HAPSITE顶空操作培训

HAPSITEER/SmartPlusTraining

HAPSITEER/SmartPlus培训HeadspaceSamplingSystem

顶空采样系统2HSSModuleOutline

HSS模件概要HSSAssembly

HSS装配HSSTheoryHSS原理HSSInternalStandards

HSS内部标准PreparingBlanks/Samples准备空样/样品RunningAnalyze运行分析QuantitationReports定量报告ContaminationIssues污染问题3WhatistheHeadspaceSamplingSystem什么是顶空采样系统HAPSITEaccessory

HAPSITE辅件Samplingsystemfor:采样系统用于:Water水Soil土壤Liquids液体DetectsVOCs检测VOCsQualitativemethods定性方法Quantitativemethods定量方法PPBtoPPTrangePPB至PPT量程4HSSAssemblyHSS装配InsertachargedbatteryintotheHAPSITE将充足电的电池插入HAPSITEDisconnecttheHAPSITEpowersupplycord断开HAPSITE的电源电缆连接5ConnectingtheY-CableforStationaryUse为台式用法连接Y-电缆

Asthenameimplies,thecableformsaY正如其名,电缆呈Y形Joinedend

连接端Splitends

分叉端6ConnectingtheY-CableforStationaryUse为台式用法连接Y-电缆ConnectthejoinedendtotheHAPSITEpowersupplycord

将连接端连接至HAPSITE的电源电缆NOTE:

Alignthedotsonthecablewiththedotsonthecord注:

对准电缆上的点与电源线上的点7ConnectingtheY-CableforStationaryUse为台式用法连接Y-电缆ConnectonesplitendofthecordtotheHAPSITE连接电缆的一个分叉端至HAPSITEConnecttheothersplitendtotheHeadspaceSamplingSystem连接另一个分叉端至顶空采样系统NOTE:

Alignthedotsonthecablewiththedotsontheinstrumentstoproperlyconnect

注:

将电缆上的点与仪器上的点对准,直至妥善地连接上8TransferLine

传输线ProvidescommunicationbetweentheHAPSITEER/SmartPlusandtheHSS提供HAPSITEER/SmartPlus与HSS之间的通讯SampletravelsthroughthetransferlinetotheHAPSITEER/SmartPlus样品经过传输线传送给HAPSITEER/SmartPlus

HAPSITEERTransferLine传输线HAPSITESmartPlusTransferLine传输线9TransferLine传输线Encompassedbyafoamsleeve外包泡沫套管Providesinsulation提供绝缘Reducespowerrequirements降低功率要求Directional方向性Multi-connectorendconnectstotheHAPSITEERUniversalInterface多接头端连接至HAPSITEER的通用接口FortheHAPSITESmartPlus,thedirectionofthetransferlineislabeleddirectlyonitHAPSITESmartPlus的传输线方向直接标注在它的上面10InsertingtheTransferLine插入传输线FortheHAPSITEER,plugtheendwiththesingleLEMO®

connectionintotheHSS对于HAPSITEER,将带有单个LEMO®

接头插入HSSAlignthereddots对准红点FortheHAPSITESmartPlus,plugthesidelabeledThisEndtoAccessoryintotheHSS对于HAPSITESmartPlus,将边上标志此端至附件端的一端插入HSSAlignthereddots对准红点11InsertingtheTransferLine插入传输线RemovetheprobefromtheHAPSITEER/SmartPlus从HAPSITEER/SmartPlus上卸下探头ToattachthetransferlinetotheHAPSITEER连接传输线至HAPSITEERScrewtheUniversalBulkheadconnectionintoplace拧上通用的防水连接件Alignthereddots对准红点InserttheLEMO®connection插上LEMO®

接头

ToattachthetransferlinetotheHAPSITESmartPlus连接传输线至HAPSITESmartPlus

Alignthereddots对准红点InserttheLEMO®connection插上LEMO®

接头

HAPSITEERViewHAPSITEER视图

12PortableHSSUse便携式HSS的用法TheHSSisdesignedforportableuse

HSS设计于便携式应用Requiresabattery

需用电池OpenthefrontdooroftheHSS

打开HSS的前门Insertthebatteryintotheslot

将电池插入槽内Thearrowonthebatterywillbefacingthebatteryreleasebutton电池上的箭头指向电池释放按钮TheINFICONlabelwillbeinthelowerleft-handcorner

