, only one of toe right Comments were received Indicating thot standard. manufacturer* eg dtapenten resins spe- instruments In this sensttMtr range art The regulation tar loading and unload oBteaBy commented that the dhpersion delicate end require continuing matute- ing Unas In 161.61(b) (1) has bens re min standard should be made less nance. The portable hydrocarbon detec vised to clarify that tt applies only to stringent, only two at several grades of tor is required for leak detection and for Hues that on disconnected after each dispersion resins made by tote company measuring vinyl chloride concentrations loading or unloading operation. Perma cannot meet the 1000 ppm Unfit. The Inside the equipment before opening it. nently installed pipelines that are opened propoeed standard takes Into considera A 6 ppm sensitivity is not needed hi Infrequently for Inspection or matnto tion that come resina an more difficult either ease; end the required eensitivttar nance, for example; are covered by toe to strip than others by providing for has been changed to 10 ppm in the pro opening of equipment regulation rather averaging among different resins. mulgated standard. thin Um umI ttfif (8) Ttoftoy, reporting, aat record- The proposed standard contained a Kgnlfttioo. kooptng. Thera are several relatively single regulation for comprcmors. The _1he regulation tor tnprocces waste- minor changes in toe testing, reporting, promulgated standard has separate regu water fa tot proposed standard could and recordkeeping requirements, a pro lations for rotating and reciprocating have bean mktotarpretsd to require in vision has bean added to 101.67 which compreeeora This is consistent with hav dividual treatment of wastewater require* that stack gas samples token ing separate regulations for rotating and streams. Beotian 61.65(b) (f)(1) of too with Tbst Method 106 an to be analyzed reciprocating pumps in both tha pro promulgated standard rlsrifiss tost within M home. This is consistent with posed and promulgated standards. wastewater streams that are required to too requirements in the proposed Test Section 61.66 of the propoeed standard be treated (Le- those containing greater Method 106. The promulgated standard , provided for the use of equivalent meth than 16 ppm vinyl chloride) can be com also specifies toot in averaging toe re ods of control which have been approved bined to be treated. However, waste sults of too throe runs required by Test by SPA. The promulgated standard re water streams that contain greater than Method 106. a teas-weighted average Is quires that the plant owner or operator 10 ppm vinyl chloride cannot be com to be used. submit a request for determination of bined with wastewater streams that con One eommentar requested tost the equivalency within 36 days of the pro tain less than lQ ppm vinyl chloride be oxygen content and moisture content be mulgation date If the alternative control fore treatment; Le- dilution cannot be specified for the 10 ppm concentration method Is intended as the Initial means need to meet the standard. standards. The propoeed standard speci of control. The purpose of thfc k to pro The commenters recommended several fied that tha vinyl chloride concentration vide time for SPA to evaluate the method changes in the --<-> limits which k to be corrected to 10 percent oxyyen before the plant has to be In oompHanoc have not been Incorporated into toe (wet basis) If combustion k used as toe (for existing sources, 66 days after the promulgated standard. These an dis control measure, in the promulgated promulgation date). SPA also suggests cussed in the following paragraphs. standard, thk requirement hoe been ex that this request for determination of It was recommended that the icquiro- panded to aU control measures. equivalency be accompanied by a re ment for double mechanical seals on A provteteQ has been added to the quest for waiver of eomplianee pursuant pumps, compressors, and agitators be re promulgated standard which states that to section 112(e) (1XBHU) of the Act moved because the single seals currently if a reactor is also mad ss a stripper, the The request for a waiver for compliance used on this equipment have small emis reactor opening emkslons may be deter should provide for the esse where SPA sions and are more reliable than doubts mined Immediately following toe strip determines that a method k not equiv mechanical seals. EPA Is aware that seeh ping operation. Xf a reactor k also used alent and the plant needa to purchase fugitive Pinkston source, such ee one as a stripper, toe resin k in toe reactor other equipment In no case win the pump, taken by Itself csumb relatively whan it k opened. Thk means that vinyl waiver of compliance be extended beyond small emissions. Fugitive emissions con chloride in the resin which has already two yean from the date at promulga sidered as a whole are a significant been stripped to acceptable levels can tion. source of emissions, however, and the In eacapa from the resin and become part There an several wording darifleations which have been made in the pro mulgated standard. The definition for "In vinyl chloride service" (| 60.CU1)) hag been elsrifled by stating that It means equipment that contacts vinyl chloride as well as equipment that con tains vinyl chloride. This would Include such equipment ss agitators. Word! have been added to If 0iJ3, 61.63, and 61.64 to clarify that the 10 ppm emission limits do not have to be met when equipment has already been opened in compliance with the regula tion for opening of equipment. Equip ment that has met the opening of equipment regulation can contain more than 10 ppm vinyl rhlorlde and would bo in violation of the standard if thk statement were not included. The requirements far stripping potgr tent of toe standard k to reduce these. Double mechanical seal pumps are com monly used in the industry for smkafcm reduction. Sealless pumps or oqutvaknt systems sre available os options to double mrtianlf1 miIi, The commenters recommended to- wealing the averaging time for the 10 ppm Unfits and the emission limits far reactor opening and stripping to 90 days. Some of the commenters apparently thought that the 10 ppm limits had to be met on an instantaneous basis. However, since the performance test for determin ing compliance consists of three rune for a minimum of an hour each, the aver aging time for the 10 ppm limit k at least three hours. Increasing the averaging time to 30 days for any of toe emission limits would permit higher peak emis sion levels. EPA has determined that thk k neither desirable nor necessary. of toe reactor opening loss. It Is EPA's intent that enee a resin has been stripped to the required lends, that additionsi controls are not required, under the new provision, vinyl chloride escaping from the resin after it has been stripped to acceptable levek k not counted as port of too reactor opening loss. A section requiring continuous moni toring Of stack emissions has been added to too promulgated standard. The con tinuous monitoring of stock emissions was required in toe propoeed standard. The addition of a specific paragraph for emission monitoring serves only to clarify toe requirement. The standard has been revised so that toe initial report requires a "description" rattier than a "detailed description" of the equipment used to control fugitive emissions. Several commenters pointed out that a detatted description would vinyl chloride resins to spsctftcd levek Borne commenters requested toot the contain proprietary information. EPA have been revised in If 61.04(e>, 61JT stripping levels for dispersion ferine be agrees that a detailed description in too ROHM MOUTU, VOl. 41, NO. aoi--TMUVSOAV, OCTOSiS 31. 1*74 BFG32318 UUS AND tieWATIONS Initial report la unnecemary. S edit' Ih section 6.4 of Test Method 196 tbe O) Tiny] tleoal tatonuUoa la BA mb obtain It under section 114 of Um Act and has been replaced with a requirementfor (3> One or asore poiymsis eontainlng the plant can request confidential trait a disc integrator or piantaeter for msaa- any fraction of pdymtrlied vinyl ebto- meat In accordance with 40 CTO Part I urtng peak area. This change le In re for Information It believes to be proprietary. Tbe proposed standard required that a semiannual report bo submitted erery ISO days. The proaulcated standard specifies dates for the submittal of the sponse to a comment which states that automatic integrators are unnecessarily elaborate and expenstva. A new section ga has been added to Test Method log which requires deter mination of the water vapor content of <b> This subpart does not apply to equipment wed 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 m* (86 gal). reports. It also specifies that the lint the sampling bag by measuring the am <c> Sections of this subpart other than semiannual report does not hare to be bient temperature and pressure near the 161.64(a)(1). (b). (e). and (d) do not submitted until at least six months after hag. The vinyl chloride concentration of apply to equipment wed in research and the Initial report is submitted. tbe bag can then be reported on a dry development If the reactor used to po The standard has been revised to elim bests. A provision for hi*yig the rigid lymerise the vinyl chloride processed In inate the requirement to record the cause container for leaks has been added to the equipment baa a capacity of greater of any leak detected by the vinyl chlo action 7.4 of Tat Method 106. than 0.19 nf (50 gal) and no more than ride detector, the action taken to repair The only change In Test Method 107 is 4.07 m* (1100 gal). the leak, and the amount of time re quired to repair the leak. SPA Is con cerned onlv that leaks are detected and repaired. That this has been dooe can bo established by looking at the strip chart record of measurements made by the vinyl chloride detector. These records am still required for the portable hydrocar bon detector however. Several commentators recommended that the companies be allowed an extra two weeks to submit to EPA data from the initial performance test. They also recommended that they submit tbe data by regular mall rather than registered mail. EPA has not adopted either of these recommendations. A source is supposed to be In compliance with the standard within 90 days of the promulgation of the standard. The standard requires that the emission tests be done within the 90 day period, and permits an extra 30 days for determination of results. The purpose of using registered mall Is to document the fact that emission data have been sent and received. This way If the results are lost in the mall, there the provision tn Section M3 for use of Cerbopek C as well as Csrtopak A. Aothobctv: avetton 111 at the dm Afcr Act as aDM by no. 4(a) at Pub. I* 91-604. 