Delta V4.3.6 - George Fox University
Contents
1. 6 3 csl METTRA RI T 3 2 3 5 4 2 4 4 Dios atcha ches eaves deacons canoes 3 11 Setting the conditions for displaying contour lines 4 13 Setting the measurement range from 1D NMR data HETCOR 4 8 Setting the measurement range from 1D NMR data HH COSY 4 7 Setting up the sample 1 7 cin e PM E AT 2 3 solvent 3 2 3 5 4 2 4 4 SO NL R 2 4 Specifying an NMR lock solvent 2 7 Spectrometer Control window 1 4 Spinning the sample 1 9 Starting 2D NMR measurement 4 10 Starting measurement 3 6 5 1 Starting one button measurement 2 4 Starting the Delta program 1 1 T T RM T 2 3 Temp State 2 4 Threshold level eerren 4 14 To expand a spectrum horizontally 3 12 To expand a spectrum vertically 3 12 To expand a spectrum vertically and horizontally at the same time 4 17 THES IET E E A 4 13 total time 3 3 3 5 4 3 4 5 V Version number eenne 6 7 Viewing information about the jobs in the queue 5 3 X X Hg WIOU uere ERES ERE Crede ls 4 3 x domain 3 2 3 5 4 2 4 5 X BITSBE La siint 3 3 3 5 4 2 4 5 X points 3 2 3 5 4 2 4 4 X BUISB irirna 3 3 3 5 4 5 X SWeep sssess 3 3 3 5 4 3 4 5 NM ECA ECX TU 3 Y y pulse 4 5 y_domain2. 2 6 Changing the display range 3 10 Changing the display ranges 4 17 comment 3 2 3 4 4 2 4 4 DIDI eo inr toe rr n a 2 3 Connecting to the spectrometer 1 3 Contour line level button 4 13 CUr TM oe PEE emer recent 2 3 II JKMeCXTTE 3 11 LUST OG BAT sanitised 3 10 E uror Ino MO aniio cesta 3 11 D Data filename een 2 7 Deleting measurement 5 2 Delta Console window 1 1 DUP CIOPW Gu ice cinia Maias Ele bii lakes 6 7 Disconnecting from the spectrometer 1 4 displaying the present status 5 1 NM ECA ECX TU 3 E Ejecting the sample 1 6 Ending 2D NMR measurement 4 10 Ending measurement 3 6 Ending one button measurement 2 5 Ending the Delta program 1 2 Expanding and resetting spectra in the 1D Processor window 3 12 Exp riment T1868 ecd ee vip etn 3 1 Experiment Tool window 3 2 3 4 4 2 4 4 F FHEBADIB Lone HI ERE 2 3 G Global directory aas recep e ann 3 1 6 7 H Hard disk capacity iceren 2 7 HETCOR measurement 4 4 HH COSY measurement 4 1 Highest peak seeene 3 13 HON ooneHiE HR IIIS TOR 2 4 I Mai a ATTE E T 3 11 irr_domain 3 5 lj c A E 3 5 Laak ii MR TE E T T 3 5 J j_constant e 4 4
3. on 2 1 STARTING AND ENDING MEASUREMENT uu eter 2 3 Lr Glee MERAEREDIEN TrabditnieH ERI TAn 2 6 gl airs Ue UL pm NUN ers I errr tts rere TUE 2 1 2 ONE BUTTON MEASUREMENT 2 1 GENERAL Automatic measurement which can be performed by simply clicking one button is called one button measurement When one button measurement is performed a series of conditions for sample settings measurement processing and plotting and their combinations are called methods The following methods are displayed in the Automation window Table2 1 Preset methods and measurements Method Measurement Sequence name Proton 1D H normal measurement single pulse ex2 1D H normal measurement single pulse ex2 Presaturation 1D homo gated decoupling A utomatic solvent elimination single pulse ex2 method Carbon 1D PC normal measurement single pulse dec ex2 1D H normal measurement single pulse ex2 Proton and Carbon 1D PC normal measurement single pulse dec ex2 1D PC normal measurement single pulse dec ex2 Carbon and DEPT 135 Automatic determination of 9C atomic group by means of DEPT dept ex2 1D PC normal measurement single pulse dec ex2 Carbon and APT 1D PC normal measurement single pulse dec ex2 Edited DEPT A utomatic determination of C sence atomic group by means of DEPT pt 1D H normal measurement single pulse ex2 Proton and COSY Homonuclear 2D H H COSY COSy ex2 1D H normal measurement single
4. 100 0 200 0 2 cre 02TH 0 0 s 3 trapezoids 0 80 4 zerofill 1 5 fft 1 TRUE TRUE fy 0 1 0 2 0 3 04 05 06 07 08 09 10 11 12 13 14 15 16 17 X seconds 1H Gain OFALSE Polit 1 0 10 20 30 40 50 60 70 80 90 abundance 12 0 110 10 0 90 80 70 60 50 40 30 20 10 0 1 A X parts per Million 1H pp 50 ats X Offset and x sweep are set to the offset and range values of the area where the 1D NMR data is displayed B Setting the measurement range from 1D NMR data HETCOR l Expand the processed 1D NMR data to the range to be used for 2D NMR measurement 2 Click on the button in the Experiment Tool window 3 Click on the View X button 4 4 faahe Experiment Tool cosy exe The mouse pointer changes to 3 4 Move the mouse pointer to the position of the processed 1D data PC 1D NMR data for example and click the left mouse button 4 8 NM ECA ECX TU 3 NM ECA ECX TU 3 4 2DNMR MEASUREMENT 41D Processor single pulse dec 1 jdf PPM HEP 1 H PC 0 1 0 2 X seconds 13C 200 0 X parts per Million 13C wae 100 0 Se xoa 2 sexp 2 0 Hz 0 0 s 3 trapezoid3 O 80 75 4 zerofill 1 5 fft 1 TRUE TRUE a M JFALSE Order Gain ligt mnn mj p ss Jom J m J
5. PID MBE The default plotting is performed 4 16 NM ECA ECX TU 3 4 2DNMR MEASUREMENT ae 4 3 5 Changing the Display Ranges The Cursor Tool bar is used to expand and reduce spectra c For how to display the Cursor Tool refer to Section 3 3 4 For the details of the Cursor Tool refer to the separate volume Processing U ser s Guide E To expand a spectrum vertically and horizontally at the same time l Select the Zoom mode from the Cursor Tool or press the key on the keyboard The Cursor Tool mode becomes Zoom 2 Move the mouse pointer to the position that will become the lower left corner of expansion in the display area 3 Press and hold down the left mouse button and move the mouse pointer to the position that will become the upper left corner of expansion in the display area 70 6 lt 0 50 40 30 20 140 8 0 z j 1 E E p E Bon E gt b ga 70 sa 0 d 3 o6 m D i44 X parts per Million 1H 4 Release the left mouse button The spectrum is expanded vertically and horizontally at the same time B To return the spectrum display to its previous conditions Press the key on the keyboard to return the display to its previous conditions You can do this up to 16 times e Backspace i af HE sf D c oO co c 2 NM ECA ECX TU 3 4 17 4 2DNMR MEASUREMENT When you do this both vertical and horizontal expansions return to their
6. When you press the Backspace key both vertical and horizontal expansions return to their previous values You cannot selectively return only the vertical or horizontal size to its previous value To return the spectrum display to its initial conditions Press the key on the keyboard All horizontal and vertical expansions return to their initial values E X age io Page NMECA ECX TU 3 3 13 2D NMR MEASUREMENT Chapter 4 explains the procedures for the basic 2D NMR measurement in the order of measurement data processing and plotting It is assumed that the Delta system has been connected to the spectrometer and that the sample setup sample loading NMR lock resolution adjustment and other preparations for measurement have already been performed If you are not ready to start measurement carry out the procedures in Chapter 1 Preparation for measurement 41 SETTING 2D NMR MEASUREMENT CONDITIONS 4 1 amp Ll HA COSY TEORSULOPDIBDILU S ai er er reer ore nnn et ENUE FAEERDEOFE Ep eter ene IE 4 BRL RETLOR MESUM eto Hec iiR DM ERIPN EH ME AR MODE H NM HHeliERUE 4 4 4 1 3 Setting the M easurement Range from 1D NMR Data 4 6 42 STARTING AND ENDING MEASUREMENT nmm 4 10 423 DAIA PROCESSING OF 2D NER aosserisiniteu usn vds DM HOP EU 4 11 4 3 1 Displaying Data Using 2D Viewer een mmm 4 12 4 3 2 Setting the Conditions for Displaying
7. ere 4 5 o 4 5 y offset 4 5 y points 4 2 4 4 Z ZOOM a ccc ccc cece cee cuucceceuunncennseues 311 NM ECA ECX TU 3 3
8. 1H abundance The 2D processed data is saved Then the version number increases automatically under the same filename l To save 2D processed data in the 2D Viewer window under a new filename l SelectFile Save As from the menu bar The SaveData File window opens tl Save Data File e Path usr people aabe files data Iz Format JEOL Delta Filter Directory Filename Version Filename entry box Fig 6 5 Save Data File window 6 4 NMECA ECX TU 3 NM ECA ECX TU 3 6 SAVING AND LOADING DATA 2 Type any filename in the filename entry box le When creating a new directory after specifying a directory name in the Path input box click on the button Create the directory and move it After that enter the filename to save it into the filename entry box 3 Click on the Ok button The 2D processed data is saved under the specified filename 6 5 6 SAVING AND LOADING DATA R L 6 2 LOADING DATA 1 Click on the button in the Delta Console window 4 aahe Delta BIE File Processors Viewers Tools Analysis Acquisition The Open Data for Processing window opens HA A Open Data for Processing ES Path Ausr people aaherfiles date Format JEOL Delta 4 Filter Ja Directory Filename o Version display box jsingle_ pulse i Data version List box Data information display box Fig 6 6 Open Data for Processing window 2 Click on the name of
