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JNM-ECA Series JNM-ECX Series JNM-ECS Series

1. alale 14 37166 s 12 0 11 0 100 90 80 70 60 50 40 30 20 10 0 10 20 P X parts per Million 1H Mode Weighted Linear Inv Recovery 4 Peak Height 2 Click on the Peak Pick button Peak picking is carried out If required before picking peak change threshold level and noise level so that small signals or peaks having fine splitting which T value does not need may not be picked up NM ECA ECX USA 3 1 15 1 RELAXATION TIME MEASUREMENT 1 16 4 aabe Curve Analysis gibberellic_acid_ti_analysis 2 jdf x 120 110 100 90 80 70 60 6 3021 62838 5 7650 A X parts per Million 1H Mode Weighted Linear Inv Recovery j Peak eight E fn 3 Click on the Select button in the cursor tool Peak mode 4 Move the mouse pointer onto the X ruler of the spectrum display range press and hold down the left mouse button The curser appears 5 Move the cursor to the position which crosses to the top of the peak to obtain the current relaxation time and release the mouse button A peak position mark appears at the position at which the mouse button was released 4 aabe Curve Analysis gibberellic_acid_t1_analysis 2jdf OE 14 37166 s FIFI Thousands 1 0 12 0 11 0 100 90 80 70 60 50 40 30 20 10 0 10 20 1E N Veoh torne 3 48 S5neRuS QB DoT SHASAARA mn m Ti ri r r a N 6 3021 62838 5 7650 5
2. ae one ae 8 When tuning of Proton is complete click on the GO button Then the message of Carbon13 appears At this time the NMR system is already prepared for tuning iiA aabe Inform Please tune coil LF1 to 13C and click GO when complete probe_coarse NONE 9 Adjust the sensitivity of indicator for Carbon13 tuning If LEVEL METER of the head amplifier chassis is out of range or does not move far adjust the button and knob of METER GAIN 10 Check that no stick is attached for Carbon13 In nuclei other than Carbon13 since there are nuclei that need a stick refer to the data provided at delivery time 11 Adjust the LF TUNE dial of the probe first to minimize the LEVEL METER display and next adjust the LF MATCH dial Adjust the LF TUNE dial and LF MATCH dial several times to minimize LEVEL METER reading e v B 4 LF TUNE dial LF MATCH dial 4S When adjusting tuning precisely refer to section 4 4 3 How to adjust tuning precisely for Carbon13 12 When the tuning is complete click on the GO button The ordinary measurement of Carbon13 starts NMECA ECX USA 3 4 9 4 MEASUREMENT OF SR MAS 4 4 3 How to Adjust Tuning Precisely for Carbon13 1 Turn the LF MATCH dial to minimize the deflection of LEVEL METER 2 Turn the LF TUNE dial to minimize the deflection of LEVEL METER M ake a note of the deflection F1 of LEVEL METER at this time 3 Turn th
3. 0 0 s 3 trapezoida USS 80 100 d zerofill 1 fft 1 TRUE TRUE Ji US lc J Fig 1 6 nD Processor window 2 Click on either of the Process File And Put In Data Slate button or Process File And Put In Data Slate button Normally click on the i button Clicking on the button performs the data processing specified in the processing list for the first to the nth measurement data sets and displays the processed data sets in the Data Slate window Clicking on the button performs the data processing specified in the process ing list for the first to the nth measurement data sets and displays the processed data sets in the Data Viewer window 1 8 NMECA ECX USA 3 1 RELAXATION TIME MEASUREMENT if an appropriate window function and phase correction values are not known Display a set of relaxation time measurement data as 1D slice data in the 1D Processor window and obtain an appropriate window function and phase correction values by following Step 1 to 6 below then process and display the data according to Step 7 1 Click on the X button in the nD Processor window 4 aabe nD Processor double_pulse 1 jdf File PreTransform Window Tr Transform PostTransform Display Preferences Click on one of above buttons 2 Click on the Axes button to display the slice position setting screen and set the slice data to the number of points from the number of sets 1 n in the relaxation time measured
