Document rB86ojzVMrx1k6LZ34rm95kOa

CALVERT CITY PLANT INTEROFFICE MEMORANDUM To: R. C. Lietzau From: B. D. Helms Personnel Monitoring Vinyl Chloride Date: 18 February 1982 Copies: 2Sr< 0T:CTd^Sfal*-^" y/r- G. N. Boyd has completed the field comparison of Reiszner badges versus the pump method for determining employee exposure to VC1. The results (attached).show excellent agreement. I recommend we change to the badge method of monitoring for VCl. The accuracy will he rechecked in three months with standard gas. Also area field comparisons with the pump method should be made every three months. Your approval is requested. B. D. Helms AP00040027 \ IPWC. ESCAMBIA PLANT INTEROFFICE MEMORANDUM C. A, Pendergrass Prom: Re: D. E. Hoffman Prepressurizer for VC1 Headspace Analysis Date: Copies: 26 August 1983 R. H. Sroufe J. W. Kadlec T. J. Regan Tl oUmlll Nnuollll B. Rose CqJuMaK. B. Helms S. Prescott J. Barr L. W. Allen J. Spata SUMMARY A recent change in the Federal Register method 107 requires pre pressurizing sample vials with nitrogen prior to analysis on the VC1 headspace analyzer. The Escambia QC Lab has fabricated a pre pressurizer in accordance with the required drawings. Initial testing has shown a minimal change in results. If no comments to the contrary are received by 15 September, the pressurizer will be put into service on that date. Discussion The September 7, 1982 Federal Register included a method for prepressurization of vials with nitrogen. These changes are underlined In Attachment I. Drawings of the required apparatus were secured, and the Escambia Instrument Department was assigned the task of building it. This proved to be a lengthly job because most of the parts used by B. F. Goodrich to build the prototype are no longer commercially available. APCI attorneys determined equivalent parts were acceptable and in some cases had to be fabricated at Escambia. The prepressurizer has now been completed, installed, and piped in to the nitrogen supply. Senior Lab Technician R. E, Zeiger has done the necessary cross checking of control samples to determine the effect of the vial prepressurization. Preliminary analyses showed double peaks appearing at pressures above 19 psig. Method 107 calls for the highest pressure possible without double peaks, so 19 psig was chosen as the prepressure level. Several vials were pressured up, put In the hot bath, and allowed to sit overnight to be certain there was no leakage through the septum or cap. Finally, several samples of different concentrations were run both with and without prepressurization. The data is tabled below. AP00040028 C. A. Pendergrass PrePressurizer for VCl Headspace Analysis 2- - 26 August 1983 FINISHED PRODUCT DRY RESIN1 - PPM Atmospheric Prepressurized 52 32 44 53 54 54 43 85 2I 43 1I 11 PROCESS SAMPLES SLURRIES. - PPM Atmospheric Prepressurized 436 308 187 176 106 93 154 135 287 294 81 86 79 72 167 168 68 63 69 65 174 187 180 190 456 470 247 224 527 486 124 127 326 336 189 180 These initial tests indicate a mean drop of 1 ppm at the normal operating range of below 10 ppm for dried resin and a mean drop of 7 ppm at the higher levels. As expected* there is apparently no significant difference when adding the prepressurizer. CONCLUSION The nitrogen prepressurizer is installed in the Escambia QC Lab. Initial results Indicate it is operating correctly and will be put in service on September 15, 1983. DEH:bg D. E. Hoffman AP00040029 ~zrt. '.1 ATTA C/y sW A/T~ `.cr / *rol. 47, / Tue?...;..-. dArttcmbf'r 7. 17 ;; ' R'dcs ana lleculatlons 3C15S i rui l . .upendix C. Tlic ICir.O. *.:j lanur.rv 19. 1931. with an o: :viarc l to extension 10 February 10,1931. i ;J ,-... ::;.rrr.:.ntior. of Five comment !_h irr '.vure received `i ^ rr.u-n-.v.i.-. --.a.-, ' -L) column ;ct;.:.or. :\j the .-nded e/isci rt con'ierr.inp issues rvinive to the prouoaud lest methods. The comments .';nci:dLr_ : .s to pu.-. :1s a method for j GU samplen.Jiysis. have been carefully considered: and wi- --determined to be r.p;;rr,pride by ` r'.7": v:-->-'.!ber 7, >! JJ.-.car.- .;or. (l) of the Clean 'l ,\.r Ac*., ii-uida! rev.-iw of this i niiemRkiniavailable only by the the .-'.uministrator. changes have been mada in the proposed revisions to the toil methods. Procedures 1 ur.J 2 of Appendix C ware proposed and published in the .j filing of a coition tor review in the U.S. i Fci.-rcl Register April 18.1900 (45 FR | lourt oi Appeals for tha District of 2CGS0). Public comments were solicited I Columbia Circuit within SO days of at the time of proposal. The public [ today's puh.icatior. i/t this rule. Under comment period was from April IS, 1900, cscticn 307(L:{2) of the Clean Air .Act. ; to August 21,1980. the requirements that are the subject of No comment letters were received. today's notice may not be challenged inter in civil or criminal proceedings SI" .i/icant Comments and Changes to I broucht by EPA to enforce these, tho Proposed Test Methods [ requiremarts. . . ` Comments on the proposed revisions .-.ODnsssas: Summary of Comments and to the test methods -were received from Responses. The summary of comments industry, industry counsel, enghtcering j .id responses for the proposed test ; methods m.ay bo oiuoined from the U. 5. firms, and equipment manufacturers. A detailed discussion si these comments "PA Library [MD-35j. Research Triangle and responses can be found in the .S'orch Carolina 27711. telephone number I3~.fi 5-11-2777. Please refer to summary or comments and responses which is referred to in the addresses "RevisedTori Metnuds 105 and 107-- soction of this preamble, The summary dammary of Comme.i.s and Responses, , EPA 450/3-66-002." The document of comments and responses serves as the basis for the revisions which have : contains (1) a summery of the changes been made to tha test methods between .nade to the test methods since proposal proposal and promulgation. The major and (2) a .i jrr.mory ol ail the public comments and responses are comments made on the proposed summarized in this preamble. Most of ruvisetl methods ar.d the the comment letters contained multiple Administrator's responses to the comments. The comments have been comments. divided into the following areaj: } Dorkei. A docket, number A--CO-3G, contain;;-._ .^.formation considered by Proposal of Revised Test Methods 108 and 107 EPA in tits development of the test .