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
乌云数据主营高性价比国内外云服务器,物理机,本着机器为主服务为辅的运营理念,将客户的体验放在第一位,提供性价比最高的云服务器,帮助各位站长上云,同时我们深知新人站长的不易,特此提供永久免费虚拟主机,已提供两年之久,帮助了上万名站长从零上云官网:https://wuvps.cn迎国庆豪礼一多款机型史上最低价,续费不加价 尽在wuvps.cn香港cera机房,香港沙田机房,超低延迟CN2线路地区CPU...
木木云怎么样?木木云品牌成立于18年,此为贵州木木云科技有限公司旗下新运营高端的服务器的平台,目前已上线美国中部大盘鸡,母鸡采用E5-267X系列,硬盘全部组成阵列。目前,木木云美国vps进行了优惠促销,1核1G/500M带宽/1T硬盘/4T流量,仅35元/月。点击进入:木木云官方网站地址木木云优惠码:提供了一个您专用的优惠码: yuntue目前我们有如下产品套餐:DV型 1H 1G 500M带宽...
hostodo从2014年年底运作至今一直都是走低价促销侧率运作VPS,在市场上一直都是那种不温不火的品牌知名度,好在坚持了7年都还运作得好好的,站长觉得hostodo还是值得大家在买VPS的时候作为一个候选考虑项的。当前,hostodo有拉斯维加斯和迈阿密两个数据中心的VPS在促销,专门列出了2款VPS给8T流量/月,基于KVM虚拟+NVMe整列,年付送DirectAdmin授权(发ticket...
飞鱼星1260为你推荐
courses163urlcss存在问题的应用软件名单(2020年第四批)支持ipad支持ipad支持ipad支持ipad《个人收入的分配过关检测》南京医科大学合同管理系统ipadwifiipad wifi信号差怎么办
电信服务器租赁 查询ip地址 Vultr 美元争夺战 搜狗12306抢票助手 服务器架设 国外网站代理服务器 e蜗 合租空间 空间合租 厦门电信 1元域名 台湾google 西安服务器托管 我的世界服务器ip 免费的域名 实惠 移动王卡 中美互联网论坛 cdn加速技术 更多