1、TOCyAPCTBEHHbIN CTAHIAPT PECIIYBJINKH KA3AXCTAHPOMbIIEHHOCTb HETAHAA H TA3OBAAMeTon onpenenemna conepxkaHna coexHHeHni cepbl H nerKHxyreBonopooB B npHpoHoM ra3e H ra30BOM TONJHBe c NOMOIbIO ra3oBoixpomaTorpaoHH H aTOMHO-3MHCCHOHHOrO eTeKropaCT PK ACTM I 6968-2011ASTM D6968-03(2009)Standard Test Meth
2、od for Simultaneous Measurement of SulfurCompounds and Minor Hydrocarbons in Natural Gas and Gaseous Fuels by GasChromatography and Atomic Emission Detection(IDT)M3 aHHe o中HIHaJIbHoeHaHHbli rocylapcTBeHHbli cTaHnapT Ka3MHCT OCHOBaH Ha ASTM D 6968-03(2009)Standard Test Method for Simultaneous Measure
3、ment of Sulfur Compounds and MinorHydrocarbons in Natural Gas and Gaseous Fuels by Gas Chromatography and Atomic EmissionDetection,aBTopckoe npaBo npHHamexnr ACTM MHrepHemHe,100 Bapp Xap6op IpaiB,BecT KoHekmeH,IIITaT IIHHceJbBaHHs,19428,CIIIA.IIepen3aeTca c pa3pemeHneM ACTMMHTepHemHen.KoMHTeT TexHnY
4、ecKoro perynHpoBaHHa H MeTpoJorHHMHHHCTepcTBa HHIyCTPHH H HOBLIX TexHOJOrH Pecny6JIHKH Ka3axcTaH(ToccraHaapr)AcTanaCT PK ACTMI 6968-2011TOCYIAPCTBEHHIM CTAHIAPT PECIHyBJIHKH KA3AXCTAHIPOMLIIIIEHHOCTL HETHA H A3OBAMeron onpeneneHua conepaHun coeHHeHui cepLI n nerkuxyreBoIopoIoB B upHpoIHoM ra3e H ra3
5、0BOM ToHIHBe c HomoI(Lio ra30BoXpoMaTorpaHH H aToMH0-3MHCCHOHHoro eTeKTopaIaTa BBeeH 2012-07-011 O6acTL pHMeHeHHAHacrogmni cTaHnapT ycTaHaBIHBaer Meron onpeneneHn conepaHn coeuHeHnMcepLI H HerKHX yrHeBOOpOIOB B HPHPOHoM ra3e H ra30BOM TOIHBe or 0,04 Mr/M3(20HHKorpaMM)o 200 Mr/M3(100 000 HHKorpaMM)B
6、0,25 cM3 o6pa3ua c noMOmBIo ra3oBoMxpoMaTorpaun(GC)n aTOMHO-3MHCCHOHHoro nereKTopa(AED).YrIeBOnOpO BKHOaOTOTeJIbHbIe aJIHQaTHueckHe KOMIOHeHTLI OT C4 0 C6.IIPIMEIAHHE ApoMarneckne KoMnoHeHT H rpyn yrneBonoponoB,KnaccH中Hupyerca BCOOTBeTCTBHH C HOMepoM yrnepona no C12,TaKHX,KaK C6-C7,C7-C8,C8-C9 H C9-
7、C10,H T.I.Hacromni cTaHnapT HPHMeHHM K GC-AED c HCHOL3OBaHHeM CHeHHaILHLIXKaJIHIX KOJIOHOK.IPHMEIAHIE B 3ToM aHaH3e MoryT 6bTL HCHOL3OBaHLI aILTepHaTHBHLMe GC KOJOHKH H napaMeTpLIupHopa,onTHMH3HpoBaHHble I pa3HHX THIoB ra3oo6pa3Horo TomIMBa,HpH ycHOBHH,TTO byneTOCTHHyTO cooTBeTCTByomee pa3eeHne coeI