84 8tat. 1099 (49 UA.C. 19970-7; Section 114 at tbe Clean Air Act, as added by sec. 4(e) of Pub. L. 91-404,94 Stat. 1687, end amendad by pub. It. as-ais, see. 0(e) (4). as Stat. 3W (49 UAjO. 18S70-8); Section S01(e) of tbe Clean Air Act, aa amendad by aae. 19(e) (S) at Pub. L. 11-604, S4 Stat. 171S (49 VAO. 1967g(a)). Dated: October 13. 1979. JonrQmuu, Acting Administrator. Part 91 of Chapter I, Title 40 of the Code of Pederal Regulations is amended as follows: The table of sections for Part 61 is amended by adding a list of sections for new Subpart P and Part 61 is amended by adding a new Bubpart P reading as follows: tobpert F WsWeeel Emlssien Standsnl far Vkq4 066* Cblertde -- 1.60 Applicability. 01.S1 Definitions. <1.61 OafiaidMM. Terms used in this subpart are defined In the Act, in subpart A of this part, or In this section as follows: (a) "Ethylene dlchloride plant" in cludes any plant which produces ethyl ene dlchloride by reaction of oxygen and hydrogen chloride with ethylene. (b) "Vinyl chloride plant" Includes any plant which produces vinyl chloride taQTftny pxocNia - (e) "Polyvinyl chloride plant" includes any plant where vinyl chloride alone or In combination with other materials is polymerised. <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 tbe vessel by the physical state of the material the gauge dis charges. () "Typo of resin" means the broad classification of resin referring to the basic manufacturing process for produc ing that resin. Including, but not limited to, the suspension, dispersion, latex, bulk, win be no question that they were sent 4142 emission standard for ethylene dl- sail snlntl/m mmmw (6) rest method. Test Method 100 has been changed to recognise that on a gas chromatograph equipped with a Chromosorb 102 column, acetaldehyde may Interfere with the vinyl chloride peek. When a sample is expected to contain ehlorlds plants. fl.83 emission standard for vinyl chloride plants. 144 Kmlsilon standard for polyvinyl chlo ride plants. 1.68 emission standard tor ethylans dt- chloride, vinyl chloride and poly (f) "Grade of resin" means the subdlvieton of resin classification which de scribes it as a unique resin, Le., the most exact description of a resin with no fur ther subdivision. (y) "Dispersion resin" means a resin acetaldehyde, a secondary column as de scribed m section 4.3.2 must be emnloved. Man spectroscopy or another absolute analytical technique is required to con firm the vinyl chloride peak obtained with the gas chromatograph, only If peak -resolution with tbe secondary column la not successful. In section 4.1.4, aluminized Mylar hags can be substituted tor Tedlar bogs. EPA now has data to allow this substitution, 61.86 6147 6148 vinyl chloride plants. equivalent equipment and procedures. Xmlealon monitoring. manufactured in such swsy as to form fluid dispersions when dispersed In a .plasticiser or ptasttclzer/diluent mlx- ei.es Initial report. 61.70 Semiannual report. <h) "latex resin" means a resin which 61.71 Bccordkacpiog. 16 produced by a polymerization process Atraourr: Section us of the Clean Air Act as added by sac. 4(a) of Pub. L. S1-S04, M Stat. 1DS5 (43 UA.C. 1S670-7); section 114 which initiates from free radical catalyst sites end is sold undried. (i) "Bulk resin' 'means s resin which of the Clean Air Act, as added by cee. 4(a) is produced by a polymerisation process of Pub. L. 91-004. 84 Stat. 1687, and emended in which no water is used. provided that the samples sre analysed by rub. h. M-519, sec. 6(a) (4). M Stat. SSS <J) "Inprocess wastewater" means any within 24 hours of collection. (49 UA.C. 19570-9); section 901(a) of too water which, during manufacturing or In section 9.1.3 of Test Method 106 the requirement to use "oxygen gas" bos been replaced with "oxygen gas or air, as Clean Air Act, ae amended by sec. 19(e)(9) Of Pub. L. 91-004, St Stat. 1719 (48 UA.C. 18578(a)). processing, comes into direct contact with vinyl chloride or polyvinyl chloride or results from the production or use of required by the detector." Several com- Subport F--Notional Emission Standard any raw material. Intermediate product, mentors stated that most pas chromato lor Vinyl Chloride finished product, by-product, or waste graphs arc designed to use hydrogen and nir for their flame detectors. When used (61.60 Applicability. product containing vinyl chloride or polyvinyl chloride but which has not in this way, they are ennoble of detect <a> This subpart applies to plants been discharged to a wastewater treat ing 0.5 ppm vinyl chloride in sir. This is which produce: ment process or discharged untreated ss sensitive enough for monitoring the 10 (1)Ethylene dlchloride by reaction of wastewater. ppm emission limits stipulated in Uio oxygen and hydrogen chloride with (k) "Wastewater treatment process" standard. ethylene. Includes any process which modifies KDSBAl BEQISTEt. VOL 41, NO. JOS--IHUStoAV, OCTOSft II, 19F4 BFG32319 MUSS AND HOUUHONS | MAS fee vinyl (or Eta veaetar If the ptefifc bag. *ad pH. wwlljr tor the IwaitiiicliiiiiiwiNMittwnQM ef which Is to remove ftivl chloride trees water to nwt reqidrosMote r* **-- gnbpart,. An owner or operator of a ring! cMwrtde plant thaBoompty with the roqnira- menuof this seirilew and 1#1-68. <a Vinyl chloride formatted and puri fication: The concentration of rinyl stripper) la the plant praam flow Vs aoftwexeeod If ppes. except m provided In Attnt. IMS requirement does not to oqxlpmant that has boon opened, is old of operation, and mat the requirement lit I 61.63(b) (to (i> before <l> "In rinyl chloride wnrioe"___ chloride to all exhauot gaeoo discharged that a piece of equipment ccntetoe or to the atmosphere from any onelpmetit (d> Monomer recovery system. The ii contact* either a liquid that la at laaat M percent hr wtebt vinyl chloride or a CM that ie at laaat 1C percent far -- vinyl chloride. (m> "Standard operatine ______ meaaa a formal written procedure ra cially adopted far the plant owner or operator and available on a routine taeeie to umm rfttpfffltfMt tot ctnytai ont the procedure. (n) `'Run" oMane the net period of tune durinc which an emtedon sampte 1* collected. (o) "Ethylene dichloride purification" include* any part of the procom of ethyl ene dichloride production wfeteh foDoon ethylene dichloride formation and In which finished ethylene dtchloridc ie used in rinyl chloride foraatten and/or purification is not to exceed 10 ppm, ex cept m provided tn 101.00(a). This re quirement doee not apply to equipment thathas been opened, is out of operation, and met the leqmrssnept to 101A0(b> (8i u> before faetng opened. | 6IA4 KmMaa standard far eotyriarl chloride * An owner or operator of i chloride plant shall odmply with the re quirements of title section and 101.00. (a> Raacter: The feBowinc require ments apply to reactors: il> The concentration of rinyl chlo ride in an exhaust gases discharged to the atmosphere from each reactor is not to exceed 10 ppm, except m provided hi concentration ef rinyl chloride In all ex- >--gain* discharged to the atmos phere from each monomer recovery sys > teas ie not to exceed If ppm, except as provided in I ftAS(a). Ihls requirement dees not apply to equipment that tun been opened, is out of operation, and met the requirement la 161J8(bX6Xi> be fore being opened. (q> Eouroee following the stripper(s>: The following requirements apply to omtesimia ef rinyl chloride to the *t- meophera from the combination of aU eoureae following the stripper (s) (or the raaetorts) if the plant has no ttrip- por(s)l in the plant process flow In cluding but not limited to. eentrinigm. emetatraton* WffMl mten* dry* ers, conveyor air dtochargas. baggers, produced. paragraph <a><2> of this section and storage containers, and inproeem waste- (pi "Vinyl chloride purifleotioa" In* 161.M(a>. cludee any part of the proceee of vinyl (D The reactor opening loss from each <1) In polyvinyl chloride plants using chloride production which follows rinyl weetor ie not to exceed 0.03 g rinyl stripping technology to control Vinyl chloride formation and in which finished chloride/Kg (0.00003 lb vinyl chloride/ chloride emissions, the weighted avenge rinyl chloride i* produced. lbi of polyvinyl chloride product, with residual rinyl chloride concentration in (q) "Reactor" includes any yeses! In the product determined on a dry solids all grades ef polyvinyl chloride resin which rinyl chloride Is partiallyor totally basis. This requirement applies to any processed through the stripping opera polymerised into polyvinyl chloride. vessel which Is used as a reactor or as tion on each calendar day, measured (r) "Reactor opening lorn" means the both a reactor and a stripper, la the Immediately after the stripping opera emissions of rinyl chloride occurring bulk process, the product means the tion is completed, may not exceed: when a reactor is vented to the atmos phere for any purpoee other than an gross product of prepotymertoattea and postpolymerixation. emergency relief discharge se defined in (3> Manual vent valve diaebarge: Ex f Ol.OOte). (s) "stripper" includes any vaseel in which residua! vinyl chloride is removed from polyvinyl chloride rosin, except' bulk min, tn the slurry fora by the an of host and/or vacuum, in the case of bulk resin, stripper includes any vows! which is used to remove residual rinyl chloride from polyvinyl chloride mtai immediately following the polymerisa tion step in the plant process Bow. 