9. Select Display High Res Load Y Projection b Select a file 1D NMR data is pasted onto the projection display area of the Y axis NM ECA ECX TU 3 4 15 4 2DNMR MEASUREMENT B When 1D NMR data is displayed on the 1D Processor window 1 Click on the button 4 2D Viewer cosy 2 jdf File Options View Project Sicing Expansion Tools Analysis Display D 2 To paste 1D data onto the X axis a Select Display High Res Load X Projection 2D Viewer cosy 2 jdf File Options View Project Siicing Expansion Tools Analysis Display NUI a ee project Y l Load X Projection X Projection m o Load Y Slice Load Y Projection The mouse pointer changes to x b Move the mouse pointer onto the displayed 1D NMR data and click on it The 1D NMR data is pasted onto the slice or projection display area of the X axis 3 To paste 1D data onto the Y axis a Select Display High Res Load Y Projection The mouse pointer will be changed to a finger shape b Move the mouse button on the displayed 1D data and click 1D NMR data is pasted onto the projection display area of the Y axis 4 3 4 Plotting This section explains how to perform the standard plotting For the details about the settings refer to the separate volume Processing User s Guide Click on the button in the 2D Viewer window 4 14 2D Viewer cosy 2 jdf w rnx File Options View Project icing Expansion Tools Analysis Display
10. The spectrometer executes measurement on a first in first out basis ta aabe Experiment Tool single pulse exz File Tools View Options s LL 4 nL zl N Commands for starting measurements can be issued repeatedly even if another measurement is being performed After one measurement finishes the next meas urement will be started under the stored measurement conditions ital aabe Spectrometer Control This mark indicates hat measurement is being executed Current measure 3 l 84541223 ment that is being single pulse executed 17 SEP 2003 15 02 06 Atsushi Abe 32 Next measurement that is waiting to be executed This mark indicates that next measure ment is waiting to be executed B Ending measurement W hen the measurement finishes the data processing window opens c To stop the measurement during operation refer to Chapter 5 Queuing 3 6 NMECA ECX TU 3 3 1DNMR MEASUREMENT o 3 3 1D NMR DATA PROCESSING After measurement is complete data is automatically forwarded from the spectrometer and the following processing is automatically executed e Correction of the DC components of FID Free Induction D ecay e Multiplication by window functions e FFT Fast Fourier Transformation e Automatic phase correction This section explains data processing following phase correction W hen measurement is completed the following 1D Processor window opens dM te aa
11. 1 Preparations for measurement 31 SETTING 1D NMR MEASUREMENT CONDITIONS 3 1 3 11 Setting H M easurement Conditions eene 3 1 3 1 2 Setting PC M easurement Conditions 3 4 3 2 STARTING AND ENDING MEASUREMENT asian obiit een 3 6 ss ID NMRDATA PROCESSING saieribiiatHy d MIS HE DEAHERER HARD br ERAN 3 7 Ao Auge Baseline C OITECUDDL eeu bise PRFER ENERO FOHER siue PUM RU REUS 3 8 3 3 2 Automatic Peak Detection and Automatic Integration 3 9 Be essen eee anaes 3 9 3 3 4 Changing the Display ROB niin idi rM FERE DEUR HP edema 3 10 NM ECA ECX TU 3 3 IDNMR MEASUREMENT i 3 1 SETTING 1D NMR MEASUREMENT CONDITIONS 3 1 1 Setting H Measurement Conditions 1 Click on the Expmnt button in the Spectrometer Control window Fig 3 1 Open Experiment window 2 Click on the ay button in the Open Experiment window A list of the Experiment files in the Global directory is displayed 3 Select the measurement mode single pulse ex2 from the Open Experi ment window and click on the Ok button The Experiment Tool window Fig 3 2 opens This Experiment Tool window consists of the four sections Header Instrument Acquisition and Pulse 1 The Experiment files contain the measurement modes standard measurement conditions and steps for processing data The file type is ex2 2 The Global directory is the directory in which the standard files supplied
12. 1 4 1 1 HH COSY Io gi S EN 4 1 4 1 2 HETCOR Oe du HR ENIEMO TE RPMER RM HR M MN 4 4 4 1 3 Setting the M easurement Range from 1D NMR Data 4 6 4 2 STARTING AND ENDING MEASUREMENT nmn 4 10 a3 DATA PROCESSING OF 20 NMR aiesitrisiitetnREA FOE REF RD 4 11 4 3 1 Displaying Data Using 2D Viewer 4 12 4 3 2 Setting the Conditions for Displaying Contour Lines 4 13 E353 Pm IDO NMR DS o ien i ima Hi REHU bp EUH bb RYE 4 15 4 3 4 PISIS uineimpnE ee UR EIE FEE UE trado ee FERES RAD 4 16 4 3 5 Changing the Display Ranges Lacasiaere ec otrikin Feri pb xlix Ere Kain 4 17 5 QUEUING 5 1 COMMAND FOR STARTING MEASUREMENT nnne 5 1 Qe UEUN vH HEHM MIT T REMULEN HIER MACH IM 5 2 NM ECA ECX TU 3 i C 1 CONTENTS 6 SAVING AND LOADING DATA EI SOUND EB ouai MEIERIEMNMIENA EIE EH MD 6 1 6 1 1 Saving the measured data FID eee 6 1 Bl Saino Proceed DA eo msn pire EpR ernie 6 3 ES LOADING DAD eerste PUIENIUNID MEAM 6 6 INDEX C 2 NMECA ECX TU 3 PREPARATION FOR MEASUREMENT Chapter 1 explains the startup and shutdown of the Delta program sample setup sample loading NMR lock automatic resolution adjustment and other operations to be carried out prior to measurement 11 STARTING AND EXITING THE DELTA PROGRAM nmm 1 1 12 CONNECTING TO AND DISCONNECTING FROM A SPECTROMETER 1 3 13 SAMPLE PREPARATION 1 3 1 Check Prior to Sample TSOP OM va
13. Contour Lines 4 13 ES PEUDSID NMR BRE eee eee ree rrr Reenter on Ene NE Man oer 4 15 434A PIOWNO arians EEEN 4 16 4 3 5 Changing the Display Ranges essroisiisisiriinirenanainianniaa 4 17 NM ECA ECX TU 3 4 2DNMR MEASUREMENT 4 1 SETTING 2D NMR MEASUREMENT CONDITIONS This section explains how to set the conditions for measuring H H homonuclear 2D NMR HH COSY and C detection heteronuclear 2D NMR HETCOR 4 1 1 HH COSY Measurement l Click on the Expmnt button in the Spectrometer Control window 4 aabe Open Experiment BA Path usr delta global experiments me Filename Version _ l Fig 4 1 Open Experiment window 2 Select the measurement mode cosy ex2 from the list displayed in the Open Experiment window and click on the Ok button The Experiment Tool window opens NM ECA ECX TU 3 4 1 4 2DNMR MEASUREMENT 4 11 aabe Experiment Tool cosy exz File Tools View Options absolute value COS cess interactive global 2d cosy abs list Edit j auto gain pua pe niter bint ef eb E E Lp force tune save aborted THe nmm jeol Total Collection Time 00 28 22 Fig 4 2 Experiment Tool window 3 Setthe necessary parameters The parameters which are usually used are explained below c For information about other parameters refer to the separate MEASUREMENT user s manual 4S Parameters can be displayed by double clicking on Header Instrume
14. HETHOD Carbon Gradient Shin GROUP Carbon est time 0 48 35 EXPERIMENT Carbon OH SLOT 1 File usr people aabe Fig 2 2 Auto Queue window B Ending one button measurement After one button measurement ends remove the sample according to the following procedure l Using the Auto Queue window make sure that the one button measurement has completed If the method name has disappeared from the Auto Queue window the one button measurement is complete 2 Open the Sample window 3 Click on button The sample will be ejected from the SCM Make sure that the Sample State display changes to the eject condition 4 Remove the sample from the SCM insertion port NM ECA ECX TU 3 2 5 2 ONE BUTTON MEASUREMENT L 2 3 CANCELING MEASUREMENT To cancel the measurement during one button measurement operate as follows 4 aabe Automation Queue scc2 nmjeol co jp lt 2 gt x Ema METHOD Proton Gradient Shin GROUP Proton est time 0 01 40 f gt EXPERIMENT Proton ON SLOT 1 File usr people adhbe METHOD Carbon Gradient Shin GROUP Carbon est time 0 48 35 EXPERIMENT Carbon ON SLOT 1 File usr people aabe The numbers D and are referred to in the following steps Click on the Method part of one button measurement that you want to chancel in the Auto Queue window c amp CD in above figure The method is highlighted Be s
15. Job Info window eseese 5 3 L Loans ID AER o eee in b oot 4 6 LOSNIO CR i daran river HORE Ode 6 6 Loading the sample 1 8 LOO Se Ale irons 6 7 Lock Status 2 4 INDEX M M eau e 3 11 M easurement conditions 2 7 Vili e TO TT 2 1 Molecule eeeenese 3 11 N BEER IO oo arte MERE 1 9 NOIRS BUB Los enseliieiexbiis bid idxkibidins 4 14 Notify MCN TEE 2 4 O One button measurement 2 1 Open Data for Processing window 4 6 6 6 Open Experiment window 3 1 P Pasting 1D NMR data 4 15 Peak sseeeeeenm eee 3 11 dic MT EEN E PA 3 11 PICE WE TTE ERTTNOOPUNS 3 11 EIN errn 3 11 xiii RT 2 7 3 9 4 16 Preparation for one button Mic E HIP 2 3 Preset DUtON ccccceseeseeeeeeeeeeeereeess 4 13 Pet IG AEEA 2 7 Processing condition sssssee 2 7 Due Lion 4 3 DO m a 4 3 pulse_angle_1 4 2 pulse angle 2 4 2 Q ELI 01 RETE 5 2 R recvr gain 3 2 3 5 4 2 4 4 Reference e 3 11 VEztllo CR RTT 3 11 relaxation delay 3 3 3 5 4 2 4 5 Rename Data File to window 6 2 Fatigues ean 3 13 4 18 S sample id 3 2 3 4 4 2 4 4 Samale he Orink 1 6 Sample Status 2 3 Sample window eeeene 1 5 Save Data File window 6 3 Saving Processed Data
16. Open Experiment window and click on the Ok button The Experiment Tool window opens 4 14 aabe Experiment Tool hetcor exe File Tools View Options Fig 4 3 Experiment Tool window 3 Setthe necessary parameters The parameters which are usually used are explained below c For information about other parameters refer to the separate MEASUREMENT user s manual Parameters can be displayed by double clicking on Header Instrument Acquisition or Pulse sample id Name to identify sample comment Comments on measurement data auto gain Normally do not check this box for 2D measurement solvent Solvent used for NM R lock recvr gain Set the gain which was used for PC 1D measurement x points Number of data points on the f axis scans Number of scans to accumulate y points Number of data points on the f axis j constant J value 4 4 NM ECA ECX TU 3 4 2DNMR MEASUREMENT ommum um relaxation delay Pulse delay time 4 Verify the necessary parameters Parameters can be displayed by double clicking on Header Instrument Acquisition or Pulse x domain Observation nucleus Carbon x Offset Observation center frequency ppm X Sweep Observation range ppm y domain Irradiation nucleus Proton y offset Irradiation center frequency ppm y sweep Irradiation range ppm total time A pproximate time necessary for measurement x pulse PC pulse width to be used for measurement y pulse tH pulse width to be us