INFICON的标签位于左下角13PortableHSSUse便携式HSS的用法Pushbatteryintoslotuntila“click”isheard将电池推入槽中,直到听见“咔哒声”Verifythatthebatteryissecurelyfastened证实电池已被牢固地固定住14NitrogenCanister

氮气瓶Insertthenitrogencanister插入氮气瓶15TurningontheHSS

将HSS的电源onPressdownonthePOWERswitch按下电源开关ThePOWERswitchisatoggleswitch电源开关是扳钮开关Oncepressed,itwillreturntoitsoriginalposition一旦按下,它将回到原位ThewordPOWERwillilluminate文字指示灯POWER亮

IftheHeadspaceispoweredbytheHAPSITEpowersupply,theRMTPOWER(RemotePower)willalsoilluminate如顶空使用HAPSITE的电源,RMTPOWER(遥控电源)也亮

Closethefrontdoor关上前门16PreparingAnalyze准备分析TheHAPSITEER/SmartPluswillautomaticallybeginpreparingaHeadspacemethodHAPSITEER/SmartPlus将自动开始准备顶空方法Allcomponentswillbeheatedtotheirsetpointtemperature全部组件将加热至它们的设定温度AutoTunewillberun自动调谐将运行ConcentratorCleanoutwillberunifaconcentratorisinstalled如安装浓缩器将运行浓缩器清理17HSSTheoryHSS原理VOCscollectasagasintheheadspaceabovetheliquidorsolidsample在液体或固体样品上,VOCs作为气体收集在顶空中Samplesneedtoheatfor~15-20minutestoreachequilibrium需将样品加热~15-20分钟,达到平衡EquilibriumoccurswhentherateofVOCsleavingthesampleisequaltotherateofVOCsreturningtothesample平衡发生于当VOCs离开样品与返回样品的速率相等时

VaporPhase蒸气相LiquidorSolidPhase液相或固体18DeterminingEquilibrationTimes确定平衡时间AREA面积19HSSSamplingHSS采样TheHeadspaceneedleisconcentricandhastwoopenings

顶空针头是同心的,有两个开口Sample

isdrawninfromthetopopening

样品从顶开口引入Nitrogen

isbubbledoutofthebottomopening

氮从底开口涌出20SensitivityTree

灵敏度树状图HighConcentration高浓度LowConcentration低浓度LowSensitivity低灵敏度HighSensitivity高灵敏度ER_HSS_PPT_StandardHSS_Tri-Bed_PPT_Standard(low低ppt)ER_HSS_PPB_StandardHSS_Loop_PPB_Standard(low低

ppb–high高ppt)ER_Air_Tri-Bed_PPB_StandardAir_Tri-Bed_PPB_Standard(low低

ppb–high高

ppt)Survey

速查HAPSITEER:>1ppmHAPSITESmartPlus:>10ppmER_Air_Tri-Bed_PPM_StandardAir_Tri-Bed_PPM_Standard(low低ppm–high高ppb)21HSSInternalStandardsHSS内部标准Thematrixoftheinternalstandardmustmatchthesamplematrix内部标准的基质必须与样品的基质匹配Liquidsamplesusealiquidinternalstandard液体样品使用液体的内部标准Gassamplesuseagasinternalstandard气体样品使用气体的内部标准TRISandBPFBaregasstandardsTRIS和BPFB是气体标准

ThesestandardswillnotbeautomaticallyinjectedintotheHAPSITEduringaHSSrun在HSS运行过程中,这些标准不自动注入HAPSITE中HSSinternalstandardsareliquidHSS内部标准是液体Standardsmustbemanuallyinjectedintoeachsamplevialusingasyringe必须用针管手动将标准注入至每个样瓶中22HSSInternalStandardsHSS内部标准Internalstandardsareusedas:内部标准用作为:Areferenceforquantitativemethods定量方法的参考Anaidtoestimateconcentrations帮助估算浓度4componentmix4成分的混合物(p/n071-748)Fluorobenzene氟苯

