HAPSITE頂空操作培訓(xùn)

HAPSITEER/SmartPlusTraining

HAPSITEER/SmartPlus培訓(xùn)HeadspaceSamplingSystem

頂空采樣系統(tǒng)2HSSModuleOutline

HSS模件概要HSSAssembly

HSS裝配HSSTheoryHSS原理HSSInternalStandards

HSS內(nèi)部標(biāo)準(zhǔn)PreparingBlanks/Samples準(zhǔn)備空樣/樣品RunningAnalyze運(yùn)行分析QuantitationReports定量報(bào)告ContaminationIssues污染問題3WhatistheHeadspaceSamplingSystem什么是頂空采樣系統(tǒng)HAPSITEaccessory

HAPSITE輔件Samplingsystemfor:采樣系統(tǒng)用于:Water水Soil土壤Liquids液體DetectsVOCs檢測VOCsQualitativemethods定性方法Quantitativemethods定量方法PPBtoPPTrangePPB至PPT量程4HSSAssemblyHSS裝配InsertachargedbatteryintotheHAPSITE將充足電的電池插入HAPSITEDisconnecttheHAPSITEpowersupplycord斷開HAPSITE的電源電纜連接5ConnectingtheY-CableforStationaryUse為臺式用法連接Y-電纜

Asthenameimplies,thecableformsaY正如其名,電纜呈Y形Joinedend

連接端Splitends

分叉端6ConnectingtheY-CableforStationaryUse為臺式用法連接Y-電纜ConnectthejoinedendtotheHAPSITEpowersupplycord

將連接端連接至HAPSITE的電源電纜NOTE:

Alignthedotsonthecablewiththedotsonthecord注:

對準(zhǔn)電纜上的點(diǎn)與電源線上的點(diǎn)7ConnectingtheY-CableforStationaryUse為臺式用法連接Y-電纜ConnectonesplitendofthecordtotheHAPSITE連接電纜的一個(gè)分叉端至HAPSITEConnecttheothersplitendtotheHeadspaceSamplingSystem連接另一個(gè)分叉端至頂空采樣系統(tǒng)NOTE:

Alignthedotsonthecablewiththedotsontheinstrumentstoproperlyconnect

注:

將電纜上的點(diǎn)與儀器上的點(diǎn)對準(zhǔn),直至妥善地連接上8TransferLine

傳輸線ProvidescommunicationbetweentheHAPSITEER/SmartPlusandtheHSS提供HAPSITEER/SmartPlus與HSS之間的通訊SampletravelsthroughthetransferlinetotheHAPSITEER/SmartPlus樣品經(jīng)過傳輸線傳送給HAPSITEER/SmartPlus

HAPSITEERTransferLine傳輸線HAPSITESmartPlusTransferLine傳輸線9TransferLine傳輸線Encompassedbyafoamsleeve外包泡沫套管Providesinsulation提供絕緣Reducespowerrequirements降低功率要求Directional方向性Multi-connectorendconnectstotheHAPSITEERUniversalInterface多接頭端連接至HAPSITEER的通用接口FortheHAPSITESmartPlus,thedirectionofthetransferlineislabeleddirectlyonitHAPSITESmartPlus的傳輸線方向直接標(biāo)注在它的上面10InsertingtheTransferLine插入傳輸線FortheHAPSITEER,plugtheendwiththesingleLEMO?

connectionintotheHSS對于HAPSITEER,將帶有單個(gè)LEMO?

接頭插入HSSAlignthereddots對準(zhǔn)紅點(diǎn)FortheHAPSITESmartPlus,plugthesidelabeledThisEndtoAccessoryintotheHSS對于HAPSITESmartPlus,將邊上標(biāo)志此端至附件端的一端插入HSSAlignthereddots對準(zhǔn)紅點(diǎn)11InsertingtheTransferLine插入傳輸線RemovetheprobefromtheHAPSITEER/SmartPlus從HAPSITEER/SmartPlus上卸下探頭ToattachthetransferlinetotheHAPSITEER連接傳輸線至HAPSITEERScrewtheUniversalBulkheadconnectionintoplace擰上通用的防水連接件Alignthereddots對準(zhǔn)紅點(diǎn)InserttheLEMO?connection插上LEMO?