17. Open Data for 1D Processor window using the buttons One is a local directory The other is a global directory Normally the user uses the local directory Local directory Clicking on the N button displays a list of the files in the local directory in the middle of the O pen Data for 1D Processor window The local directory is specified in DATA in the delta_configure file Global directory Clicking on the al button displays a list of the files in the global directory in the middle of the Open Data for 1D Processor window Because the global directory cannot be used for writing itis not used to store data The global directory is specified in GLOBAL in the delta configure file NM ECA ECX TU 3 6 7 INDEX 7 PC measurement conditions 3 4 1D NMR data processing 3 7 1D Processor window 3 7 4 7 H measurement conditions 3 1 A Annotation sseeeeeenee 3 11 ABDIV BUDDOPLu cm ovre n dip tandi 4 14 auto gain 3 2 3 4 4 2 4 4 Automatic baseline correction 3 8 Automatic integration ceecee 3 9 Automatic peak detection 3 9 A utomatic resolution adjustment 1 9 2 7 Automation window 2 3 Auto Queue window 2 5 B ESAO RTT RT 4 14 BIS EIN Loa recto ieeaace liene dieu 4 14 Bottom sSlid r ueserprtdus ad MORE MOdUA 4 13 C Canceling measurement
18. Processor window Automatic peak detection and automatic integration are carried out and the results are displayed in the lower spectral display area in the 1D Processor window Ps H aabe 1D Processor single_pulse 1 jdf File Options PreTransform Window Transform PostTransform Display Preferences am ia o 3 s o Jes e onore D EM 5 213 l dc balance 0 FALSE E 2 sexp 2 Hz 0 0 s 3 trapezoida U 80 4 zerofill 1 5 fft 1 TRUE TRUE Fi 0 1 0 2 3 0 4 05 06 0 7 08 09 L0 11 12 13 14 15 16 17 ali E 4 100 0 200 0 12 0 11 0 10 0 90 80 70 6 0 50 Sii 34 n Jt 11 bw TE 25733 24623 A parts per Million 1H PP sore Amnis 3 3 3 Plotting The standard method of plotting is as follows Click on the ial button in the 1D Processor window E 4X4 aabe 1D Processor single pulse 1 jdf IEEE File Options PreTransform Window Transform PostTransform Display Preferences ais aralera s ee e eJ x E 13 os 6 nn 2c id aeaa aala The processed spectrum in the lower display area is plotted on paper NMECA ECX TU 3 3 9 3 1DNMR MEASUREMENT 3 3 4 Changing the Display Range B Usage of Cursor Tool bar The Cursor Tool bar is used to expand or reduce spectra The Cursor Tool bar is available in each display area This section explains basic usage of the Cursor Tool bar e To display the Cursor Tool bar Mov
19. and click on the OK button les When creating a new directory after specifying a directory name in the Path input box click on the button Create the directory and move it After that enter the filename to save it into the filename entry box 4 Start measurement W hen measurement is complete the data is saved with the specified name B Specifying a saving file name after measurement W hen you did not specify a filename before measurement the measured data is saved With a filename specified in the Experiment Tool window Change this saved filename using the following procedure l Select File C hange Working File from the 1D Processor or nD Processor window The Rename Data File to window opens amp Save Collected Data To x Path Ausr people aaberfiles data4 Filename entry box Fig 6 3 Rename Data File to window 2 Type any filename in the filename entry box le When creating a new directory after specifying a directory name in the Path input box click on the button Create the directory and move it After that enter the filename to save it into the filename entry box 3 Click on the Ok button T he filename of the measurement data FID changes to the specified filename If that filename exists the version number is incremented by one 6 2 NMECA ECX TU 3 6 SAVING AND LOADING DATA 6 1 2 Saving Processed Data mM To save 1D processed data in the 1D Processor window under the same
20. buttons 3 To finish viewing click on the Close button TheJ ob Info window is closed NM ECA ECX TU 3 5 3 SAVING AND LOADING DATA Chapter 6 explains how to save NMR data and how to load data from a file Be 1 031 51540 eom 6 1 6 1 1 Saving the measured data FID enn 6 1 6 12 5aving Processed Dala ERREUR 6 3 ER 29718 D e A MH M M ENG 6 6 NM ECA ECX TU 3 6 SAVING AND LOADING DATA 6 1 SAVING NMR DATA 6 1 1 Saving the measured data FID The measured data FID is saved automatically A file name for the saved data is specified as in the following procedure B Specifying a file name for saved data before measurement l Specify the file name to the data you want to save in the filename of the Experiment Tool window 4 aabe Experiment Tool single pulse ex2 File Tools View Options File name active global std proton autophase list Edit 4 F E save aborted i am jeol co jp Total Collection Time 00 01 03 Fig 6 1 Experiment Tool window 2 When specifying the directory to save click on filename or on the Browse button The Save Collect Data to window opens 44 Save Collected Data To Path usr people aaberfiles date File name entry box Fig 6 2 Save Collect Data to window NM ECA ECX TU 3 6 1 6 SAVING AND LOADING DATA 3 After moving to the directory to save enter the file name to save it in the Name entry box
21. filename Click on the button in the 1D Processor window iia aabe 1D Processor single pulse 1 jdf File Options PreTransform woe Transform PostTransform Display Preferences ale ea ex a ols a t ae e rS EETESESTERES ET E B The 1D processed data is saved Then the version number increases automatically under the same filename E To save 1D processed data in the1D Processor window under a new filename l SelectFile Save As from the menu bar The SaveData File window opens ts Save Data File Path usr people aaberfiles data Filename entry box Fig 6 4 Save Data File window 2 Type any filename in the filename entry box les When creating a new directory after specifying a directory name in the Path input box click on the button Create the directory and move it After that enter the filename to save it into the filename entry box 3 Click on the Ok button The 1D processed data is saved under the specified filename NM ECA ECX TU 3 6 3 6 SAVING AND LOADING DATA m unum E To save 2D processed data in the 2D Viewer window under the same filename Click on the button 4 4 2D Viewer cosy 2 jdf File Options View Project 53e Expansion Tools Analysis Display ay See 3 ETE S EIER project L mj z 8 z a d 120 11 0 100 9 0 80 7 0 6 0 5 0 4 0 3 0 2 0 1 0 10 200 10 20 X parts per Million
22. from J EOL are stored The files in this directory cannot be changed NM ECA ECX TU 3 3 1 3 IDNMR MEASUREMENT 4 51 aabe Experiment Tool single pulse exz ker m cse in sample id comment auto gain filter limit ef be M E LM Torce ine save aborted TRAC TTA Le Total Collection Time 00 01 03 Fig 3 2 Experiment Tool window 4 Setthe necessary parameters Thefollowing parameters are usually used c For information about the other parameters refer to the separate volume USER S MANUAL MEASUREMENT Parameters can be displayed by double clicking on Header Instrument Acquisition or Pulse sample id Name to identify sample comment Comment on measurement data auto gain If you want the instrument to adjust the receiver gain automatically click on the button to mark it with a check mark The results that were acquired using the automatic gain will be displayed on the M aster Console window and the Spectrometer Control window solvent Solvent used for NMR lock If the NMR lock was already used on the Sample window or another window the solvent used has already been set recvr gain Receiver gain if automatic gain is not selected x points Number of data points to measure in each scan scans Number of scans to accumulate 5 Make sure that other necessary parameters are set appropriately 4S Parameters can be displayed by double clicking on Header Instrument Acquisition or Pulse x domain Observ
23. mee PP ne nm T x_offset and x_sweep are set to the offset and range values of the area where the 1D NMR data is displayed 5 Click on the View Y button as well The mouse pointer changes to the shape of a finger 6 Move the mouse pointer to the position of the 1D data H 1D data for example and click the left mouse button y offset and y sweep are set to the offset and range values of the area where the 1D NMR data is displayed 4 9 4 2DNMR MEASUREMENT 4 2 STARTING AND ENDING MEASUREMENT B Starting measurement and displaying the present status Click on the Submit button in the Experiment Tool window The measurement is entered into the spectrometer control computer s queue The spectrometer executes measurement on a first in first out basis The command for starting measurement can be issued repeatedly even if another measurement is being performed After one measurement finishes the next meas urement will be started under the stored measurement conditions This mark indicates hat measurement is being executed Current measure 34660231 ment ur IS being absolute value COSY execute 99 SEP 2003 18 20 28 Next measurement that is waiting to be executed This mark indicates that next measure ment is waiting to be executed B Ending measurement W hen the measurement finishes the nD processor window opens c To stop the measurement during operation refer to Chapter
