Bruker布魯克核磁共振儀器上機(jī)操作規(guī)程完整

核磁上機(jī)操作設(shè)置導(dǎo)向打開氣源，調(diào)節(jié)到0.5Pa的輸出壓力。常溫下可以用壓縮空氣，變溫實(shí)驗(yàn)室要使用高純氮。依次按下BSM流子上的|ockOn-Off卜［LiftOn-Off］按鈕啟動(dòng)程序;將里面的樣品彈出，換上要做的樣品。按下BSM流子上的|LiftOn-Off］按鈕啟動(dòng)程序;確定樣品已經(jīng)下去之后（“down"顯示綠色）點(diǎn)選主菜單SpectrometerDataAcquisitionGuide打開實(shí)驗(yàn)設(shè)置向?qū)А?、新建文件：點(diǎn)擊NewExperiment;或輸入命令"new/",得到如下圖：【NAME文件名；【EXPNQ試驗(yàn)號(hào)（一般1411;13C-21;其他雜核--31）;【PROCNO處理號(hào)；【USER:老師名；[Solvent]：選擇要進(jìn)行試驗(yàn)的樣品所用的笊代試劑；[Experiment]選擇所需做核磁譜的類型（建議打開已知的文件夾，在此基礎(chǔ)上新建，此時(shí)新建文件的實(shí)驗(yàn)設(shè)置參數(shù)與已知文件夾相同）。2、查看通道：點(diǎn)擊FrequencyRouting；或輸入命令"edasp”，確認(rèn)選擇實(shí)驗(yàn)核種及連線。注意：只有19F事可能需要改動(dòng)連線，其他只需要看，而不需要改動(dòng)。3、鎖場(chǎng)：點(diǎn)擊Lock,選擇需要鎖場(chǎng)的笊代試劑；或者直接輸入“l(fā)ock_笊代試劑簡(jiǎn)稱（如lockh2o）”。4、查看溫度：只有在變溫實(shí)驗(yàn)時(shí)才需要用到。5、調(diào)諧：點(diǎn)擊ProbeMatch;或者輸入“atma"（自動(dòng)調(diào)諧），或者"atmmi'（手動(dòng)調(diào)諧）。6、SampleRotation:依需求決定樣品，是否需要旋轉(zhuǎn)及轉(zhuǎn)速設(shè)置。一般液體轉(zhuǎn)速為20Hz,現(xiàn)在大多數(shù)樣品不提倡旋轉(zhuǎn)。7、勻場(chǎng)：點(diǎn)擊shim圖標(biāo)或者輸入shim命令，得到如下圖：|Shiwiig-top^hi*guiOptions0Editauto-shimdefinition("tune")fileOAuto-shimaccording"tune"fileOAuto-shimaccording"tune"fileforcurrentprobeOManualshimusing"soft"shimkeyboardCManualshimusing"hard"sNimkeyboard(')Gradientshimming「ramiinmneiine，予?■TopShirriJ，r，nl，rrl，nr，enIQK][G-III幽之后可以選擇勻場(chǎng)方式，如Gradientshimming、Topshim。另外也可以直接輸入“topshim”（三維勻場(chǎng)），or“gradshim”（Z方向梯度勻場(chǎng)）而直接進(jìn)入勻場(chǎng)，不會(huì)出現(xiàn)以上對(duì)話框。8、查看參數(shù)：點(diǎn)擊Acquisitionpars;或者直接輸入命令“eda”。得到如下圖:niiejin-songwei-110704-1#11E:oiejiinSpectrumProcPar?AcquParsTttlePuiseProgPeaksintegralsSampleStructureF2c11S?因法一V#4Installedprobe'notdefinedTWidthTWidthSW[ppm]205847SWH[Hz]6172.839AQ(s]2.6542580FIDRES[HZ]0.188380FW[HZ]7716.05SpectralwidthSpectralwidtnAcquisitiontimeFidresolutionFilterwidthWidthReceiverNucleusDurationsPowerProgramProbeListsWo&tJieLockAutomationMiscellaneoususerRouting▼ExperimentPULPROGAQ_modIDNSDSTDOzgsoqseq|E]CurrentpulseprogramAcquisitionmcdeSizeoffidNumljerofsewnsNumberofdummyscansLoopcountfor'tdO'32766l&21▼widirriSW[ppm]SWH[Hz]AQ[s]FIDRES[HZ]FW[Hz]20,5847SpectralwidthSpectralwthAcquisitiontimeFidresolutionFilterwiath61728392￡5425800.18B3607T1605▼ReceiverRGDW印5]4ReceivergainDwelltime81,000DWOV網(wǎng)DECIMai.aao1OversamplingdwelltimeDecimationrateofdigitalfilterTExperimentPULPROGzgso[..][E]CurrentpulseprogramAQinodqseqAcquisitionmodeTD32768SizeoffidNS16NumberofscansDS2NumberofdummyscansTDO1Loopcountfor'tdO1

