1、40603HayeHne:D 4239-00CTaHnapTHbin Meton nccnenoBahna cepbl npnaHann3e npo6 yrng n KoKca c ncnonb3oBaHneMMeTOnOB cKnraHna B BbIcOKOTeMnepatyphonTpy6uaton neun4D42390603HayeHne:D 4239-00CTaHnapTHbin MeTon nccnenoBaHna cepbl npn aHann3e npoo yrnaMKOKCac Ncnonb3oBaHneMMeTOOBcXKNraHNABBbIcoKoTeMnepatyph
2、on tpybyaton neunDaHHbin CTaHnapT nMeeT Hen3MeHHoe 0603HayeHne D 4239.HoMep,cnenylownnHenocpencTBeHHo 3a 0603HayeHneM,yka3blBaet ron nepBoHayanbHoro npNHATNA WnN,Bcnyuae N3MeHeHnn,ron nocne Hero N3MeHeHNA.HoMep B kpyrnblx cKo6Kax yka3blBaeT ronnocneAHero ono6peHn9.BepxHnn MHneKc nncnnoH(E)yKa3blBaeT
3、 Ha penaKTopckneN3MeHeHNA,BHeceHHble C MOMeHTa nocne Hero onoopeHna wnw N3naHNA.1.06nacTb npnMeHeHnA1.1.aHHble MeTonbl nccnenoBaHna oXBaTblBaoT Tpn anbtephaTNBHblenpouenypblC cnonb3oBaHneM MeTOnOBBBbIcoKoTeMnepatyphon Tpy6uaton neyn c uenbho 6bIcTporoonpeneneHna conepxaHna cepbl B npobax yrna n kokc
4、a.1.2.aHHble MeToAbl nccnenoBaHna n3noxeHbl B cnenyloweM nopanke:Pa3nenblMemoo ABKnoyalowwn npouenypbl onpeneneHna conepxaHna cepbl6-9nocpeCTBOM KWCNOTHO-OCHOBHOrO TWTPOBaHNAMemoo BBbIcoKoTeMnepaTypHbln MeToA cxKnraHnA,BKnOyalownn npouenypbl onpeneneHna conepxaHna cepbl10-13nocpenCTBOM MO OMeTpNyeck
5、oro TWTpOBaHNAMemod CBbICoKoTeMnepatypHbINMeTon cKnraHnA,BKnoyalownn npouenypbl onpeneneHna conepxkaHna cepbl14-16nocpenCTBoM nornoweHNA WHopakpacHoro n3nyueHNA1.2.1.Npn ncnonb3oBaHnn aBToMatnyeckoro o6opyAoBaHnaanaBbinonHeHna noooro N3 3TNX MeTOnoB NccnenoBaHna naHHblenpouenypbl MoryT 6bITb Knaccno
6、nunpoBaHbl KaK NHcTpyMeHtanbHbleMeTonbl.Ing onpeneneHna conepxkaHna cepbl B npobax yrna n KokcaHeKoTopble npon3BoANTenn npennaraoT o6opynoBaHne nna yronbHonnpoMblwneHHOCTN,npenycMatpnBaloweeBO3MOXKHOCTbTakoronpoBeneHna aHanv3a1.3.aHHblu cmaHdapm He noopa3yMeeaem aopecauulo sonpocoe nomexHuke6e3onacH
7、ocmu,CB93aHHbIX c e20 npuMeHeHueM.ycmaHoeneHue Haonexawux Mep no mexHuke 6e3onacHocmu uoxpaHe300po6b9,a makke onpedeneHue npumeHumocmuHopMamuBHbIX 02paHuyeHuu do Hayana npumeHeHug daHHo20cmaHdapma gengemca omeemcmeeHHocmblo nonb3oBameng.CM.nn.7.8M15.21 DaHHbin MeTon nccnegoBaHna HaxoAnTca B opncAuku
8、nn KoMMTeTa ASTM D-5 no yrnto nKokcy n ABnAeTcA npAMoN OTBeTCTBeHHOCTbIO nonKoMNCCNN D02.21 no MeTonaM AHann3a.Tekywee n3naHne 6bino ono6peHo 10 anpena 2000r.Ony6nnKoBaHo B nione 2000r.nepBOHayanbHo ony6nMKoBaHo Kak D 4239-83.npeanocne Hee n3naHne D 4239-9751Copyngh ASTM,100 Barr Harbor Drive.West C