24. previous values You cannot selectively return only the vertical or horizontal size to its previous value B To return the spectrum display to its initial conditions Press the key on the keyboard T he horizontal and vertical scales return to their initial values eer qe eg ERE 4 18 NM ECA ECX TU 3 QUEUING This chapter explains how to start measurement and how to control queues 51 COMMAND FOR STARTING MEASUREMENT nn 2 1 JU MERC UD P 2 2 NM ECA ECX TU 3 5 QUEUING uim m 5 1 COMMAND FOR STARTING MEASUREMENT B Starting measurement and displaying the present status Clicking on the Submit button in the Experiment Tool window enters the measurement into the spectrometer control computer s queue and the spectrometer executes measurement on a first in first out basis ta aabe Experiment Tool cosy ex2 File Tools View Options The command for starting measurement can be issued repeatedly even if another measurement is being performed After one measurement finishes the next measure ment will be started under the stored measurement conditions tal aahe Spectrometer Control Tools Config Queue Machine Options This mark indicates hat measurement is being executed Current measure 84541223 ment that is being single pulse executed 17 SEP 2003 15 02 06 Next measurement that is waiting to be executed This mark indicates that next measure ment
25. pulse ex2 Proton and DQF COSY H double quantum filter COSY dqf cosy ex2 1D H normal measurement single pulse ex2 Proton and NOESY i 1H NOE correlation measurement noesy ex2 1D H normal measurement single pulse ex2 Proton and TOCSY TOCSY TOtal Correlation pened Spectroscopy single pulse ex2 Hetcor single pulse dec ex2 single pulse ex2 Flock single pulse dec ex2 NMECA ECX TU 3 2 1 2 ONE BUTTON MEASUREMENT Method Combination 1 Gradient COSY Gradient DQF COSY Gradient TOCSY Gradient PS NOESY Gradient HMQC Gradient HMQC with y proj Gradient HM BC Gradient HMBC with y proj Gradient HMQC TOCSY HMQC TOCSY with y proj Combination 2 2 2 0 Sequence name Measurement 1D H normal measurement single pulse ex2 1D PC normal measurement single pulse dec ex2 Automatic determination of C atomic group by means of DEPT Homonuclear 2D H H COSY COSy ex2 Heteronuclear 2D C H COSY hector ex2 dept ex2 1D H normal measurement Homonuclear 2D H H COSY 1D H normal measurement tH double quantum filter COSY single pulse ex2 cosy pfg ex2 single pulse ex2 dqf cosy pfg ex2 1D H normal measurement single pulse ex2 TOCSY tocsy pfg ex2 1D H normal measurement single pulse ex2 tH homonuclear NOE correlation noesy pfgzz pn ex2 1D H normal measurement single pulse ex2 1D PC normal measurement single pulse dec ex2 H observation heteronuclear correlation hmqc_pfg
26. 5 Queuing 4 10 NM ECA ECX TU 3 4 2D NMR MEASUREMENT 2 4 3 DATA PROCESSING OF 2D NMR This section explains data processing immediately after completion of NMR measurement When measurement is complete Data will be sent from the spectrometer to the processing computer and the nD Processor window will open Data will be processed according to the process list in the pulse sequence AnD Processor cosy 1 jdf DE File Preiransioniu Whulew Cransfona Pestiransform Disphey Preferences as jajaj Y parts per Million 1H 120 110 100 90 __X parts per Million 1H Fig 4 6 nD Processor window If you change the processing conditions click on the 1 button to display the process list If you click on the 1 button again after changing the process list processing will be executed again according to the changed contents 4 nD Processor cosy 1 jdf File PreTransform Window Transform PostTransform Display Preferences fede EFECAN 3 fft 1 TRUE TRUE 4 ppm 5 abs 6 thresh 1 1 7 symmetrize Cosy 24 8 transpose Fig 4 7 nD Processor window Process list display screen NM ECA ECX TU 3 4 11 4 2DNMR MEASUREMENT 4 3 1 Displaying Data Using 2D Viewer Click on the button in the nD Processor window 4 3 nD Processor cosvy 1 jdf File Preiransioruu Siew CIrausfiorur fustiransform ineniey Preferences Jr ed e o a BEE
27. EOL Ltd 1 2 Musashino 3 chome Akishima Tokyo 196 8558 Japan Telephone 81 42 543 1111 Facsimile 81 42 546 3353 URL http Avww jeol co jp Note For servicing and inquiries please contact your JEOL service office NOTATIONAL CONVENTIONS AND GLOSSARY B General notations CAUTION Points where great care and attention is required when operating the device to avoid damage to the device itself ES Additional points to be remembered regarding the operation Se A reference to another section chapter or manual 1 2 3 Numbers indicate a series of operations that achieve a task A diamond indicates a single operation that achieve a task File The names of menus commands or parameters displayed on the screen are denoted with bold letters File Exit A command to be executed from a pulldown menu is denoted by linking the menu name and the command name with a dash For example File E xit means to execute the Exit command by se lecting it from the File menu Keys on the keyboard are denoted by enclosing their names in a box B Mouse operation M ouse pointer An arrow shaped mark displayed on the screen which moves with the movement of the mouse It is used to specify a menu item command parameter value and other items Its shape changes ac cording to the situation Click To press and release the left mouse button Double click To press and release the left mouse button twice quickly D
28. INSTRUCTIONS CONTENTS INDEX JNM ECA Series JNM ECX Series JNM ECS Series Delta V4 3 6 TUTORIAL MANUAL tL N INME epa AU Printed in Mp J NV ECA Series J NMECX Series J NMECS Series Delta V4 3 6 TUTORIAL MANUAL JNM ECA Series JNM ECX Series JNM ECS Series This manual is designed for new users of the JNM ECA JNM ECX or JNM ECS series FT NMR system who want to perform 1D or 2D NMR measurement It explains the basic procedures for operating the system For details of individual operations refer to the on line User s Manual Please be sure to read this instruction manual carefully and fully understand its contents prior to the operation or maintenance for the proper use of the instrument B L NOTICE e This instrument generates uses and can radiate the energy of radio frequency and if not installed and used in accordance with the instruction manual may cause harmful interference to the environment especially radio communications e The following actions must be avoided without prior written permission from JEOL Ltd or its subsidiary company responsible for the subject hereinafter referred to as JEOL modifying the instrument attaching products other than those supplied by JEOL repairing the instrument components and parts that have failed such as replacing pipes in the cooling water system without consulting your JEOL service office and adju
29. MEASUREMENT v o 1 3 2 Sample Loading NMR Lock and Automatic Resolution Adjustment Sample loading NMR lock and automatic resolution adjustment are performed using the Sample window dW aabe Sample scc nm jeol co jp Field Strength Helium Nitrogen 11 7473579 T I 99 85 95 Sample State Spinner Temperature O A Sry ProbeID 2692 my 13H Current 178 dC asma Target 4 25orac gt LLLA yl Shim Groups zl fa Ao Ad 165 aha pe j Lu The numbers D to are referred to in the following steps Fig 1 9 Sample window B Loading the sample e When an auto sample changer is not installed Insert into the SCM the sample which was set in the sample insertion port of the SCM Click on the 4i button in the Sample window ce D A in Fig 1 9 W hen the sample load completes the flask icon becomes full as shown below 5 e When an auto sample changer is installed l Seta sample to the slot of the auto sample changer 1 8 NMECA ECX TU 3 1 PREPARATION FOR MEASUREMENT 2 Set the slot numbers place a sample of the auto sample changer into the Slot of the Sample window c amp CD B in Fig 1 9 After carrying a sample to the top of the SCM insert it into the SCM When sample loading is complete the flask display changes as follows 5 9 B Spinning the sample Usually you measure the sample while spinning it I
30. N 6 A new 2D Viewer opens and projection data other than 2D data are displayed 4A 2D Viewer cosy 2 jdf File Options View Project icing Expansion Tools Analysis Display DIODE project Y Projectio Em tt 1 1 1 5 display area 2D data display area 120 110 10 0 90 8 7 0 6 0 5 0 4 0 3 0 2 0 1 0 0 X parts per Million 1H E E E 5 a i gt Fig 4 8 2D Viewer window 4 12 NM ECA ECX TU 3 4 2DNMR MEASUREMENT 4 3 2 Setting the Conditions for Displaying Contour Lines The 2D Viewer window is used to set the levels of the contour lines The Level Tool window is used to change the levels of the contour lines l Click the right mouse button to display the pop up menu and select Level Tool Logarithm Base b Display i Units 5 W Contour nm T Mesh Surface BI d Stack 4 F image 5 as patial Contour 6 if Draw Components b Datadex iD Datadex 2D gt save Curren View Vi Restore Saved View Sh p TheL evel Tool window opens IES Bounds Bias Contour line level button 24 pe Top slider Preset button i slider Bottom slider Threshold level Noise level Base level r 07 CONES Apply button Fig 4 9 Level Tool window Preset button Allows you to set the number of contour lines by selecting the 2 4 6 8 12 or 24 preset button Contour line level button The level of contour can be set manually by clicking on its button to h
