chromatography飞鱼星1260
飞鱼星1260 时间:2021-05-19 阅读:()
AgilentTechnologiesAgilent1260InfinityIIHT-ELSD(G7826A)-ForMolecularWeightDeterminationTechnicalNoteHT-ELSDforMWDThe1260InfinityIIHT-ELSD(G7826A)canprovidealinearizedanalogueoutputwhichallowsthedetectortobeusedasalinearconcentrationdetectorreplacingrefractiveindex(DRI)orInfraRed(IR)inHT-GPCapplications.
Themainadvantageofusingthisdetectorforthisapplicationisthesignificantincreasedsensitivityofthehightemperatureevaporativelightscatteringdetector(ELSD)comparedwiththeDRIandIR;typically,theELSDis30timesmoresensitivitythanaDRI.
ThisincreasedsensitivityenablesdetectionofmuchlowerconcentrationwhichisessentialfortheanalysisofUHMWPEsamples.
DeterminationofthePowerFunctionTheELSDsignalinthefunctionofconcentrationislinearized,basedonapowerlawfunction:ELSDsignalintensitykELSDconcentrationaELSDTheexponent,αELSD,definedbyLinFintheinstrumentinterfaceissolventdependentbutNOTpolymertypedependent.
InTable1onpage2belowarepredeterminedPowerfunctionforcommonhightemperatureGPCsolvents.
Table1ELSDparametersfordifferentsolventsforHT-GPCofpolyolefinsSolventPolymersPowerReferencesTCBPS,PE,PP1.
612[]1,o-DCBPS,PE,PP1.
20butylalPS,PE,PP1.
35[3]xylenePS,PE,PP1.
40[4]Ifanewsolventisusedthatdoesn'thaveapredeterminedPowerfunctionthenyou'llneedtomeasurethearearesponseforseveralconcentrationsofaccuratelypreparedsolutionsintherange5–500g/ml[5].
Plottheresponseagainstconcentrationandfitthedatatoapowerfunctionasdescribedinreference[2].
ThepowercoefficientwhichbestfitsthedataistheonetobeusedasLinFparameterfortherespectivesolventandtestconditions.
2DeterminationofthePowerFunction1A.
Boborodea,S.
O'Donohue,Newevaporativelightscatteringdetectorforhightemperaturegelpermeationchromatography,,Int.
J.
Polym.
Anal.
Charact.
,vol22,no7,631-638(2017)2A.
Boborodea,S.
O'Donohue,Linearizationofevaporativelightscatteringdetectorsignal,Int.
J.
Polym.
Anal.
Charact.
,vol22,no8,685-689(2017)3A.
Boborodea,A.
Brookes,Polyolefincharacterizationindibutoxymethanebyhightemperaturegelperme-ationchromatographywithanewevaporativelightscatteringdetector,Polym.
Test.
,vol64,217-220(2017)4A.
Boborodea,F.
Mirabella,S.
O'Donohue,PolyolefinCharacterizationinXylenebyHigh-TemperatureGelPer-meationChromatographywithaNewEvaporativeLightScatteringDetector,Chromatographia,vol81,no3,419-424(2018)5A.
Boborodea,A.
Brookes,Investigationofsamplepreparationforhightemperaturegelpermeationchroma-tographyusingalowsolventconsumptionmethod,Polym.
Test.
,vol63,210-213(2017)3SettingUptheInstrumentSettingUptheInstrumentOncethepowerfunctionhasbeendeterminedfortheoperatingsolventitcanbeenteredontheinstrumentviathesecondsub-screenasshownbelow:MainScreenSub-screen1Sub-screen2Navigationbetweenthescreensisachievedbythearrowsonthekeypadwhenthecursorisonthearrow.
Sub-screen2allowschangestothefollowingelectronicparameters:DefaultRangeLinFLinearizationfunction1.
01.
00–2.
00ZEROBaselinepositiontheinstrumentiszeroedto100.
1–10SCALEScalingfactortoincreasepeakheightafterlinearizationfunctionapplied1.
01–354SettingUptheInstrumentOncetheLinFhasbeensetforthesolventbeingused,eachdatapointiscorrectedbythefollowingequation:CorrectedELSDELSDSignal1LinFTheneteffectisthatsignalislinear(seefigurebelow),buttheapparentsignalsensitivityisreducedandthereforetocompensateforthislossinsensitivitytheScalecanbeappliedtoamplifythesignalagain.
Figure1OverlayofPS135kchromatograms,concentrations:5to500g/mlFigure2PeakareaversusconcentrationlinearcorrelationovertwoordersofmagnitudeToobtaincorrectmolecularweightsthezerooffsetvalueappliedneedstosetthebaselineasclosetozeroaspracticallypossiblewithoutthedatabeatorbelowzeroorthecalculationwilljustreturnzeroandthuslossofdata.