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 emergmxy manual vent valve discharge means a discharge to m* atmeephere which not have been avoided fay taking meas ures to prevent the discharge. Within it days of any discharge to the atmeephere from any manual vent valve, the owner or operator of the source from which the (i) 3000 ppm for polyvinyl chloride dispersion resins, excluding latex resins: (U) 400 ppm for all other polyvinyl fhfgfMf rsstav* latex resins, averaged separately for each type of res in: or (3) m polyvinyl chloride plants con trolling rinyl chloride emissions with technology other than stripping or in addition to stripping, emissions of vinyl ehloride to the atmosphere may not <1)3 g/kg (0408 lb/lb) product from the strtpper(s) ter reactor(s* u the plant has no strtpper(s) ] for dispersion MAS Emission slendsrd lev ethylrwr discharge occurs shall submit to the Ad polyvinyl chloride resins, excluding latex dMdoride pleats. ministrator a report tn writing contain resins, with the product determined on a An owner or operator of an ethylene ing information on the source, nature dry solids basis: dlehloride plant shall comply with the requirements of this section and I 8143. (a)Ethylene dlehloride purification: The concentration of rinyl chloride tn all exhaust gases discharged to the at mosphere from any equipment used In ethylene dlehloride purification is not to exceed id ppm, except m provided in I <1.6S(a>. Tide requirement doee not and cause of the discharge, the date and time of the discharge, the approximate total vinyl chloride loss during the (tiecharge. the method used for determining the rinyl chloride lose, the action that was taken to prevent the discharge, and measures adopted to prevent future dis charges. ib* 8trippar: The concentration of vinyl chloride to all exhaust gases dis charged to the atmosphere from each <M> 0.4 g/kg (0.0004 lb/lb) product from the strippers roe raactor(s) if the pleat hw no etripper<e>] for ell other Polyvinyl chloride resins, including latex resine, with the product determined on a dry solids beds. 101.63 Emlwlon -tamlard fur rtlh i.-nr dMtlurhle. vinyl rMnrMe snd puli vinyl eblnrlde plant*. An owner or operator of an ethylene apply to equipment that has been opened, is out of operation, and met the requirement In 161.63(b) before being opened. (b> Oxyehlorlnation reactor: Except as provided In f61.08(a>, emissions of vinyl chloride to the atmeephere from each oxyehlorlnation reactor are not to exceed 0.2 g/kg tire 100 percent ethylene dlehloride product from the oxychlorination process. stripper ie not to exceed If ppm. except m provided tn iflJSta). This require ment doee not apply to equipment that has been opened, is out of operation, and met the requirement in f 81.86(b) (> <0 before being opened. (c* Mixing, weighing, and holding containers: The concentration of vinyl chloride in all exhaust gases discharged to the atmosphere from each mixing, weighing, or holding container in rinyl chloride service which precedes the dlehloride, vinyl chloride, and/or poly vinyl chloride plant shall comply with Uw requirements ef this section. (o> Relief valve discharge: Except for an emergency relief discharge, there is to be no discharge to Uie 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 10 days of any relief valve discharge, HOftM tcotSTft. vol si. ho. iov--TMUttoav, ocroem si. tere S d O S f'S f'Z BFG32320 4fMf MUSS AND ICGULATIONS the owner or operator of the source {ran system from which the concentration of ride is to be reduced so that the equip which Um relief valve discharge occurs vinyl chloride in tbe ewhauet gases doss ment contains no sears than 3.0 percent than submit to tbe Administrator i n> not exceed 10 ppm; or equivalent ee tay rotate vtagi chloride or MN6 mJ (36 port in writinc eontointoe tnfermnttan provided in II1JS gal) at vinyl chloride, whichever is on the source, nature and cause of the (M1 Rotating ooanpressor: Vfcwrt kugr atjdanderd temperature and discharge, tbe date and time of tbe dis chloride smtaskmc front scab an all ro charge, the approximate total vinyl chlo tating comptsaaen in vinyl ehtaMs (I) Any vinyl ddoride removed from ride loss during the discharge, the meth service are to be minimised by Installing the equipment m accordance with para od used for determining the fhfl chlo compressors with double mechanical graph (h)(6)<l> ef this section le to be ride leas, tbe action that was taken to seals, or equivalent as provided in 161J6. dueled through a control system from prevent the discharge, and measures If double mechanical seals are used, vinyl which the concentration of vmyl chlo adopted to present future discharges. chloride emissions from tbe seals am to ride in the exhaust gases does not exceed (b) fugitive emission sources: be minimised by maintaining tbe pres 16 ppm, or equivalent as provided in (1) Loading and unloading lines: Vinyl sure between the two seals so that any HIM. chloride emissions from loading and un- leak that occurs is into the compressor; (3) Samples: Unused portions of sam leading linos which are opened to the by ducting any vinyl chloride between ples containing at least 16 percent by atmosphere after each loading or un the two seals through a control system weight vinyl chloride are to be returned loading operation are to be minimised from which the concentration of vinyl to the process, end sampling techniques as follows: chloride in the exhaust gases does not are to be such that sample containers in (1) After each loading or unloading exceed 10 ppm; or equivalent es provided vinyl chloride service are purged into a operation and before opening a loading in f 61.66. closed process system. or unloading line to the '<< mosphere, the <lvi Reciprocating compressors: Vinyl (6) Leek detection and elimination: quantity of vinyl ca'-' ido in all paria of chloride emissions from seals on all re Vinyl chloride emissions due to leaks each loading cr unloading line that are ciprocating compressors in vinyl chloride from equipment in vinyl chloride service to be opened to the atmosphere is to be service are to be minimised by installing are to be minimland fay instituting and reduced so that the parts combined con double outboard seals, or equivalent es implementing a formal leak detection tain no greater than 0.0038 m* (0.1S ftf) provided in 161.66. If double outboard and elimination program. The owner or of vinyl chloride, at standard tempera seels are used, vinyl chloride emissions operator shall submit a description of ture and pressure; and from the seels ere to be 'minimized by the program to the Administrator for <ti)' Any vinyl chloride removed from maintaining the pressure between the approval. The program is to be sub a loading or unloading line in accord two seels so that any leak that occurs Is mitted within 45 days of the effective ance with paragraph (b)(1) (1) of this into die compressor; by ducting any date of these regulations, unless a waiver section is to be ducted through a central vinyl chloride between the two seals of compliance is granted under 161.11. system from which the concentration of through a control system from which the If a waiver of compliance is granted, the vinyl chloride in the exhaust gases does concentration of vinyl chloride in the program is to be submitted on a date not exceed 10 ppm, or equivalent as pro exhaust gasas does not exceed 10 ppm; scheduled by the Administrator. Ap vided in 161.66. or equivalent as provided In 161.68. proval of a program win be granted by (3) Slip gauges: During loading or un (v) Agitator: Vinyl chloride emissions the Administrator provided he finds: loading operations, tbe vinyl chloride from seals on all agitators in vinyl chlo (1) It includes a reliable and accurate emissions from each slip gauge in vinyl ride service are to be minimised by in vinyl chloride monitoring system for de chloride service are to be minimised by stalling agitators with double mechani tection of maior leaks and Identification ducting any vinyl chloride discharged cal seals, or equivalent as provided in of the general area of the plant where a from tbe slip gauge through a control 161.66. If double mechanical seals are leak is located. A vinyl chloride monitor system from which the concentration of used, vinyl chloride emissions from the ing system means a device which obtains vinyl chloride In the exhaust gases does seals are to be minimised by maintaining air samples Inn one or more points on not exceed 10 ppm. or equivalent as pro the pressure between the two seals so a continuous sequential basis and ana vided in f 61.66. that any leak that occurs is into the agi lyses the samples with gas chromatog (3) Leakage from pump, compressor, tated vaesel: fay ducting any vinyl chlo raphy or, if the owner or operator as and agitator seals: ride between tbe two seels through a sumes that all hydrocarbons measured (1) Rotating pumps: Vinyl chloride control system from which the concen are vinyl chloride, with infrared spectro emissions from seals on all rotating tration of vinyl chloride tat the exhaust photometry flame ion detection, or an pumps in vinyl chloride service are to be gases does not exceed 16 ppm; or equiva equivalent or alternative method. minimized by installing sealless pumps, lent as provided in 161.66. (it) It includes a reliable and accurate pumps with double mechanical seals, or (4) Leakage from relief valves: Vinyl portable hydrocarbon detector to be used equivalent as provided in 161.06. If chloride emissions due to leakage from routinely to find smell leaks and to pin double mechanical seals are used, vinyl each relief valve on equipment in vinyl point the major leaks Indicated by the chloride emission from the seals are to chloride service are to be minimised by vinyl chloride monitoring system. A be minimised by maintaining the pres installing a rapture disk between the portable hydrocarbon detector means a sure between tbe two seals so that any equipment and the relief valve, by con device which measures hydrocarbons leak that occurs is into the pump; by necting the relief valve discharge to a with a sensitivity of at least 16 ppm ducting any vinyl chloride between the process line or recovery system, or equiv and Is of such design and size tliat it can