▼ReceiverRG4ReceivergainDW||JS]81,000DwelltimeDWOY[ps|81ODDOversamplingdwelltimeDECIM1DecimationrateofdigitalfilterDSPFIRM5向p（stand日E）7DSPfirmwarefilterDIGTYF#6日it（digiti工已「nminstallEd!）*DigitizertypeDIGMODanalogvDigitizationmodeDR16DigitizerresolutionDDR0DigitaldigitizerresolutionDE[psi115.71P「巳一scandelayHPPRGNnormal7PreamplifiergainPRGAINhighVHighpowerpreamplifiergainDQDMODEaddVDigitalquaddetectionmodePH_ret[degree]0.000Re匚elverphasecorrectionOVEPFLWIgnoreAccumulationoverflowcheckingFRQLO3N0OOseivefrequencyshiftreduction▼Nucleus1NUC1offEdit.Observenucleus□1[HZ]515757Transmitterfrequencyoffset□1P[ppm]17.199TransmitterfrequencyoffsetSFO1[MHZ]2998751576TransmitterfrequencyBF1[MHZ]2998700000Basictransmitterfrequency通常需要確認(rèn)的有圖譜的中心點(diǎn)（O1P.O2P、圖譜寬度（SW掃描次數(shù)（NS,依使用者樣品特性而有所調(diào)整。其余參數(shù)不需要輕易改動(dòng)。PULPRQG常規(guī)選擇zg30;13C選主舉zgpg30（pg：去耦）；需要壓制溶劑峰時(shí)選擇zgpr；定量碳譜選擇zgig或者zgig30AQ-mod除了31P和19F（范圍較寬）選擇qsim,其余都是DQDNS掃描次數(shù)（與樣品濃度、信號(hào)強(qiáng)度等相關(guān)）。DS空掃次數(shù)（查看PULSEPRQB看有沒有具體要求，沒有做過的，都要查看一下，有的還對(duì)NS有要求）O1P需要壓制溶劑峰時(shí)，在此輸入溶劑峰的位置。9、讀取90°脈沖參數(shù)：點(diǎn)擊ProsolPars;或者直接輸入“getprosol點(diǎn)擊時(shí)反應(yīng)較慢，建議直接輸命令計(jì)算增益：點(diǎn)擊ReceiveGain；或者直接輸入“rga”。開始實(shí)驗(yàn)：點(diǎn)擊go或者直接輸入命令“zg”。但是對(duì)于“go”和“zg”,二者還是有很大區(qū)別的。二者對(duì)于所給條件下的第一次試驗(yàn)來說是沒有區(qū)別的。但是當(dāng)做完第一次后再次進(jìn)行這種操作的時(shí)候，“go”所產(chǎn)生的結(jié)果是得到的是兩次試驗(yàn)疊加的結(jié)果；而“zg”所產(chǎn)生的結(jié)果是重新掃描產(chǎn)生的結(jié)果，兩個(gè)結(jié)果不會(huì)出現(xiàn)疊加的情況。采集數(shù)據(jù)過程中的各種操作命令：“tr”保存已采集的數(shù)據(jù)而原先設(shè)定所要采集數(shù)據(jù)的計(jì)劃繼續(xù)進(jìn)行；“halt”保存已采集的數(shù)據(jù)而原先設(shè)定所要采集數(shù)據(jù)的計(jì)劃中止。“stop”直接從采集數(shù)據(jù)的狀態(tài)中退出來而不保存已采集的數(shù)據(jù)。進(jìn)入圖譜處理：直接輸入“efp；apk；abs"（分別是傅里葉變換及相位轉(zhuǎn)換處理、自動(dòng)相位校正、自動(dòng)?；€）回車，進(jìn)入處理界面進(jìn)行圖譜詳細(xì)處理。其他常見應(yīng)用：13C-NMR寬帶去耦，參數(shù)設(shè)置如下：