-.uthods and docket number OAQPS 79- One commenter frit that EPA should j Part 2 that contains background publish a notice in the Federal Register informal:.,r. pertaining to Appendix C to clarify the November 18,19S0, notice ..:e available for public inspection on Test Methods IC3 and 107 (45 FR between LtwO a.m. cr.d 4:00 p.m.. Monday 7G348) as to whether the changes in the through Friday, at EPA's Central Socket methods were proposed or final Euciion (A-130), West Tower Loboy. amendments. The EPA considered the Gollery i. 431 M Street. S.W., suggestion to be reasonable: and a Washington. D.C. 20460. A reasonable notice was published in the Federal ;be may be charged for copying. Register on January 9,1981 (48 KR 1319) to clarify that the ..r.nnges in Methods I FOR FUSTitn INFORMATION CONTACT; 106 and 107 publisfted on November 18. Roger T. Shigchara. Emission 1980. were proposed changes. Measurement Branch. Emission Standards and Engineering Division iMD-iy), U. S. Environmental Protection Sarno/e Analyst's Procedure---Method 100 ' Agency. Research Triangle Park. North One commenter suggested that Carolina 27711. telephone [919) 54 *-- Sedan 7.2.2. Preparation of 237. Chromatograph C..i,bratian Curve, be Public Participation changed to require calibration at lecsi onco every 3 hours, of continuous The revised test methods were operation of tho ciromatcgtaph. proposud and Dublin.--d in the Federal whereas the meth.-.a requires daily Register on NovemLwr 13.1930 [45 r'R calibration. The EPA lias decided it 7t'34u|. Public comments were solicited would bo an unnecessary burden to at the time of proposal. The public arbitrarily set 8 hours as a cutoff point .omrnont period was from November 13. for valid calibrbth,.i. However, the comment has identified the need for instruction ir. the method as to the use of multiple calibration curves in data ..UerpreUition. und Section 7,2.2 has uccu revised to provide) that instruction. Or.c commenter questioned the use of Figure 103-2 because it appeared to illustrate a standards preparation .procedure different from the one described in the method. Figure 103-2 did illustrate u different sample preparation procedure and has been deleted from tne method. Sample Collection and Analysis Procedure--Method 107 One commenter ouostloned_the_n&rL tor"tne samota prauressurization . prijccGure min is included in the revised test meinoq. Tip Agency believes the prepressurtzatici procedura is valid as , p^aprc-ssur!2a:ior. o;"snm?:a vials prior (,/ 18 ibiaiyiis nas yuan snown to produce t SjvalJBS '.Vfi.th agree wttn theoretical r}* VaLJU. A tViBtif lijdflfHH:-. ii <iuW*oT dy tms tecr.niqua r.as ueerLaailgd In the. ot.iiiograpny section of th-t method as an aid in tno use 01 tnis proceuure. Quality Assurance--Method 106 One commantcr requested that Section 5.2.4. Audit Cylinder Standards, further describe commercial gas manufacturers as an alternative source of these standards. Tha Agency considered - nsquest to oc reasonable, and Section l-u.i nas been revised to define the acceptability of audit cytindors abtuinoa from commorcinl gas manufacturers. Docket The docket is an organized and complete file ofthe information considered by KA-\ in the development of this rulemaking. The docket is a dynamic file, since material is added throughout the rulemaking development. The docketing system Is intended to allow members of (he public and industries involved to readily identify .1 nd locale documents so that they car. intelligently and effectively participate in the rulemaking process. Along with the statement of basis and purpose of the proposed und promulgated test methods end EPA responses to significant comments, the contents of the docket wil: s^rve as tho racord in case of judicial review (Secdon -i 07(d)(7)(A)}. Miscellaneous This ruicmbi.ms does not impose any additional emission measurement requirements on facilities affected by this rulemaking. Rather, this rulemaking revises the teat methods -*toJ which the .If / AP00040030 * 'I - . I AJ 'l *:'4i.s:nr / Vr-I. 47, 1 ,!>!?.:".v. Si'TUn,n!;c n?l Ktigulalions V,.'tt'.r.il |f!7--.l.itumiii.-UrM ns Vinyl CM.uh.i; .-null'll (ri .!. :iir. Vm\ cidoriiir. even .'I 5.3.9 ('emulators. For required gas Ci;r,Ui.!i <.i :r. <ir:>'i!S n;nv, low ppn; i: must nrver n: venl nsidn cyikuMrs. .irul Vinvi v,, ...ruin Wii:>'iil fi* i'nivvinvl Iho I'liiur.-.i After v,,.Ir V ivn litii'ii r..:t I 'ei.bsn.ic.i Vial Fre-Pressurizer. vurrv. uol iinn i.... Introduction Pcrforr'.nr,-.! of I lux rvu'HV'd 'dsu-iUl :i:>i altcvr.plrd by pursuits um';t:ntli;ir v.'ili: i];.~ operation if u gjs chronnlu^ruph |GC|, itur by (hose who ure unfiirr.iii.'ir with sonrou Sampling. because kn.nvhuJye beyond the scope of this prcwnlnlion is rcquirnd. C:iru must be exercised to prevent exposure of sampling personnel (o vinyl chloride, a carcinosen. 1. Applicability nud Principle. 1.1 Applicability. Thi* method applies to the measurement of tlic vinyl chloride monomer fVCNt] content of inprooes* wastewater samples, ant) thn residual vinyl chloride monomer (RVCM| cnnte.nl of polyvinyl chloride (FVC) resins, wet cake, slurry, and lolex lanipirs. It cannot lie used fur polymer in fused forms, such us sheet nr cubes. This method is not acntplrible where methods from Section ;M-![hl of the Cirnn '`.'.T.or Act. 33 Li.S.C. (231 i;i seq. |lhe F*<W,il Water Pollution Control Amendments d IM'*:'. 113 .JOwniMti by tint C.:.n VAjIit Act .1 Ki7f; .. .`r.nc.iplii. Tint h.iMx tormethod re.nil s to the vapor notMiitriuni th.it is established between RVCM. PVC resin. wler, and air in a closed syslem. Tho HVCM in n PVC resin will equilibrate rnpidly in a closed vessel, provided that lIte tcmpernlure tae PVC rosin is muinUunrd above tho nsh transition temperature of that specific resin. 2. Range and Sensitivity. Thelower limit of detection of vinyl chloride will vary according to the chrumatoqrnph used. Values reported include 1 * and 4 x 1D~7 ntR. With proper calibration, the upper limit may r.Ti.-iiw.fn. , rrn.i:! tvi.-ilrrl ;i;-inr t<> r.inv TDruJernmTr.ecoic ri'ir.nv;.': vial (nun liie insiiiiincni KixiiJfi nroiectivo shield. iBlueprint availab Vanil.ild!*. \ us nrsi he . en!d t'mv.iqh .i >ni J Cfil bnpporl Section. Emission hyprnl.trmic tuti'dte oiinni-finn to an uctivotod XitMxurumrnt Branch. Office of Air Quality i h'irnruil tube l> pn-i mi reliMSir of vinyl :'mu'.ifiii mui Stnndnrds, Environmental chloride a le u j.iij.srninry sitinospbei'C. Thu Prutuclitju Agency. Mail Drop 18, Research charcoal r.v.isl be replaced prior to vinyl Trianma I'.