接頭

ToattachthetransferlinetotheHAPSITESmartPlus連接傳輸線至HAPSITESmartPlus

Alignthereddots對準(zhǔn)紅點(diǎn)InserttheLEMO?connection插上LEMO?

接頭

HAPSITEERViewHAPSITEER視圖

12PortableHSSUse便攜式HSS的用法TheHSSisdesignedforportableuse

HSS設(shè)計(jì)于便攜式應(yīng)用Requiresabattery

需用電池OpenthefrontdooroftheHSS

打開HSS的前門Insertthebatteryintotheslot

將電池插入槽內(nèi)Thearrowonthebatterywillbefacingthebatteryreleasebutton電池上的箭頭指向電池釋放按鈕TheINFICONlabelwillbeinthelowerleft-handcorner

INFICON的標(biāo)簽位于左下角13PortableHSSUse便攜式HSS的用法Pushbatteryintoslotuntila“click”isheard將電池推入槽中,直到聽見“咔噠聲”Verifythatthebatteryissecurelyfastened證實(shí)電池已被牢固地固定住14NitrogenCanister

氮?dú)馄縄nsertthenitrogencanister插入氮?dú)馄?5TurningontheHSS

將HSS的電源onPressdownonthePOWERswitch按下電源開關(guān)ThePOWERswitchisatoggleswitch電源開關(guān)是扳鈕開關(guān)Oncepressed,itwillreturntoitsoriginalposition一旦按下,它將回到原位ThewordPOWERwillilluminate文字指示燈POWER亮

IftheHeadspaceispoweredbytheHAPSITEpowersupply,theRMTPOWER(RemotePower)willalsoilluminate如頂空使用HAPSITE的電源,RMTPOWER(遙控電源)也亮

Closethefrontdoor關(guān)上前門16PreparingAnalyze準(zhǔn)備分析TheHAPSITEER/SmartPluswillautomaticallybeginpreparingaHeadspacemethodHAPSITEER/SmartPlus將自動開始準(zhǔn)備頂空方法Allcomponentswillbeheatedtotheirsetpointtemperature全部組件將加熱至它們的設(shè)定溫度AutoTunewillberun自動調(diào)諧將運(yùn)行ConcentratorCleanoutwillberunifaconcentratorisinstalled如安裝濃縮器將運(yùn)行濃縮器清理17HSSTheoryHSS原理VOCscollectasagasintheheadspaceabovetheliquidorsolidsample在液體或固體樣品上,VOCs作為氣體收集在頂空中Samplesneedtoheatfor~15-20minutestoreachequilibrium需將樣品加熱~15-20分鐘,達(dá)到平衡EquilibriumoccurswhentherateofVOCsleavingthesampleisequaltotherateofVOCsreturningtothesample平衡發(fā)生于當(dāng)VOCs離開樣品與返回樣品的速率相等時(shí)

VaporPhase蒸氣相LiquidorSolidPhase液相或固體18DeterminingEquilibrationTimes確定平衡時(shí)間AREA面積19HSSSamplingHSS采樣TheHeadspaceneedleisconcentricandhastwoopenings

頂空針頭是同心的,有兩個(gè)開口Sample

isdrawninfromthetopopening

樣品從頂開口引入Nitrogen

isbubbledoutofthebottomopening

氮從底開口涌出20SensitivityTree

靈敏度樹狀圖HighConcentration高濃度LowConcentration低濃度LowSensitivity低靈敏度HighSensitivity高靈敏度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內(nèi)部標(biāo)準(zhǔn)Thematrixoftheinternalstandardmustmatchthesamplematrix內(nèi)部標(biāo)準(zhǔn)的基質(zhì)必須與樣品的基質(zhì)匹配Liquidsamplesusealiquidinternalstandard液體樣品使用液體的內(nèi)部標(biāo)準(zhǔn)Gassamplesuseagasinternalstandard氣體樣品使用氣體的內(nèi)部標(biāo)準(zhǔn)TRISandBPFBaregasstandardsTRIS和BPFB是氣體標(biāo)準(zhǔn)