(250μg/mL微克/毫升)Chlorobenzene-d5

氯苯-d5

(250µg/mL微克/毫升)1,4-dichlorobenzene-d4

1,4-二氯苯-d4

(250µg/mL微克/毫升)Bromopentafluorobenzene

氟溴苯(BPFB)

(500µg/mL微克/毫升)23HSSInternalStandardAdditionConcentrationCalculation

HSS内部标准添加物浓度计算

V1C1=V2C2InitialVolumexInitialConc.=FinalVolumexFinalConc.0.010mLx250mg/mL(IS)=20mLx?

FinalConc.mg/mLFinalConc.=0.125mg/mL=0.125ppm=125ppbKeepthesameunitsonbothsidesoftheequation公式的两边保持相同的单位Internalstandardconcentrationwillvarybasedonsamplesize内部标准浓度基于样品大小而变更2424HSS内部标准添加物浓度计算

V1C1=V2C2

初始容积x初始浓度=最终容积x最终浓度

0.010毫升x250微克/毫升(IS)=20毫升x

?

最终浓度

微克/毫升

最终浓度=0.125微克/毫升=0.125ppm=125ppb公式的两边保持相同的单位内部标准浓度基于样品大小而变更25HSSInternalStandards

HSS内部标准FinalconcentrationsofvariousISadditions

各种IS添加物的最终浓度SampleConfigurationAddition10mLWater20mLWater5gSoil10gSoilLoopMethod(HAPSITESmartPlusonly)PPBmethod(HAPSITEERandSmartPlus)10µLof250µg/mLIS0.250µg/mL(250ppb)0.125µg/mL(125ppb)0.500µg/g(500ppb)0.250µg/g(250ppb)10µLof500µg/mLIS(BPFB)0.500µg/mL(500ppb)0.250µg/mL(250ppb)1.000µg/g(1ppm)0.500µg/g(500ppb)PPTmethod(HAPSITEERandSmartPlus)1.0µLof250µg/mLIS0.0250µg/mL(25ppb)0.0125µg/mL(12.5ppb)0.0500µg/g(50ppb)0.0250µg/g(25ppb)1.0µLof500µg/mLIS(BPFB)0.0500µg/mL(50ppb)0.0250µg/mL(25ppb)0.1000µg/g(100ppb)0.0500µg/g(50ppb)26HSS内部标准各种IS添加物的最终浓度样品配置添加物10毫升水20毫升水5克土壤10克土壤环方法(仅HAPSITESmartPlus)PPB方法

(HAPSITEER和SmartPlus)10微升的250微克/毫升IS0.250微克/毫升

(250ppb)0.125微克/毫升(125ppb)0.500微克/克(500ppb)0.250微克/克(250ppb)10微升的500微克/毫升IS(BPFB)0.500微克/毫升

(500ppb)0.250微克/毫升(250ppb)1.000微克/克(1ppm)0.500微克/克(500ppb)PPT方法

(HAPSITEER和SmartPlus)1.0微升的250微克/毫升IS0.0250微克/毫升

(25ppb)0.0125微克/毫升

(12.5ppb)0.0500微克/克(50ppb)0.0250微克/克(25ppb)1.0微升的500微克/毫升IS(BPFB)0.0500微克/毫升(50ppb)0.0250微克/毫升(25ppb)0.1000微克/克(100ppb)0.0500微克/克(50ppb)27PreparingBlank/Samples

准备空样/样品Ingeneral,HSSsamplesarepreparedasfollows:一般,HSS样品准备如下:Liquids液体Fillvials½full

注入样瓶½满

20mL20毫升Solids固体

Use10grams

用10克Donotblockneedleopening切勿阻塞针头的开口Inject10µLinternalstandardforPPB(orLoop)methods为PPB(或环)方法注入10微升内部标准Inject1µLinternalstandardforPPTmethods为PPT方法注入1微升内部标准28PreparingBlank/Samples

