1、nnai&ntTrhnninnirkQii-gvvwHW«ww*j|aiwAgilent7500aICP-MS現場培訓教材安捷倫科技化學分析儀器部7500aICP-MS現場培訓教材培訓目的:根本了解7500aICP-MS硬件操作.掌握化學工作站的開機,關機,參數設定,學會數據采集,全定量分析的根本操作培訓準備：1、儀器設備：Agilent7500aICP-MS?Babington高鹽霧化器.2、氣體準備：?«備三瓶高純Ar氣,接上減壓閥后,將三氣瓶并聯后輸出到7500aICP-MS的Ar氣的進氣口./或用液Ar罐.要求純度為99.9995%?俞出壓力為0.7Mpa&

2、#177;3.5%Babington高鹽霧化器.3、循環水：?循環水的要求為：Flow=5L/Min.;溫度：15-20C;壓力：230-350Kpa3351PSI神環水中參加一定量IPA,預防生菌.4、排風：密求排風量為：57.5m3/min4.78.1m/s.Agilent7500Series7500aICP-MS化學工作站根本操作步驟：、開機:1、開pc顯示器、打印機.2、開PC主機.(password:3000hanover)3、開ICP-MS7500a電源開關.(儀器前面的電源開關)4、雙擊桌面的“ICP-MSTop圖標進入工作站,如下列圖所示:IIIOI日一nu*|I>|-r

3、AlPII.：1、笳rCALFJ5、點擊“ICP-MSTop畫面的“ICP-MSInstrumentcontrol圖標進入下列圖所示的儀器控制畫面.點擊“Vacuum菜單,選擇“VACUUMON進行抽真空程序,儀器由Shutdown-Standby轉換.litfftuii.c.七二：竄vi-alii5"土JGG網3*可以點擊“Meters圖標,進入如下列圖所示的畫面,選中真空的顯示選項進行壓力監測.最多可選5項IF/BKPressure-接口及背壓閥壓力.AnalyzerPressure-分析器壓力.TMP一分子渦輪泵.*轉換的時間較長,一般30-60Min左右.Th目yIW<

4、&i*hT*T>!a&iiI48il-IrMTwpLEHhdMiftT«mp&<：L5i/ET«nrui*ur»ILIiriflaiiiin|nrr4uiT.rcimcipchfmiiaiifi1'j-IJi罡機旦IT口*0冷趾I%勒一如"iR:13Cjtc.IHcteIFF»：>一OrtJ4fSMPlAkeW&Br/&eM四冏./iF海I口二krLlffZjMCPririh*nhirthcmm;*6、儀器狀態轉換為“STANDBY狀態后.開氣Babington高鹽霧化器0.7M

5、pa,循環水、排風.樣品管必須放入DIW中,假設連有內標管,亦放入DIW中.點擊下列圖所示的點火圖標進行點火,儀器由Standby-Analyst轉換.*檢查確認蠕動泵的樣品及排液管工作正常.卡上蠕動泵管,并調整流速.兩圈廢液管和內標管,一圈半樣品管.-排液平滑.氣體及液體排列均勻；-檢查儲廢液罐液位.*可以點擊“Meters圖標,選中氣體、功率、霧化器溫度的顯示選項進行監測.最多可選5項gMbwt1|4tCP-MfiTw-C1HB：曹1口BbrtgJwWt一畫PPMWrit.W臥工口LClWFM*假設停機在“Standby模式,開機只須1、6步二、調諧：1、點火后,30Min預熱儀器,點擊I

6、CP-MSTop畫面的“Tuneffi標進入下列圖所示的調諧畫面.rHKfcr-sjmflnl-lirpOrttwrhHtrtAnflJyM«l+in'rJ<%fliquHPH-iH=TfhJmblfllp珂金1、i冒T&#白二Qw蝦3/%?巾內屋中步戶外4"VFiCHHM'llLMETHCIlDFICiaifetation|rFFAlJLTXC：VrFC：HFMV1lCABIR1|三|Sequence|nFFAUIT.RCZZICFCHEflt與FCUFh|Intgi4linTinnerQlSanolrigRonw#0L一一-JL1_nrMq

7、PiAF-actorpaiATiiM.er.HAAsatun»>P/AFacx-crbeTaraac-4uhifigddt-a.pD-LExini.r步生xtIH通與10電幽獷JOjLSC1ft.|T日口：SJL&I：=Itp-MGF虎L方.0口咽MP-MXO.暮耳冷£>工.必0,甘03L.7調諧畫面:2、將樣品管放入10ppb調諧液中.假設連有內標管,將內標管亦放入DIW中.點擊"靈敏度圖標,進入靈敏度調諧畫面.如下列圖所示,點擊"Acq.Parameters"菜單輸入采集的質量數為7、89、205,156/140CeO/