-u k. M.C. 27711.) , chloride brnalcii-.rousjh, 7. A'.m.nums. Use only reagents that are o G. Apparatus. chronmtoqr.'iphic grade. 0.1 Sampling.Tho following equipment is 7.1 Analysis. The following items are required: required far analysis: 0.1.1 Glass bottles. 80-ml (2-oz) capacity, with wax-lined screw-on jops, for PVC,, . sanip'ur*. ' f. ft.1.2 Glass Vials. S0-r.il cnpuc.ily 1 lypo- 7.1.1 Hytirogcn. Zero grade. 7.1.2 Nitrogen. Zern grade. 7.1.3 Air. Zero grade. '' 7.2 Colibralion. The following Hems era v\id. sealed wilhTcilon faced Tuf-Bond discs, for water samples. G.l-3 Arihnsive Tape. To prevent loosening tif bottle lops. 0-2 Sample Recovery. The following equipment i* required: 11.2.1 Class Vials. Wilh butyl rubber soptg, Pcrkin-lllrncr Corporation Nos. QlOR-OKiH (slats vmls/i OCX) 1-0720 leray butyl rubber srplum. piu;i style). Olfis^ujI (butyl rubber, srpt.i). or equivalents. The souls must be required for oati'braiion: 7.2.1 Cylinder Standards (4). Gas mlxtui aliindjuas (50-. 500-. 2000- and 4000-ppm vir chloride in uiiroyen cylinders). The tester may use cylinder slundurds to directly prepuru chnimaingraph calibration curve drsnribi'd in Section 9.2. if the following ''"condition* are met: Ml The manufacturer certifies the gna composition with an accuracy of 3 percent or better [see Sectu r.iiuir from butyl rubber. Silicone rubber seals 7.2.1.1). ihi The manufacturer recommends urf not ef'.cu'IJUblo. u.2.2 An.iivnral Oalunoo. Capublu of maximum shelf liTe over which the gas concentration does not change by greater * wainhing (o 3O.0001 q;am. than 2:5 percent from the certified value, (c 0.2.3 Vial Sealer. Ferkin-Elmer Mo. 105OJDft. or ofjuivtlant. G.2.4 Syringe. 100-jil mpacily. precision serins "A" Nq. 010025. or equivalent. 6.3 Analysis. The following equipment is The manufacturer affixes the date of gas cylinder preparation, certified vinyl chlartdi concentration, and recommended maximum shelf life to Lhc cylinder before shipment lo the buyer. required: 7.2.1.1 Cylinder Standards Certification. 6.3.1 Gas Chromatograph. Pcrkin-Elmer The manufacturer shall certify the Corporation Model F--10. F--12. or F-45 i lead* coneontwinn of vinyl chloride in nitrogen L Spann Analyser, or equivalent. Equipped with Cuic. \..r...-r liy i;t. aifocliy analysing each buckflush accessory. 8.n.2 CnrnmoloRTtkpSic Cuiutnns. St.ilnlfl** Stool 1 m oy 3.2 mm *nd 2 m by 3,2 mm. bojh, / < cylinder quo ih) calibrating fit*analytical procedure Dii the day of cylinder inttlyai*. cco`liiubrr4uit:cc ;M.i.s unalyiical procedure, the T be extended os needed. containing 50/fl0-meah Porapiik Q.'The r manufacturer shall use, minimum, a 3- 3. Interferences. Tito chromntojjraph columns and the corresponding operating parameters herein described normally provide an adequate resolution of vinyl chloride: however, resolution intsrfrrences may be encountered on some sources. analyst may use other r.cluirms provided that the precision and accuracy of the analysts of vinyl chlurido standards ora nut impaired end ]\q has avaiUtbie lor review Information confirming that there is adequulc resolution of the vinyl chloride peak. (Adeqtiuie point calibration curve, II is recommended that tho manufacturer maintain (1) e highconcentrntion calibration standard {betwer 4000 and 800n ppm) lo prepare his calibrat. curve by nn appropriate dilution technique and (2| a low-concentration calibration Therefore, the chroma Iftftraph operator shall resolution is defined <is an aren overinp nl standard (belwcen SO and S00 ppm) to veri select the column and operaI ins parameters not more than 1(1 percent of the vinyl chloride the dilution technique used. If Ihedifferenc best smtud to his particular analysis peek by an interfemnt peuk. Calculation of bvtwren the apparent concentration read requirements, subject to the approval of the area overlap is explained in Appendix C. from the calibration curve and Ihe true . Administrator. Approval is automatic f'rucedurc 1: "Determination uf Adequate concentration assigned to the low*' provided thus Ihe tester prndur.oa confirming C!irotn-itoyr;j|'hic Peak Resolution,`*1 Two concentration calibration standard exceeds data through an adequate supplemental 1.33 m columns, cuch containing l percent percent of the true concentration, (be analytics! technique, such us analysis with a Carliowiix 1500 on Curbop.uk 0. have been manufacturer shell determine the source of different column orCC/mnss spectroscopy, suggested for samples containing error and correct it, then repeat the 3-polol arid has ihe dau available for review by the acetaldehyde. calibration. * Administrator, 6.3.3 Thermometer. 0 lo 1U<V C. urnimte 7.2.1.2 Verification of Manufacturer*! I. Procinon oiul ttrprotluc.ihilily. An lo 0.1' C. Aurkin-Elmer No. 1U5-OIOD, or Calibration Standards. Boforejuino, th,e Inlcrlsborulory comparison bulwuen seven equivalent. manufacturer shuil verify eacficalibration laboratories of throe resin samples, I'nr.h u|ilil 041.4 S.iinnleTriiy Thnrmnstm Rysiom. standard by (a) comparing It togas mixtures into three purls, yielded a standard deviation Pcrkin-EbniT No. 105-0103. or cquivnbint. prepared (with (J9 molu percenfw^I of 2.03 percent for a sample with n mean of 8.3.5 Sitptri. S.indwic.lt type, for aulomntic chlnridn) in accordance with the procedure 2.09 ppm. 4.1G perennt for a sample with a dosina. 13 tnm. I'crkin-EJmer No. 105--100R, or described in Section 7,1 of Method 106 or by mean of l.Gd ppm, and 5.23 percent for * equivalent. tb) calibratins it against vinyl chloride sample with a mean of C2.GG ppm. 0.3.C Intvcculor-Rerxirdi'T. Ilnwlekt- cylinder Standard Reference Materials 5. Safely. Do nut ridcnM vinyl chloride to Pur.k.'ird Mi>dvi or rt|iiivnl<:nt, (SRM'a) prepared by the National Bureau of the laboratory ;tlutosphere during preparation 0.3.7 Filter Drier Assembly (3|. Porkin- Standards, if such SRM't are available. The of standards. Venting or purging with VCM( Etmrr No. 2230117. or eipiivalenl. agreement between the initially determined sir mixtures must hu held to a juiitimum. G.3.U Suup Film Flowmeter. Hewlett ; concentration value and the veriftcslioa When they are required, the vapor most be Packard Nu. ut(>l-On3, or equivalent. concentration value mutt b* wR___ -oj.r*'- -- ........................... ' wvy&t t AP00040031 V rgdurai i-icj2:xtr:r 39175 percent. Tbs manuf.u.turur nmtl ri-n!y ail lurution stands rc!s on a lime int< r<. ,ii i-iiTiiuno total !i: [TS], Tills :s requuud fiic crvtcul.ilimt th ?"CM. ,( "wurn s tena ln;v, errors will occur on resin r.uv.ples bciirti.sA of inaditquatc lime for head' consistent wiih llio shell life of t:i c\ uwivr .