□B!%Er心。TflPSPII2Avn師阿2gAdainiET就盯□B!FileEdit?“ProcessingAnalysisOptionsWindowHelp口3?曷總MIdJr人4力』姐也生相生■喋應(yīng)?11加;I顏女校殘反以G強(qiáng)r1arwser'basaGrcqs助神■h[]Aninr>DTiHeHS492UUZ1101151￡:uailafyaiighwlny―_—?tdiC:\BnjkErtTOP5PKt□Admiiisiratarj口EwralayangduotangtdhaaiinosogoiiOhaailnllD2l3G-phactungTMgmgHS492DQ?l1Q1討己10-期口e-Qli-zg3D@Dl2-co$ygpQf*h/MnuurneH5492edlS-nmcpndijf?imomrY忙H眄m￡3m.Mc闡卯sisp22l*1.ftjnorofineHS492日（□15?夠193cli&si6-[jeiiti35:L，1-AfflDfomEH眄1017-depBD；,?1-AjnoTjrneH&192：目口伯-C?WL*1-AmnolfriEHS495+二iDaretaffil-tJihvdrate-HSJ?!+口則如川冊(cè)1#1J1U3nil30-110527-1#tjgongyueta-nOTn-i#+jgDrgyuer>im?ib?tjgongyijela-llD71l-3+Jgongyueta-nOTlH#+□irinoteHn.hytiiochloilflfe-HtjinEzniid-HS532on9D3ai#+jluchefijTiEi-l107<l&-1*+JmushroonHJ912V6*JNramsandJ-DHSO+_jteTini3lnmcle-w^820D6D6+—即酗M1061D■修wa---m>AVSpecEnjniFro[.Pira此耳JP*T烷FUsePragPeaksinteyafeSshciIeStruciureFidrnS1LT的tistaNBdpKbenotdefinedbpeimEntWWthReceiverNucitusDuratjcnsPowerProgramPrateU$l$wotiwesAutamatnnMKelaneousUserRoutingTE^eriment刖LPROGAQ_fflOdTDNSDSTDOTWOsw|ppm|iSWH附AQ國(guó)FIDRES|HZ|FW網(wǎng)*igpga口廠區(qū)1CurrertpulseprogramDQD65596口AuysniDnmodeSGEafhdNLirtieraTscansNurrtierafdhfmy$cansLoapt&untforW3S936?SpHE-dUlspectralnvldUhAcqursrtjonDmeFHresalJDcnFilerwWDi24118a4611.3632196036fi79B12900000TRecewerRGdwbjs]DWOV㈣DECIMDSPFRMDGTYPDGMODER1B39Q4RetEr^rgainMBOD2.S00BMMOvEraampIngOwelHireDecmaticnrsate討dgitsinitersharpytandarcf：DSPitnmreriterHADC+*Cijtiiertypedgtal7□grtnRiDnmode17□gtEer『四口皿口口DOR1口利巾曄rresduiinn氏周HPPRGNPRGAMDQCWCEPH_ref[degrBe|nvFPFi、tt_向Pre-scandetayPreamplhergainHighpowerpreamplOer典力DigWiquad出尼巾m力29nonnal丫h咖vaddoocoPecEivErphasecoirerton■ImimiFntinnepfHitwrhprkinn'irrirrp_mlH91?-M￡1DW[網(wǎng)DWOV(|JS]DECIM203002.600DSPFIRMDIGTYPDIGMOD17DRDDRDE[ps]HPPRGNPRGAJNDQDMODEPH_ref[degree]OVERFLWFRQLO3N▼Nucleus1NUC101[HZ]01P[ppm]SF01IMHZ]BF1[MHz]▼Nucleus2NUC202[Hz]O2P[ppm)SFO2[MHz]BF2[MHZ]DwelltimeOversamplingdwelltimeCedmationrateofdigitalfilterDSPfirmwarefilter1130Edit,..100606099995100.6226299100.6127690400.13160054001300000DigitizertypeDigitizationmodeDigitizerresolutionDigitaldigitizerresolutionPrejeandelayPreamplifiergainHighpowerpreamplifiergainDigitalquaddetectionmodeReceiverphasecorrectionAccumulationoverflowcheckingObservefrequencyshiftreductionObservenucleusTransmitterfrequencyoffsetTransmitterfrequencyoffsetTransmitterfrequencyBasictransmitterfrequency2ndnucleusFrequencyoffsetof2ndnucleusFrequencyoffsetof2ndnucleusFrequencyof2ndnucleusBasicfrequencyof2ndnucleusDEPT?:協(xié)助確定伯仲叔碳，如下圖，可將13GDEPT135和DEPT90t匕較，可確定碳的種類。