8、Ce氧化物,70/140Ce2+/Ce雙電荷,并選中“Plot,“Channel號,點擊“OK按鈕.點擊“Start按鈕啟動采集.點擊“Stop按鈕停止采集.確認靈敏度、氧化物、雙電荷是否到達表一的要求.否那么調整參數.哂H出.1洞I口.(hq(J-口LJ.J3錨,也#麟Hrf,J'»<|OCFAULJMC：UPCMI.MHHWLTiIOUSH.,-F-.*(DErAOLTCCJPC-HEMllTaEaUCNCEk互r扇面尸回四雨兩闡|口1.|如詬*r-yrrurnriuitH7Kn-ns-IeilhlelEarBrar-a-Jr-JrBrar-ryrrr/JrJr-a

9、rFkk筍LLLLLLF帕0|TestItemspec.MassAxisLi(7)如.1amuY(89)如.1amuTl(205)3.1amuMassResolution(at10%)0.65-0.8amuSensitivityLi:>6400(0.1sec.,10ppb)Y:>16000Tl:>600Oxide(CeO/Ce)<1.0%DoublyCharged(Ce2+/Ce)<3.0%點擊“Start按鈕啟動采集.點擊3、點擊“峰型/質量軸調諧圖標,進入峰型/質量軸調諧畫面.0ILM.ESMTrfH0,rM：+rfi凡.|M>_f*fcr-3iUMBA

10、mJi,1!-«.jM'J-lfT-«L'HA*Hdr>H->.|入=HNi1JUT1梟“Stop按鈕停止采集.確認峰型/質量軸是否到達表一的要求.否那么調整參數*一般左邊缺省的顯示項調中對大多數用戶足夠.如要添加,如下列圖所示,點擊“Acq.Parameters菜單,進行添加.|Hl2t3f田*'|Bicrmi;td>_citurQkiCIjd5g包四里翁望D7仁隼仁1味IIIlMKU!：；lC3UIN4：l|»EIAJULT.：中6-11必0口俯63EFrlljjijlE三三三三cccccCCCCCCGr-c匚口留西胃

11、口昌nDlliWMd!LfeVPAiM¥>*ldHhI1I：-：|調諧參數及其含義:roi<icari一廿單nypwMjuiiu串EiumrujiLii'u%?hlrtfnuir口廿RFR?w&r1200Waris1200ct148WotUNcfmalyfix»d3t1300WatlaSarripeDepIFi6mn4to9mmSenstrwly,be"/areofOxHesand2+.Torch-H4M>4»>AutoAdjiuEtformaxsens-rtivirrTorch-VAAutoAdjustforme

12、wBentitiwiily.Csrri電rGab1.2L'mh1.0to1.4UrrmSriBHivity,bewareofOtidssand2*.MakeijpGss,口NoneApplic-atianiSpecificOplion6型AwW匕匕修iffrti«dAvitiLtoiffir舊dAv3ihblsiffiftwdFeril-FUrrp0.1rpGNoneSamplefIcnrale.S/CTemparcNoneStabiliry«Dfplasms.Extraction1-150iVerts-200to-100VolteAdjustforrrxw&

13、;«n6irtiviiyBExtrsetl'On2-70Vols-11Olo-40VeitsAdjis：1foritlmn心田wily二白nzwl1.3-1OOVc4te-130to-40VottsAdjjsIfeemaxbgthsliviiLy日n二鑰2“Vog+Otp+15Adj*tforrrewsnrfivityOmegaBios35VotB-45to-20Adjustforfkatithponsecurve.Onrega(+)+&Veils0to+20VcitsAdjustfcrffkatresponsecurve.Onnega?-)-5Volte-20toO

14、VoteAdjustfcrfIsitresponsecurveeQPFocu*3Volts0to*1OVottsAdjuslformew2n雨vily.AMJ口目inU&evaluefromSTDTuneFieAsrenuredResokibonhighmasses.AMJOffsetL-teevalluefromSTDTuneFieAsrequred1%-EiOlLJliGnb1mas-Ees.AxisGainvalu#fromSTDTun»FieAersqurvdcalibrationhih>mastie4AxisOffsetLteevaluefromSTDTuns

15、FieAsrquiredMasscaibrallmallmsfis.es.HsAbBisib-20Vote-4OtoOVeilsAdjustformaxseniBrtiv!iit>,QPBias+2VoIlBoto+eVehsAdjustifthetopofpeaklooikssplh.CtecrimrilcfUfc.wHiwfiromSTDTuneFi*5>.11F4*dLieaAmpI0r號檔七Ifcmienoise.FlilseHVUevaliusfromSTDTuneFie1200to3500VotsIncreaseSensitiviity.AnalogHV隼Mu靜from