ThesestandardswillnotbeautomaticallyinjectedintotheHAPSITEduringaHSSrun在HSS運(yùn)行過程中,這些標(biāo)準(zhǔn)不自動注入HAPSITE中HSSinternalstandardsareliquidHSS內(nèi)部標(biāo)準(zhǔn)是液體Standardsmustbemanuallyinjectedintoeachsamplevialusingasyringe必須用針管手動將標(biāo)準(zhǔn)注入至每個(gè)樣瓶中22HSSInternalStandardsHSS內(nèi)部標(biāo)準(zhǔn)Internalstandardsareusedas:內(nèi)部標(biāo)準(zhǔn)用作為:Areferenceforquantitativemethods定量方法的參考Anaidtoestimateconcentrations幫助估算濃度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內(nèi)部標(biāo)準(zhǔn)添加物濃度計(jì)算

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

FinalConc.mg/mLFinalConc.=0.125mg/mL=0.125ppm=125ppbKeepthesameunitsonbothsidesoftheequation公式的兩邊保持相同的單位Internalstandardconcentrationwillvarybasedonsamplesize內(nèi)部標(biāo)準(zhǔn)濃度基于樣品大小而變更2424HSS內(nèi)部標(biāo)準(zhǔn)添加物濃度計(jì)算

V1C1=V2C2

初始容積x初始濃度=最終容積x最終濃度

0.010毫升x250微克/毫升(IS)=20毫升x

?

最終濃度

微克/毫升

最終濃度=0.125微克/毫升=0.125ppm=125ppb公式的兩邊保持相同的單位內(nèi)部標(biāo)準(zhǔn)濃度基于樣品大小而變更25HSSInternalStandards

HSS內(nèi)部標(biāo)準(zhǔn)FinalconcentrationsofvariousISadditions

各種IS添加物的最終濃度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內(nèi)部標(biāo)準(zhǔn)各種IS添加物的最終濃度樣品配置添加物10毫升水20毫升水5克土壤10克土壤環(huán)方法(僅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

準(zhǔn)備空樣/樣品Ingeneral,HSSsamplesarepreparedasfollows:一般,HSS樣品準(zhǔn)備如下:Liquids液體Fillvials?full

注入樣瓶?滿

20mL20毫升Solids固體

Use10grams

用10克Donotblockneedleopening切勿阻塞針頭的開口Inject10μLinternalstandardforPPB(orLoop)methods為PPB(或環(huán))方法注入10微升內(nèi)部標(biāo)準(zhǔn)Inject1μLinternalstandardforPPTmethods為PPT方法注入1微升內(nèi)部標(biāo)準(zhǔn)28PreparingBlank/Samples

準(zhǔn)備空樣/樣品PrepareablankusingVOC-freewaterandinternalstandard用無VOC的水和內(nèi)部標(biāo)準(zhǔn)準(zhǔn)備空樣VerifiesthattheHeadspaceandtheHAPSITEER/SmartPlusareoperatingproperly證實(shí)頂空和HAPSITEER/SmartPlus的運(yùn)行正常

Propergasflow氣流量正確Acceptablepressure壓強(qiáng)可接受Monitorscarryoverorcontamination監(jiān)測殘留或污染29PreparingtheBlank/Samples

