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Avance 300 MHz NMR Spectrometer Operating Instructions using
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1. Tol toluene d8 Process Data Plot Editor Lock nucleus Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe File Edit View Spectrometer Processing Analysis Options Window Help NMR Step By Step 090 05B8B8 2 3 4 AML Sm NV A aa 27276 et ZMAJA n QM gt e atte A sample_1d_1H 3 1 CiBrukeriTOPSPIN Training Create New Dataset 1D Experiments 2D Experiments Browser Last50 Groups Alias g Man Spectrum ProcPars AcquPars Title PulseProg Peak Lock Fid gues Training Tune and Match sample_1d_13C Shimming sample_1d_1H i 2 0 1 2930 Acquire SD 3 2930 e 1 1H Cyclosporin Process Data sample_10 Plot Editor amp Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe File Edit View Spectrometer Processing Analysis Options Window Help NMR Step By Step Dange aBel sa AM ios 272 68 2 FEMA QAQAQo QMe eos ett Browser Last5D Groups Alias N AL sample_1d_1H 3 1 C Bruker TOPSPIN Training CABrukeriTOPSPIN guest Training 0 sample_1d_13C sample_1d_1H 1 zg30 10 2 zg30 3 2930 e 1 1H Cyclosporin 0 sample_1d a Fire N MARKE HM Spectrum ProcPars AcquPars Title PulseProg Peak Create New Dataset 1D Experiments 2D Experiments Lock Fid Tune and Match o Shimming Acquire Halt Process Data Plot Editor 6 Start the experiment by clicking Acquire in NMR Step By Step If at the end of the experiment the signal is weak yo
2. Avance 300 MHz NMR Spectrometer Operating Instructions using TopSpin v 2 1 1 Logon e Click on ID icon and enter your password e Double Click on TopSpin e Ifthe lock window does not open click Y to open it 2 Insert Sample Place sample into the spinner and adjust the height with adjusting gauge When placing your sample in the spinner do not touch the spinner with bare hands use a kim wipe e Your sample should touch the bottom of the gauge e Remove the black cap from the top of the magnet Press Lift On Off button on the BSMS keypad and WAIT until you can hear air stream before inserting your sample e Press the Lift On Off button on the BSMS keypad to lower your sample The Effect of Improper Sample Depth on Gradient Shimming LN no oc ame pam par Sample at Proper sample at Improper Depth Depth E FE a NOTE TopSpin has replaced CPAN used in XWIN NMR with NMR Step By Step 3 Create a new Dataset by clicking on Create New Dataset in NMR Step By Step NAME file name case sensitive no spaces no brackets and no forward or backward slashes EXPNO Increment starting from 1 PROCNO usually 1 DIR do not change USER do not change Solvent no need to change Experiment Dirs do not change Experiment do not change TITLE no need to fill in yet e Click OK to setup your new data set E Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe File Edit V
3. e File Edit View Spectrometer Processing Analysis Options Window Help NMR Step By Step Dea A 6 Bla 3d LK AM TL FEIN EA A Be Create New Dataset 1D Experiments 2D Experiments File Options Help Source C Bruker TOPSPIN expistan nmrpar v Search in names td_15N inept 1d 1HSensitivity KERNE carton_020 Peak Lock Fid Tune and Match Shimming Acquire Halt Process Data Plot Editor 1d_13CSensitivity 1d_15N id tHes 1d_carbon_nodec 1d lineshape 1d proton Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe File Edit View Spectrometer Processing Analysis Options Window Help NMR Step By Step Create New Dataset 1D Experiments Dal 6 Bad 3 4 AMA TE LAA 2 RBRB ZMAJA n aM e o rie atte Browser Last50 Groups Alias N Ml sampie_ 1d_1H 3 1 C Bruker TOPSPIN Trainin 2D Experiments 5 an Spectrum ProcPars AcquPars Title PulseProg Peak Lock Fid gues O Training Tune and Match sample_1d_13C Shimming sample_1d_1H 1 2930 Acquire 2 z930 Halt gt 3 2930 H Cyclospo Process Data 1 1HCy sample_1d Plot Editor 4 Start the experiment by clicking Acquire in NMR Step By Step Note that you do not need to shim your sample as this was already done prior to the proton spectrum Type ns in the command line to change the number of scans to 150 5000 depending upon your sample During the experiment you can view your spectrum by typing tr in the comma