* 2J l.'h'-persiM . `'iu K lurry a:ic t I.mu > tc<* c:is oquilibriiiru. Thi* nor.nitfon can be simuiarris said. !. i:.'X Su r-.i'ifs. T'...: ..'.n'..:i ;.ib iiluviiti not hr .ivmi.irii ity rur.nina cuverai standard gas &. Procci/ure. fii'. ri'ii. Sunipli- ir.uri! ! lii,->n>u-:;\ly mixed, '...{ttj-ios at various prrssjies araund the 8.1 Sampling. lisiuy a lured viil {lured. inciniiir.-j scptuiii r. ..vtiinleu prosatire, and tliun svlucllng the 3.1.3 PVC Sampling. Allow the r<*min or mid aluiniuum ca;i| add { p;irt*xiru'>ifiv eight |-.iqh'*st prosaure that does not produce a slurry to flow from a tup or the t.-m* ',r suo ;hi.-iH (11.25 to 0.35 y) <.f slurry uf !a:i'\ using d-MiO.n irtiixtiun. All samples and standards until Mic tt'P line has been w.-ll purved. nirdicino dropper. This s.uuiul hr dur.o liiujit bo pressurised for 05 seconds using the are of "V is are rsixlure m vinyl ' 4ter _ l urvs as '3 ;rer ; Section " :nds a ' 4 Extend ami Ml a GO-ml sample botllu under iKe Up. and immediately tighten ;i v.p mi (lie boUle. Wrap adhesive tape nround tha cap and botilc to prevent the cap from lommiuut- Place an identifying label on each bottle, and record the date. lime, und sample location both on the bottles and in a.lug Injok. 8.1.2 Water SampHna. Prior to use, the 50mi viola (without the discs) must be* enuped with aluminum foil and healed in u muiflo furnace al -tOO" C for at least 1 hour to destroy or remove any organic matter tnnl cmml interfere with analysis. At thr* sampling location fill the vials bubble-free to overflowing so that a convex meniscus forms at the top. The excess vralor is displaced as the sealing disc is carefully placed, with the Teuon si-if: down, on the opening of the vial. Place the aluminum seal over the disc anti the neck of the vial, ami crimp into plana. Affix an identifying label un the botMn. and IniaiuJiiilely after r.dxini'. Sun! inn vial ui soon .is possible. Cuterniiiio sr.nii'ii; weight (0.0001 g|. After prepreasurization. condition the vial for 1 hour nt hit* C in the Analyzer bath. Determine the TS on the slurry sample (Section C-3.5). 541.4 Inproccss Wastewater Samples. Using a tared vial (tared. including septum nnd .aluminum cap) quickly add approximately 1 cc uf water using a medicine til upper. Soul the vlni as soon ns possible. Determine sornpie weight ( -- 0.01301 ts). Prnprnssurize the vial, and then condition for l tu 2 hours as required at go* C ir. tne analyzer bath. 8.3 Analysis. 8.3.i Preparation of Equipment. Install tha chromatographic culumn and condition overnight at ICO" C. In the first operation. . Pnrapok columns must be purged for 1 hour at 230" C. vial pr<:pr:uriser. The vial .s then placed into :i.u UQ' C canuiiionir.c bam and tested - fur leakage by placing a drop of water on the septum at the needle hole. A clean, burr-free needle is mandatory. ______ ... ourner <-\ir supply, set regulato^on cylinder to read 50 psitj. Set reguialor on chromatograph to supply air to burner at a . rate between 230 and 300 cc/min. Check with bubble flowmeter. '` cl. Hydrogen Supply. Set reculator on-* cylinder to read 30 paig. Set regulator on chromatograph to supply approximately 33 5 cc/min. Optimize nydrogen flow to yield the r\osl sensItivA oqtactor respnniB without rxiingmshing the name. Check flow with ` bubble meter end record this flow. **> 0.3.4.2 Tcmpnrature Adjustments, Set *. " t tcmpornlurcs as follows: * ; a. Oven [chromntogrnph column). 140* C. >:r * ; <IS* (c) .; loride :mum nt to 4 4 ition. record the date. lime, amt sample localion both on the dais and in .i log book. All samples must be kept refrigerated until uniiiyzcri. 3.2 Sample Recovery. Samples must be run wi thin 24 hours. 8.2.1 Resin Semples. The weight t.f the resin used must be between 3-5 nnd 4.5 grams. An exact weight must be oblaincd Do not connect the oxil cad of Ihc column to the detector while* conditioning, i iycro.-jon und dir to the detector must be turned off while tha column is disconnected. a.3.1.1 How Rata Adjustments. Adjust flow rates AS follows: a. Nitrogen Carrier Gas. Set regulator on cylinder to read 50 psiq. Sat regulator on chromatograph to produce a flow rate of tiO.tl b. Dosing Una, 150" C. c.'i:i|ficlton Blank. 170" C. d. Sample Chamber, Water Temperature." aa* C i.o* C. " ....... . 8.3.1.3 Ignition of Flame Ionization Detector, ignite the detector according to tho '' manufacturer's instructions. ', 3.3.3.4 Amplifier 3ular.ee. Balance the amplifier according to the manufacturer's , ; i.'en in -ach cal {*. To i n 3- iod .ih* tween 'ration %iue verify ranee ad . (0.0001 g) for each sample. In the case of suspension resins, a volumetric cup can be prepared for holding the required amount of sample. VVhen the cup is used, open the simple bottle, and add the cup volume of renin to the tared sample vial (larcti. including septum and aluminum ncp|. Obtain ilio exact sample weight, add 303rU or about two equal drops of distilled water, und immediately seal the vial. Report this value nn the data sheet: it is required for ciilculati jn of RVCM. In the case of dispersion resins, the cup cannot be used. Weigh the sample In an aluminum dish, transfer the sample to the tared vial, and accurately weigh it in the vinl. Afirr jroprcMuriz.ilion of ihp samples. condition cc/piln. Accurately measure tho flow rate nt the oxi> end of the column using tho soap film flowmeter and a stopwatch, with the oven and column at the Analysis tempurnture. After the instrument program sutunrens ic tho "S" (backflush) mode, adjust the nitrogen pressure regulator to exactly balance Ihc nitrogen flow rate at the detector as was obtained in ihe "A" mode. 1>, Vial Propmsaurizcr Nitrogen. After the nilrngen carrier is act. solve Inc loilowinq equation and adjust the pressure cr. the vial prepressurizer accordingly i ^ B !wl " Pw2 733" - 10 k ?! instructions. iiV, 8.343 ".. v.i\.i:,;a:nr the Chromatcgraph. Frugrnm t.i unru.T.ntugrapn as follows: a. I--Dus;,-.3 or Injection Time. The normal selling is 2 seconds. b. A--" Anal} ail Time." The normal setting is approximately 70 percent of the VCM retention tiino. When this timer terminates. Hiu programmer initiates backflushing of the first column. c. D--backflushing Time. The normal ' sotting is double the `'analysis time." d. W--Stabilization Time. The normal setting is 0.5 min to 1.0 min. ' e. X--Number of Analyses Per Sample. The normal selling Is one. them for a minimum oi l hour in the 90* C 8.3.3 Preparation of Sample Turntable. 