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
RAKsmart推出7.59美元/月，云服务器产品Cloud Server，KVM架构1核1G内存40G硬盘1M带宽基础配置
近期RAKsmart上线云服务器Cloud Server产品，KVM架构1核1G内存40G硬盘1M带宽基础配置7.59美元/月！RAKsmart云服务器Cloud Server位于美国硅谷机房，下单可选DIY各项配置，VPC网络/经典网络，大陆优化/精品网线路，1-1000Mbps带宽，支持Linux或者Windows操作系统，提供Snap和Backup。RAKsmart机房是一家成立于2012年...
PIGYun中秋特惠：香港/韩国VPS月付14元起
PIGYun发布了九月份及中秋节特惠活动，提供8折优惠码，本月商家主推中国香港和韩国机房，优惠后最低韩国每月14元/中国香港每月19元起。这是一家成立于2019年的国人商家，提供中国香港、韩国和美国等地区机房VPS主机，基于KVM架构，采用SSD硬盘，CN2+BGP线路(美国为CUVIP-AS9929、GIA等)。下面列出两款主机配置信息。机房：中国香港CPU：1core内存：1GB硬盘：10GB...
EdgeNat 新年开通优惠 - 韩国独立服务器原生IP地址CN2线路七折优惠
EdgeNat 商家在之前也有分享过几次活动，主要提供香港和韩国的VPS主机，分别在沙田和首尔LG机房，服务器均为自营硬件，电信CN2线路，移动联通BGP直连，其中VPS主机基于KVM架构，宿主机采用四路E5处理器、raid10+BBU固态硬盘！最高可以提供500Gbps DDoS防御。这次开年活动中有提供七折优惠的韩国独立服务器，原生IP地址CN2线路。第一、优惠券活动EdgeNat优惠码（限月...
飞鱼星1260为你推荐
-
界面winrar5伺服器chromeTestto机构appleIntentsandroid支持ipad支持ipad勒索病毒win7补丁win7有针对勒索病毒的补丁吗css下拉菜单如何用css3做导航栏下拉菜单迅雷快鸟迅雷快鸟支持移动宽带提速吗