ForTCB,therecommendedZerovalueis0.
1,butthisvaluecanbeslightlyincreasedupto1forsolventspresentingahigherlevelofbaselinenoise.
ToensurethatthebaselineissettothezerooffsetvaluebeforeeachrunweadviseusingCable(G7826-60015)withtheAgilent1260InfinityIIHTGPCSystemwhichisconnectedbetweentheInjSyncatthebackofthecontroldrawerandtheAuxI/OportattherearoftheHT-ELSDpriortoeachrun.
ThesamecanbeachievedforthirdpartyusersbyusingCable(0890-0055)withbothInjectSyncandAutozerolinesconnectedtotheinjector.
5Example–AnalysisofSRM1475aExperimentalConditionsExample–AnalysisofSRM1475aExperimentalConditionsAgilent1260InfinityIIHighTemperatureGPCSystem(G7820B)interfacedtoanAgilent1260InfinityIIHT-ELSD(G7826A).
Table2ChromatographyConditionsMobilephase1,2,4Tricholobenzene+250ppmBHTColumns3xPL-OlexisColumns,7.
5mmx300mmColumnOventemperature160°CFlowRate1.
0mL/minInjectionvolume200LConcentration1mg/mlforSRMPE1475aCalibrationStandardsEasiVialsPSstandardsPS-HTable3DetectorConditionsXfer(Transferlinetemperature)160°CNeb(Nebulisertemperature)160°CEvap(Evaporationtemperature)120°CGas(Gasflowrate)0.
4SLMSmth(smoothingfactor)60LED(Lightsourcepower)100%LinF1.
61Zero0.
3Scale16Example–AnalysisofSRM1475aAnalysisofPESRM1475sampleAnalysisofPESRM1475sampleEightanalyseswereperformedonPESRM1475sampleduringseveraldays,usingthesamesettingforthepowercoefficientforELSD,LinF=1.
61.
TheoverlayoftheobtainedchromatogramsinFigure3onpage6showsanexcellentreproducibility:Figure3OverlayofchromatogramsofPESRM1475sample7Example–AnalysisofSRM1475aAnalysisofPESRM1475sampleTheaveragemolecularweights,presentedinTable4onpage7areinexcellentagreementwiththeexpectedvaluesprovidedbyPESRM1475certificate(Mn=18310,Mw=53070g/mol,Mz=138000g/mol).
Table4AveragemolecularweightsdeterminedfromtheHT-ELSDchromatogramsusingconven-tionalGPCandpolystyrenecalibrationstandards(EasivialPS-H)InjectionMn(g/mol)Mw(g/mol)Mz(g/mol)NIST1475(01)1824257925145027NIST1475(02)1835357648144716NIST1475(03)1831457537143238NIST1475(04)1841157434142142NIST1475(05)1796056259138325NIST1475(06)1795056369140288NIST1475(07)1804456323139180NIST1475(08)1817056434139052ThefollowingMarkHouwink-SakuradaparameterswereusedinthecalculationtoconvertthePolystyreneequivalentmolecularweightvaluestoPolyethylenevalues:KPS=19*10-3mL/g;αPS=0.
655KPE=39*10-3mL/g;αPE=0.
725Example–AnalysisofSRM1475aAnalysisofPESRM1475sample*G7826-90020**G7826-90020*G7826-90020Edition:08/2018PrintedinGermanyAgilentTechnologies,Inc2018AgilentTechnologies,IncHewlett-Packard-Strasse876337WaldbronnGermanyThelinearizedELSDsignalisindependentofmolecularweightandthisisdemonstratedbytheexcellentagreementbetweentheMWDobtainedwithclassicalDRIdetectorandtheonegivenbyELSD,aspresentedinFigure4onpage8:Figure4ComparisonbetweenMWDobtainedwithDRIdetectorandELSDinTCBat160°CforPESRM1475sample
Themainadvantageofusingthisdetectorforthisapplicationisthesignificantincreasedsensitivityofthehightemperatureevaporativelightscatteringdetector(ELSD)comparedwiththeDRIandIR;typically,theELSDis30timesmoresensitivitythanaDRI.
ThisincreasedsensitivityenablesdetectionofmuchlowerconcentrationwhichisessentialfortheanalysisofUHMWPEsamples.
DeterminationofthePowerFunctionTheELSDsignalinthefunctionofconcentrationislinearized,basedonapowerlawfunction:ELSDsignalintensitykELSDconcentrationaELSDTheexponent,αELSD,definedbyLinFintheinstrumentinterfaceissolventdependentbutNOTpolymertypedependent.
InTable1onpage2belowarepredeterminedPowerfunctionforcommonhightemperatureGPCsolvents.
Table1ELSDparametersfordifferentsolventsforHT-GPCofpolyolefinsSolventPolymersPowerReferencesTCBPS,PE,PP1.