4. him finished is displayed before continuing g Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe File Edit View Spectrometer Processing Analysis Options Window Help NMR Step By Step 0 A Parameter Sets rpar 1d x File Options Help Source C Bruker TOPSPIN exp staninmripar Bro Search in names Search Create New Dataset 1D Experiments 2D Experiments ou eak Lock Fid 1d_13CSensitivity 1d_15N 1d 15Ninept 1d _1HSensitivit 1d_1Hes 1d_1Hpr 1d_31P 1d_JMOD ne carbon D20 1d carbon_nodec Tune and Match 1d_proton Shimming Acquire Halt Process Data Plot Editor p Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe File Edit ENANA bis Options Window Help NMR Step By Step O a O sc Description bp EA UE BB te Create New Dataset 2 72 8 e Acetic acetic acid d4 eole alt te Acetone acetone d6 1 D Experiments Browser Lad cene benzene d6 BrukeriTOPSPIN Training 2D Experiments Sa AcquPars Title PulsePrag Peak Lock Fid 5 5 Trail CD3CN_SPE LC SPE Solvent Acetonitrile Tune and Match sf CDCI3 chloroform d Shimming s CH3CN D20 HPLC Solvent AcetonitrivD20 E CH30H D20 HPLC Solvent Methanol D20 Acquire oC D20 deuteriumoxide Halt C DEE diethylether d10 Dioxane dioxane d8 103 ome dimethylether d6 DMF dimethylformamide d7 DMSO dimethylsulfoxide d6 EtoD ethanol d6 H20 D20 90 H20 and 10 D20 MeOD methanol d4 Pyr pyridine d3 THF tetrahydrofurane d8
5. his button may not be visible due to the size of the screen and if you click Y the save and return button will be visible 5 Peak Picking Click 4 to open the Interactive Peak ar OH E ROE ruker ol EN as Joe File Edit View Processing Analysis Options Window Help NMR Step By Step x x gt DsaP8B Bau 4 AM Fl 3d 4 A Be Picking window an ka Sr Browser Last50 Groups Alias N E sample_1d_1H 4 1 CiiBruker TOPSPIN Training To select peaks click the Define Region EAS ES ia a xaa 20 draining F N0 DonrY utton which will change to green E yap P 40 27 ppm 136 37 Hz Se 2 2930 Define new region Click and drag the mouse to draw a box ice around the peaks you would like to be picked Alternatively click j to manually pick BETEN Jasik LL Ll e AU individual peaks by using the mouse to select the center of the desired peak Click El to save peaks and return to your spectrum amp Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe 6 Set your title by clicking the Title tab above your a Edit View Processing Analysis Options Window Help NMR Step By Step spectrum Return to your spectrum by clicking the Spectrum tab 7 Plot your spectrum by clicking Plot Editor in NMR Step By Step Consult the xwinplot manual for detailed instructions on plotting and printing your spectrum Dah 6S dA 440 1 Sin Vm A Be 227 68 2 FMAIQAAQA lo aW e oje arts Br
6. iew Spectrometer Processing Analysis Options Window Help NMR Step By Step 0908608058234 44 Tapa 272828 FEMA QAQQAAo AM e e gt a 7314 Browser Last50 Groups Alias N D C Bruker TOPSPIN Create New Dataset 1D Experiments 2D Experiments Lock Tune and Match lt Shimmin amp New g Acquire Prepare for a new experiment by creating a new data set and Halt initializing its NMR parameters according to the selected experiment type For multi receiver experiments several datasets are created Process Data Please define the number of receivers in the box below Plot Editor NAME sample_1d_1H EXPNO 1 PROCNO 1 DIR CABrukenTOPSPIN USER Training Solvent C6D6 v Experiment Dirs C Bruker TOPSPIN exp stan nmrparfuser v Experiment Use current params TITLE 1 Receivers 1 2 8 H NMR 1 Read in standard IH parameter set by clicking 1D Experiments in NMR Step By Step e select the appropriate parameter set usually 1d proton e Click Read Click OK 2 Lock by clicking on Lock in NMR Step By Step e Choose your solvent from the menu e Wait until Lock Finished is displayed before proceeding 3 To start automatic tuning and matching click Tune and Match in NMR Step By Step e Wait until atma finished is displayed before proceeding 5 To shim click Shimming in NMR Step By Step This will start a process called TopShim e Wait until TopS
7. nd line wait for the message checklockshift finished for the first tr of the experiment after this wait for data stored as and click Process Data in NMR Step By Step e When the signal is strong enough click Halt in NMR Step By Step e Wait until checklockshift finished is displayed before processing your data How to Log off Press lock on off on the BSMS keypad to turn the lock off and press lift on off on the BSMS keypad to eject the sample e Remove your sample replace the black cap on the magnet and turn off the air flow by pressing lift on off on the BSMS keypad Exit TopSpin and click OK Log off the computer under the Start menu and select log off and log off
8. ove the mouse until all peaks left and right of the biggest peak are also positive e Click El to save and return to your spectrum 3 Calibrate your spectrum using a reference peak ES 3 3 1 1 1 C Bruker TOPSPIN Training JE rei gt t N co Click A to enter the Spectrum ae IE Cal bration window i Ce Using the mouse select the center of your a reference peak you may need expand the area around the reference peak prior to 24 entering the calibration window Enter the desired value and click OK Cursor frequency in ppm 7 27 Click to return to your spectrum 4 Integrate Click T to enter the Interactive Integration window Delete all integrals created automatically during data processing by clicking T to select all integrals then click UN To select integral regions click the Define Region button which will change to green Click and drag the mouse on either side of a peak to define a integral region If you need to expand a region of the spectrum be sure to that the Define Region button is NOT green then click and drag the mouse on either side of the region you would like to expand See How to look at your spectra section To calibrate the integration right click on the desired integral and select Calibrate Current Integral Enter the number you wish and click OK When finished click El to save your integrals and return to your spectrum NOTE that the t
