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
npidc：9元/月，cn2线路（不限流量）云服务器，金盾+天机+傲盾防御CC攻击，美国/香港/韩国
npidc全称No Problem Network Co.,Limited（冇問題(香港)科技有限公司，今年4月注册的）正在搞云服务器和独立服务器促销，数据中心有香港、美国、韩国，走CN2+BGP线路无视高峰堵塞，而且不限制流量，支持自定义内存、CPU、硬盘、带宽等，采用金盾+天机+傲盾防御系统拦截CC攻击，非常适合建站等用途。活动链接：https://www.npidc.com/act.html...
丽萨主机122元/每季，原生IP,CN2 GIA网络
萨主机(lisahost)新上了美国cn2 gia国际精品网络 – 精品线路，支持解锁美区Netflix所有资源，HULU, DISNEY, StartZ, HBO MAX，ESPN, Amazon Prime Video等，同时支持Tiktok。套餐原价基础上加价20元可更换23段美国原生ip。支持Tiktok。成功下单后，在线充值相应差价，提交工单更换美国原生IP。!!!注意是加价20换原生I...
DMIT(8.72美元)日本国际线路KVM月付8折起,年付5折
DMIT.io是成立于2018年的一家国外主机商，提供VPS主机和独立服务器租用，数据中心包括中国香港、美国洛杉矶和日本等，其中日本VPS是新上的节点，基于KVM架构，国际线路，1Gbps带宽，同时提供月付循环8折优惠码，或者年付一次性5折优惠码，优惠后最低每月8.72美元或者首年65.4美元起，支持使用PayPal或者支付宝等付款方式。下面列出部分日本VPS主机配置信息，价格以月付为例。CPU：...
飞鱼星1260为你推荐
-
SAProute支持ipad支持ipadApplicationsios5photoshop技术什么是ps技术itunes备份怎样用itunes备份iphoneiphonewifi苹果手机怎么扫二维码连wifi迅雷下载速度迅雷限制下载速度要设置多少迅雷雷鸟迅雷会员每日免费抽奖，抽中迅雷的雷鸟披肩了,要钱吗联通合约机iphone5联通苹果5合约机套餐费