31. OO0L 5th BLD sccd OWHED ECH400 R amp D DEHO sceh OWNED ECA5SOO R amp D DEHO sccb OHHED ECABOO R amp D DEHO SET J sewn Jf View co vy The numbers D and are referred to in the following steps Fig 1 3 Spectrometer Control window NM ECA ECX TU 3 1 3 1 PREPARATION FOR MEASUREMENT 2 Using the mouse select the spectrometer you want to connect to by clicking on its name in the list in the Spectrometer Control window amp in Fig 1 3 3 Click on the Connect button L7 Q in Fig 1 3 If the connection is carried out correctly the message Connect is displayed in the Spectrometer Control window as shown in Fig 1 4 a faabe Spectrometer Control Queue State OWNED Selected Job UNKNOWN Fig 1 4 Spectrometer Control window after the spectrometer is connected B Disconnecting from the spectrometer Click on the Unlink button in the Spectrometer Control window M A aabe spectrometer Control Queue State OWNED Selected Joh UNKNOWN Fig 1 5 Spectrometer Control window Spectrometer is connected W hen the spectrometer is disconnected the Spectrometer Control window returns to the display shown in Fig 1 3 1 4 NM ECA ECX TU 3 1 PREPARATION FOR MEASUREMENT ur 13 SAMPLE PREPARATION This section explains how to insert the sample into the SCM 1 3 1 Check Prior to Sample Insertion Check to make sure that no other sample is inserted in the SCM as follo
32. ation nucleus Proton 3 2 NMECA ECX TU 3 NM ECA ECX TU 3 X Offset X Sweep total time x pulse relaxation delay 3 IDNMR MEASUREMENT ae nr Observation center frequency 5 ppm Observation range 15 ppm Approximate time necessary for measurement Pulse width to be used for measurement Pulse delay time 3 3 3 IDNMR MEASUREMENT 3 1 2 Setting C Measurement Conditions l Click on the Expmnt button in the Spectrometer Control window The Open Experiment window opens 2 Click on the ay button in the Open Experiment window A list of the Experiment files in the Global directory is displayed 3 Select the measurement mode single pulse dec ex2 from the Open Experiment window and click on the Ok button The Experiment Tool window opens 4 14 aabe Experiment Tool single pulse dec exe File Tools View Options I EF EPET TEE EENET LE B o ut EN E T pam 5 uL zi a F 4 T zl my aH ta 4H wg qu ee qu T EE active global std carbon autophase list Edi z am peol co Total Collection Time 00 47 27 Fig 3 3 Experiment Tool window 4 Setthe necessary parameters Thefollowing parameters are usually used c For information about the other parameters refer to the separate volume USER S MANUAL MEASUREMENT Parameters can be displayed by double clicking on Header Instrument Acquisition or Pulse sample id Name to identify sample comm
33. be 1D Processor single pulse 1 jdf File Options PreTransform Window Transform PostTransform Display Preferences aeaoe EET Ae n 100 0 200 0 2 sexp 0 2 H2 Dils 3 trapezoida U 80 4 zerofill 1 5 1 TRUE TRUE CA 4 m3 m F m E ua Tf m j D i 12 0 110 100 9 0 80 70 60 50 40 230 20 10 A parts per Million 1H Fig 3 4 1D Processor window NMECA ECX TU 3 3 7 3 IDNMR MEASUREMENT 3 3 1 Automatic Baseline Correction 1 Click on the button in the 1D Processor window An item Base Correct is added to the process list 2 Click on the Process button The spectrum with the baseline corrected is displayed in the lower spectral display area process list e tl aabe 1D Processor single pulse 1 jdf File Options PreTransform Window Transform PostTransform Display Preferences aaaea oasa E Daine wal E a GME a e s ec ia 5 fft 1 TRUE TRUE 6 machinephase EE anm 100 0 200 0 01 02 0 3 04 0 5 06 07 08 09 10 11 12 13 14 1 5 16 1 7 ad _ T X seconds 1H Division None TI n Width 10 20 230 40 50 60 70 80 9 0 0 120 11 0 100 90 80 70 68 5 0 40 30 20 10 0 10 20 parts per Million 1H PP sez sph 3 8 NMECA ECX TU 3 3 1DNMR MEASUREMENT 3 3 2 Automatic Peak Detection and Automatic Integration Click on the button in the 1D
34. conditions for general organic compound samples are used for one button measurement If you want to measure the sample under special conditions perform the measurement using individual operations e Hard disk capacity and data filename Make sure that there is free space to save data before performing one button measurement The results of one button measurement are saved in a file with a specified file name to which the method name is added If the filename already exists a new file With the version number one higher will be created e Processing condition In one button measurement parameters for data processing are prespecified If you want to perform your own specific data processing perform it later using the data that has been saved in the file e Plotting In one button measurement data will be plotted automatically Therefore make sure that chart paper is set in the printer correctly and that the printer is online before starting one button measurement NMECA ECX TU 3 2 7 1D NMR MEASUREMENT Chapter 3 explains the procedures for the basic 1D NMR measurement in the order of measurement data processing and plotting It is assumed that the Delta system has been connected to the spectrometer and that the sample setup sample loading NMR lock resolution adjustment and other operations prior to measurement have already been performed f you are not ready to start measurement prepare for measurement according to Chapter
35. d the mouse pointer on the spectral screen changes to 9M 2 Move the mouse pointer to the position that will become the upper end of the expanded Y axis 3 Drag the left mouse button to the position that will become the lower end of the expanded Y axis 4 Release the left mouse button 10 0 Mr pep TH inpune A 80 70 69 5 The spectrum is expanded vertically To expand a spectrum horizontally l Select the Zoom mode from the Cursor Tool bar or press the key on the keyboard The Cursor Tool mode becomes Zoom 2 Move the mouse pointer to the position that will become the left end of the expanded X axis 3 Drag the left mouse button to the position that will become the right end of the expanded X axis 4 Release the left mouse button Il ij ra ely i i Il I f M fi ill TE nm i T A X parts per Million 1H The spectrum is expanded horizontally 3 12 NM ECA ECX TU 3 3 IDNMR MEASUREMENT To adjust the display to the intensity of the highest peak displayed Press the key on the keyboard ee The highest peak in the spectral region displayed at present is expanded or reduced to fit within the screen To return the spectrum display to its previous conditions Press the key on the keyboard to return to the previous conditions You can return to the previous conditions up to 16 times E 6 OUR E JE C
36. e ee Wotity Noty n and Dept 135 iaz A Fig 2 1 Automation window U sually the name of the sample is used Enter a comment Sample number of the automatic sample changer M essages about the present sample status such as LOADED and EJECT Set temperature used during temperature control Present sample temperature 2 ONE BUTTON MEASUREMENT T emp State L ock Status Solvent Notify Hold Specify whether or not to carry out temperature control using the temperature controller Present status of the NM R lock Select the sample solvent Information is sent to the specified E mail address when measure ment is complete In order to use this function it is necessary to per form the basic setting before using mail Even when a sample number is changed Notify E mail address is placed on hold B Starting one button measurement Click on the desired method button M easurement starts Method buttons Ji Pe Pd an eee F delta autamation auto Proton Presaturatisu qal nas qai quce cante a pip i a RETS C Larbon Proton and Carbon b Carhon and Dept 135 Proton and COSY Proton and TOCSY cii C acr adient COSY W hen measurement starts the Auto Queue window opens as shown in Fig 2 2 NM ECA ECX TU 3 2 ONE BUTTON MEASUREMENT on Gradient Shin GROUP Proton est time 0 01 40 i gt EXPERIMENT Proton ON SLOT 1 File usr people aabe
37. e the mouse pointer to the spectral display area in which you want to display the Cursor Tool bar The Cursor Tool bar is displayed at the upper right in the spectral display area CERCEI 10 20 30 40 50 60 70 80 LE j i 1 120 11 0 100 90 80 70 60 50 40 30 20 10 10 20 parts per Million 1H Tab button Operation buttons Key command Mode button used in the button selected mode Fig 3 5 Normal display of Cursor Tool bar e To minimize the Cursor Tool bar Click on the tab button The Cursor Tool bar changes from the normal display shown in Fig 3 5 to the minimized display shown in Fig 3 6 Fig 3 6 Minimized Cursor Tool bar To return the minimized Cursor Tool bar to the normal display Click on the tab button The minimized Cursor Tool bar returns to the normal display shown in Fig 3 5 3 10 NM ECA ECX TU 3 3 IDNMR MEASUREMENT i e To switch the Cursor Tool mode l Move the mouse pointer to the mode button at the right end of the Cursor Tool bar then press and hold the left mouse button Thefollowing thirteen modes are displayed under the mode button Zoom To expand reduce or move spectra Select To select data or a geometry R egion To display a selected region in another geometry Cursor To correct the baseline or to display the difference between two points Reference To set a chemical shift reference axis marker Peak To execute a peak pick Pic