612[]1,o-DCBPS,PE,PP1.
20butylalPS,PE,PP1.
35[3]xylenePS,PE,PP1.
40[4]Ifanewsolventisusedthatdoesn'thaveapredeterminedPowerfunctionthenyou'llneedtomeasurethearearesponseforseveralconcentrationsofaccuratelypreparedsolutionsintherange5–500g/ml[5].
Plottheresponseagainstconcentrationandfitthedatatoapowerfunctionasdescribedinreference[2].
ThepowercoefficientwhichbestfitsthedataistheonetobeusedasLinFparameterfortherespectivesolventandtestconditions.
2DeterminationofthePowerFunction1A.
Boborodea,S.
O'Donohue,Newevaporativelightscatteringdetectorforhightemperaturegelpermeationchromatography,,Int.
J.
Polym.
Anal.
Charact.
,vol22,no7,631-638(2017)2A.
Boborodea,S.
O'Donohue,Linearizationofevaporativelightscatteringdetectorsignal,Int.
J.
Polym.
Anal.
Charact.
,vol22,no8,685-689(2017)3A.
Boborodea,A.
Brookes,Polyolefincharacterizationindibutoxymethanebyhightemperaturegelperme-ationchromatographywithanewevaporativelightscatteringdetector,Polym.
Test.
,vol64,217-220(2017)4A.
Boborodea,F.
Mirabella,S.
O'Donohue,PolyolefinCharacterizationinXylenebyHigh-TemperatureGelPer-meationChromatographywithaNewEvaporativeLightScatteringDetector,Chromatographia,vol81,no3,419-424(2018)5A.
Boborodea,A.
Brookes,Investigationofsamplepreparationforhightemperaturegelpermeationchroma-tographyusingalowsolventconsumptionmethod,Polym.
Test.
,vol63,210-213(2017)3SettingUptheInstrumentSettingUptheInstrumentOncethepowerfunctionhasbeendeterminedfortheoperatingsolventitcanbeenteredontheinstrumentviathesecondsub-screenasshownbelow:MainScreenSub-screen1Sub-screen2Navigationbetweenthescreensisachievedbythearrowsonthekeypadwhenthecursorisonthearrow.
Sub-screen2allowschangestothefollowingelectronicparameters:DefaultRangeLinFLinearizationfunction1.
01.
00–2.
00ZEROBaselinepositiontheinstrumentiszeroedto100.
1–10SCALEScalingfactortoincreasepeakheightafterlinearizationfunctionapplied1.
01–354SettingUptheInstrumentOncetheLinFhasbeensetforthesolventbeingused,eachdatapointiscorrectedbythefollowingequation:CorrectedELSDELSDSignal1LinFTheneteffectisthatsignalislinear(seefigurebelow),buttheapparentsignalsensitivityisreducedandthereforetocompensateforthislossinsensitivitytheScalecanbeappliedtoamplifythesignalagain.
Figure1OverlayofPS135kchromatograms,concentrations:5to500g/mlFigure2PeakareaversusconcentrationlinearcorrelationovertwoordersofmagnitudeToobtaincorrectmolecularweightsthezerooffsetvalueappliedneedstosetthebaselineasclosetozeroaspracticallypossiblewithoutthedatabeatorbelowzeroorthecalculationwilljustreturnzeroandthuslossofdata.
ForTCB,therecommendedZerovalueis0.
1,butthisvaluecanbeslightlyincreasedupto1forsolventspresentingahigherlevelofbaselinenoise.
ToensurethatthebaselineissettothezerooffsetvaluebeforeeachrunweadviseusingCable(G7826-60015)withtheAgilent1260InfinityIIHTGPCSystemwhichisconnectedbetweentheInjSyncatthebackofthecontroldrawerandtheAuxI/OportattherearoftheHT-ELSDpriortoeachrun.
ThesamecanbeachievedforthirdpartyusersbyusingCable(0890-0055)withbothInjectSyncandAutozerolinesconnectedtotheinjector.
5Example–AnalysisofSRM1475aExperimentalConditionsExample–AnalysisofSRM1475aExperimentalConditionsAgilent1260InfinityIIHighTemperatureGPCSystem(G7820B)interfacedtoanAgilent1260InfinityIIHT-ELSD(G7826A).
Table2ChromatographyConditionsMobilephase1,2,4Tricholobenzene+250ppmBHTColumns3xPL-OlexisColumns,7.
5mmx300mmColumnOventemperature160°CFlowRate1.
0mL/minInjectionvolume200LConcentration1mg/mlforSRMPE1475aCalibrationStandardsEasiVialsPSstandardsPS-HTable3DetectorConditionsXfer(Transferlinetemperature)160°CNeb(Nebulisertemperature)160°CEvap(Evaporationtemperature)120°CGas(Gasflowrate)0.