16、iSTDTuneFi?700to20DOVoltsExlwid»ddynorriicraog#.、P/AFactor調諧:將樣品管插入PAfactor調諧溶液(Sc(45),In(115),Bi(209)100ppb一內標稀釋得到).在靈敏度調諧窗口觀察Sc(45),In(115),Bi(209)元素靈敏度,待穩定后,點擊“Tune菜單,選擇“P/AFactor在下列圖所示的“P/AFactorTuning窗口添加Li(6)、Sc(45)、Ge(72)、Y(89)、In(115)、Tb(159)、Bi(209)3Xj總¥3季型宜Z3Z3再京直3AlItV三J三,.口DrrA

17、OLrcmcpckemiiWCbJMljveHLilUTBCCCPCIlt.M'LliWALim兀系.“rIh|nrmTH5U匚皆1仁門£1!1"1丁匕口5點擊“Run按鈕,儀器將自動得到P/AFactorTuning報告.四：試劑準備及方法建立試劑準備：或EnvironmentalCalibration及10ppmAg,As,Se,Cd,Pb,Ni,校準標液及PAFactor調諧溶液:?AgilentCalibrationVerificationStandard(Part#5183-4682)Standard(Part#5183-4688,1000ppmFe,K,

18、Ca,Na,MgCu,Zn等.)- HNO3.- DI水.- AgilentTuning溶液：10ppbLi,Co,Y,Ce,Tl.?PAFactor溶液：將Part#5183-4680,10ug/mLLi6,Sc,Ge,Y,In,Tb,Bi)稀釋100倍,得到PAfactorTune溶液(100ppbLi6,Sc,Ge,Y,In,Tb,Bi).標液：?用1%HNO3稀釋CalibrationVerificationStandard(Part#5183-4682)或EnvironmentalCalibrationStandard(Part#5183-4688,1000ppmFe,K,Ca,Na

19、,Mg和10ppmAg,As,Se,Cd,Pb,Ni,Cu,Zn等)至U1000和500倍,得至USTD1和STD2.?準備1ug/L和2ug/LHg在1%HNO3中,作為STD3和STD4.?空白1%HNO3為STD0O?準備1ug/mL內標(ISTD)溶液.稀釋(Part#5183-4680,10ug/mLLi6,Sc,Ge,Y,In,Tb,Bi)得到.?準備tapwater于1%HNO3中.方法建立:1、在"ICP-MSTop畫面,點擊“Methods菜單,選中"Editentiremethod.2、進入“EditMethod"窗口LS!-*3E*EbIup

20、/DttAULIInFFAUIT.CCZ：VFHFhA1ACABIRArwthnxfInFFAiJIT.MrJCFCHFMlliMFTHqiDg|ICP-mTT色LJCJi.I_|70小1_3.一|川尸：tHtiFEHHtaQjlr匚Ehfl-MjAnalvBMMflHnndvXtjhheCHmi-ihH叫purEinTolfflp迪/后GT白La,J財%*晚n?3、如上圖所示,選中除DataAnalysis外選項,點擊“OK按鈕,進入以下回面.口山Jbjg45一157|IgP-Mk5cA叫E|也nBQ港/比.馬備0國4、在“MethodComments中輸入方法注解.如“ThisisEPA2

21、00.8method.,選中“DataAcquisition",點擊“OK按鈕,進入以下畫面.5、 如下列圖所示,在“SelectSampleType畫面,將CalStd、QuantBLK>Sample保留在右邊框中.點擊“OK按鈕.國1融Q直11,.百.卜蝦始產蛆aj?MathodnFFAUIT.M匯-CZFCHF萬TH<?nF*Caifcradon|dFFAUIT.C-C*IICIPCZHFfllM：1Ali1曰*Seq«eino&|nFFAUIT.S-U即CPCHF,£FQUf+BUS*SB與市"R假設®0獷IIicp

22、-m&1XAI一口:竄.,I7口W£一Ir：l四16404dQ0H3g必6、 在"interferenceequation窗口,選中EPA200_8,如下列圖所示,干擾方程列于窗口中.點擊“OK按鈕itp-ewirnp-furhiiRAI-orr/nrfaijufjm/nrjjmmt.c參照"ApplicationHandbook中的應用.7、在“AcquisitionMode!畫面,選中“Spectrum選項,點擊“OK按鈕8、在“PeakPattern窗口,選中"FullQuant(3),然后點擊“PeriodicTabe進入下一畫面.Na,