准备空样/样品PrepareablankusingVOC-freewaterandinternalstandard用无VOC的水和内部标准准备空样VerifiesthattheHeadspaceandtheHAPSITEER/SmartPlusareoperatingproperly证实顶空和HAPSITEER/SmartPlus的运行正常

Propergasflow气流量正确Acceptablepressure压强可接受Monitorscarryoverorcontamination监测残留或污染29PreparingtheBlank/Samples

准备空样/样品Add20mLofVOC-freewaterintothevial在样瓶中添加20毫升无VOC的水Cleanthe10µLglasssyringethreetimeswithmethanol用甲醇清洗10微升玻璃针管三次Allowsyringetocompletelyfillwithmethanol针管可完全充满甲醇Discardexcessmethanolintowastevial将过量的甲醇倾倒入废瓶中30Practicepropersyringetechniqueusingmethanol用甲醇实习正确的针管技术Drawthesyringeplungerbacktothe1µlmark将针管柱塞拉回至1微升标记处Insertthetipofthesyringeneedleintothemethanol将针头的针尖插入甲醇中Becarefulnottomovetheplunger注意不要移动柱塞Carefullydrawtheplungerbacktothe2µlmark小心地将柱塞拉回至2微升标记处Withdrawthesyringefromthevial从样瓶中撤回针管Becarefulnottomovetheplunger注意不要移动柱塞PreparingtheBlank/Samples-SyringeTechniques准备空样/样品-针管技术31PreparingtheBlank/Samples-SyringeTechniques准备空样/样品-针管技术Drawtheplungerbackuntilthereisa1µLplugofliquidbetweenthe1µLand2µLmark抽回柱塞直到有1微升液体在1微升与2微升标记之间Plungerwillbedrawnbackto~4mL柱塞被抽回至~4毫升

Injectthisliquidintoawastevial将此液体注入废瓶中Disregardsmallairpocketsthatmayappearneartheplunger不管柱塞附近是否出现小空气泡Repeatthissameprocedureforsamplepreparation为样品准备重复此同样顺序32InsertingBlankandPurgeVialintotheHSS

将空样和冲净样瓶插入HSS中OpenthetoplidontheHeadspace打开顶空的顶盖Lifttheneedleassembly提升针头组件Placethestandardblankintoawell

将标准空样置入槽中Placeanemptyvialintoanotherwell将空的样瓶放入另一个槽中ThisisthePurgeVial这是冲净瓶33InsertingBlankandPurgeVialintotheHSS

将空样和冲净样瓶插入HSS中Centertheneedleovertheseptumandgentlyinsertitintothevialforthestandardblank为标准空样对中隔膜上的针头,将它插入样瓶Needleguidescanbeusedtohelppositiontheneedle针头导向有助于针头定位Closethetoplid盖上顶盖

Allowtheblanktoheatfor15-20minutes让空样加热15-20分钟34RunningAnalyze

运行分析TouchRUNANALYZE

按运行分析Nitrogenfromtheheadspaceneedleandbubbleintothesample来自顶空针头的氮,泡状进入样品ThiswillpurgethesampletoreleaseVOCsdissolvedinthewater这将冲净样品,释放溶解在水中的VOCs35CollectingaSample

收集样品CollectingSampleForscreen收集样品用于窗口TheHeadspacewillautomaticallycollectasample顶空将自动收集样品

Noactionisrequiredfromtheuser用户无需动作SamplingisDonescreen采样完成窗口Samplecollectioniscomplete样品收集完成Again,noactionisrequiredfromtheuser同样,用户无需动作36GRAPHView

图形查看Compoundswillbedisplayedonthefrontpanel化合物将显示于面板上GRAPHisthedefaultview图形是默认查看Displaysthechromatogramduringtherun显示运行过程中的色谱图Displays:显示:CompoundName化合物名RetentionTime滞留时间TICTICMax37CMPDIDView

CMPDID查看

ThedatacanbeviewedasalistbytouchingCMPDIDduringarun在运行过程中,按CMPDID

可查看数据清单Displays:显示:CompoundName化合物名CASNumberCAS数RetentionTime滞留时间NetFit纯拟合38PurgeHeadspace