two seals through a control system from alent as provided in 161.66. be used to measure emissions from local which the concentration of vinyl chlo (5> Manual renting of gases: Except ized points. ride In the exhaust gases does not ex ceed 10 ppm; or equivalent os provided in f 61.66. <il) Reciprocating pumps: Vinyl chlo ride emissions from seals on all recipro as provided in I61.64ia>(3>. an gases which are mnnunUy vented from equip ment in vinyl chloride service are to be ducted through a control system from which the concentration of vinyl chloride HU) It provides for an acceptable cali bration and maintenance schedule for the vinyl chloride monitoring system and portable hydrocarbon detector. For the vinyl chloride monitoring system, a dally 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 in the exhaust gases does not exceed 16 ppm: or equivalent as provided in i 61.66. <6) Opening of equipment: Vinyl chloride emissions from opening of equipment (including lending or unload ing lines tliat are not opened to the at mosphere niter each loading or unload ing operation) are to be minimised as follows: <it Bolore opening any equipment lor span check is to be conducted with a concentration of vinyl chloride equal to the concentration defined as a leak ac cording to paragraph (b> (6> <vi * of tills section. The calibration is to be done with either: (A> A calibration gas mixture pre pared from the gases specified in sections tween tbe two seals through a control any reason, the quantity of vinyl chlo 6.3.1 and 531 of Test Method 106. ot FfDitAl MOISTft, VOL 41, NO. J05--THUSSOAY, OCTOSM 31, 1076 BFG32321 I BUM AHO neuunUM ,> * vinyl chloride tot sgftotol M.il mf thi aooranriate oanMntratton of ftnjl eUtrM. U a calibration gw cylin der k ured. Um mink mart to toast* mbit to the National Bureau of Stand ards or to a grarimetrically caUteatad vinyl chloride permeation tube. ISM gal hi volume lor which an mis sion limit to prescribed to OlASOs) (0) (1) prior to opaalng the equipment nod using TMt Method 104. a portable hydro carbon detector, or an equivalent or al (g> Unlsss otbarwiso specified, the owner or operator Shan use teat Test Methods in Appendix B to this part for each teat as required by paragraphs (g)(1), (g)(3), (g)(3), (g)(4), and (to) The location and number of potato ternative method. The method of meas <g> () of thto section, unless an equiva to to monitored and the frequency at monitoring provided for in the program are acceptable when they are compared with the number of pieces of equipment urement to to meet the requirements in * 61.07(g)(5) (1) (A) or (g)((g)(1)(B). | 61.66^ Eqwlvalenl equipment and pen* lent method or an alternative method has been approved by the Administrator. B the Administrator finds reasonable grounds to dispute the results obtained tat vinyl chloride service and the stag and by an equivalent or alternative method, physical layout of the plant. (> It contains an accwtable plea of action to to taken when a leak to de* tGctod* (vi> It contains a definition of leak Upon written application from an own er or operator, the Administrator may approve use of equipment or procodurn which have been demonstrated to his to may require the use of a reference method. If the results of the reference and equivalent or alternative methods do not agree, the results obtained by the reference method prevail, and the Ad which to acceptable when compered with satisfaction to to equivalent in terms of ministrator may notify the owner or the background concentrations of vinyl reducing vinyl chloride emissions to the operator that approval of the method chloride in the areas of the plant to to monitored by the vinyl chloride monitor ing system. Measurements of background concentrations of vinyl chloride in the areas of the plant to be monitored by the vinyl chloride monitoring system are to be included with the description of the program. The definition of leak for a given plant may vary among the differ ent anas within the plant and to also to change over time as background con' centrations in the plant are reduced. ( Inprocess wastewater: Vinyl chlo 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 to to to submitted to the Administrator within 30 days of the effective date. For a now source, any request for using an equiva lent method to to be submitted to the Administrator with the application for approval of construction or modification required by 101.07. previously considered to to equivalent or alternative to withdrawn. (1) Test Method 100 is to be used to determine the vinyl chloride emissions from any source for which an emission limit to prescribed in |l 01.02(a) or <b> 01.03(a). or || 01.04(a) (1), (b). (c), or (d). or from any control system to which reactor emissions are required to be ducted in 101.04(a) (3) or to which fugi tive emissions are required to be ducted in It 01A5(b> <1) (ii>, (b)(3), (b)(5>. (b)(0) (ii>, or (b)(0) (h). ride emissions to the atmosphere from inprocess wastewater are to to reduced as follows: (it The concentration of vinyl chlo ride in each lnprocess wastewater stream containing greater than 10 ppm vinyl chloride measured Immediately as it leaves a piece of equipment and before being mixed with any other inproceee wastewater stream to to to reduced to no more then 10 ppm by weight before being mixed with any other inproceee wastewa ter stream which contains less than 10 ppm vinyl chloride; before being exposed to the atmosphere, before being dis charged to a wastewater treatment proc ess; or before being discharged untreated as e wastewater. The paragraph does apply to water which to used to displace vinyl chloride from equipment before it is opened to the atmosphere in accord ance with 161.64(a) (3) or paragraph (b)<6> of this section, but does not apply to water which is used to wash out equip ment after the equipment has already been opened to the atmosphere in ac cordance with |l.64(a><3> or para graph (b) (6) of this section. (iii Any vinyl chloride removed from the inprocess wastewater in accordance 161.47 Embalm testa. (a) Unless a waiver of emission testing is obtained under 101.13. the owner or operator of a source to which this subpart applies shall test emissions from the source, (1) Within 00 days of the effective date in the ease of an existing source or a new source which has an Initial startup date preceding the effective date, or (2) Within 90 days at startup In the ease 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 tost to afford the Administrator the opportunity to have an observer present during the test. (c> Any emission tost to to to con ducted while the equipment being tested is operating at the maximum production rate at which the equipment will to op erated and under other relevant condi tions ss may be specified by the Adminis trator based on representative perform ance of the source. (d) Each emission test is to consist of three runs. For the purpose of deter mining emissions, the average of results of ail runs is to apply. The average to to (i) For each run. one sample to to be collected. The sampling alto to to be at least two stack or duct diameters down stream and one half diameter upstream from any How disturbance such as a bend, expansion, contraction, or risible flame. For a rectangular cress section an equivalent diameter is to be determined from the following equation: equivalent dtometr-2 length+width The sampling point in the duet to to be at the centroid of the cross section. The sample to 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 to to contain a minimum volume of 50 liters corrected to standard conditions. <U> Far gas streams containing more than 10 percent oxygen, the concentra tion at vinyle chloride as determined by Test Method 104 is to be corrected to 10 percent oxygen for determination of emissions to using the following equa tion: Cn, Ci 10.0_________ 20.0--percent (J* with paragraph (b> (9) (i) of this 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 provided bo computed on a time weighted basis. ie> All samples are to to analyzed within 24 hours, and vinyl chloride emis sions are to be determined within 30 days after the emission test. The owner or ^(wwi'lwP "TV MwtnlnUn I rinvl cliloriih* in thrrtjumt gam, cocmtal lo in \ki CTCfitiimrtrwilo(t <4 vinyl (MnritW- :w* IMImhI hjr Tf* Method Ktt. 9J"lVttrM Mygen in thr ambient uir ut in! 41.04. operator shall report the determinations (c) The requirements In paragraphs to the Administrator by a registered _ ftmutant eondHton*. MJiolVfcrtil pijpjmi in tlm amhiriit air :tl ftmntanl ratHtllton*. ntittm it* w (t(l>. (b)(2). (b)(5). (b)(6). (b)(7) and (b> (0) of this section are to be in corporated into a standard operating procedure, anr made available upon re letter dispatched before the close of the. next business day following the deter mination. if) The owner or operator shall retain MTfnt Otyftnt to widt h t In* ctgrrv non U Indie# inmW* I'cmmt Oi*Pfir*m oxyam in thr rt(i;w4 * m--Mfud by Uffcrrmt MclboU 3 in ApporaH* A of Kart *l aC t bio flutist rr. quest for inspection by the Administra at the plant and make available, upon (ill) For those emission sources where tor. The standard operating procedure is request, for inspection by the Adminis the emission limit to prescribed in terms to include provisions for measuring the trator. for a minimum of 2 years records of mass rather than concentration, moss RoctAt eeoiSTfe. vot. 41, no. ios--muesoAv. octosu t. tore 24548007 BFG32322 MIS AND RSOMATIQMr to kg/166 kg ante teat k also need as a stripper. Um deter- detection, or an eqtovaleat or alterna ft* determined tv w be udi tauMdkWir fcl- tive method. The vinyl chloride monitor- equation: Um stripping tamton. tog system umd to asset the requirements <D Inept u provided In paragraffe to 16148<b) ((1) may ba used to meet (g)(6) ta) ot tit* section. the the requirements eC this section. cpentng km la to ba determined (e> A dsgy span cheek is to be con Cai' cv tolMIMMHl Dnatt* M ttaul chteMs at mm 'VatttacmUatritatf/laJwirialala IdmnlMMl aiMnanla. IM-Cmiwfcm kctur hr pen. X-Ft1wUm nla (ktfkl, (3) Teat Method 107 to to ba wad to tee following equation: c IT (rtO)ClOr*) (Ct) W-Cuauekyu(UMiT*darlai**.