23、Mg,K,Ca,Fe,V,Cr,9、點擊“ClearAll按鈕,再選中要分析的元素及ISTD元素,如:As,Cu,Ni,Zn,Hg,Pb,Cd等及內標元素ISTDSc,Ge,In,Bi.10、擊“OK按鈕,進入下一畫面.xjMasses.口叫|川,2040008010CPSeteueiyMassIntegrationtimeperPoint：|0B30sec120140ISO18020CPeriodicTableMassScaleArquisitionTimeAcquisition;52X)6000secRepetitinn：,TotalTime：156seeOKCancelHelpDetec

24、tor;(AutoCheckParamctfirEnterIntegrationTimeseelMassHem.perPuinlpgrMas古Deteutur57Fe59Co60Ni63Cu66Zn72Ge75As77網62Se105(Cd)107Aq108(Cd)111Cd115In118(In)202Hg205Tl206(Ph)207(Pb)20KPh209Bi3000)(msec303030卸303003003030300303003030303030ra-r,(w'"oooooogg9g99oo.uo.oo.oaoooooooooooo.&o,o'o&

25、#39;,6o,0s60,OSOOSpectrumAcquisitionParameters11、選中“SeteveryMass,在“Repetition窗口輸入“3或“2.然后在“IntegrationTimesec窗七,設定為0.3sec;Se,Cd,Hg-2sec;As-1Sec.NoError12、點擊“CheckParamete股鈕,假設error,那么檢查參數.點擊“OK按鈕,進入下一"PeristalticPumpProgram®面.13、在“PeristalticPumpProgram'窗口,設定uptakespeed:0.3rps;uptaketi

26、mea008c1占擊-一二OK按鈕,進入下一畫面.LinkedCalibrationHiewasupdated.AieyousureUiattiieupdatedflicnameissavedtothemethod?16、點擊“Yes；方法設定完畢.采集數據：1、將內標ISTD管放入1ug/mLISTD溶液中,樣品管放入1%HNO3溶液中.在“Tuning窗口檢查ISTD元素(Ge,In,Bietc)RSD.應小于5%.2、在“ICPMSTop'畫面,點擊“AcquireData菜單,選中“MainPanel,進入下畫面.Fl.4y口匚：*-a3、點擊AquireData'菜單

27、,選中"AquireData選項,進入下一畫面.4、將樣品管放入STD3(1ug/LHg),輸入文件名,(STD3.D,路徑為C:ICPCHEMDATA),OperatorName(User),DilutionFactor(1.00),樣品名(Hg1ppb).點擊"Acquire：進入下一畫面.5、當采集完成后,點擊“Tabulate/Mass",檢查ISTD元素(Ge,Sc,In,Bi)RSD,應小于5%.6、重復35采集完其它STD.當采集完成后,點擊“Tabulate/Mass,檢查ISTD元素(Ge,Sc,In,Bi),RSD應小于5%.7、 重復3-5采

28、集完樣品,如Tapwater在1%HNO3中,文件名為“waterl.D."8、 重復3-5采集完空白,如1%HNO3或DIW,文件名為“CK1.D'.全定量數據分析:1、點擊“DataAnalysis菜單,選擇“MainPanel.進入分析畫面,點擊“Calibrate菜單,選擇“EditCalibrationSetting一進入設定畫面.匚41匕lAiaiEtaLslBMl匚MlA1MaMnlh£ndCl-biMiiDfiTKte:i-pb.rhI-EHwtik匚ai>cJutuirAoihsri-3abi“UW|f1/iS-D-SOl：JM*»

29、E4r»l皿口n>TUdmVI?|Prwii"ibMkj,S-lrtpe赤*,u的PM仆FMUSTDW>i“WM44>iCOibC-3Aj19I;,ivdafd|DuMrYMW|CmphD«i*l|OFF©rtin11itinOFFftmn.0/1nmUlFFndinB<|/lnctLtriDFF0mn«O/I口mnnrnncmnVQ/I,n所口1呃v0,才iijonnfwrimnn口mnmnn日由口iann5DOOioan口n門門門卻！？加加mIHQngG,出I-EL°,J«m1-'.|7F

30、MJ】h.jjr*£d"1-g*k叫I&8JS3L*：J42、如上圖所示,選中“New進入下一畫面如上圖所示,選中“ExternalCalibration,“LoadMassesfromCurrentAcq.Params點擊“OK按鈕,選擇"Yes進入下一畫面.3、右鍵點擊所有帶()元素,如77(As),206(Pb),點擊“DeleteElementsHS-TDWuilhiUdHl1L2JLi一orr口3口*_»orrO-DOOira口尸尸"EIJ.nOFF門3門.OFFODOD.1.口卜卜UI.SJUDFF口DOD一orr"