'eeds 5 e of dnt on lures ure ir by bath. Do not exceed 5 hours. Note.--Roma aluminum vial caps have a center section that must be removed prior to placing into sample trey. If tha cup is not removed, the injection needle will be damaged. B.2.2 Suspension Resin Slurry and Wat C.tka Samples. Decant the water from a wet cuke sample, und turn the sarnpio ho!tin upside down onto a paper towel. Wait for the water to drain, place approximately 0.2 to 4.5 urami of ihc wnt eake sample in a Ixriid viol Where: TiAmblent temperature. "K. Tt^CondiUor.ing bath tamperiiiiira, 'K. P.sGas chromatograph absolute dosing pressure (analysis mode), k l',i. P.iaWHlervapor pressure DO' C {520.5 mm l lg). Water vapor pressure @ 22* C (19.It mm 11^). 7.S0 n mm 1 Ig per 1c Ru. 1U k PaoFactor to adjust thr prepressurized pressure to slightly less Before placing any sample into turntable, be - certain that ihe center section of the aluminum cap has been removed. AH samples and standards must be pressurized for SO seconds by using the vial prepressurizer. The numbered sample vials should be placed in the corresponding numbered positions In the turntable. Insert samples in the following (. urdnr ' Position 1 and 2--Old 2000-ppm standards far conditioning. These are necessary only after the analyzer has not been used for 24 (tared. including septum and aluminum c:np| thnn the dosing pressure. hours or longer. u of The ned (7s nnd seal immediately. Then determine the sample weight {-0.0003 g). All '.,nnp\-s must he prepressurized nnd then conditioned for 1 hour ul GO' C. A sample of wet cakq is usad to Unrvutseof gauge errors, the iipparnttis may jn-ar-pressurizn the vi.il. If Ihc vial jv*sure is .it nr highcT than the dustnq yrcssuie, an audible double injection will occur, if the vial Position 3--30-ppm standard, freshly prepared. Position 4--500-ppm standard, freshly prupured. AP00040032 V ,/n i'isiior;:: :/ Vnt, .|7. 17.T ;v. SfDUsiiin'f " IbHl! ilu!;:s ;mi Koyuittliitns n PosiUi'i." &--HLaO-iipm si.iiitluril- frijsisly preparm;. Position ft--mOO-iipm standard, tri.-sltly prepared. Position 7--Sinnp.i: No. 7 |T!tis is liir iirsl sample of lint day. La.I is given nr; 7 lo he consistent with tiu> turntable and thu inlrgrii.'nr printout.) After ati samples havr* been pcis-honr;!, insert trie second set of ni).. .V)b-. iyxio-. anu 4d0i1-?pm standards. Samples, iurlijrling jldniiftrcis. must be comhtionod in the unlh of 90` C for 1 hour {rot lo exceed S hours). 8-3.4 Start Chroiruitnsrupii I'rrymm. When all samples. including standards. have been conditioned at UO' C for I hoar, start the analysis program necordhtj! to the manufacturer's inrtruclior.s. These Instructions must be carefullv followed when starting and sloppmc a proernm to prevent dumngc to the dosing assembly. D.3.3 UHtermuirtf.cn ofi'S. Vor wot cake, slurry, resin solution, and PVC latex samples, dolerniine TS fnr each sample by nccurulely weighing approximately 3 lo 4 grams cT sample in an aluminum pan buhir* anti after placing in a draft oven it05 to 110* Cl. Sumpi- $ must tm dried lo iMnst-'.nt weight. After first weighing, return the pan to tho oven for a shori period of time, and then rewnigh to verify compirrlc dryness. The TS arc then cnlculutuu us the final sample weight divided by initial sample weight. P Calibration. Calibration 1* to tie performed each 8-hour period when the instrument is used. Each day. prior lo running samples, the column should be conditional by running two 2000-ppnt standards front the previous day. 9.1 Preparation of Standard*. Calibration standards sre prepared as follows: Piece tOOfil or about two equal drops of distilled water in the sample vial, then fill thu via] with ill# VCM/nilrouen alnndarrl. rapidly seal \he sepUirn. *ni seal vAVh lha aluminum cnp. Use a X*in. stainless slcfl line from the cylinder lo the vial. Do not use rubber or tygon tubing- The sample line from the cylinder must be purged (into a properly vented hoodl for several rulnnlus prior m filling the vials. Alter purging, reduce 11m flow rate lo 5Q0 to 1(X'*0 cc/min. I'l.-.ro rod of tubing into vial [nenrluuiomf. Position a septum on lop of the vial, pressing it against the X-in. filling tube to minimize the star of the vent opening. This is necessary to mimimjr.e mixing air with thu standard in the vial. Each vial is to be purged with standard for 90 seconds, during which time tho filling tube is gradually slid in the lop of the vinl. After the 90 seconds, the tuba is removed with the septum, simultaneously smiling the vial. Practice will be necessary tu develop guild technique. Rubber gloves should lm worn during the above otmratwns.Thi; cr;fhJ vinl must ihan be pressurised for OT) using Hie vjuLPrrpw murnierLTi-srifia viul for leakage by placing u drop of water on the septum in the nuuuic bole. 11.2 Preparation of Chromatograph Calibration Carve. fd.V. .i::r: toi-ii-ppm suini-ircl sa;ur Run ll'.u uauiuniioii :-,iiu;i1es in "M. t: ".< Kami1 in.iiiiiiir .is le.roii.r vaiui'i . -a A.. !i;r iot'-jratu.* u 'o.i ..nuriti for i*.j. ; ttiiiKiiird sa.Ti;ile, versus ti,. .V.u r.nnwr.iM'.'.rtS of mnyl ui'cvblv. ir.ie.ii stan.inrU si.rnaic. Draw u .-.iraiuht line through dm audits derived by the least squares method. Iff. Calcijia.'ars 10.1 Response Factor. If the calibration curve described in Section U-2 passes through zero, a response racier. R(, may be used to compute vinyl chloride concentrations. To compute a responds factor, divide any particular A. by the corresponding Cr *f - 7" r C q. 107-1 Where: A, *Chromatograph nroa counts of vinyl diiurifi.- for dm sample, !',,* Ambient a turn.spheric pressure, mm lfj> ` K, -. it.oiponse factar (n area counts per p*>m ,, VCM. Ti Ainluenl iuburetnry temperature. *fC. r~ ; M. Muincuitir weight u( VCM, C2.5 g/ ' .' ' llUlIl!. ' ti--l v'oliiiui! cT thu vapor phase, cm'. ' K -C.i.s const.ini. (02JC0 ctrij) (mm lig/ `*vr:, .tinlo) ( Jv .n S.un pic weight, g. K, --! Icnry's L;iw Constant for VCM in ' I'VC DO' C, 6.S2X10'`g/g/mm Hg. '"T If ihr ciilibrntinn carve doetfnot pass- ' ibrniitth r.rrn. the calibration curve must be "V,;J emplovod to calculate each sample cunccntr.iiion itniosa the error introduced by : ' using <j parlicul.tr Rf is known. . 