8、uHeH.Hacromn Mero ncmrraHn He upeHa3HaeH HeHTHKaunn BCex BHIOB cepLL.Heu3BecTHbIe coeHHeHn cepI H3MepgIoTc KaK MoHo-cepoconepxamne coeuHeH.O6meecoepaHne cepLI B o6pa3ue MoeT 6LITL onpeeneHo nyTeM CyMMHpOBaHn conepaHn cepLIBcex BHIOB.IIPHMEIAHME Hacromul Meron He aBngerca noxpO6HLIM aHanM3oM yraeBono
9、ponoB(DHA)H HeBbIXBJIeT Bce BIbI yrIeBonoponoB.KoMnoHeHTI aIMOaTqeckux yrIeBonopoIOB,KoTopble ere,qeM H-TeKcaH,6eH3on,Tonyon,3THn6eH3on,p-KcHnOL n o-KcHoLI(BTEX),onpenenIoTcH oTneLHO.3HaeHMX OIKHLI BLIpaKaTLC B eMHMuaX BenHHH MeXyHapOHO CHcTeMLIeIMHI.B HacTomeM cTaHIapTe He npeycMorpeHo paccMoTpeHHe
10、 Bcex BonpocoB o6ecHeeH6e3onacHoCTH.loL3OBaTeL cTaHapTa Hecer OTBeTCTBeHHOCTL 3a yCTaHOBIeHHecoorBeTcTByIomHX HpaBHn TexHHKn 6e3onacHoCTH H oxpaHLI Tpyna,a Takke onpeIeneHHeupHroHOCTH HOpMaTHBHLIX orpaHneH no pHMeHeH HacTomero cTaHIapTa.2 HopMaTHBHLIe CCLIJIKHIn upHMeHeHH HacTomero craHnapTa He6XOHM
11、 cneyIomn cCLLIOHLIHOPMaTHBHbM OKyMeHT:CT PK 1.9-2007 ocynapcTBeHHa cHcTeMa TexHnuecKoro perynmpoBaHna PecHy6nKnKa3axcTaH.lopanoK npHMeHeHA MexnyHapOHLIX,perHOHaTLHLIX H HaIMOHaILHLIXcTaHapToB HHOCTpaHHLIx rocyapcTB,pyTHX HOpMaTHBHLIX IOKyMeHToB Ho cTaHIapTH3aHHH3aHne oHHaILHoeCT PK ACTM I 6968-2011
12、B Pecny6nnke Ka3axcTaH.ASTM D1265-05*Standard Practice for Sampling Liquefied Petroleum(LP)Gases(Manual Method)(TexHonorHn o6pa3uoB ra3a xnkoro TOIIHBa(KT),PyuHoi MeTon).ASTM D1945-03(2010)*Standard Test Method for Analysis of Natural Gas by GasChromatography(Meron HcnbrraHni a aHann3a mpupomHoro ra
13、3a npn noMomn ra3oBoixpomarorpaiH).ASTM D1946-90(2006)*Standard Practice for Analysis of Reformed Gas by GasChromatography(TexHonorun w aHann3a Heore3aBonckoro ra3a npn nomomn ra3oBoMxpoMarorpaHH).ASTM D3609-00(2010)*Standard Practice for Calibration Techniques Using PermeationTubes(TexHOnOrHH KaHop
14、oBKH C HCIOJb3OBaHHeM KanuIapHbIX TpyooK).ASTM D4626-95(2010)*Standard Practice for Calculation of Gas ChromatographicResponse Factors(TexHonorHH noncyera KogoHIHeHTa yyBCTBHTenbHoCTH ra3oBoxpoMarorpa中HH).ASTM D5287-08*Standard Practice for Automatic Sampling of Gaseous Fuels(TexHoJOrHH I aBToMaTHye
15、cknx npo6 ra3006pa3Horo TOIIHBa).ASTM D5504-08*Standard Test Method for Determination of Sulfur Compounds inNatural Gas and Gaseous Fuels by Gas Chromatography and Chemiluminescence(MerouHcnbrTaHni a onpeneneHna coemHeHnn cepbr B npnpo HoM ra3e H ra3006pa3HOM TonHBenpH nOMOIIH XpoMaTorpaoHH H XeMHJF