~ 1SS-Dually ef riayl ebtarMi u ooe U>o*phri* uwd W Clnka/m*. H-OpmabaMUrtripa CW-ppm hy rahmM TtnyVeMertdr m drimaimd by ducted for each vinyls chloride monitor ing system used. Far all at tha emhsion sources Ueted to paragraph fa) ot this action, except tha onefor which an emis sion Umlt Is prescribed to 16142(b), the dally span cteck is to be conducted with a concentration at vinyl chloride equal to 10 ppm. Far the amission source for which an emission Umlt is prescribed in determine the concentration of vinyl chloride to each lnproceaa wastewater stream for which n errimlca limit is pmacribedta(01.f ' (1). <3> When a i . ,l.ig operation is That Mathad MS pr i parUhla hrdrawrtao detaetor whk-h pMamiiva hydrwcarhwoa with a pppaitiTlty af at lasat 10 ma V-Nutter f hmehca Mam tha mattor wrnlmt apiaid tath ataiwtihm. r-Jlrawi ka af polyrhiri ahlwtda pradaaad par hatchlntha namhrrpfhttchnUnm thr rmstpr 161.63(b), the daily span cheek la to be conducted with a concentration of vinyl chloride which is determined to be determined to be equivalent to the emis sion limit for tb**. source based on the used to attain the emission Unit to 161.- amission test n 'by (67.67. The 64(e), emissions are to ba determined calibration Is to be done with either: using Test Method 107 as follows: iA) if Matbod 100 is used to deter (1) A calibration gas mixture pre (I) The number of strippers and sam mine the concentration of vinyl chloride pared from the gases specified in sections ples and the types and iradsa of resin to (Cb), the sample ia to be withdrawn at *4.1 and 644 of Test Method 106, or be sampled an to be determined by the a constant rata with a probe of sufficient (2) A eaUbratlan gas cylinder con Administrator for each individual plant length to reach the vessel bottom from taining the appropriate concentration of at the time of the test baaed on the Um manhole. Samples are to be taken vinyl chloride. If a calibration gas plant's operation. for 5 minutes within 6 inches of the ves cylinder is used, the analysis must be (ill Each sample is to be taken imme sel bottom. 5 minutes near the vessel traceable to the National Bureau of diately following the stripping operation. center, and 5 minutes near the vessel top. Standards or to a gravimetrlcafly cali (lil) The corresponding quantity of (B) If a portable hydrocarbon detec brated vinyl chloride permeation tube. material processed by each stripper is to tor is used to determine the concentra 61.69 Initial report. be determined on a dry solids basis and by a method submitted to and approved by the Administrator. <iv) At the prior request of the Ad ministrator, the owner or operator shall provide duplicates of the samples re quired in paragraph (g)(3)(l) of this section. (4) When control technology otter than or in addition to a stripping opera tion is used to attain the emission limit in 161.64(e), emissions an to be deter mined as follows: U) Test Method 106 Is to lie used to determine atmospheric emissions from all of the process equipment simultane ously. The requirements of paragraph (g) (1) of this section an to be met. (II) Test Method 167 is to be uaod to determine the concentration of vinyl chloride in each lnproceaa wastewater stream subject to the emission limit pre scribed to 161.64(e). The mass of vinyl 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 4 inches of tha vessel bottom, one near the vessel center end one near the vessel top. Measure ments are to be made at each location until the reading Is stabilised. All hydro carbons measured are to ba assumed to be vinyl chloride. (C) The production rate of polyvinyl chloride iZ) is to be determined by a method submitted to and approved by Um Administrator. <U) A calculation based on the number of evacuations, the vacuum Involved, and the volume of gas in the reactor ia hereby approved by the Administrator as an al ternative method for determining reac tor opening loss for postpolymerisation reacton in the manufacture of bulk resins. (a) An owner or operator of any source to which this iubpart applies shall submit a statement ta wilting notifying the Administrator that the equipment and procedural specifications to li 61.65 (b)U), <1(2). (b)(3). (b)(4), (b)(5). (b)(6), (b)(7), and (b)(6) are being implemented. (b) (1) In the ease 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 60 days of the effective date, unless a waiver of compliance is granted under 161.11. along with the informa tion required under 161.10. If a waiver of compliance is 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 so days of the chloride in kg/100 kg product in each | 61.60 Emiul--n monitoring. initial startup date. in process wastewater stream is to ba de termined by using the following equa tion: c____ [C 10-1 (1001 where: Cn-kg rtiiyl chbriilr MS ks predwrt. 4 t'e-th* rwiH-nitniUmi of efiiyl rliMdt m amrand be Tret Method 107. C-rilR be (ate In I/hr. drtmnlnedln oererdoncw with methud whk-h hue been mhmlUrd to amUpproml hy U>e Ailiniidelrelor. ir2t--CrruoimhtrntiieMw bmrli*ar(Whrc/phor)m. .drienadnrd la error*, wire with wr-thud * lih-h bee been nilmdtlrd mid appeared by the AiliuiuMmlar. ' i a) A vinyls chloride monitoring sys tem is to be used to monitor on a con tinuous basis the emissions from the sources for which emission limits are pre scribed in f 61.62(a) and (b>. f 61.63(a). and ( 61.64(a)(1). (b>. (c>,and <d>.and far any control system to which reactor emission are required to be ducted to ( 61.65(b) <l>(ii). and (b)(3). ib)S>. <b> 6)<11), and (bHDHii). b) The vinyl chloride monitoring sys tems) used to meet the requirement in paragraph <a> of this section is to be a (c) The statement is to contain the following information: (1) A list of the equipment installed for compliance, (2) A description of 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 (101.65 (b) (1X1) and (b)(6)U). (4) A statement that each piece of (5) The reactor opening lorn for which device which obtains air sampcls from equipment is installed and that each an emission limit is prescribed in 101.04 one or more points on a continuous piece of equipment and each procedure (a)(2) is to be determined. The number sequential basis and analyses the samples is being used. of reactors for which the determination with ras < hromotography or, if the owner 8 61,70 Siwiknsiul n port. ia 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 or operator assumes Hint ail hydrocar bons measured arc vinyl chloride, with infrared spectrophotometry, flame Ion <a)<2> is to be determined. The number source to which this subpart applies shall submit to the Administrator on Septcm- FCOctAl tfotsrte. VOl. <I, NO. 205--THUSSDAY, OCTOSM >1. 197* BFG32323 *:3 fear U and March U of Mchymra report of 3 hours for each grade of note which may be mafia immediately following too ill writing containing to* inftwmatiou to being procweed, whichever to amiefw- required tr this Mctiw. H> flat --I annual nport to to bo mbenlttart f(snow fMot The sample to lobe taken ae tho reein flows out of the stripper and Mam- I *1.71 tUeerdkeeptan. ing tho first full 6 month nportinc period Mfled by resin type and grade and the (a) The owner er operator at any after the initial report to cubmitted. date and time the sample was taken aouree to which this subpart applies shall (b) (1) fettwcin<fanattli|MDm The corresponding quantity of material retain the foDowing information at the or a new aouroa which haa an initial processed by each stripper over the tone aouree and make It available for inspec atartup data preceding the effective date, period represented by the sample during tion by the Administrator for a mini the fliat report to to be aubraltted within toe eight hour period, to to bo recorded mum of two years; ISO days of the effective data, unlaaa a and identified by natal type end grade (1) A record of too looks detected by waiver of compliance la granted under and the date and time it wpreaante. the vinyl chloride monitoring system, as i U1. If a waiter at compliance to (ill) The quantity at material proc required by 131JS(b>(3), including toe granted, the lint report to to bo ubalttad on a date scheduled fey the Ad- mhustrator. (2) In the eaaa of a new aouree which did not hare an Initial startup date pre ceding the affective date, the first raport to to bo submitted within IN days of the initial startup date. (c) Unless otherwise medfled. the owner or operator shall tae the Test Methods In Appendix B to this part to conduct emission teste as required by paragraphs (0(2) and (e)(3) of this section, unless an eauhralent or an alter native method has been i pprovad by the Administrator. If the Administrator finds reasonable grounds to dispute tho results obtained by an equivalent or al ternative method, he may require the use of a reference method. If tho results of essed by the stripper to to be determined on a toy aotMe basis and by a method submitted to and approved by too fid- (iv> At too prior request of the-Ad ministrator, tho owner or operator shall provide duplicates of too remitter re quired In paragraphs (c)(2)(1) and (e) (2) (U) Of this aar-thm (v) Tho report to too Administrator fay toe owner or operator is to ineluda the vinyl chloride content found in all the samples required in paragraphs (e)(2) (i> and (e) (2) (ID of this section, aver aged separately for each type of resin, over each calendar day and weighted ac cording to toe quantity of each grade of resin processed by the atripperfe) that calendar day, according to toe following equation: concentrations of vinyl chloride as measured, analysed, and recorded by the vinyl chloride detector, the location of each measurement and the date and ap proximate time at each measurement. (2) A record of tho leaks detected during routine monitoring with the portable hydrocarbon detector and the action taken to repair the leaks, as re quired Iqr 131.39(b) (3), Including a brief statement explaining the location and cause of each leak detected with the portable hydrocarbon detector, the date and time of the leak and any action taken to eliminate that leak measured in accordance with 131.33. (3) Bor the relief discharges from reactors subject to toe provisions of 131A5(a>, a daily operating record for each reactor, including pressures and the reference and equivalent or alterna tive methods do not agree; the results obtained by the reference method pre vail. and the Administrator may notify the owner or operator that approval of Ar'r~ Or'r 2. Appendix B is amended by adding Test Methods log and 107 as follows: lOS--OmumunoK or Vntn Statkwut fioouexs the method previously considered to be Pa, Ma,+Ptitat+ .... equivalent or alternative to withdrawn. (1) Tho owner or operator shall in clude tat the report a record of any emis ------------ -- - -- IWlatunM or this method should not bo attempted by pswous unfamiliar with tho A-94 hour avwaes wntnm at type T, into Is operation of a gas chromatograph, nor by sions which averaged over any hour period (commencing on the hour) are in excess of the emission limits pre scribed in II 31.62(a) or (b>. 