38. ed for measurement x Offset x sweep y offset and y sweep can be set from 1D NMR data which has already been processed For the procedure refer to Section 4 1 3 Setting the measurement range from 1D NM R data NMECA ECX TU 3 4 5 4 2DNMR MEASUREMENT 4 1 3 Setting the Measurement Range from 1D NMR Data To measure H H homonuclear 2D NMR H 1D NMR data is necessary To measure H detection heteronuclear 2D NMR or C detection heteronuclear 2D NMR H 1D data and PC 1D data are necessary If 1D data is already loaded in the 1D Processor window proceed to B Setting the measurement range from 1D NMR data If these 1D NMR data are not yet displayed in the 1D Processor window load data in the 1D Processor window from the file as follows E Loading 1D data 1 Click on the I button in the Delta Console window ata aabe Delta File Processors Viewers Tools Analysis Acquisition Delta NMR Processing and Control Software Copyright 1990 2003 by JEOL USA Inc Fig 4 4 Open Data for Processing window 2 Using the mouse select the 1D NMR data from the data file list in the Open Data for Processing window 3 After you selectthe file from the Open Data for Processing window click on the Ok button The data is loaded and the 1D Processor window opens 4 6 NM ECA ECX TU 3 4 2DNMR MEASUREMENT m B 4X 4 1D Processor single pulse 1 jdf File Options PreTransform Window Transform P
39. eds a large amount of memory in the system slowing down the processing of the program Set the levels according to the following procedure Click on the bottom contour line level button Determine the bottom level of the contour lines using the bottom slider Determine the top level of the contour lines using the top slider Select the number of contour lines you want to display from the preset buttons e Click on the Apply button ceo cgo 4 14 NM ECA ECX TU 3 4 2DNMR MEASUREMENT 4 3 3 Pasting 1D NMR Data This section explains how to paste 1D NMR data onto the slice or projection data display area in the 2D Viewer window It is assumed that 1D NMR data on which data processing such as FFT was already performed is stored on the hard disk or is displayed in the 1D Processor window B When 1D NMR data is stored on the hard disk 1 Click on the button 4 14 2D Viewer cosy 2 jdf w irix File Options View Project 53i Expansion Tools Analysis Display 2 To paste 1D data onto the X axis a Select Display High Res Load X Projection 2D Viewer cosy 2 jdf File Options View Project Siicing Expansion Tools Analysis Display Gel wee paosgs project Y HighRes LoadXSlice Fai EN e Load Y Slice Load Y Projection b Select a file ID NMR data is pasted in the projection display area of the X axis 3 To paste 1D data onto the Y axis a
40. ent Comment on measurement data auto gain If you want the instrument to adjust the receiver gain automatically click on the button to mark it with a check mark 3 4 NMECA ECX TU 3 NM ECA ECX TU 3 3 IDNMR MEASUREMENT C solvent Solvent used for NMR lock If the NMR lock was already used on the Sample window or another window the used solvent has been set recvr gain Receiver gain if automatic gain is not selected irr noise Noise source for irradiation Normally WALTZ is used x points Number of data points to measure in each scan scans Number of scans to accumulate irr domain Irradiation nucleus Proton irr offset Irradiation position 5 Make sure that other necessary parameters are set appropriately Parameters can be displayed by double clicking on Header Instrument Acquisition or Pulse x domain Observation nucleus Carbon13 x Offset Observation center frequency 100 ppm X sweep Observation range 250 ppm total time Approximate time necessary for measurement x pulse Pulse width to be used for measurement relaxation delay Pulse delay time 3 5 3 IDNMR MEASUREMENT 3 2 STARTING AND ENDING MEASUREMENT This section explains how to start and end 1D NMR measurement and how to confirm the measurement status B Starting measurement and displaying the status Click on the Submit button in the Experiment Tool window The measurement is entered into the spectrometer control computer s queue
41. ex2 1D H normal measurement single pulse ex2 H observation heteronuclear correlation spectroscopy hmqc_pfg ex2 1D H normal measurement single pulse ex2 1D PC normal measurement single pulse dec ex2 tH observation heteronuclear long range correlation spectroscopy hmbc pfg ex 1D H normal measurement single pulse ex2 tH observation heteronuclear long range correlation spectroscopy hmbc_pfg ex2 1D H normal measurement single pulse ex2 1D PC normal measurement HM QC TOCSY 1D H normal measurement HM QC TOCSY 1D H normal measurement single pulse dec ex2 hmqc tocsy pfg ex2 single pulse ex2 hmqc tocsy pfg ex2 single pulse ex2 1D PC normal measurement Homonuclear 2D H H COSY H observation heteronuclear correlation spectroscopy single pulse dec ex2 cosy pfg ex2 hmqc pfg ex2 NM ECA ECX TU 3 2 ONE BUTTON MEASUREMENT 2 2 STARTING AND ENDING MEASUREMENT B Preparation for one button measurement e Setting the sample in the SCM c Insert the sample according to the procedure in Section1 3 Sample preparation Opening the Automation window Click on the Auto button in the Spectrometer Control window The Automation window opens Filename Comment Slot Sample Status T emp Set Curr T emp NM ECA ECX TU 3 4 53 aabe Automation scc2 nm jeol co jp File Sample Ten ser Mesci Curr Temp vma Terp atate remporr 4l Lock Status pu Solvent EAA r
42. f you want to measure the sample without spinning proceed to BINMR lock Click on the button lt s in Fig 1 9 W hen the sample starts spinning the toppled top will be upright as shown below B NMR lock Select the solvent to be used for NMR locking and execute the NM R lock command 1 Select the solvent to be used for NMR locking from the Solvent list box gt 3 in Fig 1 9 If the solvent does not appear in the list box move the slider at the right side of the box 2 Click on the amp b button in Fig 1 9 W hen the NM R lock operates the messages LOCK ON and IDLE are displayed at the bottom right of the L ock C ontrol section 3 Click on the button ce in Fig 1 9 W hen the following message window appears optimization of the Lock Phase will be performed dM aabe Inform 7 aabe Inform sce nm jeolco jp scca nm jeolLco jp INFO INFO Optimizing Lock Phase Finished Optimizing Lock Phase within 45 degree window Optimization started Optimization finished E Automatic resolution adjustment Specify the axes for automatic resolution adjustment ce in Fig 1 9 Select Z1 Z2 from the pulldown menu When selection is complete resolution adjustment for Z1 and Z2 axes starts automatically NM ECA ECX TU 3 1 9 ONE BUTTON MEASUREMENT Chapter 2 explains automatic measurement using one button operation 2 l 2 2 d 2 4 NM ECA ECX TU 3 fis 4 07 re
43. i a surgkicio bes ek ryREHE Apo RERUUN PERI KE HE P ohm 1 5 1 3 2 Sample Loading NMR Lock and Automatic Resolution A djustment 1 8 NM ECA ECX TU 3 1 PREPARATION FOR MEASUREMENT 1 1 STARTING AND EXITING THE DELTA PROGRAM This section assumes that the data system has started normally and that the login Operation is complete c For starting the data system and login refer to the separate manual on the Workstation B Starting the Delta program NM ECA ECX TU 3 Double click on the ll Delta icon on the screen The Delta program starts and the Delta C onsole window opens A faabe Delta File Processors Viewers Tools Analysis Acquisition Delta NMR Processing and Control Software Copyright 1990 2003 by JEGL USA Inc Version 4d 3 Beta 09 15 03 17 23 Linux 21 CFR part 11 technical features are enabled Fig 1 1 Delta Console window 1 1 1 PREPARATION FOR MEASUREMENT B Ending the Delta program After measurement or NMR data processing is complete terminate the Delta program as follows l SelectFile Quit in the Delta Console window First point to File in the menu bar in the Delta Console window and press and hold the left mouse button A pull down menu appears Then while holding down the left mouse button move the mouse to highlight Quit in the pull down menu and release the left mouse button there aahe Delta Fite vocessors Viewers Tools Analysis Acqu
