1、EAEPAJbHOE ATEHTCTBOnO TEXHYECKOMY PEryJPOBAHIO METPOOrHAOHAJbHbIFOCT PCTAHAAPTPOCCMCKON57804-中EAEPAU2017PACTBOPTEJM OPTAHYECKMETAOEHCOEPKAWE X CMECMeTog onpegeneHng pacTBOpMOct ranoreH-MOHOBM3AaHne onunanbHoeMocKBaGnCTaHAapTHHPoPM2017FOCT P 57804-2017HAUMOHAbHbI CTAHAAPT POCCCKO EAEPAUPACTBOPTEJM O
2、PTAHYECKE TAJOEHCOAEPKALLME IX CMECMMeTog onpegeneHnA pacTBopMocTn ranoreH-MOHOBHalogenated organic solvents and their admixtures.Test method for halide-ions water-solubilityAaTa BBeAeH-2018-06-011 06nactb npMeHeHHacTou cTaHgapt ycTaHaBnnBaet MeToAbi onpegeneHng pacTBopnMoctn ranoreH-nOHOB.1.1 MeToA
3、bi 1,2 n 3-HacToune MeTogbi pacnpocTpaHoTcA Ha onpegeneHne n3BneKaeMbIX BogoiranoreH-noHoB B ranoreHcogepxawnx opraHn4ecknx pacTBopnTenAx n ux cMecAx.MeToAbi He pacnpocTpa-HoTc Ha onpeAeneHne TopnA-oH n3-3a pacTBopMocT TopAa cepe6pa.1.2 MeToA 4-gaHHbi MeToA pacnpocTpaHgeTcA Ha onpegeneHne xnopnA-noH
4、oB B ranoreHcoepxa-Lx opraHn4ecknx pacTBopnTenAx n x cMecAx.1.3 3Ha4eHnA,3anncaHHbie B eAnHnyax cncTeMbi CN,cunTaKoT cTaHAapTHbiMn.HnKakne Apyrne egn-HLbI 3MepeH He BKn4eHbI B CTaHAapT.1.4 B HacToAueM cTaHgapte He npeAycMoTpeHO paccMoTpeHMe Bcex BonpocoB 6e3onacHOCT,cBA-3aHHbIX c cnonb30BaHeM gaHHbi
5、X MeTogoB cnbiTaH.onb3oBaTen HacTowero cTaHAapTa HeceT oT-BeTCTBeHHOCTb 3a co6niogeHe npaBnn 6e3onacHOCTH n oxpaHbi 3AopoBba(nepcoHana),a Takke onpegena-eT Lenecoo6pa3HOcTb npMeHeHnA 3aKoHogaTeNbHbix orpaHn4eH nepeg ero cnonb3oBaHeM.2 CyuHOCTb MeToAOB2.1 MeTobi1,2 n 3anoreH-noHbi,npncyTcTByoune B ra
6、noreHcogepxanx opraHnecknx pacTBopnTenx,n3BnekaioT Bo-go n ocaxqaoT B Bnge ranoreHnga cepe6pa,conn c HnTpaTom cepe6pa.KonnuecTBo npncyTcTByounx ra-noreHoB onpegengioT nyTem cpaBHeHnA MyTHOCTn oOpa3ya c 3BeCTHbIM CTaHAapToM.B ACTnnpoBaHHOMBoge,a takke Bo Bcen ncnonb3yemon cTeknHHon nocyge He gonxHbi
7、npncyTCTBoBatb ranoreHnAbi.2.2 MeToA 4AaHHbi MeToA ocHoBaH ha onpegeneHn nOHn3npyeMbIx xnopnAoB TuTpoBaHnem ayeTaTa pTyTn,nc-nonb3y s-AneHnKapoa30H B KaecTBe HAnKaTopa.3 Ha3HaeHne n npnMeHeHne3.1 AaHhble MeToAbi cnbiTaHn ncnonb3yioTc An o6ecneyeHn npon3BoAcTBa n tpe6oBaHn k no-cTaBngeMon npogykyn.T