131.33(a), or II 3144(a)(1). (b>, (o).or (d).or for any control system to which reactor emissions art required to be ducted in 131.34(a) (3) or to which fugitive emis q-T5irrodaattm(tjr T, rates evvrtlMSka pscleC, ia k. T.-Typs at nun; MX ... elan fe Wd aambsr otrasta tjrpm predated dame tea St* iMVPHMt Af--Oaocrntrstlon at vinyl OMh b oa* esfb f grads Oi raate. Is ppm. P-TraOoMoa at end* Oi ns Mouth, la ktT thorn who are tmlhmlllor with oourco sam pling, ae thorn are pony details that are beyond tho scope of this presentation. Care mutt ho taarohad to pravont exposure of oampllng porootmol to vinyl chloride, a car- "lTprtnctpto and Applicability. U An Integrated hag aaacpte ct stack gaa rcateteUig vinyl chloride (ehloreathyisna) sions are required to bo ducted tat 131A3 (b)(1)(U), (b) (2). (b)(S). (b)(3)(11),or (b)(3) (11). The emissions are to be meas ured In accordance with 131.33. (2) In polyvinyl chloride plants for which a stripping operation to used to (vi) The owner or operator shall re tain at the aouree and make available for inspection by the Administrator for t minimum of 2 years records of all data needed to furnish the Information re to subjected to chromatographio analysis. ai^BxiK m g^mgg^m mroix^ro^agmu ngHBiur. U The method is applicable to the muiuremsat ct vinyl chloride la stock fame froa ethytone dichloride, vinyl chloride and poly vinyl chloride manufacturing ptoccues. ex cept whore the vinyl chloride is contained in attain the emtotoon level prescribed In 16i.34(e). the owner or operator shall include tat the report a record of tho vinyl chloride content in the polyvinyl chloride resin. Test Method 107 is to be used to determine vinyl chloride content quired by paragraph <c)(2)(v) of this particulate matter. section: The records are to contain the foDowing information: (A) The vinyl chloride content found 1. Bangs and Sensitivity. The lower limit ot detection win vary mcoordmg to the chromatograph used. Values reported Include 1 x 10-' mg and x 10-' in all the samples required in paragraphs mg- (e) (2) (i> and (c) (2) (il) of this aecttoo, S. Interferences. as follows: (i> If batch stripping is used, one rep resentative sample of polyvinyl chloride resin to to be taken from each batch of each grade of resin immediately follow ing the completion of the stripping, and grade aud the date and time the batch to completed. The corresponding quantity of material processed in each stripper batch is to be recorded and iden tified by resin type and grade and the date and time the batch to completed. (li> if continuous stripping is used, one representative sample of polyvinyl chloride resin is to be taken for each grade of resin processed or at intervals identified by the resin type end grade and toe time and date of toe sample, and (B) The corresponding quantity of polyvinyl chloride resin processed by the stripper(s), identified by the resin type and grade and toe time end date it represents. (3i 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). Emissions are to be deter mined in accordance With 161.37(g) (5>, except that emissions for each reactor arc to be determined. For a reactor that Is also used as a stripper, the determination Acetaldehyde, which can occur lu some vinyl chloride sources. wUl interfere with the vinyl chloride pock from the Chromoeorb 102 column. Bee sectlone tu and 6.4. If resolu tion ot the vinyl chloride peak is still not satisfactory for a particular (ample, then chromatograph parameters can be further altered with prior approval of the Admin istrator. If alteration ot the chromatograph parameters falls to nootre the vinyl chloride peak, then supplemental confirmation of the vinyl chloride peck through an absolute analytical technique, such as mam spectro scopy, must be performed. 4. Apparatus. 4.1 Sampling (Figure 1). 4.1.1 Probe--8talnlem steel. Pyre* glass, or Teflon tubing according to stack temper- JO I FfDMAl HOIST!!, VOL 41, NO. 70S--THUtSOAV, OCTOMt 31, 1774. BFG32324 4M1V atm% neb equipped with a glam wool plug i mnn partleutete mates*. 4.14 BMpplallwa Ttflon, M mb outside probe to bag. A new tmuaed place Is saapioyed Ul Mop wa for each scries of bag samplss Oft otmtlHulso Rase gfn Bow In 4.IJ Mala ft) and ftiaili (S) atatalaaa A Raaginta. It ta naammry that aU reasteel qukn-eonnoets, with baa ahecka (cno gt--i *ri ef nbi iimatmraphlii graits i injection at pair without) loaatad aa *sn M llawa 1. At Oaalyrie 4.1.4 Tadlar bags, 100 Utar capacity Ta ftslal SiUttai cm or I. m-Xm . The sewage vwlwo for tbase tero areas eontain sample. Ttflon bap ara aat soeept- grade, (or chromatograpbla carrier gaa. abla. Alumlnlard Mylar baas amp ba aaad, S.14 Hydrogen pi Eero grade. provided that tha samples ara aaalyaad 0.14 Oxygen gaa, or Air. as required by Oompere tha ratio of a. to A. for tha vinyl wtthia M boon of coUaattaa. 4.14 Rigid leakproof eontalners for 4.1.4. with oovertng to protect oootaata (ran sun light. 4.1.4 needle valr 'Met sample flew rata. 4.1.T Pump--leak-free. Mlniqrum eapoo- ltjr 0 lttaia par wtinuta. . 4X0 Charcoal tuba--Ta pmwnt adaula- rion of vinyl chloride to atmosphere la vleln- Ityof samplers. 44J blow aaatar--Pot ubaarrbig Haapli flow rata; capabla of maaaurlag a how raaga (Torn 0.10 to ijoo Utar par minute. 4.1.10 Connaetlng tubing--Teflon, 44 mm outalda dlamatar, to essembli aampla train (Flgura 1). 4.1.11 Pitot tuba--Type 0 (or equivalent). attaehad to tha proba ao that tha sampling flow rata can bo regulited proportional to tha ataek gaa velocity. 4i Sampla recovery. 44.1 T-iblng--ration, a.4 mm outalda diameter, to connect bag to gaa chromato graph aampla loop. A saw unuaad pieoa la employed for each aeriea of bag campice that oonetltutea an amlaslon teat, aad h to be dla- carded upon conclusion of analysis of tboaa baga. 41 Analyata. 44.1 Oaa chromatograph--With flame tha datester flare grade. 4 Calibration. AAl Vinyl chloride, M4+%--Per prep aration ot standard gaa mtzturae. 44 Calibration cylinders (S), optional One each of 00.10 and 6 ppm vinyl ehloride m nitrogen with certified analysis. Analyata most be traceable to MBS (National Bureau of Statuterda) or to a grevtmetrlcally cali brated vinyl chloride paraaaattou tuba. 044 Nitrogen gaa Two grade, for prep aration of standard gaa mixtures. 0. Procedure. 4.1 Sampling. Assamble Uw aampla train aa in Figure 104-1. Perform a bag leak aback according to Bsetlon 7.4. Obearvo that aU oonnsetloas between tha bag and tha proba ara tight. Place tha and ot tha probe at the centroid of the stack and start tha pump with the media valve adjusted to yield a flow of 04 lpm. After a period of tbm suflldant to purge tha line several tunas has elapsed, connect tha vacuum llna to the bag and evacuate the bag until tha rotam eter indicates no flow. Than reposition tha aampla and vacuum Unco and begin tha ac tual sampling, keeping tha rate proportions! to tho stack velocity. Direct the gae exiting the rotameter sway from sampling pe--"nutf At the end of the sample period, chut off the pump, disconnect the aampla Urn from tho chloride aampla with tha same ratio for tha standard peak which Is rtoaast In bright. As a guideline, if these rattae differ by mom than 16%, tha vinyl chloride pack may not bo pure fpeariMy acetaldehyde Is preeent) and tha meander1' column should bo em ployed (see Sect* ' it. 04 Measure the isUaat temperature and barometric yrmsure near the bag. (Aasume tha relative humidity to bo 100 percent.) Prom a water saturation vapor pressure table, determine tha record and water vapor con tent cf the bon. 7. OallbratiCB and Standards. 7.1 Preparation of vinyl chloride standard gas mixtures. Bvaouate a slxtaan-lnch square Tadlar bag that has passed a leak check (described in Section 7.4) and mater In 8.0 liters of nitrogen. While tha bag la filling, oaa the 04 ml syringe to inject 360*1 of M.9+% vinyl chloride through the wall of the bag. Upon withdrawing the syringe needle, lmmsdlataly cover the resulting hole with a piece of educates tape. This gives a concen tration of 50 ppm of vinyl chloride. In a like manner use the other syringe to prepare dilu tions having 10 and 6 ppa vinyl chloride concentrations. Place each bag on a smooth surface and alternately depress opposite sides of the bag 60 times to further mix the gases. Ionization detector, potantiemetrie atrip chart recorder and 1.0 to BA ml heated aam pllng loop In automatic eamplo ealve. 441 Chromatographie imlwmit--Wtalwlaa atari, 3.0 x 34 mm, nontalnlng 60/10# maab Chromoaorb 101. A secondary oolum ot OB BP-96, ao% P. atalnless on 00/00 atael. 3.0 mmasxh AW Chfcmeaarb 64 aim. win ba bag. and disconnect the vacuum Una from tha bag container. Protect the bag container from sunlight. 64 Sample storage. Sample bags must be kept out of direct sunlight. Whan at all pos sible, analysis is to ba performed within 34 hours of aampla collection. . 44 Sampla recovery. With a place of Tef 74 Determination of vinyl chloride re tention time. This section can ba performed ,simultaneously with Section 7.3. Establish chromatograph conditions Identical with thorn in Section 64 above. Sat attenuator to Z 1 position. Flnh the sampling loop with zero hrilnaa or nitrogen and actirate the sample vulva. Recced the Injection time, required If acetaldehyde la present, if uaad. lon tubing identified for that bag, connect a the sample loop temperature, tha column the 8P-96 column la placed after tha Ghreeno- bag inlet valve to the gas chromatograph temperature, tha sorrier gas flow rate, the aorb 103 ooinmn. Tha combined nohmnnt aampla valve. Switch the valve to withdraw chart speed and tha attenuator setting. should then bo operated at 110*0. 