反相高效液相色谱法测定工业高盐废水中含氟有机酸含量杨先武

385May201820185ModernChemicalIndustry1221*1．3100272．310023、、。SHIM－PACKVP－ODSC184.6mm×150mm5μm40mmol/LKH2PO4pH=3.00.6mL/min50℃195nm。Ｒ≥0.99922～1000μmol/L0.002～0.01μmol/L96.2%～109.4%。CODO657．72A0253－4320201805－0233－05DOI10．16606/j．cnki．issn0253－4320．2018．05．053Determinationofcontentoffluorine-containingorganicacidsinhighsaltindustrialwastewaterbyreversed-phasehighperformanceliquidchromatographyYANGXian-wu1CHENXian-jin2LIJie2HOUZhao-yin1*1．DepartmentofChemistryZhejiangUniversityHangzhou310027China2．EngineeringTechnologyCenterZhejiangＲesearchInstituteofChemicalIndustryHangzhou310023ChinaAbstractAreversed-phasehighperformanceliquidchromatographyＲP-HPLCmethodisdevelopedtodeterminesimultaneouslytrifluoroaceticacidpentafluoropropionicacidandheptafluorobutyricacidinhighsaltwastewater．Itisconfirmedthatsomeperfluoroorganicacidsaredifficulttogetoxidizedbypotassiumdichromate．Thesampleisdilutedordissolvedwithwater．ThetestiscarriedoutonaSHIM-PACKVP-ODSC18column4.6mm×150mm5μmwithacolumntemperatureat50℃．Gradientelutionisperformedbyusingamixtureofacetonitrileand40mmol·L－1KH2PO4pH=3.0asthemobilephasewithaflowingrateof0.6mL·min－1．Thedetectionwavelengthissetat195nm．Thelinearcorrelationcoefficientsforvariousfluorine-containingorganicacidsarenolessthan0.9992．Thelinearrangesarein2－1000μmol·L－1andthedetectionlimitisbetween0.002and0.01μmol·L－1．Therecoveryrateisintherangeof96.2%－109.4%．Keywordsreversed-phasehighperformanceliquidchromatographyfluorine-containingorganicacidshigh-saltindustrialwastewa[e-mail]1968－、[e-mail]。1－3COD、TOCF－。4、、、5。COD、TOC、F－。6。。－7－9、10－14、915－1617－18。·332·38533。11.1LC－10AvpPlusSPD－10AvpPlus、LC－10ATvpCBM－10AvpPlus－AL104。A1.0mmol/L、、B1.0mmol/L、、。1%。、、、＞99.0%、＞99.0%、HPLC、、、。1.2SHIM－PACKVP－ODSC184.6mm×150mm5μm50℃ABpH3.040mmol/L0.6mL/min20μL195nm0～10minA15%40%10～25minA40%15%5min。1.31419。2.0g0.0001g25mL0.45μm5mL。。22.12.1.1C18。1213C18。SHIM－PACKVP－ODSC18、ZOＲBAXEclipseXDB－C18HypersilODS2C18、2SHIM－PACKVP－ODSC18。ZOＲBAXEclipseXDB－C18HypersilODS2C18ZOＲBAXEclipseXDB－C18SHIM－PACKVP－ODSC18。SHIM－PACKVP－ODSC181。aVP－ODSC18No．6082238bVP－ODSC18No．60329701—2—3—1SHIM－PACKVP－ODSC182.1.240mmol/L190～370nm1nm2。2、192、192、193.7nm。190nm190、195、200、205nm210nm320。195nm3·432·20185。abc22.1.3－、－40mmol/LpH3.040μmol/LA3。3－－40mmol/LpH3.03。－40mmol/LpH3.0。3SHIM－PACKVP－ODSC182.1.4－pH5、10、20、40、60、80mmol/L40μmol/LA、、、4。440～80mmol/L1.5。40mmol/L。1—2—3—440mmol/LpH2.0、2.6、3.0、3.6、4.0、4.435。5pH3.0～4.0。pH3.0。1—2—3—5pH2.23yx331。1、/μmol·L－1ＲLOD/μmol·L－12～1000y=2356.4x－218770.99920.00242～1000y=2307.4x－102400.99970.00252～1000y=2103.4x+7866.90.99980.0102.372。21.8%～4.9%·532·385。2.410%10。A10、20、40μmol/L。2/μmol·L－1/μmol·L－1/μmol·L－1n=7/%ＲSDn=7/%11.201020.7294.6～100.22.52031.2096.3～101.12.64051.2099.3～102.81.820.211030.74101.8～109.43.62039.6396.2～102.54.94060.7499.1～106.83.6—109.7896.9～103.13.02020.19100.2～107.63.84040.0399.2～102.42.12396.2%～109.4%。2.51.0mmol/LAB40μmol/L6。6、、。0.45μm。A—B—632.610%103。1、27。3/μmol·L－11264.31513.47—211.2020.21—3341.28672.79—49.7614.19—abA—B—C—730.5mmol/L0.02mmol/L＜0.5mmol/L。2.7CODHJ828500mg/LCOD214。B85%4/mg·L－1COD/mg·L－1/mg·L－150027.9919.72482.0925013.6011.67246.7150019.4421.37—25016.3310.439.2650019.4424.6940.1125011.6614.5421.47·632·20185250mL8。48、、。。abc8。3、、、、。1．DB32/939—2006S．2006－07－26．2．GB18599—2001、S．2002－07－01．3．GB8978—2002S．2003－07－01．4．－2－－3－CN103787854AP．2014－05－14．5．A2/OJ．20126331－34．6．CODD．2013．7．－J．－2010463241－243．8PatrycjaMako＇sAndreFernandesGrzegorzBoczkaj．Methodforthedeterminationofcarboxylicacidsinindustrialeffluentsusingdis-persiveliquid-liquidmicroextractionwithinjectionportderivatizationgaschromatography-massspectrometryJ．JournalofChromatographyA201715172926－34．9．D．2012．10AnaCarolinaMouradeSenaAquinoMniaStremelAzevedoDeiseHelenaBaggioＲibeiroetal．ValidationofHPLCandCEmethodsfordeterminationoforganicacidsinsourcassavastarchwastewaterJ．FoodChemistry2015172725－730．11MarinaCocchiPaoloLambertiniDanielaManzinietal．Multivariateanalysisoforganicacidsinfermentedfoodfromre-versed-phasehigh-performanceliquidchromatographydataJ．Ta-lanta201817815－23．12．J．2010312126－127．13．J．201383613－14．14．J．20133091089－1095．15．、、－J．2012304384－390．16WangFenglianCaoMinyiWangNanietal．Simplecoupledultra-highperformanceliquidchromatographyandionchromatographytechniqueforsimultaneousdeterminationoffolicacidandinorganicanionsinfolicacidtabletsJ．FoodChemistry20182391562－67．17．J．200720440－47．18．J．2015347454－458．19．2007C．2007．20．5－．2010191621－22．21．HJ828—2017S．2017－05－01．■·732·