44. ighlight it Top slider D etermines the maximum intensity of the contour lines Bottom slider D etermines the minimum intensity of the contour lines NMECA ECX TU 3 4 13 4 2DNMR MEASUREMENT Bias slider D etermines the signal intensity between the ones specified by the top slider and the bottom slider M oving the bias slider changes the slope of the middle curve shown in Fig 4 8 Moving it upward results in drawing more contour lines at the lower level of the signal intensities Noise level Automatically set after data processing is completed Threshold level Automatically set after data processing is completed and used for peak picking in 2D processing B ase level Zero level of the signal intensity Set it to the lowest level in the L evel tool window Apply button Clicking on this button redraws the contour lines at the set levels 2 Adjustthe levels of the contour lines in the Level Tool window Set the minimum intensity based on the noise level Set the number and intensity of the contour lines to be drawn between the minimum intensity and the maximum intensity in the L evel Tool window 4 Level Tool ole Bounds Bias 24 Noise level 5i ES Ee Ls L5 EL 30 0 EA 10 0 EG 10 0 si Usually few or no contour lines are set to levels below the noise level Setting the contour level below the noise level displays the contour lines of noise and ne
45. instrument inappropriately controlled or managed for the maintenance e After installation or delivery of the instrument if the instrument is required for the relocation whether it is within the facility transportation resale whether it is involved with the relocation or disposition please be sure to contact your JEOL service office If the instrument is disassembled moved or transported without the supervision of the personnel authorized by JEOL JEOL will not be held responsible for any loss damage accident or problem with the instrument Operating the improperly installed instrument might cause accidents such as water leakage fire and electric shock e The information described in this manual and the specifications and contents of the software described in this manual are subject to change without prior notice due to the ongoing improvements made in the instrument e Every effort has been made to ensure that the contents of this instruction manual provide all necessary information on the basic operation of the instrument and are correct However if you find any missing information or errors on the information described in this manual please advise it to your JEOL service office e n no event shall JEOL be liable for any direct indirect special incidental or consequential damages or any other damages of any kind including but not limited to loss of use loss of profits or loss of data arising out of or in any way connected with the
46. is waiting to be executed Fig 5 1 Displaying the status of the queue NMECA ECX TU 3 5 1 5 QUEUING B Deleting measurement You can delete measurements in the queue using the following procedures How to delete specified experiment l Click on the measurementto delete from the Spectrometer Control window The specified measurement is highlighted 2 Click on the B button in the Spectrometer Control window A window appears to verify deletion Are you sure you want to delete the selected experiment from the queue __ Fig 5 2 The window that verifies the queue to delete 3 To delete the queue click on the OK button How to delete all experiment from the pending queue l Select Queue Delete in the Spectrometer Control window jz Spectrometer Control Tools Config Machine Options sy i i y F Fig 5 3 The window that verifies the queue to delete 2 To delete the entire queue click on the OK button 5 2 NM ECA ECX TU 3 5 QUEUING B Viewing information about the jobs in the queue You can view the details of a job in the measurement queue as follows l Double click on the job whose information you want to view in the Spec trometer Control window TheJ ob Info window opens 4 Job Info for scc nm jeol co jp single pulse ex Atsushi Abe single pulse 814125313 Fig 5 4 Job Info window 2 Display the parameter you want to make sure of using the arrow AV
47. isition zx a ke En 5 IT Tirri 3 2 T J LT L l i 4 D Verify Quit The Confirm window opens tal aabe Confirm Are you sure you want to exit Delta All Windows Will Be Closed Unsaved Files May Be Deleted Fig 1 2 Confirm window 2 Click on the OK button The Delta program ends 1 2 NMECA ECX TU 3 1 PREPARATION FOR MEASUREMENT Cr e CONNECTING TO AND DISCONNECTING FROMA SPECTROMETER The Delta program can be connected with two or more spectrometers through the network in the JNM ECA ECX series FT NMR instrument For this reason before NMR measurement it is required to connect the Delta program with the spectrometer you will use After NMR measurement disconnect the NMR spectrometer from the Delta program Here we will explain how to connect and disconnect the Delta program and the NM R spectrometer B Connecting to the spectrometer 1 Click on the ea button in the Delta Console window Delta NMR Processing and Control Software Copyright 1990 2003 by JEOL USA Inc The Spectrometer Control window opens and a list of the currently available Spectrometers appear in the list box c amp Fig 1 3 The spectrometers which are marked as FREE are available for connection The spectrometers which are marked as OW NED are currently being used PUES Tools Tools Contig Quse pp ine Options Sh Jachine Siku 2 FREE ECA500 5th BLD al D sec3 OWNED ECAB
48. k To set the slice position of 2D data or read peak positions Integral To perform integration Annotation To display an annotation in the geometry PIP To display a selected part of the geometry within the present geometry Phase To adjust the phase Molecule X To display a structural formula and molecular formula in the geometry M easure M easure distance between peaks c This chapter explains only the Zoom mode For more information about the other modes refer to the separate volume USER S MANUAL DATA PROCESSING 2 Move the mouse pointer with the left mouse button still pressed to the mode you wantto select and release the mouse button The Cursor Tool bar changes to the buttons for the selected mode e To select a button Click on the button you want The button you clicked on changes to appear selected or pressed The explanation of the selected button is also displayed at the bottom right of the spectral display area c Clicking the middle mouse button on the mode button with displays a list of the buttons which can be used in the currently selected mode and an explanation of these buttons You can select the button you want to use from the list NMECA ECX TU 3 3 11 3 IDNMR MEASUREMENT B Expanding and resetting spectra in the 1D Processor window To expand a spectrum vertically 1 Select the Zoom mode from the Cursor Tool bar or press the key on the keyboard The Cursor Tool mode becomes Zoom an
49. nt Acquisition or Pulse sample id Name to identify sample comment Comments on measurement data auto gain Normally do not check this box for 2D measurement solvent Solvent used for an NMR lock recvr gain Set the gain which was used for normal H measurement x points Number of data points on the f axis Scans Number of scans to accumulate y points Number of data points on the f axis pulse angle 1 Flip angle 90 deg in Cosy pulse angle 2 Flip angle 90 deg or 45 deg in Cosy relaxation delay Pulse delay time 4 Verify the necessary parameters 4S Parameters can be displayed by double clicking on Header Instrument Acquisition or Pulse x domain Observation nucleus Proton x offset Observation center frequency ppm 4 2 NM ECA ECX TU 3 4 2DNMR MEASUREMENT ae ae X sweep Observation range ppm total time A pproximate time necessary for measurement x 90 width 90 pulse width pulse 1 First pulse width to be used for measurement pulse 2 Second Pulse width to be used for measurement JS X Offset and x sweep can be set from 1D NMR data which has already been processed For the procedure refer to Section 4 1 3 Setting the measurement range from 1D NMR data NM ECA ECX TU 3 4 3 4 2D NMR MEASUREMENT 4 1 2 HETCOR Measurement l Click on the Expmnt button in the Spectrometer Control window The O pen E xperiment window opens 2 Select the measurement mode htcor ex2 from the list displayed in the
50. ostTransform Display Preferences sug 2 gig sal ais Lo Ano Pres 2 Pres xij sc ia EH al PPM 1 de_balance 0 FALSE 2 sexp 0 2 Hz 0 s 3 trapezoids 0 80 4 zerofill 1 5 fft 1 TRUE TRUE 100 0 200 0 0 1 02 0 3 04 0 5 06 07 08 09 10 11 12 13 14 1 5 16 17 1 J Ir X seconds 1H Order fol Gain _ JFALSE Lmjqa H nno mj W EE JE End EXEYEI PP er Ap 0 10 20 30 40 50 60 70 80 9 0 120 110 100 9 0 80 7 0 60 50 40 30 20 10 0 10 20 X parts per Million 1H Fig 4 5 1D Processor window 4 If the loaded 1D NMR data is FID perform data processing such as FFT phase correction and reference setting referring to Section 3 3 1D NMR data processing If data processing has already been executed proceed to the next step B Setting the measurement range from 1D NMR data HH COSY l Expand the processed 1D NMR data to the range to be used for 2D NMR measurement 2 Click on the button in the Experiment Tool window 3 Click on the View X button Aa abe Experiment Tool cosy ex2 File Tools View Options The mouse pointer changes to 1 NM ECA ECX TU 3 4 7 4 2DNMR MEASUREMENT 4 Move the mouse pointer to the position of the processed 1D data and click the left mouse button 41D Processor single pulse 1 jdf File d PreTransform Window Transform PostTransform id Preferences T HAME