16、OMHHecLeHIHH).ASTM D5623-94(2009)*Standard Test Method for Sulfur Compounds in LightPetroleum Liquids by Gas Chromatography and Sulfur Selective Detection(Meron ncmbrramnionpeneneHna coeHHeHni cepbI B KIKOM neTponeHoM 9oHpe npn noMonn ra30BOMxpomaTorpaoHH H onpereneHna BbroopKH cepbl).ASTM D6228-10*
17、Standard Test Method for Determination of Sulfur Compounds inNatural Gas and Gaseous Fuels by Gas Chromatography and Flame Photometric Detection(Meron HcmbrraHni a onpeneneHna coemHeHnn cepbI B npHpomHom ra3e H ra3006pa3HOMTONHBe npH noMOIIH xpomaTorpaoHn H IaMeHHo-ooToMerpHyeckoro ereKTHpoBaHHa).AS
18、TM E840-95(2005)*Standard Practice for Using Flame Photometric Detectors in GasChromatography(TexHOJOrHH II&HCnOJb30BaHHa maMeHHo-OToMeTpnqecKHx eTekTopoB Bra3oBo xpomarorpaonn).ISO 19739:2004*Natural gas-Determination of sulfur compounds using gaschromatography(TIpupombri ra3-onpenenemne coeHemni c
19、epbI npn nomomn ra3oBonxpoMaTorpaHH),GPA 2199*OnpeeneHne cnemnonuecknx coeHeHni cepbl.IIPHMEYAHHE TIpH nom3oBaHHH HacToAIHM cTaHnapToM uenecooopa3Ho npoBepHTb eHcTBHeCCbLOqHbIX cTaHHapToB no exeroHo H3HaBaeMoMy HHoopMaLHOHHoMy yka3aTeo no COcTOHHIO Ha Tekym ron H cooTBeTcTByIOmHM exkemecsHo H3HaBaeM
20、bIMHHopMaIHOHHbIM yKa3aTeM,onyOJHKOBaHHbIM B Tekymem roy.ECJH CCbIOYHbI OKyMeHT 3ameHeH(H3MCHeH),TO IIPH IIOJb30BaHHH HacTOHIHM CTaHnapToM cJeayer pyKoBOHCTBOBaTbCa 3aMeHeHHbIM(H3MCHeHHbIM)HoKyMeHTOM.ECJIH CCbLIO EbI oKyMeHT OTMeHeH 6e3 3aMeHbI,TO nOJOeHHe,B KOTOpOM AaHaCCbIIKa Ha Hero,npHMeHseTC&B
21、yacTH,He 3aTparHBaromeH 9Ty CCLLIKy.IIpHMeHseTC B COOTBeTCTBHH C CT PK 1.92CT PKACTMI6968-20113 TepMHHLI,onpeneeHH H 0603HaeHHA3.1 CokpameH:3.1.1 06mee coKpameHne yreBonOpOHLIX coeMHeH cHO3yerc Io6o3HaeH Hcna aToMoB yrnepoa B coeHeHn.IlpeHKc HcHoL3yeTc I o603HaeHHpopMLI yrnepoHo uenn,re HnHn HHec o6
22、o3Haaer qncno aToMoB yrnepona(HanpHMep,o6LH 6yraH=n-C4,H3oneHTaH=i-Cs,annparneckne yrneBonopon,KoTopble Takenee,yem n-reIITaH,HO He Taxenee yem n-oKTaH=C7-C8).3.1.2 CoeHHeHn cepH 06LH 0603HaaoTC HaaLHLIMH 6yKBaMH(XHMHeCKHMHIM opMynaMn,HanpuMep,MerHIMepKarraH=MeSH,nMerHncym=DMS;Kap6oHHLHL cymH=COS,Tp