9、onshohocken,PA 19428-2959.United States2Copyright by the American Society For Testing MaterialsNed Dec0517:27:1820014D42392.HopMaTNBHble ccbinKn2.1.CmaHdapmbl ASTM:D 346 MeToanKa oT6opa n nonroToBKn npo6 Kokca npoBeneHnnabopaTopHbix aHann30BD 1193 Cneunonkaunn no peareHTHon Bone3D 2013 MeTon noAroTo
10、BKn npo6 yrna ana npoBeneHna aHanw3a3D 2361 MeTon nccnenoBaHna conepxaHna xnopa B yrneD 3173 MeTon nccnenoBaHna npoueHTa BnaxKHocTn npn aHann3e npo6 yrnaW KOKCaD 3176 MeToAnKa nepBMyHoro aHann3a yrna n Kokca2D 3180 MeToAnKa pacueta aHann3oB yrna n Kokca no pa3HbIM MaccaM2D 4208 MeTon nccnenoBaHna o6
11、wero xnopa B yrne nocpeAcTBOM cxKnraHnaB Kncnopo Hon 60M6e/MeTO OM c ncnonb3oBaHneM 3neKTpoxnMNyeckoronaTyNKaD 4621 VHCTpyKuna no KoHTponio KayecTBa B opraHn3aunax,npoBoAwnxOT6op npo6 nnn nccnenoBaHne yrna n KoKcaD 5142 MeTonbl nccnenoBaHna npn npoBeneHnn TexHnyeckoro aHann3anpo6 yrna n Kokca nocpeA
12、CTBOM MHCTpyMeHTanbHblx npouenyp3.KpaTkoe n3noxeHne MeTonoB nccnenoBaHnA3.1.Memoo A-BbicokomeMnepamypHblu MemooC米U2aHU9,BKnoyarowuu npouedypbl onpedeneHua codepxaHuacepblnocpedcmeoM KucnomHo-OCHOBHO20 mumpoeaHuB3Be山eHHagnpo6a cxknraeTca B Tpybuaton neyn B noToke Kncnopona npwMNHNManbHon pa6ouen Temn
13、epatype 1350C.B npouecce ropeHnaBcA cepa,conepxawaaca B npobe okncngeTca o ra3006pa3HbIXoKcMAoB cepbl(AMoKcnn cepbl,SO2,n Tpnokcnn cepbl,SO3),a xnop,conepxaunnca B npo6e BbICBo6oxnaeTca B Bnne Cl2.3Tn nponyKTbl,3aTeM a6cop6npyloTca B pacTBope nepekncn Bonopona(H2O2),rneOHn pacTBopAloTCa c 06pa3oBaHn
14、em pa36aBneHHblx pacTBopoBcepHon(H2SO4)n conaHon(HCI)KNCnoT.KonnyecTBo 06onxnonyynBwnxca KNCnoT Hanpamylo 3aBNCNT OT KonNyeCTBa cepbl nxnopa,npncyTCTBylownx B nepBOHayanbHon npo6e yrna.Kak TonbKooobeMbl KaxKnon N3 npNCyTCTByHOWNX KVCnOT onpeneneHbl,CTaHOBNTCA BO3MOXKHbIM paccyNTaTb npoueHTHoe conepx
15、kaHve cepbl Bnpobe.3.1.1.aHHbIn MeTon pa3pa6oTaH c yueToM ncnonb3oBaHna aHann3atopoBcepbl cepnNhoro npon3BOACTBa,KoTopble nonKHbl 6bITb KannopoBaHblHa3TanoHHbIX BewecTBax(SMRs)ycTaHoBneHnaKo30onuNeHTOB N3BneyeHna Nnn co3naHna KanvopoBoyHON KpVBoN,OCHOBaHHON Ha nvana3oHe conepkaHna cepbl B aHanv3npye
16、MbIXnpobax yrna n Kokca.2 Exeo copHuK cmaHdapmoe ASTM,TOM 5.06.3 ExeaoHbl c6opHuK cmaHdapmoe ASTM,TOM 11.01.0Copyright by the American Society For Testing MaterialsNed Dec0517:27:1820014D4239NPVMEYAHNE 1 3neMeHTbl,N3HayanbHo npNCyTCTBylowe B yrne,HeMewaloT wccnenoBaHnio npn npoBeneHnn MeTona A(nn.3.