4. 0870 4 8088 M X parts per Million 1H Mode Weighted Linear Inv Recovery Peak Height Aes l 100 0 300 0 abundance 30 40 50 60 70 80 90 100 110 120 130 14 0 NM ECA ECX USA 3 NMECA ECX USA 3 1 RELAXATION TIME MEASUREMENT a one ae The selected peak values change to yellow and a peak intensity table is created When printing out the T values of two or more signals collectively drag cursor around the peak area All peaks listed up by peak picking in the area are selected and numerical markers become white 1 RELAXATION TIME MEASUREMENT 1 2 2c Obtaining relaxation times by approximate calculation Step 3 WE To select an approximate calculation equation Select the desired approximate calculation equation in the approximate calculation equation selection box The selected approximate calculation equation is displayed in the approximate calculation equation display box Q A faabe Curve Analysis gibberellic_acid_t1_analysis 2 jdf Y 14 37166 s Thousands 12 0 11 0 100 90 80 70 60 50 4 6 3021 62838 5 7650 Ss X parts per Million 1H Mode WeghtalLinerine Recovery feces ens 1 fan Approximate calculation equation selection box Approximate calculation equation display box z 2 Mary 8 0 90 10 0 110 120 130 140 approximate Description calculation equation Weighted linear least sq
5. 2 1 2 RELAXATION TIME DATA PROCESSING sci sissnrmncenaimeiacmnmtnane 1 5 1 2 1 Loading Relaxation Time M easurement D ata cccscssessssreesssseesessreesens 1 5 1 2 2 Processing Relaxation Time M easurement D ata cccsscssesessessssreeseees l 7 Lea Foun ertansiorming Sten 1 cuuniinminaciandusiinwaunwaanawan 1 8 Leao eM ee T A rdinara 1 12 1 2 2c Obtaining relaxation times by approximate calculation Step 3 1 18 LAS Pte ie tee gt RENS eeni 1 20 NM ECA ECX USA 3 1 RELAXATION TIME MEASUREMENT 11 RELAXATION TIME MEASUREMENT There are three kinds of relaxation times T Tip and T Section 1 1 explains the method of T measurement which is frequently performed 1 1 1 Relaxation Time T Evaluation To obtain T with high accuracy array measurement is performed using the variable of recovery times To set the variable of recovery times to appropriate values the approximate T of the sample must be determined first This section describes the method of a simple T evaluation by means of inversion recovery E Simple T evaluation method using T measurement mode by means of inversion recovery If a peak changes as a single exponential function the observed magnetization M tr is expressed as a function of the relaxation delay time t by using the inversion recovery method M t M 1 2exp t T From this equation it is found that T can be evaluated from the delay time when the observed magnetiza
6. ECX USA 3 3 DOSY MEASUREMENT aa Threshold Threshold level of the peak to used for processing W hen Threshold is 0 the default value of Delta software is used Species Set the total number of components expected Peaks Set this to the maximum number of the diffusion coefficient expected for each chemical shift 4S In the L M arquardt method set Peaks to 1 Ratio In the SPLMOD method set this to the minimum ratio of the different diffusion coefficients having equal chemical shift 4S This parameter applies only to the SPLM OD method Error Set this to the permissible error in the SPLM OD method as decimal Example When Error is 0 2 the permissible error is 20 4S this parameter applies only to the SPLM OD method Gamma Set this to the gyromagnetic ratio of the nucleus used for processing 4 Click on the Process File And Put In Data Viewer button Data processing is performed and DOSY data is displayed iat aabe 2D Viewer pst_manual 3 jdf lt 2 gt ae a z 5 z E 120 110100 90 80 70 60 50 40 30 20 10 10 20 01 03 OF X parts per Million 1H abundance 5 Repeating steps 3 and 4 obtain the search condition for the diffusion coefficient in the suitable range Logarithmic display of diffusion coefficient axis In the diffusion coefficient axis logarithmic display may be more legible Here the procedure for logarithmic display is explained 1 Set cursor tool to Select g
7. T as an initial value relaxation delay Value at least 5 times the expected T fal faabe Experiment Tool double pulse ex2 File Tools View Options 7 Click on the Submit button M easurement is carried out 8 Perform data processing in the 1D processor window and adjust the phase on the phase correction panel in the 1D processor window to turn the peak downward 9 Increase tau_interval in the Experiment Tool window and perform measurement again Perform the phase correction on the obtained spectrum using the same phase correction values as those obtained in Step 8 W hile you repeat this operation the peak reverses and then turns upward During the process the tau_interval at the time when the peak disappears is obtained This is the null point You can obtain an approximate value of T by multiplying the null point by 1 4 E Setting the parameters 1 After you obtain the null point enter the approximate value of T multiplied by 10 into relaxation delay The peaks in the spectrum have different T values However enter 10 times the maximum T value in the peaks used for the T measurement 2 Based on the obtained approximate value of T set tau_interval to array parameter array variable To enter the array parameter for T measurement by the inversion recovery method be sure to array the values in order from the greatest value The arrow buttons NMECA ECX USA 3 1 3 1 RELAXATION TIME MEASUREMENT Switch bet