23、er6yTHn TpHcyH=DTB-TS rerparHpoTHoaH=THT H THOaH).4 KpaTkoe coepanne MeToa HcuLITaHni4.1 Or6op n aHam3 mpo6 ra3oo6pa3HLIx coeHeHi cep BeTc cHoXHo 3anaeiB CBA3H c peaKHOHHO cHOCO6HOCTL 3THX coeHHeHn.O6pa3u co6paoTc H XpaHTC BKoHTeiHepax,KoTopLie He pearnpyoT Ha cepHncTLle coeAMHeHM(HanpuMep,KOHTeHepL
24、 H3HepKaBeome crann c ToHKo KpeMHe3eMHo noKnanKo n TeapHMe KOHTeHepI cnOnponMneHoBo apMaTypo HH HM nOnO6HIe).I o6ecHeeHHA TOTHOCTH O6pa3HOBKOHTeHepI c o6pa3uaMH OKHLI 6ITL 3anOnHeHL H oeHI He MeHee Tpex pa3.Io6ecneeHH HaeHLIX pe3yLTaTOB a6opaTopHoe 6opyIOBaHHe OHO OLITL HHePTHLIM.Ip6I OHLI LITL HCII
25、TaHLI nO CTe4eH cpoKa XpaHeH.4.2 0,25 cM o6pa3ua ra3oo6pa3Horo TonIMBa BBOMTC B ra3oB xpomaTorpad,reo6pasen mpoxonMT epe3 30 MerpoByIO KoNoHKy HaMerpoM 0,32 MM.MoKeT 6LTLHCHOL3oBaHa KOoHKa c 6onee IHpOKHM IHaMerpoM 0,53 MM,I 6onee ToqHoro pa3neIeHn/HapyeH HHx peneoB.4.3 ATOMHO-3MHCCHOHHIe eTeKTopLI.
26、Bce coeHHeHH cepLI H yrepoOB MoryT 6ITL6HapyKeHLI aHHLIM MeTOOM.GC-AED 6 pa3pa6oTaH HeaBHO I aHaIH3a 6LIMHCTBa3eMeHTOB,B TOM HCe cepL H yrnepoIa.AED HcHOL3yeT CBI HHnyuMpoBaHHyIo renHeByIoIa3My I OTeneHn MOneKyn H aTOMHLIX/BO36yXICHHLIX 3neMeHTOB PH BLICOKOTeMeparype 5000 C.XapaKTepHLe JHHHH H3y4eHM
27、A OT KOHKPeTHIX aTOMOB06HapyKHBaIoTC OTOIHOIHLIM JIyeBLIM eTeKTopOM(PDA).BL6pOCH cepI H3MepIoTCapH 181 HM.BLI6pocLI yrepoa H3MepHoTC B IHana3oHe oT 193 HM o 179 HM.KONMecTBOH3nyaemoro cBeTa Ha KaKno IHe BOHLI nponopHOHaILHO KOHeHTpa cepLI HIMyrnepoa.B6pocH yrnepona H Bonopoa TaKke MOXHO H3MepHTL pH
28、498 HM H 486 HM,coorBeTCTBeHHO.HX BOnOpOHorO H3MepeH ONKeH 6LITL HOCTpOCH KBapaTHHLrpayHpoBaHHL rpaHK.GC-AED upearaer oeHL BLICOKyIO cTeneHL H36paTeLHOCHocO6HOCTH n poKn InHaMecKn Iana3oH I O6HapyeHn pa3IHHLIX THIOBcoeuHeHa.PyKoBOIcTBo no HpHMeHeHHIo AED,KaK n XeMHIOMHHeCueHTHoro leTeKTopaCepLI(BCC)
29、pHBeeHO B ASTM D5504.4.4 Ipyrue neTeKTopLI.IaHHMe MeToI HcHITaH HCHOL3yIOTC,npene Bcero,IaTOMHO-3MHCCHOHHOro neTeKTopa.MeTo GC MOKeT 6LITL HCHOL3OBaH c pyTHMHeTeKTopaMH,KOTopbIe HMeOT lOcTaTO4HyO yBCTBHTeJIbHOCTL H peaKIMO Ha BCeKOMHOHeHTLI cepL H yreBOnOpOI B TPe6yeMOM IHana3oHe H3MepeHni.CoBMeCTHOeHCHOIL3oBaHHe IeTeKTopoB FID-SCD cOoTBeTCTByIOT IaHHIM KPHTepHAM.3