444 now maters (3) Rotameter type. gaa from the bag through tha sample loop. Plumb the equipment so tbs sample gas Record peaks 'and detector responses that occur In the abeenoe ef vinyl chloride. Main 0 to 100 ml/min capacity, with flow control peases from tha aampla valve to tha leak-free tain conditions. With tha equipment plumb trivet. 44.4 Oaa regulators- Por required gas pump, and than to a charcoal tuba, followed by a 0-100 ml/mln rotameter with flow con ing arranged MeMMaWy to Section 64. flush tha sample loop tor 30 seconds at tho rets ot cylinders. trol valve. 100 ml/mln with one of the vinyl chloride 44 0 Thermometer--Accurate to ana de 6.4 Analysis. Sat the column temperature calibration mtxtuiaa and activate the sample cree centigrade, to msosure temperature cf to 100* O tha detector temperature to 180* valve. Record tha Injection time. Select the heated sample loop at tune ot sample injee- tion. 44.0 Barometer--Accurate to 6 mm Hf. to measure atmospheric presaura around got chromatograph during aampla analyata. 44.7 Pump--Leak-free. Minimum capac ity 100 ml/mln. 4.4 Calibration. 4.4.1 Tubing--Teflon, 0.4 mm outalda diameter, separate plecee marked for each calibration concentration. 4.44 Tedlar bap--Blvtean-lnch aquam size, separate bag marked for each calibra tion concentration. 4.4.3 Syringe--04 ml, gaa tight. 44.4 Syringe--60*1, gas tight. C. and tha sampla loop temperature to 70* C. When optimum hydrogen and oxygen flaw rates have been determined verify and main tain these flow rates during all chromato graph operations. Using aero helium or nitrogen aa the carrier gaa. aatablMi a flow rata In tha range consistent with the manu facturer's requiremanta for satisfactory de tector operation. A flow rate of approxi mately 40 ml/mln should produce adequate separations. Observe the beer line periodi cally and determine that the notes level baa stabilised and that base line drift baa eaaaad. Purge the sampla loop for thirty seconds at tha rata of 100 ml/mln. than activate tha sample valve. Record tho Injection time (the position of tha pan on tho chart at tha time peek that corresponds to vinyl chloride. Measure tha dietsues on tbs chart from tha Injection time to the time at which the peak maximum occurs. This quantity, divided by tha chart speed. Is defined as the retention time. Record. 74 Preparation ef chromatograph cali bration curve. Make a gas chromatographic measurement of each standard gaa mixture (described In flection 7.1) using conditions Identical with theca listed in Section 6.3 above. Plush the sampling loop for 30 seconds at the rate of 100 ml/mln with each standard gas mixture and activate the sample valve. Recced C,, the concentrations of vinyl chlo ride injected, the attenuator setting, chart peed, peak area, mmple loop temperature, > Mention of trade names on specific prod ucts does not constitute endemement by the Environmental Protection Apncy. of aampla Injection), the sample number, the sample loop temperature, tha column tem perature. carrier gas flow rote, chart spaed column temperature, carrier gae flow rate, and retention time. Record tha laboratory pressure. Calculate A., the peak area multl- KMOAt MOinU. VOL 41. NO. JOS--THUkSDAT, OCTOOH 11, 1474 BFG32325 v aitas attenuator N* tajMtlOD MM MM tratiom hM tai iUM, nm through M pun. 1 MM MHfi W VHwV MB WNv OT' bag aampiae. ttthmr to mm fTiqsaat of this section to taquiiMd subsaqumit to tag use. n to otoo KtM ttot u bo imfnnowi prior to bog um. After M um, otto om big did not develop ImIm m tOttawa. TO iMk otort, ooanict o wotor monometir and urtoi Um big to t-U am M,0 (t-4 tat &M. Allow to stead gar 10 otottw. Aar lUrptoia aaot la tbo waMr imnoontar Indiratoo a teak. Also aback the rigid eentalaer tor taata 4-- tltif BULBflAT* (San: Aa iitwaotlto took cheek to to ptomurlae tbo bog to 6-10 am HJ> or 9-4 in. b/> ind allow to rtut overnight. A MM tag man -- a -) Woe Mb MHgito tag to Mi ttgid Mtotog, ptaM o ntiMtor in-hae totwem tbo bog bad tho pump mist. Evacuate tba tag. PeOure of tba appears to ta empty ladtootM o took. U Determine tbo aota paak follooo: > WMI IMMMtttol i SgBfltiOO lot-1 lomcae 107--Doraaimranoar or Varnaao- mg sad 4X1V* ox- With proper calibration, tba upper limit may te axtaodsd aa needed. trtAan,s-n maple peek m. A-Ths raarund pal tab. AHTito aMaunaea beta. '"to BaMPiaa. am Torn, Catnana Oowraarr er 3. Precision aad Reproducibility. Foarvnm. datum bam. Burnt, War Aa lntarlaboratory nompartoon batwaan Oaaa, am Lam flaacrub aovan laboratcrlas aif three raaln aamplaa, each spilt Into thrta parts, yielded a standard M Vinyl abtarMa ooooentretloae. TYam tbo oiUbntloo cum described la gentian TA. above, abtoet tbo value at 0, tbit corngeoto to A,, tbo aampto paak ana. Oileulita C, ao follows: Farformane* of tbto method atoould ad ta bttomptad by paraora unfamiliar wltb tbo oporatloa of a gas chromatograph. nor br ttooaa wbo arc Unfamiliar wltb sampling, or than ara many datails that aro bayond tbo deviation of 3.83% tot a aampla with a mean of 3.09 ppm, 4.18% for a aampla with a mean of IAS ppm. and 4A9% for a aampto wltb a mean of 6346 ppm. 4. Batety. DO not lolaam vinyl chloride to tha labora tory atmosphere during preparation of tand- anto. Venting or purging with VCM/alr mtx- aqmuon loo-s A#-TbemwaltnergTia,per esatta at tla bag Mata, m Cfe-Tta mcMtntfM U cMmMb t tto bf C.-TbroacotatSusa at vtayl ahbrtto IciBmlil bf the (M tataMaanpb, la pom IMk Muni praam. tM Miwtor praam isweded dartar mMteata*. era Ha. . . n>Tta atapb tap mapaeime sa the ahtotato mb at th* Urn l inalpito, *CT B<-Tta bbmtjrr praam M Uaw at iMbnto, mb lofittBflH. 1. brown. O. W,, toy. B. W. pad Stephen son, U. a. "Vinyl Chloride Mraltoring Par tbo B. P. Qoedrleb Ohaoaleal Oompaay ta loulMtl*, Dentodty." Region IV, OA Envtrofunantal Protection Agency, SurveOlanc* and Analysis DMstoa, Athene, Oaargto. team 94. 1914. A "evaluation ct A OcnscUon bad Analy- tleal Procedura lor Vinyl Cblortda la Air." by O. D. Clayton and Aaaociataa, Daeamtar IS. 1974. EPA Contract MO. 8S-6S-140S, TMk Ordar No. 3. EPA Report oM. B-VCt-L paraonnal to vinyl chloride, a aatebmgaa. 1. Prlaolpia and ApplioabUtty. 1.1 m taato far thto motbod nlataa to tbo vapor aqntlibrtnm wbieb to srtahHahsd batwaan RVCM, PVC. mala, wntar. aad air In a dosed ayitam. It baa bam demonstrated that tbb RVCM In a FVC raaln win aquUlbrata In a ninnad vmaal qulta rapidly, pro* yldad that tha tamparatura of tbo PVC raaln la malntalitod above the glam traaattien tamparatura of that apaaMto raria. 1A Tbla proeaduro to aultabla for deter mining tbo vinyl chloride monomer (VOX) eontaat of Itipromaa waatawatar aamplaa. and tbo raaldual vinyl nhlorldo monomar (HVCM) content at polyvinyl chloride <PVC) raam, wot cake, Hurt, aad latax aamplaa It cannot ta used, for polymer in fuaad form, aucb aa abaot or cubes. If o raaoiution aC tba ylnyl chloride paak to net aattofactory far o particular aampto, than chromatograph paranwten map ta altarad with prior ap proval ot tbo Administrator. If tbaro to rea son to ballava that some other bydrooarbaii with an Identical retantion tbno to praaant in the aampla, then supplemental confirma tion of tbo vinyl rtilorUla paak through aa absolute analytical techulqus, such as mass spectroscopy, should be performed. turas must ta bald to a minimum. Whaa they ara required, tbo vapor must ta routed to outside air. Vinyl chloride, area at low ppm totals, must never to seated Inside tba laboratory. After vlato have Imq analysed, tba pressure within tba rial must be vented prior to removal ham OM instrument turn table. Vlato must ta seated Into aa activated charcoal tuba using a hypodermic needle to prevent release of vinyl chloride into tba laboratory atmosphere. The charcoal must ta raplaaed prior to Tiny! chloride break through. A Apparatus. hi Sampling, SJJ Bottle*--SO ml (3 os), wltb waaad llnad screw on tops, for PVC samples. Ui Vlato--<0 ml Hypo-vlala.1 sealed wltb Teflon {seed Tuf-Baad dlaet for water earnplot, UA BlaeMeal tap* <w equivalent, to prevent loosening of bottle tops. BA Bampto recovery. BA.1 Vlato--With scale and caps. PerkinDinar Corporation No. 106-0113, or aqutveInt 8AA Analytical balance--Capable of weighing to 04*1 gram. 44. Syringe, 100 <8 Prectrion Sartos "A" Ha 010033, or equivalent. a. Bangs and SenaiUvlty. Emtatmi Method tor Vinyl Cblarldi." by Mid- Tha lower limit of detsetioa of vinyl chlo .Mention of trade names an specific prod- waat Remearch institute, laid. BPA Contract ride will vary according to tba chromato- Mo. 69-01-1003, Task Ordar Mo. 1. graph mad. Valuas reportad include 1X19-* Mroomentsl Protection Agency. 1 nm tfoisrck. vot. 4>, no. 3f--mussbav, ocresn it# m* BFG32326 U4 Via! srolor, MUa-Brar Mi 190- scaling and weighing, uHng a 100 *1 syringe. 0109 w tqvMai In the earn of dispersion r--tin, the eap U Analysis. esnnot be used. The tempi* Is itmteed 14.1 Om elwik|ii|i> Twttu weighed sppradmately in an aluminum dhh, Corporation ModH Ml >irt m- btMgni to the tend viol end weighed Ifuer. Ho. 104-0001, Of equivalent. accurately in the vial. The sample la than 7JJ Hregraaemtag the chromatograph-- UJ Chromatogripbto ooliini min. placed m the Parkln-Khpor head spaeo ana Program the chromatograph as fSUouo: IMS stee), l axll mm. WMHm M lyser (or oqulvalontl and icniMtlonid for ono Dmtng thna--The normal rating la Cubotu 1000 osi CiiHpU A, Perktn-Btoesr hour a* b0*O. Corporation No. ItMlH, or (qulntaat. Corbopek c eon bo used la plan of Carbopak Nora: floms aluminum vial capo have a oonter section which must be removed prior I. A--AnalyHe lira The normal asttlng to minutes. Ctrtau typos of mmploa eon- A. to placing into mmple tray. If not tamoitrt. tain high boning mafsrlale which eaa eanao M.9 Thermometer--# to too* O. accurate aerkmi damage to the lnjoctlon needle will interference wUh the vinyl chloride peek on to 0.1* a Perkm-Elmer Ho. 100-0100 or occur. subsequent auelyew In thorn caeca the equivalent. 