8、MeToAbi ncnonb3yioT An onpegeneHnA TpeboBaHnn K pacTBopnTenio npn eroCnonb3BaHN.BbicoKM ypoBeHb pacTBOpnMbIX B Boge xnopnAoB MOxeT yKa3biBatb Ha ha4ano pa3noe-H pacTBopTeng.4 Annaparypa n nocyga4.1 AenTenbHa BopoHKa BMeCTMOCTbO 500 CM3.4.2 Tpy6kn Heccnepa BMeCTMOCTbO 50 CM3.M3AaHne opnunanbHoe10CTP5
9、7804-20174.3 Kon6a 3pneHMenepa,BMeCTMMOCTbIO 125 CM3.4.4 KonopnMeTp nnn Typ6nAnMeTp,Ana MeTona 2.5 PeaKTNBbI5.1 CTeneHb YMCTOTbI peaKTMBOBnpn npoBeneHnn ncnblTaHnn cnenyeT ncnonb3oBaTb peaKTnBbl cTeneHn X.4.Ecnn He yKa3aHo NHoe,npennonaraeTCA,4TO Bce peaKTnBbl AOKHbI COOTBeTCTBOBaTb TeXHNyeCKNM yCno
10、BMAM KoMNTeTa aHanNTn-yecknx peaKTnBOB AMepnkaHckoro XNMNyeckoro ooweCTBa.MHa cTeneHb 4MCTOTbI MOXKeT 6bITb Mcnonb30-BaHa npn ycnoBnn,ecnn ycTaHoBneHo,4To peakTNB oonanaeT OCTaTOYHO BbICOKON cTeneHbIO YWCTOTbI npMero ncnonb3oBaHnn 6e3 yMeHbweHNa TOYHOCTN onpeneneHnA.5.2 OunweHHag Bona.Ecnn He yka3aH
11、o NHoe,cnenyeT ncnonb30BaTb AncTwnnnpoBaHHylo BOAy,Heconepkawyio ranoreHnnbl.5.3 CTaHAapTHbin pacTBop xnopnn-MoHa(1 CM3=0,0001 r CI ana MeTOnoB 1,2 w 3.CMewMBaIOT0,165 r xnopnna Hatpna c 1 n AcTnnnnpoBaHHon BOAbl,He conepxkawen ranoreHnAbl.5.4 CTaHAapTHbin pacTBop xnopna-MoHa(1 CM3 0,0000001 r Cl)an
12、a MeTona 4.PacTBopAIoT 0,0660rxnopnna Hatpna B ANCTwnnMpoBaHHoN Bone M OBODAT o 1 n.aHHbIN pacTBop nmneTkon nepeHOCAT B kon-6y BMeCTMMOCTbIO 1000 CM3,AOBOAAT Ao MeTKM BooM M nepemewnBaloT.5.5 KoHueHTpnpoBaHHa a30THa KncnoTa.5.6 PacTBop HMTpaTa cepe6pa,MonapHon KOHueHTpaunn 0,1 Monb/AM3.nonroTaBnMBar
13、oT pacTBopHNTpaTa cepeopa MonapHON KOHueHTpauln 0,1 Monb/AM,nobaBnAa 16,99 r HMTpaTa cepeopa B MepHyiokonby BMeCTNMOCTbIO 1 n OBOAAT o MeTkn ANcTNnnMpoBaHHoN BonoN,He conepxkawen ranoreHnAbl.nnonHoro pacTBopeHna HWTpata cepeopa BCTpaxnBalOT Konby,nocne yero nepeHOCAT pacTBop B CKnAHKy N3TeMHorO CTek
14、na M xpaHAT B HeN.5.7 PacTBop aueTaTa pryTn,nna Merona 4.5.7.1 MaTouHbii pacTBop aueTaTa pTyTn.PacTBopaoT 1,6 r ayeTaTa pTyTn B 500 CM3 BOAbl,conepxka-wen 3,5 CM3 a30THON KMCnOTbl.DOBOAAT AO 1000 CM3 n nepemewMBalOT.5.7.2 CTaHAapTHbin pacTBop aueraTa pTyTn.Pa36aBnAIOT 40 CM3 MaToYHoro pacTBopa ayeTa
15、Ta pTyTnAO 1000 CM3 n a30THoN KMcnoTon AOBOAAT pH Ao 1,6.CTaHAapTn3MpyIoT no 7.5.5.5.7.3 PacTBop s-AnoeHunkap6a30Ha(nna MeTona 4).PacTBopAIOT 0,5 r s-AnoeHnnkap6a3oHa B100 CM MeTaHona.6 Tpe6oBaHna 6e3onacHocTn6.1 Tpe6oBaHMa 6e3onacHocTn npn pabore c pacTBopnTenem.CnenyeT n36eraTb KOHTakTa pacTBo-pnT