DEPT135:CH3CH為正，CH2為負(fù)，DEPT90只有CH在新建文件是，experiment選擇DEPT13豉者DEPT90DEPT135參數(shù)設(shè)置如下:Broker⑶配GroupsAliasABroker⑶配GroupsAliasA日ErukerI0F5111HLIonKIRPC2猖^jdiiiLLstutaiFileEdllViewProcessing朋郵1$Oplions師MowHelp2d3d:四國(guó),曲殘區(qū)卜喟Tt1+jc：MnroPSPN-J口:也出附由finpr?jMirtni彌占增-一iEwa似的叩i口加他叫+jhaoKn09DM3i-jha(jKn11D218iJtaoxng-jAmorolfine-HS4&M07ll01,510-2^30j，011.呼口-，即rqnolfinpH鄒2rj回怖b聊必]T1-MmotME卜幽汕如網(wǎng)胸幽22!!■'?AiroromneHS432;2仿-駟30-；底內(nèi)肺=iLjl6-deptl35-□l7-dept=Qi-AiraroilineHS4S2-「田-c卿甲11-AmonoifineiW+」口優(yōu)幽斗1rtMiraFHS4%」tOtustiitao-liffiSS-i#*^(usriit3Q-11[527-1#i二gong*1叼LI#vjgcngyucfa-110711-2*jgDig^jef3-11D?11-3t^gorgyuefa-110711^+.Irinotecin-lydnjchloride-Htjline!Did-HS5320090301^tjliucrengniei-110J05-1#i3mi柳加叫Bl20Gi」眥曲＞?ni曲LiMSOtjleriffloi口皿d邛期200眥ijweipi^11Q6iM#VT'/再*^內(nèi)M1!.時(shí)DW[ps]DWOV[間DECIMDSPFIRMDIGTYPDICMODDRDDRDE|ps]HPPRGNPRGAINDQDMCDEPHref[degree]OVERFLWFRQLO3N▼Nucleus1NUC101[HZ]O1P[ppm]SFO1IMHZ]即1[MH?TNucleus2NUC202[HZ]O2P[ppm]SFO2[MHz]EF2IMHZ]20.SOODwelltime26?？贐17□versampiinq(JwielltimeDecimationrateofdigitalfilterDSPfirmwarefilter1130Edit...10060.8099,995100.6228299100.61276904001316005400.1300000DEPT9修數(shù)設(shè)置如下:DigitizertypeDigitizationmodeDigitizerresolutionDigitaldigitizerresolutionPre-scandelayPreamplifiergainHighpowerpreamplifiergainDigitalquaddetectionmodeReceiverphasecorrectionAccannulationoverflowcheckingObservefrequencyshift「巳ductimnObsen/enucleusTransniitterfrequencyoffset

TransrnitterfrequencyoffsetTransmitterfrequency

日日5ktransmitterfrequency2ndnucleusFrequencyoffsetof2ndnucleusFrequencyoffsetot2ndnucleusFrequencyof2ndnucleusBasicfrequencyof2ndnucleus-口irDW[ps|20,300DwelltimeDWOV[ps]DECIM26000OversamplingdwelltimeDecimationrateofdigitalfilterDSPFIRMsnarp(standard)VDSPfirmwarefilterDIGTYPHADC+VDigitizertypeDIGMODdigitalVDigitizationmodeDR17DigitizerresolutionDDR1DigitaldigitizerresolutionDE[ps]6.5。