準(zhǔn)備空樣/樣品Add20mLofVOC-freewaterintothevial在樣瓶中添加20毫升無VOC的水Cleanthe10μLglasssyringethreetimeswithmethanol用甲醇清洗10微升玻璃針管三次Allowsyringetocompletelyfillwithmethanol針管可完全充滿甲醇Discardexcessmethanolintowastevial將過量的甲醇傾倒入廢瓶中30Practicepropersyringetechniqueusingmethanol用甲醇實(shí)習(xí)正確的針管技術(shù)Drawthesyringeplungerbacktothe1μlmark將針管柱塞拉回至1微升標(biāo)記處Insertthetipofthesyringeneedleintothemethanol將針頭的針尖插入甲醇中Becarefulnottomovetheplunger注意不要移動柱塞Carefullydrawtheplungerbacktothe2μlmark小心地將柱塞拉回至2微升標(biāo)記處Withdrawthesyringefromthevial從樣瓶中撤回針管Becarefulnottomovetheplunger注意不要移動柱塞PreparingtheBlank/Samples-SyringeTechniques準(zhǔn)備空樣/樣品-針管技術(shù)31PreparingtheBlank/Samples-SyringeTechniques準(zhǔn)備空樣/樣品-針管技術(shù)Drawtheplungerbackuntilthereisa1μLplugofliquidbetweenthe1μLand2μLmark抽回柱塞直到有1微升液體在1微升與2微升標(biāo)記之間Plungerwillbedrawnbackto~4mL柱塞被抽回至~4毫升

Injectthisliquidintoawastevial將此液體注入廢瓶中Disregardsmallairpocketsthatmayappearneartheplunger不管柱塞附近是否出現(xiàn)小空氣泡Repeatthissameprocedureforsamplepreparation為樣品準(zhǔn)備重復(fù)此同樣順序32InsertingBlankandPurgeVialintotheHSS

將空樣和沖凈樣瓶插入HSS中OpenthetoplidontheHeadspace打開頂空的頂蓋Lifttheneedleassembly提升針頭組件Placethestandardblankintoawell

將標(biāo)準(zhǔn)空樣置入槽中Placeanemptyvialintoanotherwell將空的樣瓶放入另一個(gè)槽中ThisisthePurgeVial這是沖凈瓶33InsertingBlankandPurgeVialintotheHSS

將空樣和沖凈樣瓶插入HSS中Centertheneedleovertheseptumandgentlyinsertitintothevialforthestandardblank為標(biāo)準(zhǔn)空樣對中隔膜上的針頭,將它插入樣瓶Needleguidescanbeusedtohelppositiontheneedle針頭導(dǎo)向有助于針頭定位Closethetoplid蓋上頂蓋

Allowtheblanktoheatfor15-20minutes讓空樣加熱15-20分鐘34RunningAnalyze

運(yùn)行分析TouchRUNANALYZE

按運(yùn)行分析Nitrogenfromtheheadspaceneedleandbubbleintothesample來自頂空針頭的氮,泡狀進(jìn)入樣品ThiswillpurgethesampletoreleaseVOCsdissolvedinthewater這將沖凈樣品,釋放溶解在水中的VOCs35CollectingaSample

收集樣品CollectingSampleForscreen收集樣品用于窗口TheHeadspacewillautomaticallycollectasample頂空將自動收集樣品

Noactionisrequiredfromtheuser用戶無需動作SamplingisDonescreen采樣完成窗口Samplecollectioniscomplete樣品收集完成Again,noactionisrequiredfromtheuser同樣,用戶無需動作36GRAPHView

圖形查看Compoundswillbedisplayedonthefrontpanel化合物將顯示于面板上GRAPHisthedefaultview圖形是默認(rèn)查看Displaysthechromatogramduringtherun顯示運(yùn)行過程中的色譜圖Displays:顯示:CompoundName化合物名RetentionTime滯留時(shí)間TICTICMax37CMPDIDView

CMPDID查看

ThedatacanbeviewedasalistbytouchingCMPDIDduringarun在運(yùn)行過程中,按CMPDID

可查看數(shù)據(jù)清單Displays:顯示:CompoundName化合物名CASNumberCAS數(shù)RetentionTime滯留時(shí)間NetFit純擬合38PurgeHeadspace