10.2 Kitsidunl Vinyl Chloride-Monomer Clonr.cnirauon, (Cr.tl or Vinyl Chloride i -<r.p- Monnmcr Conuenlralion. Calculate Cm in * ppm ur nig/kg os follows: - 0T "f 1 AP + Kp (TS) T2 + \ ( " TS^ T2 Eq. 107-2 Results c.ilculotmi using these cqualitms represent conrunlrutinn bnjrd on the total sample. To obtain results based on dry I'VC content, divide by TS.. 11. Hcfmnans. \. B.F. Goodrich, Residual Vinyl Chloride Monomer Contnnt of Polyvinyl Chloride Resins. Latex. Wei Cake. Slurry and Water Sample*. 3.K. Goodrich Chemical Croup Standard Test Procedure No, 1l)05-i. B.F. Goodrich Technical Center. Avon Lako, Ohio. October U. 197s'. 2. Larons, A.R. The Diffusion of Vinyl Chloride in Polyvinyl Chloride. ACS-- Division of Polymer Chemistry, Polymer Preprints /5|2);197.11174. 3. herons, A.R. The Diffusion of Vinyl Chloride in Polyvinyl Chloride. ACS-- Division of Polymer Chemistry. Polymer Pn'prinls ;j[2):203, IS74. `' 4. lirrons. A.K., LD. Crider, C.f. Tonttnok. and J.M. VVhiiney. Analysis for Vinyl Chloride in PVC Powders by Head---Space TS~To!nt solids expressed as a decimal fraction. T,hllquilihrium temperature, 'K. Kw**HenrV. ' ,-,w Cu.-.r.t'n.t For VCM in Wrtle.-C:.7x:ir'g/3/m:n rig- Assu.iiir.g the followinu condition! are met. :l;i:su values can be lubstiluUd into Equation 107-2: P,*7S0 mm Hg. r V,Viul volume--sample'volume (Fisher vials are 22.0 cm* end Perkin-Eltner vials ore 21.0 cnv*). 'I . *23' C or 2110' K. T.-a0* C or oM* K. A HU -------TRsyni------ - 6.25.x 10'6(TSlf3635 J.Q x 10'7 <l-TSJ(SB3)j Gas Chromatograph!*, (ournal uf Applied Polymer Science. 7tt31t>9-am. t)73. 3. Mansfield, R.;\. Thu Kv.ilu.ilmn of I lonry's Law Constant [Kp) ami Wati*r Fiib.mci'tni'iil fn thu I'nrkin-Klnn'r Mnllifr.ict F-40 Gas Clirutiiutouraph. U.F. Gnndricli. I Avon Lake. Ohiu. February 10. ltf7lt 40 C1*K P;rt Gl is iimendcd by adding Appendix C as follows: Appendix C.--Quality Assurance Procedures Pwcthim l--Dvlrrminatton ofAdequate Chroinniu^rcpbic Peak Resolution In this method of dealing with resolution, the* uMent tu winch one chromatographic peek overlaps another is determined. f I'or convenience, consider the range of the i-lutum curve of each compound at running Trnm --2crln +-2tr. This ronga Is used in other rcsiiluilcn criteria, and It contains 95.45 percent of the area of a normal curve. If two AP00040033 t **?* , 7udR twister ' Vo!. -\7. JiO ./ppm 1?K." 1 f-.a! d by ar>: j-ep.iralf'U by ;i kn/wi; nmtiincrt. L. n-'C can determine the .Ttnjliim or il:<? area of curve that bus within the r.ino'.' nf thr 5:hcr. The extent to which the rto thm . urve ot a conlurntnop.t coinwrmnb-ovf>rl.ij>s tinivrvc of a compound that is under urnlysts is f.uind by inte?ratinR the cont:imir..'in: eurvi* over tho iimits b --2o\ to b-t-<r,. where o\ is tin* sixncord deviation of the sample curve. This calculation can bo simplified in several ways. Ovcrlfij) can be determined for turves oi ur.il area: then acuuil areas can be introduced. Desired inlcjtnilton cun be resolved inio two inienral* of slut nurmttl distribution function for which there are eonvenienl caicuintion proem ms end tables. An example would bo I'rrujram 15 in Texas instruments Program Manual STL 11)75. Texas instruments. Inc.. Dallas.Texas 75222. C1UJH8 cods sw-v>-w / i i\\ Si-pic:v.lutr 7. "!?H2 / ?miLh find Kcyuluiior.s 39177 J7-Z fj .k. i j i i fa AP00040034 REISZNER ENVIRONMENTAL A ANALYTICAL LAIS, INC. I The standards for calibration of the gas chromatograph should be prepared by injecting 40 uL of vapor into the headspace above 5 mL of carbon disulfide. A teflon lined silicone septum (Cat- No. 0-26) is recommended for sealing the vials and for preparation of standards. REAGENTS Only activated charcoal Cat. No. 0-21 (or 0-22 in vials) or equivalent should be used. Carbon disulfide (reagent or spectroscopic grade) should be as pure as possible to speed analysis time. CALIBRATION OF THE MONITOR The monitor should be calibrated before use if not purchased calibrated. Expose the device to a known concentration (10 ppm) of vinyl chloride for a given period of time (2 hr.). This can be done conveniently by placing the monitor in an aluminum or glass chamber (Cat. No. 0-25) with the calibration gas moving through the chamber at about 1 L per minute per monitor being exposed. Permeation tubes are probably the most accurate source of vinyl chloride while compressed gas standards are more convenient to use. The recommended procedures above should be used for charging the device and analyzing the charcoal. The calibration constanr can be calculated from the equation: .k " c t w i I I i i \ ** The same sampling and desorption procedures can be used for Freon-12. i ! pOST OFFICE BOX 3341 BATON ROUGE. LOUISIANA 7DB21 I - TELEPHONE 504 - 367-06*9 AP00040035 REISZNEB ENVIRONMENTAL & ANALYTICAL LASS. INC. MINIMONITOR RECOMMENDED OPERATING PROCEDURE FOR MEASURING VINYL CHLORIDE IN AIR Also Freon 12** 1. Pour* 1.35 g of activated charcoal (Cat. No. 0-21 or 0-22) into the MiniMonitor and attach the monitor to an individual as close to the breathing zone as is practical. 2. After exposure, normally 1 to 6 hr, pout the charcoal into a 7 nL glass vial.* Seal the vial with a teflon faced silicone septum (Cat. No. 0-26) and refrigerate the sample at -2G*C if it is to be stored for more than 8 hrs. ANALYSIS ; 1. Cool the sample to ~20*C (in a freezer) and add 5 mL of cold (dry ice) : carbon disulfide. The desorption apparatus (Cat. No, 0-24) in figure 1 ; is particularly convenient for this purpose because it allows the carbon disulfide to be measured at room temperature. i 2. Recap the vial immediately after adding the carbon disulfide and allow to l stand 30 minutes. 3. Shake che vials at 10 and 20 minutes after solvent addition. | r J 4. Inject 5 uL into a gas chromatograph equipped with a flame ionization detector. The column used should be chosen to separate possible interfering \ species that occur in the environment being sampled; however, a 6 ft 1/8 in. Chromcsorb 102 (Johns Mansville) or a 20 ft. 1/8 in, FFAP column are 1 commonly used. An internal standard that is not removed from solution bv the charcoal is recommended. ! 5. Calculate the concentration from the equation: j c * kw t ! I where j | ! k = constant c concentration of vinyl chloride, ppnr t " time of exposure, hr w * volume of vinyl chloride, yL @ 25eC ; j | : POST * To facilitate rapid addition and removal of charcoal a vibrator (engraver) may be touched to the badge clip or the MiniMonitor may be thumped during the process. I i OFFICE BOX 3341 . BATON ROUGE. LOUISIANA 70821 TELEPHONE 504 . 