Pre-scandelayHPPRGNnormalVPr巳ampllfie「gainPRGAINhighVHighpowerpreamplifiergamDQDMCDEaddVDigitalquaddetectionmodePH_ref[degree]0.000ReceiverphasecorrectionOVERFLWignore7AccumulationoverflowcheckingFRQLO3N0Observefrequencyshiftreduction▼Nucleus1NUC113CEdit...Observenucleus01[HZ]10060.30Transmitterfnequ巳ncyoffset01P[ppm]99,995TransmitterfrequencyoffsetSF01IMHZ]BF1[MHZ]▼Nucleus2100.6226296100.6127690TransmitterfrequencyBasictransmitterfrequencyNUC21HEdit..2ndnucleus02IHZ]1600.52Frequencyoffsetof2ndnucleus02P[ppm]4.000Frequencyoffsetof2ndnucleusSF02[MHZ]BF2[MHz]400300000Frequencyof2ndnucleusBasicfrequencyof2ndnucleusCOSYH-H相關(guān)在新建文件時(shí)，experiment選擇COSYGPSW

DiuIgbitOPSPIfl工1ui\SIRPC2asAihini￡tE2loE國(guó)giea國(guó)giea口白回審圖禹自idML后上J出&%達(dá)貴省固?日於Bra^Er㈤刈配呷門整l|，jCCukertTOPSPIN-jD'toruhEfitruher+Jpxtnnistratflr-」E.扇麗ng▼-jttjrtsng-JhaminOSOMSijhacMinrO?iBT白haeh叫■□Ajnorolfine-HS(l92(1071l0l±jl0-3g30iJ11-j)g30&CJ12-CE^ygp^&.ji3-hmti：g|Tidi[rL*1-AmnrnfrieHS492+□l4-hsqcetgpsls|i22,315-即即11-i^izrorneHS4921iJ16-depri351-^■-izrorneHS4.92&Ol7-depi901-WtfTBliS492tJi16-(：oiygpt)(+□Dotei禧蚱trirrdm通HS4打底0fu勁腦小110523■件￡jftjs?iitai>11O52M#tJgongyijefa-11D7lbi#t□gong^iEfa-110711-2￡jgorg^fa-110711-3tjgorg￥ufffa-lIDTlU#tjrinatecan-r^urDtnimEte-H±Jineznli[l-HS53aDt]903ttl#i.Jiurhengmei-110705-1#±二)m闿rm西的1106tjNEaimanidE^OMSO七3temDiolomll&w切目:出眸D@t^wEipinglLkllO6lCH#￡口』硒gjuW血ng?網(wǎng)1即idyttfueIjX1"^irr"tHFiEnCE?！?EF>nWin

PGgoReceivergainDW[|JS]93,600DwelltimeDWOV[|js]2.92&□versamplingdwellbmeDECIM32DecimationrateordigitalfilterDSPFIRMsnarpfstandard)VDSPfirnwareniterDIGTYPHADC+VDigitizertypeDIGMODdigitalYDigitRationmadeDRISDigitizerresolutionDDR2DigitaldigitizerresolutionDE[ps]6.50Pre-scandelayNEL1Numberofblocks(ofacquisitionmemory)HPPRGNnormalVPreamplifiergamPRGA1NnighVHighpowerpreamplifiergainDQDMODEadd3DigitalquaddetectionmodePH_ref[degree]ReceiverphaseccrrecticinOVERFLWignoreVAccumulationoverflowcheckingFRQLO3N□Obsen/efrequencysniftreduction▼Nucleus1NUC11HEdit...1HVObservenucleus□1[HZ]M近662405.66TransmitterfrequencyoffsetO1P[ppm]6.0126.012TransmitterfrequencyoffsetSFO1[MHz]dOD.1324D574001324057TransmitterfrequencyBF1[MHZ]^10013000004ao.i3ooD0aBasictransmitterfrequencyNOEH-H空間相關(guān)在新建文件時(shí)，experiment選擇NOESYPHSWNOESYPHPR般對(duì)于生物樣品）HMBCC-H遠(yuǎn)程相關(guān)在新建文件時(shí)，experiment選擇HMBCGPNDQF