8. Transform PostTransform Display Preferences ae sexp 12TH O f s Ey 3 trapezoid3 OS 80 100 E EJ D I X i i A B Click on one of above buttons 2 Click on the Axes button to display the slice position setting screen and set the slice data to the number of points from the number of sets 1 n in the diffusion coefficient measurement data Usually slice the first measurement data whose phase correction is easy to carry out easily 4 faabe nD Processor cpse_manual 1 jdf File PreTransform Window Transform PostTransform Display Preferences Slice TAR Ifpnt ninte ic me parameter input box Pl a Bill a oe Oi ca fes t gem es Aj en Aa M a Iar NMECA ECX USA 3 2 11 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 12 ae one ae 3 Click on the f msi D Slice button 6 7 r m de balance 0 FALSE 2 sexp 0 2 Hz 0 0 s 3 trapezoid3 O 80 4 zerofill 1 5 fft 1 TRUE TRUE y a get 124 a0 PI a C J gt PP i poli t L abundance 10 0 0 1 0 2 03 0 4 0 5 06 0 7 08 09 10 11 1 2 13 14 1 5 16 17 X seconds 1H 32 mT m PO 6 0 M X parts per Million 1H Fig 2 6 1D Processor window Set up suitable window function conditions changing the window function and parameter value The operation of changing the window function i
9. data Normally slice the first set of measurement data as it is easy to correct its phase t faabe nD Processor gibberellic_acid ti_analysis 1 OE File PreTransform Window Transform PostTransform Display Preferences Antes i ak Pint k Points 4 B transpose Ql fit Droints 4 gt Ia pe Slit Ser vee Slice position parameter input box ier ee Ad p poms 4 MAp P o _ 4 Oda P Poims 4 z s View a ial e E 2 zJ NMECA ECX USA 3 1 9 1 RELAXATION TIME MEASUREMENT 3 Click on the _ 1DSlice 1D Slice button 4 faabe 1D Processor gibberellic_acid_t1_analysis 1 mok aeaaeae ea a SS Snr skoal 2 sora CE 0 0 s 3 trapezoid3 O 80 4 zerofill 1 5 fft 1 TRUE TRUE 0 1 02 03 04 05 06 0 7 08 09 10 11 12 13 14 1 5 16 17 a es ey X seconds 1H Order t 14 37166 s Gain _ FALSE I P Mann A DoE Thousands 0 0 2 04 06 08 10 12 14 16 12 0 11 0 10 0 90 80 70 60 50 40 30 20 10 0 10 20 5 10 a 90 d X parts per Million 1H PP sor vk Fig 1 7 1D Processor window 4 Change the window function and its parameter values and enter an appropriate window function condition This operation is the same as that of changing the ordinary 1D data window func tion a Carry out phase correction and obtain the appropriate phase correction val
10. file _ Path usr people aaherfiles data standard_date Format JEOL Delta 4 Filter L on a i 2D 131070 23r 4M ppm s R JAN 2004 16 24 55 7 10 DEC 2002 23 33 38 double pulse Experiment Distribution Spectra Fig 1 9 Open File window 3 Select the file in which the relaxation time measurement data after a Fourier transformation is saved from the list box in the Open File window and then click on the Ok button The selected relaxation time measurement data is loaded in the Curve Analysis window 4 aabe Curve Analysis gibberellic_acid_t1_analysis 2 jdf asjal asl aaj 12 0 11 0 100 90 80 70 60 X parts per Million 1H Mode Weighted Linear Inv Recovery 4 PeakHeight Integral f inf NMECA ECX USA 3 1 13 1 RELAXATION TIME MEASUREMENT eme Ne if relaxation time measurement data after a Fourier transformation is being displayed 1 Click on the Open Data By Fingering a Geometry button in the Data Slate window 2 Click on the i Open Data File button The mouse pointer changes to the shape of a finger 3 Move the mouse pointer to the area in which the relaxation time measure ment data after Fourier transformation is displayed and click on it The selected relaxation time measurement data is loaded in the Curve Analysis window E To select a peak Either the Pick mode or the Peak mode is used to select a peak If there are a lot of peaks for T measurem