4SLMSmth(smoothingfactor)60LED(Lightsourcepower)100%LinF1.
61Zero0.
3Scale16Example–AnalysisofSRM1475aAnalysisofPESRM1475sampleAnalysisofPESRM1475sampleEightanalyseswereperformedonPESRM1475sampleduringseveraldays,usingthesamesettingforthepowercoefficientforELSD,LinF=1.
61.
TheoverlayoftheobtainedchromatogramsinFigure3onpage6showsanexcellentreproducibility:Figure3OverlayofchromatogramsofPESRM1475sample7Example–AnalysisofSRM1475aAnalysisofPESRM1475sampleTheaveragemolecularweights,presentedinTable4onpage7areinexcellentagreementwiththeexpectedvaluesprovidedbyPESRM1475certificate(Mn=18310,Mw=53070g/mol,Mz=138000g/mol).
Table4AveragemolecularweightsdeterminedfromtheHT-ELSDchromatogramsusingconven-tionalGPCandpolystyrenecalibrationstandards(EasivialPS-H)InjectionMn(g/mol)Mw(g/mol)Mz(g/mol)NIST1475(01)1824257925145027NIST1475(02)1835357648144716NIST1475(03)1831457537143238NIST1475(04)1841157434142142NIST1475(05)1796056259138325NIST1475(06)1795056369140288NIST1475(07)1804456323139180NIST1475(08)1817056434139052ThefollowingMarkHouwink-SakuradaparameterswereusedinthecalculationtoconvertthePolystyreneequivalentmolecularweightvaluestoPolyethylenevalues:KPS=19*10-3mL/g;αPS=0.
655KPE=39*10-3mL/g;αPE=0.
725Example–AnalysisofSRM1475aAnalysisofPESRM1475sample*G7826-90020**G7826-90020*G7826-90020Edition:08/2018PrintedinGermanyAgilentTechnologies,Inc2018AgilentTechnologies,IncHewlett-Packard-Strasse876337WaldbronnGermanyThelinearizedELSDsignalisindependentofmolecularweightandthisisdemonstratedbytheexcellentagreementbetweentheMWDobtainedwithclassicalDRIdetectorandtheonegivenbyELSD,aspresentedinFigure4onpage8:Figure4ComparisonbetweenMWDobtainedwithDRIdetectorandELSDinTCBat160°CforPESRM1475sample
- chromatography飞鱼星1260相关文档
- change飞鱼星1260
- hFE飞鱼星1260
- "2018年成都市中小企业成长工程培育企业名单(第一批)
- based飞鱼星1260
- absence飞鱼星1260
- 大连市公安局交通警察支队2019年度弱电维护、办公设备维护及耗材服务单位采购项目
Kinponet是谁？Kinponet前身公司叫金宝idc 成立于2013年 开始代理销售美国vps。
在2014年发现原来使用VPS的客户需求慢慢的在改版，VPS已经不能满足客户的需求。我们开始代理机房的独立服务器，主推和HS机房的独立服务器。经过一年多的发展，我们发现代理的服务器配置参差不齐，机房的售后服务也无法完全跟上，导致了很多问题发生，对使用体验带来了很多的不便，很多客户离开了我们。经过我们慎重的考虑和客户的建议。我们在2015开始了重大的改变， 2015年，我们开始计划托管自己...
数脉科技8月促销，新客减400港币，BGP、CN2+BGP、阿里云线路低至350元
数脉科技（shuhost）8月促销：香港独立服务器，自营BGP、CN2+BGP、阿里云线路，新客立减400港币/月，老用户按照优惠码减免！香港服务器带宽可选10Mbps、30Mbps、50Mbps、100Mbps带宽，支持中文本Windows、Linux等系统。官方网站：https://www.shuhost.com* 更大带宽可在选购时选择同样享受优惠。* 目前仅提供HKBGP、阿里云产品，香港...
MechanicWeb免费DirectAdmin/异地备份
MechanicWeb怎么样？MechanicWeb好不好？MechanicWeb成立于2008年，目前在美国洛杉矶、凤凰城、达拉斯、迈阿密、北卡、纽约、英国、卢森堡、德国、加拿大、新加坡有11个数据中心，主营全托管型虚拟主机、VPS主机、半专用服务器和独立服务器业务。MechanicWeb只做高端的托管vps，这次MechanicWeb上新Xeon W-1290P处理器套餐，基准3.7GHz最高...
飞鱼星1260为你推荐
-
搜狗高速浏览器Createdwin7支持ipad支付appleeacceleratorW3S是什么意思联通版iphone4s苹果4s怎么分移动版联通版电信版？联通iphone4联通iphone4合约谷歌sb为什么搜索SB第一个是google？google分析google分析打不开了？routeaddroute add 添加路由的命令，内网和外网如何同时上