沖凈頂空Apromptwillappeartopurgeattheendofeachrun每次運(yùn)行終點(diǎn),將出現(xiàn)沖凈提示Topurge,inserttheHeadspaceneedleintothepurgevial為沖凈,將頂空針頭插入沖凈瓶中Averagepurgetimeis2minutes平均沖凈時(shí)間為2分鐘Cleansresidualsamplefromtheneedle從針頭中清除殘余的樣品TouchContinue39MethodFinished

方法完畢Whenthemethodandpurgearecomplete,METHODFINISHEDwillbedisplayed當(dāng)方法和沖凈完成時(shí),將顯示方法完畢字樣40HSSBlankfromtheSmartPlus

來自SmartPlus的HSS空樣

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

來自ER的HSS空樣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

練習(xí):準(zhǔn)備HSS樣品Usea40mLvialtopreparethesample用40毫升樣瓶準(zhǔn)備樣品Add20mLVOC-freewater添加20毫升無VOC水Inject1LHSSInternalStandard注入1微升HSS內(nèi)部標(biāo)準(zhǔn)Inject1LSample注入1微升樣品PlacethesampleintheHSSandallowtoequilibratefor20minutes將樣品置入HSS,并讓它平衡20分鐘

RunMethod運(yùn)行方法ER_HSS_Tri-Bed_PPB_QuantSelectandusetheQuanttabtoviewdata

選用Quant標(biāo)簽條查看數(shù)據(jù)43Worksheet:HSSBlank工作表:HSS空樣44AccessingQuantitationReports

查訪定量報(bào)告Double-clickontheIDUnknownsicon雙擊ID未知物圖標(biāo)

Theuserispromptedtoselectthemethodtype提示用戶選方法類型SelectGC/MS選GC/MS

ClickOK單擊OK45AccessingQuantitationReports

查訪定量報(bào)告SelectHAPSITE選HAPSITEDouble-clickonthedesiredmethod雙擊所需的方法46AccessingQuantitationReports

查訪定量報(bào)告ClickBrowsetoselectthedesiredDataFile單擊瀏覽

選所需的數(shù)據(jù)文件Thepathwayforthedatafile:數(shù)據(jù)文件的途徑:ClickStart單擊

開始47QuantitationReport

定量報(bào)告CompoundsDetected檢測的化合物RetentionTime滯留時(shí)間

Concentration濃度

微克/升(ppb)48AccessingQuantitationReports

查訪定量報(bào)告IDUnknownswilllabelthepeakofeachchemicalfromthe

calibrationlibrarywitha“T”

ID未知物

將用“T”

標(biāo)志來自校準(zhǔn)庫的每個(gè)化合物的峰49QuantitationReports

定量報(bào)告UsecautionwhenusingQuantitationreports

當(dāng)用定量報(bào)告時(shí),使用警示Thereportidentifiesandquantifiesonlythechemicalsthatarespecificallyreferencedinthecalibrationlibrary報(bào)告鑒別和定量僅對校準(zhǔn)庫中特定引用的化合物Thechromatogrammustbevisuallyinspectedforadditionalpeaksthatwerenotidentifiedinthereport必須視覺檢查色譜圖是否存在報(bào)告中未鑒別的附加峰50QuantitationReports

定量報(bào)告IDtheunidentifiedpeak(s)using:ID未鑒別峰用:AMDISSearchAMDIS搜索AutomaticNISTSearch自動NIST搜索ManualNISTSearch手動NIST搜索Estimatetheconcentration估算濃度5112.5ppb(25ifusingBPFB)

HSSConcentrationEstimates

ThisformulaisusedtoestimateconcentrationofchemicalsbasedontheinternalstandardsNOTE:Thiscalculationisforaconcentratormethodusinga1μL internalstandardinjectionMaxnormalizationvalueofnearestinternalstandardMaxnormalizationvalueofcompoundofinterestXApproximateConcentration

(+/-oneorderofmagnitude)MaxnormalizationTCE