387-0675 AP00040036 ( SZKER EKVIROk'MENTAl t ANALYTICAL LABS, Mt. CERTIFICATE OF CALIBRATION The Mini-Monitor has been calibrated at least two times to assure a guaranteed maximum error of 5%. The charcoal used in calibration was PCB 20-40 mesh and was reactivated at 350* under a stream of nitrogen. To calculate the concentration of vinyl chloride use the equation: C where C * concentration w amount of gaseous pollutant in sample (y at 25C) t - tine, (hr), k constant (EESJil) MiniMonitor JJo. 641 642 647 k* 0.84 0.88 0.71 Certifying Agent Kenneth D. Reiszne' Ph.D., President 12/10/81 * The charge of PCB should be 1.35 g. POST OFFICE BOX 3341 BATON ROUGE, LOUISIANA 70821 TELEPHONE 504 * 387-0679 AP00040037 .$ZKcR EKVIHONii'EKTAL l ANALYTICAL LASS. WC. CERTIFICATE OF CALIBRATION The MiniMonitor has been calibrated at least two times to assure a guaranteed maximum error of 5%. The charcoal used in calibration was PCB 20-40 mesh and was reactivated at 350 under a stream of nitrogen. To calculate the concentration of vinyl chloride use the equation: where C a cone ent ration w amount of gaseous pollutant in sample (yi. at 25C) t * time, (hr), >m,hr k " constant vi MiniMonitor No. 622 638 639 k* 0.72 0.79 0.76 Certifying Agent Kenneth D. ReisznerPh.D., President * The charge of PCB should be 1.35 g. 10/19/81 POST OFFICE BOX 3341 BATON ROUGE. LOUISIANA 70821 . TELEPHONE 504 - 387-0679 AP00040038 =:SZ?R EKViRCKMlKTAL & ANALYTICAL LASS. :HC. CERTIFICATE OF CALIBRATION The MiniMonicor has been calibrated at least two times to assure a guaranteed maximum error of 5%. The charcoal used in calibration was PCB 20-40 mesh and was reactivated at 350 under a stream of nitrogen. To calculate the concentration of vinyl chloride use the equation: where C * concentration w = amount of gaseous pollutant in sample (y& at 25C) t = time, (hrl . k * constant v y--i -) MiniMonitor No. k* 552 546 553 0.82 0.85 0.84 i i I i 1 i Certifying Agents Kenneth D. Reiszner.jji^' Ph.D., President 7/13/81 * The charge of PCB should be 1.35 g. ' POST OFFICE SOX 3341 BATON ROUGE. LOUISIANA 70B21 TELEPHONE 504 387-0679 AP00040039 I 'EI.TAL AKlU.mCU L*.2S. f JC. CERTIFICATE OF CALIERAiION The Mip-iMcmitor has been calibrated at least tvo times to AP00040040 1 ANALYSES OF VINYL CHLORIDE MONOMER BY METHOD 107 USING THE SIGMA 2000 WITH HS 100 HEADSPACE SAMPLER SCOPE: The Sigma 2000 and HS 100 Headspace Sampler are used to analyze the vinyl chloride monomer concentration in polyvinyl chloride resins, slurries, and water samples according to Method 107 of the Federal Register, Subpart FNational Emission Standard for Vinyl Chloride, 7/30/80, pages 121:0504 121:C506. Method 107, Section 6.3.1 allows the use of a GC equivalent to the Perkin Elmer F-40, F-42, or F-45 Headspace Analyzers. PRINCIPLE: The vinyl chloride monomer, as a gas, in equilibrium with resin, slurry or water in a heated sealed vial is measured and this amount measured in the headspace is mathematically related to the amount present In the solid or 1iquid samples. APPARATUS: 1. Sigma 2000 gas chromatograph, Perkin Elmer 2. HS-100 headspace sampler, Perkin Elmer 3. Glass vials with butyl rubber septa, Perkin Elmer 4. Vial sealer, Perkin Elmer, part #105-0106 5. Stainless steel GC columns, 6' x 1/8", 3' x 1/8" bath containing 0.2X carbowax 1500 on Carbopak C. 6. Analytical balance: capable of weighing to .0001 gms. REAGENTS: 1. Hydrogen, zero grade 2. Nitrogen, zero grade 3. Air, zero grade 4. Calibration standard of 50, 500, 2000 and 4000 ppm of VCM in Nitrogen Matheson Scientific INSTRUMENT CONDITIONS: 1. Set hydrogen and air flow at rates to optimize detector sensitivity as specified in the Sigma 2000 manual. 2. Oven temperature: 70C 3. Analyses time: 6 minutes 4. Range: 1 5. Attenuation: X 8 AP00040041 6. Sample Temp.: 90C 7. Transfer Temp.: 140C 8. Thermostatting Time: 60 minutes 9. Pressurization Time: 0.5 minutes 10. Injection Time: 0.04 minutes 11. Withdrawal Time: 0.2 minutes .12 Precut Off Time: 0.00 13. Backflush on/off:: 1.00 2.00 14. Vent 1 = YES/-1 == NO: -1 PROCEDURE: 1. Prepare samples and calibration standards for analyses. a. Weigh 3.5 to 4.5 gins of resin into tared sample vial. Record exact weight to .0001 gms. b. Filter slurry samples and place 0.2 to 4 gms of the wet slurry into a tared sample vial. Determine solids on wet slurry by placing 3 to 4 grams of filtered sample in a tared aluminum weighing pan and determining initial and final weight after drying to a constant weight at 105-110DC. c. Place approximately 1 cc of water in tared sample vial and record exact weight to 0.0001 gms. d. Place 100 ul of water into each of 8 sample vials and crimp septa on tops. Purge sample line from calibration gas cylinder and place needle thru septum of sample vial. Purge vial at 500-1 OOOcc/min. for 90 seconds. By this procedure fill 2 sample vials with each of the 4 calibration gas-mixtures. 2. Load Magazine a. Position 1 and 2 should contain old 2000 ppm standards for conditioning if the instrument has not been used for 24 hours or longer. b. Position 3 - 50 ppm standard, freshly prepared. c. Position 4 - 500 ppm standard, freshly prepared. d. Position 5 - 2000 ppm standard, freshly prepared. e. Position 5 - 4000 ppm standard, freshly prepared. f. Position 7 thru 95 (as many spaces as required) should contain the samples to be analyzed. g. A second set of standards, 50, 500, 2000, and 4000 ppm should be inserted immediately following the last sample. AP00040042 3. GC and HS-100 Conditions a. Get a list of chromatographic functions. Press SECTION and ENTER Display" should read: CHROMATOGRAPHY FUNCTIONS SECTION 1 INSTR STATUS SECTION 2 ACTIVE METHOD SECTION 3 METHOD CONTROL SECTION 4 HS-100 b. List the present GC status. Press #1 and ENTER Display should read: METH #1 (Active Method) CHAN: A FID B (Channel Designation) RANGE: 1 ATTN: 8 X2 (If the cursor is positioned next to the X2 pressing or keys change the attenuation values.) ZERO: A B EQUTIME: 0.5 ACT (Status Displayed) OVEN: SET ACT Temp 1 70 (Status Displayed) Time 1 6.00 Rate 1 0 HS-100 (Status Displayed) c. List the active method. Press #2 and ENTER Display should-read: METH ^normally 1) OVEN TEMP: 70 TIME: 6.00 RATE: 0 FLOWS SET ACT ZONES SET ACT Al 0 INS A 140 140 A2 2 DET A 160 160 INJ B 140 140 AUX 1 45 RUNTIME: 6.0 ACT: (status displayed) OVEN ACT: 70.1 STATUS: (status displayed) Press ADVANCE & ENTER Should display: OVEN MAX TEMP: 150 EQUILIBRATION TIME: 0.50 CHAN: A FID RANGE 1 (won't use RUN TIMED EVENTS) AP00040043 d. List the number of the currently set up method. Press SECTION and ENTER. Press *3 and ENTER. The display should read: ENTER SET UP/V0I0 1 GENERATE/EDIT 2 DELETE 3 COPY 4 STORE SET UP 5 TRANSFER 6 PRINT 7 Press No. 1 and ENTER. Display should show: THE FOLLOWING METHODS EXIST: 1 {current method set up to run) THE SET UP METHOD IS: 1 (Must agree with method number in section 1 and 2.) ENTER METHOD NUMBER: Use if setting up a new method. e. Display conditions Set Up for HS-100 Press SECTION and ENTER. Press No. 4 and ENTr7~ Press No. 3 and ENTER. Press method no.