16、enen c KoKen.ECTb pa3nMyHble CTeneHn onacHOCTn BAblxaHnA,npornaTblBaHna KOHTakta c pac-TBopnTeneM.nonb3oBaTenio cnenyeT pyKoBOACTBOBaTbC HoBeNwnMn MeAnKo-caHnTapHbIMn npaBnnaMn,KacaHOwNMNCA WHANBNnyanbHoro pacTBopntena.6.2 KoHueHTpnpoBaHHa a30THa KncnoTa oueHb onacHa npn KOHTaKTe C KoKen nnn rna3aMn
17、.napbloueHb TOKCNYHbI N npMBOAT K Koppo3MN.6.3 Cneayer HaneBaTb 3awnTHble oukn w pe3nHOBble nepuaTkn npn o6paweHnn C HNTpaToM cepe6paM ero pacTBopaMn.6.4 AueTaT pTyTn TOKCM4eH.6.5 Tpe6oBaHna 6e3onacHocTn npn paboTe c s-AndeHnnkap6a30HOM OTCyTCTByIOT.7 npoBeneHne aHann3a7.1 MeTon 17.1.1 nepeHOCAT 100
18、 CM3 06pa3ua B nenMTenbHyo BopoHky M Ao6aBnAIoT Takon xe o6beM AMCTunnM-poBaHHoN BOAbl,He conepkawen ranoreHnAbl.TwatenbHo BCTpAXNBaIOT B TeyeHMe 2 MWHyT nA N3BneyeHNABonopaCTBopNMbix ranoreHnnOB(CM.npnMeyaHne 1).7.1.2 no3BONAIOT KMAKOCTM OTAenMTbCa OT cnoa pacTBopnTena.nepeHOCAT 50 CM3 n3BneyeHHON
19、BOAblB Tpyoky Heccnepa BMeCTNMOCTbIO 50 CMM no6aBnAlOT neCATb Kanenb KOHueHTpnpoBaHHon a30THON KMcno-TbI.nonroTaBnnBaloT CTaHnapTHbin pacTBop xnopnn-MOHOB B Tpyoky Heccnepa,nobaBnAa o6beM CTaHnapT-2FOCT P 57804-2017Horo pactBopa xnopnA-noHoB,cm3,paBHbiM nnotHOctn pacTBopnTen,n gengt ha 2 4act c Konn
20、4ecTBoMppm,3KBnBaneHTHbIM Tpe6yeMbIM XnopnA-noHaM(CM.npnMe4aHne 2).Pa36aBnAoT KaKqLM cTaHAapT Auc-tunnpoBaHHo Bogo,He cogepxawe ranoreHngoB,go o6bema 50 cm3 n go6aBnioT gecAtb Kanent KoH-yeHTPPOBaHHO a3oTHo KncnoTbi.Ao6aBnHOT 1 CM3 pacTBopa HnTpaTa cepe6pa MongpHO KOHyeHTpaynn0,1 monb/AM3 B Kaxqb 06
21、pa3ey n cTaHAapt,n TaTenbHO BcTpAxnBaHoT Tpy6Kn Heccnepa B Te4eHne 30 ceK.CpaBHnBaoT o6pa3ey co cTaHAapTamn An onpegeneHn ypoBHA xnopnAoB(CM.npnMe4aHne 3).门p nMe 4 a H ne 1-BpeM 3Bne4eHn gonHo 6bItb nocTOAHHbIM.MeAneHHo rnAponn3yeMble opraHnyecknecoeAnHeHnA,Takne Kak pocreH n TpuxnopayetnnxnopnA,Tpe
22、6ykoT npMepHo 2 MH,4To6b npopearupoBatb nonHOcTbHO.4pe3MepHoe BpeMA 3Bne4eHnA MoKeT cnoco6cTBoBatb ranoreHcogepxaMM opraH4ecKnM pacTBoptenAM ruAponn-30BaTb ce6.门p nme4 a H ue 2-Hanpnmep,ecnn npoBognnncb n3MepeHA TpnxnopatneHa,to 1,46/2 nnn 0,73 cM3 cTaH-Aapthoro pactBopa xnopnAa 6bino 6bi Heo6xoAMo
