测定环氧树脂易皂化氯含量的样品处理条件研究

ThermosettingResin274Vol.27No.420127July2012201800、、。、＞3mol/L。3mol/LNaOH80℃4hGB/T4618.2—20080.588%0.592%。。TQ323.5B1002－7432201204－0066－04【】2011－07－25【】1990—。StudyontreatmentconditionsofepoxyresinindeterminationofhydrolyzablechloridecontentHUBi－chengDONGJunLINFang－jingGAOJinCHENZheng－yuanHUHe－fengSchoolofMaterialScienceandEngineeringShanghaiUniversityShanghai201800ChinaAbstractTheeffectsofdifferenttreatmentconditionsofepoxyresinsamplesonthedeterminationofhydrolyzablechlorinewereinvestigatedbytheintuitiveanalysisandvarianceanalysisoforthogonaltestselectedreactiontemper-aturereactiontimealkaliconcentrationasfactors.Theresultsshowedthatthereactiontemperatureandtimehadsignificantinfluenceontheaccuracyofdeterminationresultsandthealkaliconcentrationhigherthan3mol/Lhadnoinfluence.Thehydrolyzablechloridecontentofepoxyresintreatedat80℃for4hourswith3mol/LalkaliwassignificantlyhigherthanthatofepoxyresintreatedaccordingtoGB/T4618.2—2008.Therelativeerrorwas0.588%andrelativestandarddeviationRSDwas0.592%.Thetreatmentconditionsforthedeterminationofhydrolyzablechloridecontentwasbothsuitableofglycidicamineandglycidoletherepoxyresin.Keywordsepoxyresinhydrolyzablechlorinecontentorthogonaltesttreatmentcondition0、、、1。。。GB/T4618.2—200822h。。JISK7243—2—2005。ASTMD1726—0315min。JISASTM。6643。。11.1、、、D.E.R.383DowSKE－1SKE－3E－51E－44。PHS－3CpH216217。1.221～2g25mL25mL。。100mL325mL。。GB/T4618.1—2008。w21。w2Cl=35.5×c2×V1－V2m0×10－w1Cl－1c2mol/LV1mLV2mLw1%m0g。22.1αβ3。。。。、。GB/T4618.2—2008A、B、C31L16452。1Tab.1Factorsandlevelsoforthogonaldesign1234A/h2345B/℃20608090C/mol·L－13.03.54.04.52Tab.2ResultoforthogonaltestsABCw2/%1A1B1C10.1032A1B2C20.1353A1B3C30.1464A1B4C40.1505A2B1C20.1186A2B2C10.1437A2B3C40.1688A2B4C30.1699A3B1C30.12510A3B2C40.15611A3B3C10.16912A3B4C20.17013A4B1C40.12814A4B2C30.16015A4B3C20.17016A4B4C10.170D.E.R383。2.22.2.1。R。。、、76273。A、B、CRA=0.024、RB=0.046、RC=0.004RB＞RA＞RC。3Tab.3Averagevaluesofdifferentlevelsandtheextremedifferencew2/%＜w2＞/%R/%AA10.1030.1350.1460.1500.1340.024A20.1180.1430.1680.1690.150A30.1250.1560.1690.1700.155A40.1280.1600.1700.1700.157BB10.1030.1180.1250.1280.1190.046B20.1350.1430.1560.1600.149B30.1460.1680.1690.1700.163B40.1500.1690.1700.1700.165CC10.1030.1430.1690.1700.1460.004C20.1350.1180.1700.1700.148C30.1460.1690.1250.1600.150C40.1500.1680.1560.1280.1512.2.2。F。FSSeF=S/Se。2。S=1f1mΣmi=1＜w2＞i2－G2n22＜w2＞iimnGf。3。Se=1feΣnj=1w2j－＜w2＞2－Σpk=1Sk33w2jj＜w2＞nSkkpfe。15f3fe6。FF0.0136=9.78F0.0536=4.76F0.136=3.29。FF0.01FF0.01F0.05FF0.05F0.1F＜F0.1。2G=2.38%16＜w2＞0.149%。24。39.67×10－5A、B、CF46.93190.531.53。4Tab.4Squaresumofofaveragedeviationofeachfactor＜w2＞/%×10－5AA10.13445.37A20.150A30.155A40.157BB10.119184.18B20.149B30.163B40.165CC10.1461.48C20.148C30.150C40.151FB＞FA＞FCFB、FA＜F0.01、。FCF0.1。。。2.2.31。1a4h。1b80℃。1c3mol/L。8643mol/LNaOH80℃4h。1Fig.1Relationshipbetweenthelevelofeachfactorandaveragehydrolyzablechlorinecontent2.35。5Tab.5Erroranddeviationindeterminationofhydrolyzablechlorinecontentsω/%/%10.170020.168－1.1830.168－1.1840.169－0.5950.17004.5mol/LNaOH90℃5h0.170%5。0.001%0.588%0.592%。。2.4GB/T4618.2—20086SKE－1SKE－3。6Tab.6Hydrolyzablechlorinecontentsofepoxyresinsdeterminatedbydifferentmethodsω/%/%/%SKE－10.1020.2150.11352.6SKE－30.0420.1460.10471.2E－510.0490.1360.08764.0E－440.0440.1450.10169.7D.E.R．3830.1030.1690.06639.1。。。3。3mol/LNaOH80℃4h。0.588%0.592%。。1.J.20108320－33.2GB/T4618.2－20082S.3.AJ．199621212－15.96