11. of the Delta Console window The Gradient Strength window opens Input value into each item of the Gradient Strength window Select 1H Proton in Nucleus and input the liquid height of the sample used into Coil length column M oreover input the frequency obtained in step 8 into the L eft position and Right position column The obtained magnetic field gradient strength is displayed on Gradient Strength window 2 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 3 MEASUREMENT OF DIFFUSION COEFFICIENT D As discussed above the measurement of the diffusion coefficient can be carried out by changing either the field gradient strength G the duration of gradient pulse 6 or the time between two FG pulses A However in the measurement in which a time parameter such as the duration of the field gradient pulse or time between FG pulses A changes you have to take into account the influences time such as relaxation Therefore the measurement by changing magnetic field gradient strength G is presently in general use The procedure for measurement of the diffusion coefficient by changing the magnetic field gradient strength G is explained below E To obtain measurement conditions 1 Stop the sample spinning and tune the probe 2 Check the 90 pulse width 4S in order to improve the accuracy of the diffusion coefficient measurement we recommend that you check the 90 pulse width of the sample you are measur ing For checking the 90
12. pulse perform an array measurement using the measurement mode single_pulse ex2 or single_pulse_dec ex2 3 Click on the Expmnt button in the Spectrometer Control window The Open Experiment window opens 4 Click on diffusion ital faabe Open Experiment Path nsrflelta glohaV experiments cosy ex2 aI cosy_pfg ex2 idept ex2 fdifference noe 1d ex2 ldqf cosy ex2 fdqf_cosy_pfig ex2 paqi_cosy_phase ex2 5 Select the desired sequence from the File name list The Experiment T ool window for setting up parameters opens 6 Input the following value if needed The values of x_pulse and gradient_max of the following are recalled automati cally from the default values in the probe file Input values when values obtained in step 2 differ from the values in the probe file 2 4 NMECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT x_pulse 90 pulse width which you obtained in step 2 gradient_max The maximum magnetic field strength T m in the system currently used For the maximum magnetic field strength input into gradient_max measure the value for every system combination of the probe and the maximum output of the FG power supply referring to section 2 2 How to measure PFG strength 7 Input values for the parameters of measurement of the diffusion coefficient The following three parameters are necessary for measuring the diffusion coeffi cient diffusion time Interval of two FG p
13. 3 CONTENTS 1 RELAXATION TIME MEASUREMENT AND DATA PROCESSING 1 1 RELAXATION TIME MEASUREMENT sesser 1 1 1 1 1 Relaxation Time T ey BGO cay nconicciemcwinrsecienseensuibener 1 1 1 1 2 Measurement of Relaxation Times T sessssesssrserrerrserreerrerreereen 1 2 1 2 RELAXATION TIME DATA PROCESSING sesers 1 5 1 2 1 Loading Relaxation Time M easurement D ata 1 5 1 2 2 Processing Relaxation Time M easurement Data l 7 1 2 2a Fourier transforming Step 1 ssssssssesrrsenrrssrrisrrrerrrnerrrnerrrrerrns 1 8 1 2 2b Selecting a peak Step 2 sssssesrsssrrenrrsnrrsnrrsnrrsnrrsnrrrenrrsnrrseres 1 12 1 2 2c Obtaining relaxation times by approximate calculation a EA A ANRA 1 18 kes PIO CaCl ar ONY Re n 1 20 2 MEASUREMENT OF DIFFUSION COEFFICIENT AND DATA PROCESSING 2 1 METHOD OF EVALUATING DIFFUSION COEFFICIENT assises 2 1 22 TOW POMESSURE PFO STRENGTH carona 2 2 2 3 MEASUREMENT OF DIFFUSION COEFFICIENT D eee 2 4 2 4 PROCESSING DIFFUSION MEASUREMENT DATA eessen 2 8 2 4 1 Loading Diffusion Coefficient Measurement Data 2 8 2 4 2 Procedure for Processing Diffusion Coefficient M easurement Die PE E eter Orr E E arr rr rr E cn emer er rc T heer 2 10 2 4 2a Fourier transformation Step 4 cnnusnciwantinesnnnnenwes 2 11 2 4 2b Extraction of peaks and creation of peak intensity table ELN EIRETIER TEET ETTET EA IE EEEE TTE PE TETTE 2 14 2 4 2c Method of obtaining diffusion coefficient by approximate Par ee EEE 2 21 24 3 Plot