31、;EW1JFRUIKII1!“一DFF口rannI-.一»aaIldhlTW.1feiWlib111iriVrihl第diHVrihilbaiiwdhii1IPll<T口*姓2田七S-=o0Kaad:H2"Jdkac-Jj,IfitIQerM!電l/通qgi.w.j皿7：.34、點擊“ConfigureAnalyte/ISTD按鈕,進入下一畫面,將45,72,115,209內標元素加到右邊區域,點擊OK按鈕.16司WeEFMv'hodtI1/iftri-SDi叱I9-I-|3口:|3北|睫0|Ilk-Edh.硬M|"7畔.t心IV.4L4E5a50z

32、ir口faIIF'r-THLiBBalI-Er.ilaiiuvn-vlt.lllFI.iiunC-al?!-mkH-iTlm="pEwt-mal,匚kbimktnC-al-bi-ailcn-Tnl«:f|"PiAr'ikCarW.AuhliWilrA-'BT*U»IImiiiImilIbMBIILIM|«i-liidiiiiiMiiy|Gh+l,i口.I.|T兒3屏1._45911«1»DiriI-日小心CX4兮3bti-B*-riS/MFI*,*|Filc-|pmHi=,L>rv>miN

33、GiidiphDn.¥¥Ife<ArwlifcWp-tiHU'"ICJpi.b.I|.*j,.IW3e«ibEe-IV111工9liJBU|VLr5、如下列圖所示,選擇曲線：Y=aX+b;選擇濃度單位:輸入元素濃度：K,Ca,Na.Mg,Fe-1000/2000ppbPPb*注意:Sc,Ge,In,Bi行,*由于Hg在STD1andSTD2無濃度,202Hg;Hg-1/2ppb所有Level在“Level2ISTD下方選擇適宜的內標；;其他元素為10/20ppb;.和“Level3列為blank,輸入“一,在“Level4和“Level5輸

34、入其濃度.IU一一“!不£rllHT"!0Hli仁：.工亡口匚KT'、tA1昨11事HMgME：匚口皿口|沁"！T臥ir:ExlvncalCahb'o'iion卜lEJiodCLbiAilwTtab:|rDIahiLEarvc.匚jbirBcJInvIWcitahiinoM«rt*wd|1ZOTZiMAdiceFIIda«VIS|Lim-s-Tabic于二7111*11J1HFUI二三三£工,FJn5JiB厘2f-ipiWDi3d-a-ri-AdX-Z?Z?Z7-WWiMj£hlMiniMofffco

35、oooFTomuOFFOOOODFr0JDQORFFQQWUFFU.WUrffnnnnOFFO.CPOOdffOFFOOMH二iriiHiir:IblbL靠.MM士士ClMJiOOCImac10OTOIO.QOIXMJ1UUUnrwiinnnuuuulO.OunKmioonaftM10.00DOi?i口口口0(MOIO.iXiDenID.DOas>：>J0.«：'2.口口M.00Am-#r一ar在1Iti1!,)-二Fipl*7H1d小fI仃門nrr口卜卜orrI3hhorrOFRisEi口"J'lTIUODOD43IIIIDtwoa3口llub

36、ll:I5TD1-FikISTDCnnc寫TO"monVPSLiff-VCl1L0,UCl3Levoq7Lcvol411dCiEOICOOIE口1ECi1i：n：N11.DO£i1DCMJIE口1.4X1口1.31：31i15itmiOQO1E.mn11Bliuuuipqfji-mo1.IMU1ML11&DQ<ciwn«n*Eb«pM«TrtlvmsnA<r叢小卜一今"I匚口曰IgwjAciEasyKT.|TINFL臨7口6、如下列圖所示,點擊“StandardFile按鈕,數據.點擊Level1,選中STD0.d

37、(STDblank),依次點擊Level2-5,選中STD1.d-STD4.D點擊“OK按鈕,進入下一畫面.點級“Clear按鈕,依次選中std0-std4路徑為.,路徑為.此E-ahbiaiieriEnL看mlEaEb4aiH>-iMethodEdit匚1/心也日的-匚廣,工匚1>«1,1匚小工彝,.1：咻士|110現匚U-5bb!aiic«Tfcfc:JEFaZCiDSMetfcdM-we口nkiiiio*VISBkw-'ik.Cohc-.T日Staild-ard*Fife$ISumnwiFIOraph0(：1口ii9hy3C:iCPCMEMMMSA

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