23、Ang kaxgoro Konn4ecTBa ppm,3KBBaneHTHoro xenaeMbiM xnopnA-MoHaM.An 2 ppm,cneAyer go6aBtb 0,73 2=1,5 cM3.TaK KaK BogopacTBopnMble ranoreHnAbi,Kak npaBnno,MeHeeHeM 1 ppm,peAko 6yAet Heo6xoguMo nogroToBTb Gonee oAHoro unu AByx cTaHAapToB.p n Me 4 a H ne 3CTaHAaptbi n o6pa3ybi cneAyer npnroTaBnnBatb oAH
24、OBPeMeHHo.AnA toro,4to6bi cBectK MMHMMyMy BnMAHMe Bo3Ayxa 3MeHeHMe MyTHOCT xnopAa cepe6pa,o6pa3ubI ocTaBngoT B TeMHOTe B TeeHe15 MMH.3To oco6eHHo BaxHo npn onpegeneHnn Hn3koro cogepxaHnA xnopnAoB(MeHee 1 ppm).XpaHeHe B TeMHOTenpeAoTBpaaeT 3MeHeHne KOHLeHTpaLN HTpaTa cepeopa.7.2 MeToA 1ATO4HOCTb MeTo
25、ga 1 MokeT 6bItb yny4weHa AnA 06pa3yoB c cogepxaHem xnopAoB MeHee 2 ppmnyTem yBenn4eHA cooTHoweHnA pactBoptenb-BoAa c 1:1 go 4:1.7.3MeToA2OnpegengioT MyTHOCTb cTaHAapToB no 7.1 n 7.2 c nCnonb3oBaHneM KonopnMeTpa unn TyponAnMeTpa.CTpoT rpauK An onpegeneH ypoBHA cogepxaH xnopAoB B o6pa3yax.7.4MeToA3M3
26、BneKaioT o6pa3ey no 7.1.AHanM3npyioT 3Bne4eHHyio Bogy c noMOubio nOHHoTo xpomaTorpacpa,koTopLin oTKanopoBaH An cTaHAapta B cooTBeTcTByouwnx qnana3oHax.AaHHbiM MeToA qaet BbicoKy1o TO4-HOCTb pe3ynbTaToB onpegeneH MyTHOCT.7.5MeToA47.5.1 lpoMbiBaoT Bco cTeknAHHyio nocygy AnctunnnpoBaHHon Bogon,He cogep
27、xawe ranoreHnAbi,go tex nop,noka 10 Cm3 nPoMbIBHOi BoAbi he 6yAet noka3biBatb HnKaKnx cegoB MyTHoCtn npu go6aBneHnn1 cM3 pacTBopa HTpaTa cepe6pa.7.5.2 lepeHOcAT 100 cM3 06pa3ya B AenuTenLHyiO BOpOHKy BMeCTMOCTbI 250 CM3,A06aBnAOT25 cM3 BOAbi,He cogepxawen xnopnAbi,n BcTpAxnBaot B Te4eHe 1 MH.DepeHOc
28、AT 06pa3ey BO BTO-pyio gennTenbHyio BOpOHKy BMeCTnMOCTbI 250 CM3 n CAnBaoT BOgy B Kon6y 3pneHMeiepa BMeCTMOCTbiO125 cM3.loBTopAHoT 3Bne4eHne ewe pa3 npu go6aBneHnn 25 Cm3 BOAbi.OObeAnHAoT n3Bne4eHHyo BoAyB Kon6e 3pneHMeiepa.7.5.3 HarpeBaioT 3Bne4eHHyio Bogy go Temneparypbi 60 AnA oTroHkn ocTaTo4Hoi
29、npo6bi.Oxna-AaHoT CMeCb AO KOMHaTHO TeMnepaTypbI.7.5.4 Ao6aBnAioT 5 KanenL pacTBopa n TuTpyioT cTaHAapTHLIM pacTBopom aueTaTa prytn go AocTne-HA KoHe4HoM To4Kn TTpoBaH oneToBoro uBeTa.7.5.5 Or6paor nnnerkom 10 cM3 cTaHAapTHoro pacTBopa xnopnga HaTpnA n nepeHocAT B Kon6y3pneHmeiepa BMeCTnMOCTbo 250 CM3.Ao6aBnAKoT 20 CM3 BoAbi,He cogepxawei xnopnAbi,n 5 kanenbpacTBopa s-AnpeHnnKap6a3oHa.TnTpyoT cTaHAapTHbiM pacTBopoM ayeTaTa pryTn gO TycKHeHnA KOHeqHoTO4KM TTPoBaHA oneToBoro BeTaCM3 xnopuna 1,00=F=MKr xopa/cM3,cM3aueTaTa pryT(1)rAe F-pakTop Ana pacTBopa aueTaTa pryT.3