-to Be used and ENTER. Press 1 (constant mode) and ENTER. The H-1QO conditions for the method specified should be displayed. Compare with the values listed for instrument conditions in this method (assuming only one method exists). This same procedure may be used to create new HS-100 methods. f. Actually start analyses by specifying 1st and last vial to be analyzed. Press SECTION and ENTER. Press No. 4 and ENTER. Press No. 2 and ENTER. The display should"read: FIRST VIAL LAST HS-PROGRAM # 1 START AT VIAL # 00 STATUS HS-100 {status displayed) Enter the number of the first vial to be analyzed. The cursor will move below the word LAST. Enter the no. of the last vial to be analyzed. The cursor will move below HS-PROGRAM #. Enter the number of the HS program being used. Normally will be no. 1. The cursor will move to a position below the first vial entered so that a second sequence of vial number may be entered if desired (nine sequences may be entered). Press ENTER to move the cursor to the right of START AT VIAL #. Enter the first vial In the first sequence from top of screen. The display will change to read STOP AT VIAL #. Enter the last vial which will be analyzed. When this Is entered the sample positions in the magazine of the HS-100 will shift to position the vial listed as first to be analyzed below the carousel. AP00040044 The current vial rotating past the sampling position of the carousel will automatically be displayed on the screen. The STATUS of the HS-100 will be displayed on the screen. The sequence will automatically start after entering the first and last vials to be analyzed. g. Setting up a new GC Method. If it is necessary to generate new GC conditions, a new GC method must be qenerated by pressinq SECTION and ENTER. Press No. 3 and ENTER. Press No. 2 and ENTER. Enter method num&er: Enter the number of the method you are creating. A menu will appear with -;he method number you specify. Enter the values you desire for GC control. Delete old sequence and prepare new sequence. The sequence can be preparedwhilethe samples are thermostating in HS-100. a. Get into LAS by typing BYEif the terminal says BASIC >. If the terminal reads PLEASE LOG ON when RETURN is hit, type in JK.JK and RETURN followed by PASSWORD? JK. The terminal will be InfTTe manager: Type in LAS to get into LAS which is designated by a READY*. b. Type: Cl,2 and hit RETURN. c. Type: DE,S,SEQ2 and hit RETURN. d. Type: PR,S,SEQ2 and hit RETURN. e. In response to channel #? Type in 2_ and hit RETURN. f. The program will ask for method? Type in ZERQ2. This method has been previously prepared for channel 2 and is simply an area percent method. g. In response to the next 3 questions the program asks simply hit RETURN and don't answer. h. The next input required is for SAMPLES. The appearance will be: SAMPLES SAMPLE-NAME BLT# PROC-FILE RAW-FILE &DIL-F STD-AMT SMP-AMT 1* The 1st response should be to type in the 1st sample name which should be the COND SAMPLE. Type in CONDI.Then type in 2 commas, , to bypass BTl#. Type in PROC-FILE name (ex: PI) and a comma. Type in RAW-FILE name (ex: R1) and a comma. Type in 100.00 and a comma for % DIL-F. Type in 1.00 and a comma for STD-AMT. Type in 1,00 for SMP-AMT. The last three responses for DIL-F, STD-AMT, and SMP-AMT only have to be typed in on the first line. They will automatically be copied for subsequent lines. Example of 1st line: CONDI, , PI, R1 , 100.00, 1.00, 1.00 AP00040045 Example of 2nd line: COND 2, , P2, R2, Example of 3rd line: S51, , P3, R3, etc. until all samples and standards have been entered. The names entered should be descriptive of the sample or std. A different process and raw file name must be associated with each name so that each chromatogram may be stored in different raw and process files, If the raw and process file names were the same for 2 different sample names the data from the second cnromatogram would simply over-write the first and the data from the 1st chromatogram would be lost. After the last sample name is entered, (should be the 4000 ppm std.) type /E and hit RETURN to end the sequence. It will respond with SUBSEQUENCE 2? Type in NO, hit RETURN. It will respond with DONE. Hit RETURN to get READY*. 5. Associate sequence with a channel. a. Type in CH, 2, SEQ2 and hit RETURN. b. In response to DONE, hit RETURN. The sequence is now ready to start putting all area slices from each chromatogram into the RAW files specified in the sequence to integrate the area slices into peaks and store this data in the specified process files. The contents of the process files will automatically appear on the 5880 printer as each sample is analyzed. 6. Turn on the Perkin Elmer recorder so the peaks may be observed as they elute. 7. Calculation of VCM results. a. Obtain areas of VCM peak at RT of 1.35min. on each printout for the 8 calibration standards. b. Type BA on tha 588C keyboard. c. Type RU, P2088 d. Answer questions as follows: NUMBER OF DATA PAIRS? 8 TYPE IN DATA PAIRS. (X, Y - RETURN) Enter each AREA, then the cone (ppm) ex: 42,000, 51 Do Not Enter the Cone First. Modifications (Y/N)? Type N if all data was entered correctly. OUTDVC? T2 AP00040046 DETAILS FOR CURVE TYPE? 0 Take values of A and 8 from equation 1 A = Y intercept B slope Y = A + (B*X) Type RU, HS. Program will ask for value of A determined above. Type in value for A. Program will ask for value of B determined above. Type in value for B. Program will ask for area of peak for first sample to be calculated. Type in area determined in step 6.a. Program will ask for weight of sample used. Type in value obtained in step 1, a, b, or c depending upon the type sample. Use uncorrected solids weight for slurry samples. Program will ask which type sample is being analyzed (1) slurry, (2) resin, (3) water. Type in a 1, 2, or 3. If the sample is a slurry the program will ask for the percent solids expressed as a aecimal and it will correct for solids. AP00040047