17、1),3a ncknioyeHneMxnopa.Pe3ynbTaTbl onKHbl 6bITb cKoppeKTnpoBaHbl c yueToM conepxaHna xnopa Bnpo6e(nn.9.1).3.2.Memoo BBbicokomeMnepamypHblu MemoocKu2aHuA,BKnoyarowuu npouedypbl onpedeneHuacodepkaHua cepblnocpedcmeoM uodoMempuyecko2o mumpoeaHua B3BeweHHaanpo6a cxknraeTca B Tpy64aton neyn npn MNHnManb
18、Hon pa6oyenTeMnepaType 1350C B noToke kncnopona o6ecneyeHnaoKncneHna cepbl.3Tn nponyKTbl,3atem a6coponpyloTca B BO HOMpacTBope,conepxawem non.Korna anokcnn cepbl oTnengeTca npnnoMo山Mpa3米MKao山eroa3a,MnKpo3 neMeHTbl nona,3Ha4 anbHOnpNCyTCTByowero B pacTBope,BOCCTaHaBnMBaoTca no nonwnaTaKnM 06pa3oM noB
19、blwaa conpoTnBneHne.CncTeMa o6HapyxkeHnAnploopa CocTONT N3 nonapl3oBaHHoro CnBoeHHoro nnatNHOBOrO3nekTpona.o6oe N3MeHeHne conpoTnBneHna pacTBopa B cocyneonpenenaeTca HemenneHHO.3aTeM TWTpaHTnonnnanponopunoHanbHo nobaBnaeTCa B cocy na npoBeneHna peakunl,noka MNKpo3neMeHTbl Mona CHOBa He OOHOBATCA B N
20、36bITKe,NconpoTNBneHve pacTBopa He noHN3NTCA o CBoero nepBoHayanbHoroypoBH9.O6beM n3pacxonoBaHHoro TNTpaHTa ncnonb3yeTcpacyeta KoHueHtpaunn cepbl B npobe.aHHbin MeTon aBngeTca3MnnpnyecKNM,n no3ToMy annapaT nonkeH 6blTb Kann6poBaH cncnonb3oBaHneM 3TanoHHoro BewecTBa(SRM).3.2.1.DaHHbin Meton pa3pa6oTa
21、H ncnonb3oBaHna c cepMMHbIMNaHann3atopaMn cepbl,o6opyoBaHHbIMn aBToMaTnyeckoroBbinonHeHna npenwecTBylowen onepaunn,n nonxKeH 6bITbKannopoBaH Ha CooTBeTCTBylowen npo6e(nn.5.4),OCHOBaHHon Hanvana3oHe npoueHTHorO conepxkaHna cepbl B Kaxknon aHanv3npyeMoNnpobe yrng wnn kokca.nPMMEYAHME 2 ng npoBeneHnanp
22、ouenyp TMTpoBaHnaMOXKHOwcnonb3oBaTb HeaBToMaTnyeckoe obopy oBaHne,npn 3TOM pacyeTbl BbinonHAIOTCABpyuHylo KBannonunpoBaHHbIM nepcoHanom na6opatopnn.Pe3ynbTnpylowanoTepa B TOYHOCTN NnM CKOpOCTM,WnN N To N apyroe,MOryT CBeCTN Ha HeTnpeNMywecTBa ncnonb3oBaHna nonHOCTblO aBToMaTnyeckoro WHCTpyMeHTanbHor
23、ononxona.3.3.MemooCBbIcokomeMnepamypHblu MemooC米U2aHU9,6knoyarowuu npouedypbl onpedeneHua codepxaHua cepbl nonoanoweHulo UHobpakpacHo2o u3nyyeHua npo6a cxnraeTca BTpy6yaton neun B noToke Kncnopona npn MNHnManbhon pa6oyenTeMnepaType 1350C c uenbho okncneHna cepbl.Bnara n TBepableHacTNUbl ynangoTCA N3
24、 ra3a noBywkaMn(ynoBnTengMn),HanonHeHHbIMn 6e3BO HbIM nepxnopaTHblM MarHneM.noTOK ra3anpoXoNT yepe3 3neMeHT,B KOTOPOM eTeKTopoM nornoweHNAMHopakpacHoro n3nyueHna(K)3aMepseTca conepxaHne nnokcnnacepbl.Anokcn cepbl nornowaeT VoK 3Heprnlo c TouHon AnMHoNBonHbl B npenenax oK cnekTpa.3Heprna nornowaeTca no MepenpoxoxneHna ra3a uepe3 kopnyc 3nemeHTa,rne nepenaeTca MoK4Copyright by the American Society For Testing MaterialsNed Dec0517:27:182001