14. Diffusion Analysis The window changes to the Diffusion Analysis mode 4 aabe Curve Analysis x 2 14 NM ECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT a Oc an E Reading the data Fourier transformed in the Curve Analysis window When Fourier transformated diffusion coefficient measurement data is saved on the hard disk 1 Click on the Get Data From File button in the Curve Analysis window 2 Click on the Open Data File button The Open File window opens i Path usr people aaberfiles date 3D Automation_Test Fig 2 8 Open File window 3 Select the file containing the Fourier transformed diffusion coefficient measurement data from the list box of in the Open File window and click on the Ok button The selected diffusion coefficient measurement data is loaded into the Curve Analysis window A aabe Curve Analysis cpse_manual 3 jdf x EISER 5 8 5 7 5 6 5 5 5 4 5 3 5 2 5 1 5 0 4 9 4 8 4 7 4 6 4 5 4 4 4 3 4 2 4 1 4 0 39 3 8 3 7 3 6 3 E X parts per Million 1H Mode Diffusion Analysis S Type fms ims NMECA ECX USA 3 2 15 2 MEASUREMENT OF DIFFUSION COEFFICIENT When Fourier transformed diffusion coefficient measurement data is displayed 1 Click on the E Open Data By Fingering a Geometry button in the Data Slate window 2 Click on the Open Data File button The mouse pointer changes to the shape of a finger 3 Move the mouse pointer to the area w
15. INSTRUCTIONS ae one ae CONTENTS INDEX JNM ECA Series JNM ECX Series JNM ECS Series Delta V4 3 6 APPLICATION USER S MANUAL AUG2007 08110241 Printed in Japan j J NMECA Seres J NMECX Seres J NMECS Senes Delta V4 3 6 APPLICATION USER S MANUAL JNM ECA Series JNM ECX Series JNM ECS Series This manual explains how to perform more advanced measurement using the JNM ECA JNM ECX or JNM ECS Series FT NMR system 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 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 adjusting the specified parts that only field service technicians employed or authorized by JEOL are allowed to adjust su
16. L http Avww jeol co jp Note For servicing and inquiries please contact your JEOL service office a NOTATIONAL CONVENTIONS AND GLOSSARY E General notations CAUTION Points requiring great care and attention when operating the device to avoid damage to the device itself BS Additional points to remember regarding the operation S 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 achieves a task Reference U seful information for you File The names of menus commands or parameters displayed on the screen are denoted with bold letters File Exit Selecting a menu item from a pulldown menu is denoted by linking the menu and the item with a dash For example File Exit means selecting Exit from the File menu Ctrl Keys on the keyboard are denoted by enclosing their names in a box E Mouse terminology M ouse pointer A mark displayed on the screen which moves following the movement of the mouse It is used to specify a menu item com mand parameter value and other items Its shape changes accord ing to the situation Click To press and release the left mouse button Right click To press and release the right mouse button Double click To press and release the left mouse button twice quickly Drag To hold down the left mouse button while moving the mouse NM ECA ECX USA
17. MAS for the preparation and the operation of the SR MAS probe The pulse sequence used for a SR M AS measurement is the same sequence as the pulse sequence used for general solution NMR measurement Therefore the basic measuring method and data processing method are the same as those of solution NMR 4S However the pulse sequence using field gradient FG cannot be used Here the method of adjustment of the magic angle the resolution and tuning the temperature controlling and the relationship between spinning speed and resolution that iS peculiar to the SR MAS NMR measurement and different from the general solution NMR measurement in the spectrometer are explained E SR MAS measurement SR MAS is the abbreviation of Swollen Resin M agic Angle Spinning It means that the resin swallenby the solvent is directly measured under the condition of several kilohertz MAS spinning The resolution of the spectrum of semisolids soft solid and high viscosity liquids will be improved by reducing the residual weak dipole dipole interaction of a sample by MAS Moreover higher resolution can be reached by averaging inhomogeneity of the local magnetic field around the rotating axis CAUTION Be sure to rotate a sample in SR MAS experiment If you measure without the air for sample spinning flowing the probe may be damaged However when you carry out the resolution adjustment using sin gle_pulse ex2 damage to the probe does not occur even if a meas