冲净顶空Apromptwillappeartopurgeattheendofeachrun每次运行终点,将出现冲净提示Topurge,inserttheHeadspaceneedleintothepurgevial为冲净,将顶空针头插入冲净瓶中Averagepurgetimeis2minutes平均冲净时间为2分钟Cleansresidualsamplefromtheneedle从针头中清除残余的样品TouchContinue39MethodFinished

方法完毕Whenthemethodandpurgearecomplete,METHODFINISHEDwillbedisplayed当方法和冲净完成时,将显示方法完毕字样40HSSBlankfromtheSmartPlus

来自SmartPlus的HSS空样

Chlorobenzene氯苯-d5(7:30)Fluorobenzene氟苯(2:50)1,4-Dichlorobenzene二氯苯-d4(14:30)Bromopentafluorobenzene氟溴苯(8:00+/-0:10)41HSSBlankfromtheER

来自ER的HSS空样Fluorobenzene氟苯(1:30)

Chlorobenzene氯苯-d5(3:35)1,4-Dichlorobenzene二氯苯-d4(6:45)Bromopentafluorobenzene氟溴苯(3:45+/-0:05)42Exercise:PreparingaHSSSample

练习:准备HSS样品Usea40mLvialtopreparethesample用40毫升样瓶准备样品Add20mLVOC-freewater添加20毫升无VOC水Inject1LHSSInternalStandard注入1微升HSS内部标准Inject1LSample注入1微升样品PlacethesampleintheHSSandallowtoequilibratefor20minutes将样品置入HSS,并让它平衡20分钟

RunMethod运行方法ER_HSS_Tri-Bed_PPB_QuantSelectandusetheQuanttabtoviewdata

选用Quant标签条查看数据43Worksheet:HSSBlank工作表:HSS空样44AccessingQuantitationReports

查访定量报告Double-clickontheIDUnknownsicon双击ID未知物图标

Theuserispromptedtoselectthemethodtype提示用户选方法类型SelectGC/MS选GC/MS

ClickOK单击OK45AccessingQuantitationReports

查访定量报告SelectHAPSITE选HAPSITEDouble-clickonthedesiredmethod双击所需的方法46AccessingQuantitationReports

查访定量报告ClickBrowsetoselectthedesiredDataFile单击浏览

选所需的数据文件Thepathwayforthedatafile:数据文件的途径:ClickStart单击

开始47QuantitationReport

定量报告CompoundsDetected检测的化合物RetentionTime滞留时间

Concentration浓度

微克/升(ppb)48AccessingQuantitationReports

查访定量报告IDUnknownswilllabelthepeakofeachchemicalfromthe

calibrationlibrarywitha“T”

ID未知物

将用“T”

标志来自校准库的每个化合物的峰49QuantitationReports

定量报告UsecautionwhenusingQuantitationreports

当用定量报告时,使用警示Thereportidentifiesandquantifiesonlythechemicalsthatarespecificallyreferencedinthecalibrationlibrary报告鉴别和定量仅对校准库中特定引用的化合物Thechromatogrammustbevisuallyinspectedforadditionalpeaksthatwerenotidentifiedinthereport必须视觉检查色谱图是否存在报告中未鉴别的附加峰50QuantitationReports

定量报告IDtheunidentifiedpeak(s)using:ID未鉴别峰用:AMDISSearchAMDIS搜索AutomaticNISTSearch自动NIST搜索ManualNISTSearch手动NIST搜索Estimatetheconcentration估算浓度5112.5ppb(25ifusingBPFB)

HSSConcentrationEstimates

ThisformulaisusedtoestimateconcentrationofchemicalsbasedontheinternalstandardsNOTE:Thiscalculationisforaconcentratormethodusinga1µL internalstandardinjectionMaxnormalizationvalueofnearestinternalstandardMaxnormalizationvalueofcompoundofinterestXApproximateConcentration

(+/-oneorderofmagnitude)MaxnormalizationTCE