DW陽DWOV[網(wǎng)DECIMDSPFIRMDIGTYPDIGMODDRsharp(standard)DW陽DWOV[網(wǎng)DECIMDSPFIRMDIGTYPDIGMODDRsharp(standard)VHADC+VdigitalV10DDPDE[網(wǎng)NBLHPPRGNPRGA1NDQDMODEPH_ref[degree]OVERFLWFRQLO3N6.501normalVhighVaddV0.000ignoreV0293.6002.92532DwelltimeOversamplingdwelltimeDecimationrateofdigitalfilterDSIPfirmwarefilterDigitizer巳DigitizationmodeDigitizerresolutionDigitaldigitizerresolutionPre-scandelayNumberofblocks(ofacquisitionmemory)PreamplifiergainHignpowerpreamplifiergainDigitalquaddetectionmodeReceiverphasecorrectionAccumulationoverflowcheckingObservefrequencyshiftreduction▼▼Nucleus1NUC11HEdit...13C01[Hz]2405.661004470O1P[ppm]6.01299,836SFO1[MHz|BF1[MHz]▼Nucleus2400.13240574006223138100.6127690NUC213CEditC2[HZ]O2P[ppm]100447899,636SFC2[MHZ]BF2[MHz]100.6326138100.6127690vObser/enucleusTranamitterfrequencyoffsetTransmitterfrequencyoffsetTransmitterfrequencyBasictransniitterfrequency2ndnucleusFrequencyottsetof2ndnucleusFrequencyolTsetof2ndnucleusFrequencyof2ndnucleusBasicfrequencyof2ndnuclleusHSQCC-H直接相關(guān)在新建文件時(shí)，experiment選擇HSQCETGPSI&P參數(shù)設(shè)置如下:Bnjwg叫LastsMcno甲51AllBg|■jCfinjkertTOPSFlN*-口口.5Ke世iruKErh^jAdinnistraior-_)E.taailaiyangt-_]duntang」hacwmraaaE^hamiil10Q18--iha(?ik期-J^naralfne4iS492Off?1101+□W-zgaOtjii-■sgaa,3cll2-tDsygj^J1-MmorornneHS4d2l3-j113-mticgpnd(t?1-AmorarnneHS；1?三DlU-加qretgpsi5P2;：^J15-2gpg30AmomlfinEHS492-,□l6-rtept1351-AmomlfineHS492GJ17-Mct90J*1-AmoronneHS492*cJie-cosygptrt_iDocetat：=i-trihvdr3tp-HS47；t^ftjshtsD-110523-1#+._jAjShtao-11D5271#+□gongyuEfa-110711-1#+j)gdngyuel>i1(Pii.2+□gongyuEfa-l10711-3!」即瓢婚110711』#?二Irinouetan-hydracNande-H■JlinHflli[l-HS532DD9D30l#iQMKhcngmei-iionK-i#*^iriU5hrao[n-Q9l2D6，jiMtazfficanlde-DMSO?_ibEmaiDlonnde-w^aaOOeDB1.jweipingjiu-i10610-1#t_iXisn^guduotarg-O9i1037En悟4期皿HIMU1E為劃舊地叫hHnwfl前’SpectrumPracParj恥quP/5mePulsePragPeaksntE9選SampleStfUCUX?FidAs闌insteiedproue-notdennedExpenmentWkittiRKEktrNucleusDurationsPowerProgramPrabeListsWUHe□xkAutonabonMiscellaneousUserRoiling<BipetiroentF2FlAFrequencyassRJLPROG.AO_modhsqcetgpsispS?11.ECurrentpulseprogramDOO■W"AfquisrtianmodeFrtWDEEcho-Annecho*Acquismanmottetar2D.3DHeaseffldTDNSDSTDO204B2564Number討scans16NumtererfdummyscsnsLoopcourtffirW1TwidthSw阿ISWH|HZ]160204165.6500Specir^wdttispecirai”dmincrementTordelayAcquisrbantimeFidresalution641D.25616667.756IN_F：|JS]6D.00AQ\s\FORES㈣FW阿015907200.0D767953.13000965.108421125D0D00FterwcnnTReceiverRGDW|MS]6192RecB^ergainDwellhue7BQ00DWOV附DECIM325024Oversamp