18. NT OF SR MAS ae ae g Shim On FID scc4 loj x Eraressinig 2 0 1 9 1 8 14 Hz X kilohertz T E J si ju Zd jsumzs j I a970 I 219703 11 68 Hz Fig 4 2 View Tool window in resolution adjustment 6 Ifthe resolution is not good adjust the resolution as followings a Open the Sample window and adjust Z1 to maximize the peak intensity b Adjust X2 and Y2 to maximize the peak intensity C Adjust Y and other axes to maximize peak intensity d Repeat steps a to c 7 Click on the STOP button after shim adjustment is complete NMECA ECX USA 3 4 5 4 MEASUREMENT OF SR MAS 4 4 ADJUSTING TUNING In order to apply RF pulses to a sample efficiently tuning is necessary operation If tuning shifts measurement conditions will change and the S N ratio of the spectrum will decrease Furthermore if tuning shifts greatly it will cause electric discharge in the probe 4 4 1 When Tuning is Necessary Tune the probe in the following cases Perform the measurement under the best conditions of both the observation and the irradiation system E When an observed nucleus is changed Tuning of the observation and irradiation system is necessary 4S The stick selection and the standard position on the dial scale of major nuclei are indicated in the table supplied with the probe When the observed nucleus is changed estimate the tuning point roughly with the numerical value from the table and then f
19. T The Points L ist appears OA era a Points List 261118 s 0 22209897 0 18622681 0 1581052 0 13378517 0 11270032 0 09489272 0 07950995 on A tn amp amp he Method of extracting Peak in Peak mode In the Peak mode the procedure for extraction of a peak and creation of a peak intensity table is as explained below 1 Click on the Peak button in the Curve Analysis window 4 aabe Curve Analysis cpse_manual 3jdf File Options 2 Y 32 mT m 12 0 11 0 100 90 80 70 60 50 40 30 20 P X parts per Million 1H a Mode Diffusion Analysis P tegra 2 Click on the Peak Pick Data button A peak pick is performed If necessary before performing peak picking adjust the threshold and noise level so that small signals and fine splitting of the peak which you do not need to obtain the diffusion coefficient may not be picked 2 18 NM ECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT p At faabe Curve Analysis cpse_manual 3 jdf OAAPRE LE Aa ala at 32 mT m o et 12 0 110 100 90 80 70 60 50 40 30 20 10 0 10 20 sCX parts per Million 1H Mode Diffusion Analysis Peak Height ae 3 Select Peak Select by cursor tool 4 Move the mouse pointer onto the X ruler in the spectrum display area and press and hole down the left button of the mouse Cursor appears 5 While continuing to hold down the left mo
20. The power processing step abs is entered in the processing list amp 4 aabe 1D Processor gibberellic_acid_t1_analysis 1 Let File Options PreTransform Window Transform PostTransform Display Preferences als 3 a OJ SJ IL peso aras Proce SIC C3 ENE aisle ate MEy Sa J 1 sinbell 0 0 100 0 2 zerofill 1 3 fft 1 TRUE TRUE 100 0 D 100 Thousands 5 display phase 01 0 2 03 04 05 06 0 7 08 09 10 11 12 13 14 15 16 17 E X seconds 1H 14 37166 s EC H BE C E a PP ue an C Proceed to Step 6 NMECA ECX USA 3 ae 1 11 1 RELAXATION TIME MEASUREMENT 1 2 26 Selecting a peak Step 2 To perform this operation the relaxation time measurement data after Fourier transformation should first be loaded in the Curve Analysis window E To open the Curve Analysis window Select Viewers Analysis Curve Analysis from the menu bar in the Delta Console window The Curve Analysis window opens Fig 1 8 Curve Analysis window E To load relaxation time measurement data after Fourier transformation in the Curve Analysis window if relaxation time measurement data after Fourier transformation is saved ona hard disk 1 Click on the Get Data From File button in the Curve Analysis window 2 Click on the k Open Data File button The Open File window opens 1 12 NMECA ECX USA 3 1 RELAXATION TIME MEASUREMENT al faabe Open
21. View Sh V _ y Z Buler fAlt Z aaah dhh Aa The Y axis changes to logarithmic display F Logarithinic X Ruler Sh Alt X W Logarithmic Y Ruler SHAY F Show Number of Points Sb AIt E F Show Ruler Type Sh Aft G l F Display Clock Time X F Display Clock Time Y NMECA ECX USA 3 MEASUREMENT OF SR MAS 4 1 OUTLINE OF SR MAS MEASUREMENT siciccmichnnnimuudneniudmauins 4 1 4 2 HOW TOADJUST MAGIC ANG cnuntiniiacaunnsonnadnwinan 4 2 43 ADIUSTHENTOFRESOCUTION sirpin rE 4 4 44 ADJUSTING TUNING sirsirisisrsiisiisrssaisisrsiiraisrsinisinnsiaraiirsenininaniiriidananiina ai 4 6 AA When Tunna Pe Saal unaa 4 6 S D eree ee E TEE E 4 6 4 4 3 How to Adjust Tuning Precisely for CarDOn13 cccscessesessesessreeseeeees 4 10 Re MS Rl OU OU cn GG LO Meemerenerererererne rr ererrret ee rrer cre rarinser merentret eter mer errr 4 11 a0 SPINNING SPEED AND RESOLUTION ticciunciimmniannaiimmnieineneas 4 12 NM ECA ECX USA 3 4 MEASUREMENT OF SR MAS 4 1 OUTLINE OF SR MAS MEASUREMENT SR MAS Swollen Resin Magic Angle Spinning is a measurement method for gel samples swollen resin of solid phase synthesis and heterogeneous systems such as tissue In order to perform this measurement it is necessary to use the special SR MAS probe which can carry out MAS measurement and the special purpose sample tube use for liquid samples which does not leak even if it rotates at several kilohertz c Refer to the manual of the SR