51. rag To hold down the left mouse button while moving the mouse To drag an item you point to an item on the screen and then drag it using the mouse NM ECA ECX TU 3 CONTENTS 1 PREPARATION FOR MEASUREMENT 11 STARTING AND EXITING THE DELTA PROGRAM 1 1 12 CONNECTING TO AND DISCONNECTING FROM A SPECTROMETER eciseichtnsietpE RENE RRIDEIDUINE III NDEH RN DM 1 3 L3 SAMPFLEPRER RATION Lrsesenitben eii nsan EEEE 1 5 1 3 1 Check Prior to Sample Insertion eem 1 5 1 3 2 Sample Loading NMR Lock and Automatic Resolution PGS TU V 1 8 2 ONE BUTTON MEASUREMENT L BENPBBAL oanensmiu nunca eee ene eae 2 1 2 2 STARTING AND ENDING MEASUREMENT nmn 2 3 2 3 CANCELING M EASUREM ENT een 2 6 EN PEREGRINI IRURE ERR MN NI PUN 2 7 3 1D NMR MEASUREMENT 31 SETTING 1D NMR MEASUREMENT CONDITIONS 3 1 3 11 Setting H M easurement Conditions eeeeene 3 1 3 1 3 Setting C M easurement Conditions ssiri 3 4 3 2 STARTING AND ENDING MEASUREMENT nnn 3 6 23 JDNHMBDSIATROLESSIEO Lastest MEINEM MIHI 3 7 3 3 1 Automatic Baseline Correction eene 3 8 3 3 2 Automatic Peak Detection and Automatic Integration 3 9 DEC EME oso PEU ERU URN 3 9 3 3 4 Changing the Display Range eeeme 3 10 4 2D NMR MEASUREMENT 4 1 SETTING 2D NMR MEASUREMENT CONDITIONS 4
52. sting the specified parts that only field service technicians employed or authorized by JEOL are allowed to adjust such as bolts or regulators which need to be tightened with appropriate torque Doing any of the above might result in instrument failure and or a serious accident If any such modification attachment replacement or adjustment is made all the stipulated warranties and preventative maintenances and or services contracted by JEOL or its affiliated company or authorized representative will be void e Replacement parts for maintenance of the instrument functionality and performance are retained and available for seven years from the date of installation Thereafter some of those parts may be available for a certain period of time and in this case an extra service charge may be applied for servicing with those parts Please contact your JEOL service office for details before the period of retention has passed e In order to ensure safety in the use of this instrument the customer is advised to attend to daily maintenance and inspection In addition JEOL strongly recommends that the customer have the instrument thoroughly checked up by field service technicians employed or authorized by JEOL on the occasion of replacement of expendable parts or at the proper time and interval for preventative maintenance of the instrument Please note that JEOL will not be held responsible for any instrument failure and or serious accident occurred with the
53. the data file you want to load in the list box 3 Click on the Ok button The most recent version of data is displayed in the 1D Processor window or nD Processor window The following information on the most recent version of data is displayed in the data information display box Time domain frequency domain unit s Time domain data FID data Hz PPM Frequency domain data Fouriertransformed data 1D 2D nD Row of data Number of data points R Ranged 5 Sparsed i 1D 16384c 256K 3 R Revision time 2 O06T 2003 13 18 43 2 0CT 2003 13 19 43 single pulse 53477498 Comment Sample ID Creation time If you want to display earlier data select the version number referring to in formation in the data information display box and click on the O k button 6 6 NMECA ECX TU 3 6 SAVING AND LOADING DATA BH Version number In the Delta program a version number is appended to each data filename Before data iS processed a new file is automatically created under the same filename with a different version than that of the original data The original data is not processed preventing corruption of the original FID data If you save data under the existing filename the data iS given a version number one higher Copied data is sometimes deleted after it is processed Therefore some of the version numbers in the file list are usually omitted B Directory You can specify two directories in the
54. the neutral position of the auto sample changer At the same time verify that the Sample State indicator changes to the ejected state 3 Take the sample out of the slot of the auto sample changer 1 6 NMECA ECX TU 3 1 PREPARATION FOR MEASUREMENT B Setting up the sample Be sure to wear protective gloves when handling a sample tube containing a poisonous sample If the sample tube breaks this allows you to avoid contact with any sample that leaks l Setthe sample tube with the sample in it in the holder Since the resolution varies according to the sample volume height it is recom mended that you standardize the sample volume An appropriate sample height is approximately 4 cm 3 8 to 4 2 cm Sample tube Rotor Holder Sample gauge Make sure that there is no gap between the rotor and the holder Center of the detection coil Align the center of the sample with this position Fig 1 8 Setting up the holder 2 Check to make sure that the air is flowing by holding your hand over the sample insertion port of the SCM f air is not flowing never insert the sample tube into the insertion port of the SCM Another sample may already have been inserted or there might be a problem with the air system 3 Put the sample in the holder into the sample insertion port of the SCM and gently release it The sample levitates on the compressed air NM ECA ECX TU 3 1 7 1 PREPARATION FOR
55. ure to click on a METHOD without clicking on GROUP and EXPERIMENT 2 Click on the Remove button ce 2 in above figure c f you click on the Remove button when GROUP and EXPERIMENT are selected by mistake cancellation is not performed correctly Perform the cancellation operation again after updating the queue by selecting O ption the Refresh Queue in the menu bar 2 6 NMECA ECX TU 3 2 ONE BUTTON MEASUREMENT 2 4 PRECAUTIONS e Specifying an NMR lock solvent The difficulties which occurs most frequently in one button measurements is an NMR lock error To prevent NM R lock errors make sure that the solvent name is entered correctly Automatic resolution adjustment If the volumes of the samples to be measured are greatly different or solid substances are present in the sample the automatic resolution adjustment takes a long time U nder these conditions the appropriate resolution may not be achieved To prevent these difficulties prepare the samples with about the same height of 4 cm and align the bottom of the sample tube with that of the sample gauge e Probe tuning The probe tuning varies depending on measurement parameters such as solvent or temperature Especially before performing a measurement such as DEPT that is sensitive to pulse width or when measuring a small amount of a sample that requires improvement of the S N ratio be sure to tune the probe e Measurement conditions The measurement
56. use of the information contained in this manual or the software described in this manual Some countries do not allow the exclusion or limitation of incidental or consequential damages so the above may not apply to you e This manual and the software described in this manual are copyrighted all rights reserved by JEOL and or third party licensors Except as stated herein none of the materials may be copied reproduced distributed republished displayed posted or transmitted in any form or by any means including but not limited to electronic mechanical photocopying recording or otherwise without the prior written permission of JEOL or the respective copyright owner e When this manual or the software described in this manual is furnished under a license agreement it may only be used or copied in accordance with the terms of such license agreement Copyright 2002 2003 2004 2007 JEOL Ltd e n some cases this instrument the software and the instruction manual are controlled under the Foreign Exchange and Foreign Trade Control Law of Japan in compliance with international security export control If you intend to export any of these items please consult JEOL Procedures are required to obtain the export license from Japan s government TRADEMARK e Windows is a trademark of Microsoft Corporation e All other company and product names are trademarks or registered trademarks of their respective companies MANUFACTURER J
57. ws 1 Connect to the spectrometer according to the procedure of Section 1 2 2 Click on the Sample button in the Spectrometer Control window The Sample window opens A A aabe Sample scc2 nm_jeol co jp 11 7473579 T ore ess Sample State Spinner Tas Fig 1 6 Sample window 3 Verify that the Sample State section in the Sample window indicates that no sample is loaded NMECA ECX TU 3 1 5 1 PREPARATION FOR MEASUREMENT Green bar Green bar Sample State s eh A sample is loaded No sample is loaded Fig 1 7 Sample State If the display shows that no sample is loaded proceed to B Setting up the sample If the display shows that a sample is loaded remove the sample according to the procedure B Ejecting the sample B Ejecting the sample e When an auto sample changer is not installed If a sample is inserted in the SCM remove it l Click on the Sample button in the Spectrometer Control window to open the Sample window 2 Click on the button The sample in the SCM is ejected Verify that the Sample State section indicates that the sample has been ejected 3 Remove the sample from the insertion port on the SCM A A e When an auto sample changer is installed Another sample has been inserted into SCM take out the sample according to the following procedure l Open the Sample window 2 Setthe Slot number to 0 The sample can be ejected from the SCM and is moved to
Download Pdf Manuals
Related Search