9. owser Last50 Groups Alias N AL sample_1d_1H 1 1 C BrukeriTOPSPIN Training ae Spectrum ProcPars AcquPars Title PulseProg Peaks Integrals Sample Structure Fid gues Training BmHjoje 9 sample_1d_13C sample_1d_1H D 1 2930 e 1 1H Cyclosporin gt 2 2930 1H Cyclosporin a Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe File Edit View Spectrometer Processing Analysis Options Window Help NMR Step By Step 0904868234444 TEN MH AE 8 27278 8 EMA QQQA aW e eo gt e art Browser Last50 Groups Alias C Bruker TOPSPIN Create New Dataset 1D Experiments 2D Experiments O sample_1d_1H 3 1 C Bruker TOPSPIN Training Spectrum ProcPars AcquPars Title PulseProg Peak Lock Fid guest Training Tune and Match 9 sample_1d_13C Shimming sample _1d_1H 1 2930 Acquire 2 zg30 H alt SD 3 z930 e 1 1H Cyclosporin Process Data ee Plot Editor SC NMR 1 Increment the experiment number by typing 1 in the command line or clicking create new dataset in NMR Step By Step and changing the EXPNO to 2 2 Read in standard 13C parameter set by clicking 1D Experiments in NMR Step By Step e select the appropriate parameter set usually 1d_jmod e Click Copy All 3 To start automatic tuning and matching click Tune and Match in NMR Step By Step e Wait until atma finished is displayed before preceding amp Bruker TOPSPIN 2 1 on NMR_OFFICE as Jo
10. rs Title PulseProg Peak Lock Fid 20 en Tune and Match sample_1d_13C en sample_1d_1H NOS 1 2930 Acquire 2 zg30 3 2030 Halt of Process Data zu Plot Editor SIDE NOTE How to look at your spectrum using TopSpin To expand a region simply click and drag the mouse over the are you wish to expand Click MM to see the full spectral width To increase or decrease the intensity you can simply use the mouse wheel or click and hold and move the mouse up or down or to make the spectrum larger click 2 or 8 to make the spectrum smaller click 2 or ii Click to reset the spectral intensity so that the largest peak in your spectrum 1s completely visible Clicking any of the arrow buttons Y 7 E AF f will allow you to navigate around on nn d b dov donb Browser Last50 Groups Alias e Experimenta ata current an past can be accessed by double A EN clicking on the desired experiment in the browser panel guest experiments can still be recalled by typing re in the command Training li d th xWinNMR sample_1d_13C ine as was done with x Win 33 sample 1d 1H HA 1 2930 Mag 1H Cyclosporin a 2 7930 2 The spectrum should be phased correctly if not phase manually e Click A to enter the Interactive Phase Correction window Click and hold Y and move the mouse until the largest peak highlighted with a red line is positive and the baseline is as flat as possible Click and hold 1 and m
11. u can increase the number of scans by typing ns n the command line and entering the desired number of scans you can then re acquire the spectrum To stop an experiment at any time click Halt in NMR Step By Step Wait until Checklockshift finished is displayed before processing your data amp Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe File Edit View Spectrometer Processing Analysis Options Window Help NMR Step By Step 0 angad 4 AM Sl Nh EAR Bt Create New Dataset 27278 e EMAIQAQQAA aM e e gt ea 32 1D Experiments Browser Last50 Groups Alias N E sample_1d_1H 3 1 CiBrukeriTOPSPIN Training 2D Experiments en Spectrum ProcPars AcquPars Title PulseProg Peak Lock Fid Training Tune and Match sample_1d_13C Shimmin sample_1d_1H 9 20 1 2930 Acquire O 2 z930 HD 3 2930 a e 1 1H Cyclosporin Process Data E Plot Editor Processing Basic 1D spectra using TopSpin v 2 1 E Bruker TOPSPIN 2 1 on NMR_OFFICE as Joe l W hen the acquisition 1S complete ie File Edit View Spectrometer Processing Analysis Options Window Help NMR Step By Step s I Dal 6S Bast AM GL Ts pl Create New Dataset checklockshift finished is displayed click on 2R7KeEMAAAQAA OAM ese AFF iD Experiments 7 4 1 1 E N l Browser Last50 Groups Alias N A sample_1d_1H 3 1 CiBrukeriTOPSPIN Trainin 2D Experiments Process Data n N R Step By Step rn Spectrum ProcPars AcquPa
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