22. a relaxation time or when changing selection of an approximate calculation formula an approximate calculation is performed automatically NMECA ECX USA 3 1 19 1 RELAXATION TIME MEASUREMENT 1 2 3 Plotting Calculation Results 1 Click on the Plot Data File button in the Curve Analysis window Items and buttons for plotting are displayed in the approximation curve display area The Plot Option window opens ata aabe Plot Options ayia per Slice 7 Slice Point X _ X walue table i value table Curve fit equation E Standard deviation o E Chi square x e _ Number of points All Slices Plots Page T h 2 Puta check mark on the buttons with the items you want to plot To print the T values of more than one peak selected in the Peak mode together click on the All Slices button 3 Click on the Plot data with current state button The items that were selected in Step 2 are plotted 1 20 NMECA ECX USA 3 MEASUREMENT OF DIFFUSION COEFFICIENT AND DATA PROCESSING 2 1 METHOD OF EVALUATING DIFFUSION COEFFICIENT osese 2 1 2 2 HOW TO MEASURE PFG STRENGTH senisisssectntesiuiepcemniitinivemdieienicneniss 2 2 2 3 MEASUREMENT OF DIFFUSION COEFFICIENT D e 2 4 2 4 PROCESSING DIFFUSION MEASUREMENT DATA eeen 2 8 2 4 1 Loading Diffusion Coefficient M easurement D ata eecsessesesesesreen 2 8 2 4 2 Procedure for Processing Diffusion Coefficient M easurement Data 2 10 2 4 2a Fourier transformatio
23. agnetization produced by a 90 pulse is in the state coherent where the phase is complete in the beginning If PFG is applied here since the Spin receives a magnetic field strength corresponding to its z coordinate the phase of the magnetization changes with the magnetic field strength If the strength of the magnetic field gradient is G the duration of the field gradient pulse is 6 and the gyromagnetic ratio is y the final amplitude of phase modulation is yGAzo for a square wave field gradient in the direction of z axis The distribution function of the phase modulation iS as follows P t 4aDt yG5 t exp 4 yG6 Dt Therefore when the coherence is reestablished due to rephasing by a second PFG after vanishing due to dephasing by the first PFG the signal intensity is as follows if the time between the two FG pulsesis A I G A 1 0 A exp D yG6 Furthermore when the influence of the diffusion between FG pulses cannot be disregarded it is corrected as follows I G A I 0 A exp D Gd A 6 3 Therefore the diffusion coefficient D can be evaluated from the formula by changing either the strength of the magnetic field gradient G the duration of the field gradient pulse 6 or the time between the two magnetic field gradient pulses A NMECA ECX USA 3 2 1 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 2 HOW TO MEASURE PFG STRENGTH In order to obtain the diffusion coefficient it i
24. ample includes molecules whose the diffusion coefficients different largely suitable decaying data may not be obtained for each kind of molecule In this case we recommend that you divide the meas urement sample into a group having a large diffusion coefficient and a group having a small diffusion coefficient and measure two times under conditions Suitable for each group separately Data Slate bpp ste dosy 36 File Options View Freies Slicing Expansion Tools Analysis Stal 5 1 4 0 l a 4 0 parts per Million 1H yz A parts per Million 1 3 4 NMECA ECX USA 3 3 DOSY MEASUREMENT a On E DOSY measurement l Stop sample spinning and tune the probe 2 Check the 90 pulse width 4S in order to improve the accuracy of diffusion coefficient measurement we recommend that you check the 90 pulse width of the measurement sample In order to check the 90 pulse perform an array measurement using the meas urement mode of single_pulse ex2 or single_pulse_dec ex2 3 Input various parameters obtained by the above procedure To obtain measurement conditions 4S Set scans so that sufficient signal to noise ratio can be obtained for every molecule groups 4 Set grad_1 amp to suitable array variable in the range of the minimum and maximum values of the variable magnetic field gradient which were used in condition setting Set grad 1_amp lx Dimension Array Type None Listed Linear i s Expon