7JJ Ouepenetoo rain alurry and wet coke analysis time muat bo adjusted to Htoalnata 54.4. rrmpu tny thmuMtit tfilnH* mmple*--Slurry must b* flltsrsd using n the Interference. An untametad beckfluxh Perkln-Rlmer Now 100-0100, or equivalent: raall Buehaar funnel with vacuum to yield system can eleo.be weed to solve this prob OJA Bepta Sandwich type, tar auto wet cake. The Altering proem must bo con lem. matic dosing, 10 aa, Ptrtdn-BUnar Ho. 100- tinued only as long aa a iteaSy ctraam of e. B--flushing The aoraal setting la oJ 1000, or dvinkat water la anting from the funnel. XxoeaHve 0J.0 Integrator - neordtr -- Hewlett - filtration time eould result In mum loss of d. 70--StahOtoetom time--The ncenol set- Packard Model S300A. or equivalent. VCM. The wet oaks mrnplo (0.10 to 44 gram) ttng to 0J minuf 0J.7 Miter drte wei Ily (0) -HtMa. la added to a tared vM (Including septum BUner Mo. 2230117, or equivalent. and aluminum eap) sad Immediately eealed. BwhHI raWH4 ra 4 UJ Soap 01m flowmeter--Hewlett Pack* Sample weight to than determined to deci 7JJ Preparation of sample turntable--Be aid Ho. oioi-ouo, or equivalent. mal places. Tha sample to than pieced in the fore placing any aupk into turntable, be 0.4 Calibration. Mdn-Bwr bead epaoe analyser (or equiva certain that tha oentar section of the alu,- 0.4.1 Regulator!--(or required gao cylndm. 0. Beagenta. lent) and eondtuonad for ono hour at 90*0. A sample of wet'cake to utad to determine n (total aoUda). This la required for calcu minum cap has been removed. The numbered --1--r1* bottles mould be placed in th* cor responding numbered positions in tbs turn 0.1 Analyila. lating the BVCm. table. Insert eamnlee In the followtnc order: 0.1.1 Hydrogen gee aero grade. 0.1J Nitrogen ga asyo grade. 0.1J Air earn grade. TJJ Dlaperetan rceln tturry mmplee -- Pceltlone 1 A a OM 3000 ppm standard* This material should not be Altered, sample for conditioning. Thmo an necessary only muat be thoroughly mixed. UMng a tared after th* analyser bee not bean used for 34 M Calibration. vial (including septum and aluminum cap) OJA Standard cylinder! (4) one each add appradmataly 0 drops (0JS to 0JS at to, 100,0000, and 4000 ppm vinyl chloride grams) of alurry or latex using a madidne la nitrogen, with oertlfled analysts. dropper. This should b* dons Immediately 7, Procedure. after mixing. Seal tbs vial as toon aa passible. 'Determine mmple weight accurate to 0J0i hour* or longer. Position 3--90 ppm standard, freshly pro- pind. Position 9--900 ppm standard, freshly pre pared. Position I loop ppm standard, freshly 7.1 J pvc tempilng--Allow the raeta grams. Total aample weight must not moved or 0J0 grama. Condition tha vial far one hour alurry to flow from a tap on the tank or sUo at W*C In the analyser. Determine the T8 prepared.' Position 9 -4000 ppm standard, freshly pro- pind. until the tap line baa been wall purged. Bx- on the Hurry temple (flsetton 7JJ). Position 7--Sample No. 7 (This to the first tend a 00 ml aample bottle un<Mr the tap. All, 7JA mproora wastewater mmptao-- ample of the day, but la given os 7 to be con and Immediately tightly eap the bottle. Wrap Doing n tared vtal (Including septum and sistent with th* turntable and the Integrator electrical tape around the eap and bottle to alummum eap) quickly add approximately printout.) 1 ee of water using a medicine dropper. Bead After all tamplaa have bean positioned. In Identifying label an each bottle, and leeced the vial as toon as point*. Determine sert th* eeoond set of 60, 900, 3000, and 4000 the date, time, and tempi* location both on ppm ttenderito. Sample*, Including stand the bottle* and In a log book. dltloa th* vtal for two hours at 90*0 in the ards must be conditioned In the bath of 7.1J Water mmpllpt Prior to use, the analyser. BO ml vlala (without the diaea) muat be 74 capped with aluminum fe|) and mufltod at 74.1 400*C for at todgi <m hour tQ doctroy or install i mpaofCMi litlngugliti eoiumn and oon- 90* C for 1 hour (pot to rated 9 hours). 744 Start chromatograph program-- mien on temples. Including standards, have been eondltlaral t ff* O tor 1 hour, start ^ S&W&XKtS:tartar* with SltttB t exit etu tion on the vlala loo. to.overflooring ao that a oonvex i ferae at tha top. 0* 0*C Do not oosuaaet tha nhimn to the detsotoc while aunt fcc oarofuBy fsOowad when atarttng tfljiwlnmiit tgjiial ajd stqpptgg pregrtta to provent damage to Tha excra watar la **74J P>taraSS^o of total solids (TS). dlie la carefully the opening of the' teal over the die* the seek of the vial and crimp Into place, AHx as Identifying label on the bottle, and teeoed the date. time, and tampla location both on tha vlala and la a log book. All tamplaa muat ha kept re frigerated until analysed. 7J Sample recovery. Hamplee must be run within 24 hours. 7J.1 Ream maples--'The weight of the resin used mutt be between 0.1 end 4J grams. An asset weight must be obtained (+0.001 gram) for each aample. In the earn 3 sus pension resins n volumetric ewp eaa be pre pared which win bold the required amount of sample. The mmple bottle Is openad. and the cup volume of resin i* added to the tared ample vial (including septum and alumi num cap). Tha vial It immediately males and the exact mmple weight Is then obtained. Report this value on the data sheet as It Is inquired for calculation of RVCU. In the cam of relatively dry reein eemplm (water a--Sat rssulator on M pUg. Srt regulator on to 14 kg/em*. Normal flows i should b* 39 to 40 oo/mlnuts. For wot cake, Hurry, roeln solution, and PTO latex tempita determine T8 for each sample by aoouroteiy weighing approxim t With babble Sow mttar. b. Burnsf air supply--Sst regulator on cyl inder to nod 90 psig- Sot regulator ta chromatograph to supply air to burner a* a rat* between 990 and BOO oc/mlnute. Cbsok ately 9 to 4 gram* of eampto In an aluminum pan before and aftar pitting in a draft oven <100 to MO* C). Semples must be dried to constant weight. After lint weighing re turn th* pan to the even for a abort pe riod of time and then reweigh to verify com 3. Hydrogen supply--8*1 rsgutotor on eyltndsr to read 90 pslg. Set regulator on chromatograph to supply approximately 35^9 ce/mlnute. Optlmlz* hydrogen flew to yield tbs most ssnsttlvs detector response without extinguishing the flame. Cheek flow with bubble meter end record this Sow 7J.U Temperature adjustments Set temperatures as foUswat a. Ovsn (chromatographto column), 90* C. b. Dosing line. 140* O. e. Injection block, 140* C. d. Sample chamber, water temperature, plete dryneao. TS to then calculated as the final (ample weight divided by Initial sam ple weight. 9. Calibration. Calibration to to be performed each eighthour period when the instrument to used. Bach day, prior to running samples, the col umn should be conditioned by running two of the previous days 3000 ppm standards. 9.1 Preparation of Standards. ' CalibreUoo standards are prepared by fill ing tha vlala with tha vinyl ehlortde/ultrogen standards, rapidly seating the septum and sealing with the aluminum cnp. Une a stainless steel Una from the cylinder to the content <0.3 weight %), 100 *1 of dletllled 90* C1J* O. vial. Do not us* rubber or tygon tubing. The water muat be Injected Into tha vial, after 7J.1J Ignition of flam* IonNation detec- sample line from the cylinder must be fHMBAl Bteiim, VOL 41, NO. SOS--1NUBSOA7, 0CT04H 11, 1*7* BFG32327 q toRM^UOp Iw WMfM^BnKl VBIlMMWrt^MW v|PVlBfWli Ttata. Aftor purplnf, Tadoea tha flow mto to mwi--My 900-1000 oo/min. PUoo 1 of Mm Into vial (mot bottom) ud aftar 6m mtnuto taowly noon toblag. Ptaoo omtuta to mi a* aooo m poulblt to mlnttoim atastafl olr with aampte. ATMr too stand* Mimbm*aaaiad. iajset iw^i of amom U Praparatlne of chromatograph caMbm- Prapara two W ppm. two #00 ppm. two 10M ppm, ml two 4000 ppm itudiiO aamplaa. tom too mUbntkm aamplaa in asaetiy too MM Mflflflor m rtfulax mmploo not IU too Integrator arm counts for oooh staadoMI mfliplo 0.. too oonoantraOcu of vinyl eUtrm is aoeh staadoifl aamplo Draw o l!ao at bom St arooflh too potato. *. oolimlotioBo U Baopoon factor. From too eallbrottoa ewn daacrlbad la aotloa U aboro. aatoot too rahM of C toot oorraoponda to A. for oaeh aaaipla. Ooa. poto too raapoaoa factor, to, for aoeh aampte. m foUooa: Equation 107-1 li Baatdnal vinyl chlorlda monomar ooa* eantratten. or vinyl oblorMo momomar oouoaatratton. Calculate 0m ao fouowa: . C--T& (S'+Jtn) Equation 107-2 ft--CtaaHiaMm aI atari ahioiMa ta tha i te ppM. f.-Ubatlorr atmosphr pnaaws, aa H*. T|-- Harm launpuatuia, X ta--Mehmlar alM cfvCM (J). V--Vataiaa tamper pirns (rial rolana hanaplt sti-WUgM taaaapia. ara X-On aemuat (kju) Jf-Haarr*! (TO, *Lfa-awjaoxnM-a*o-tXh,r VCM ta lor VCM rvc ta I at aa (appnmmaU) namir ampb.at W*0, lE>txira>r. Aalpinnlta tamparatnn. *K. imuiSSSlmGSmS" m "* *vmU,am* ig=8B: JL P-Jllaua.il*. \ 1 r--VWaatam,(tOU|. t ! HatatalhOitataOJKuilta. N Cw-^ClXM^gg) Iquttifl IOT-* aqaallm aaa Oil, PVC aa( Cr"XTl XU^ftKt(TS) Equation 107-4 r.-Tatal *a. NMk JT. auto to mmtaafl. toaulta oalculatad using aquation 101-4 rapraaant oonoantratton baaad oa too total mmpla To obtain raoalto baaafl oa flip FVO content, dtatdo bp 18, Faralas (anprualaialil waaNimtar wpl, Kaootua MT-t am DaaZapUadts tha feHaarlm: Cr"'mT, [^ io-)] Equation 107-0 10. Kafaranoaa. / 1. Botadual Vinyl Chlorlda Monomar Ooutant of Poipainyl Chlorlda attain and Wat Cako flamplaa, B. T. Goodrich Obamleol Oo. Standard Taat Frooaduro No. 1006-T. B. F. Ooodrloh Tanhnleal Cantor, Aton Lake, Ohio. January W, INI. *. Barons, A. to. "Tha Solubility at Vinyl Chlorlds la Folyrtnyl Chloride," AOa-Mvt* alon of Polymar Cbomtatry, Polymar Praprlnta IS (1): 1PT, 1974. 9. Barani, A. to, "no Diffusion at Vinyl Chlorlda la Poiytlnyl Chlorlda," ACS-Dltltaoa of Polymar Ohaotaotry, Polymar Pro- prints If (1): tot, 1*71. 4. Bitan, A. to. I*, to Crldar. C. J. Toma* nak and J. ML Whttnoy, Aaalytaa tor Vinyl Chlorlda in PVC Powdota by Haad-Bpaos Qaa Chromatography," to bo published. (P* Doc.7#-90049 POad 10-90-78;9:49 am] FEOCtAl noum, VOL 41, NO. 90S--THU9Ar, OCTOtfl 21, 1*7* BFG32328