25. bled The Open Data for Processing window appears J faabe Open Data for Processing Path fusr people aaberfiles data Format JEOL Delta Filter Directory Filename Version ay Ltt F 4 cpse manual p Version display box fidouble pulse A 3D a fhncacb Automation Test CAHE pst manual b List box a a e ee pulse dec g hsinge pulse 2D 16384c 16r 4M s mT RS 2 FEB 2004 16 11 48 2 FEB 2004 16 08 28 spin_echo_ptg 3 Data information display box Fig 3 3 Open Data for Processing window 2 Click the data file called from the list box The data information on the newest version is displayed in the data information display box as shown below Note that the format of the data obtained by the array measurement is displayed as 2D data NMECA ECX USA 3 3 7 3 DOSY MEASUREMENT m oa a ae domain Frequency domain unit Time domain data FID data He PPM Frequency domain data Fourier transformed data Field intensity LD 2D nD Row of data R Ranged S Sparsed A number of data points f2 2D 16384 16r 4 s mT R Revision_time 2 FEB 2004 16 11 46 2 FEB 2004 16 08 26 spin echo ptg 3 Comment Creation time 3 Looking at the data domain of the data information display box and select the version of stored FID from the version display box If the newest version of the data displayed in ste
26. ch 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 instrument inappropriately controlled or managed for the maintenance e After installation or delivery of the instr
27. data Fourier transformed in the direction of the X axis in step 1 1 Click on the Y button in the nD Processor window s aabe nD Processor double_pulse 1 jdf File PreTransform Window Transform PostTransform Display Preferences ca 4 a SNE foo in _ 2 sexp 0 2 Hz 0 0 s gt 3 trapezoid3 O 80 100 4 zerofill 1 iy fft 1 TRUE TRUE Click on one of above buttons 2 Select Transform DOSY in the menu bar and select the algorithm used for processing 3 Setup the various parameters There are the following parameters 4S In the nD Processor window only three parameters are displayed simultane ously When the parameters you want to change are not displayed display them by clicking the e Back to previous parameter group button or the i Advance to next parameter group button Start This is the minimum value of the range over which to search for the peak to use to measure the diffusion coefficient Stop This is the maximum value of the range over which to search for the peak to use to measure the diffusion coefficient Inter p This determines the number of points to interpolate in the diffusion coefficient axis Y axis Example When the number of data points is three and Interp is 2 thenumber of points becomes 7 after processing Original points Interpolated points In the CONTIN method values of Interp that are 15 or more are suitable 3 12 NMECA
28. decay ratio of the signal may become in the range of 10 1 to 20 1 for the maximum and minimum of field gradient strength File Options View raiect Slicing anan Tools Analysis aaolsalolelases ol o 7 0 6 0 5 0 4 0 3 0 7 0 6 0 5 0 4 0 3 0 X parts per Million 1H X parts per Million 1 E Measurement of diffusion time 1 Stop sample spinning and adjust tuning of the probe 2 Check the 90 pulse width 4S In order to improve the accuracy of the diffusion coefficient measurement we recommend you to check the 90 pulse width of the sample to measure To check the 90 pulse perform an array measurement in the single_pulse ex2 or single pulse dec ex2 measurement mode 3 Set up the various parameters obtained in the procedure W To obtain measurement conditions 4S Setup scans so that you obtain a sufficient S N ratio also for the decay signal 2 6 NMECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT a Oa Sa 4 Set grad_1 amp to a suitable array variable in the range of the minimum and minimum value of the variable magnetic field gradient used in the condition setting In measurement of a diffusion coefficient good measurement can be performed changing an array variable so that the 2nd power of the magnetic field gradient may be measured at equal intervals For this reason the array variable can be easily set by selecting Logarithmic as an Array Type and by setting the Base value to 2 Dimen
29. e Copyright 1990 2003 by JEOL USA Inc Version 4 3 Beta 10 16 03 21 55 Linux 21 CFR part 11 technical features are enabled cpse_ manual Version dis play box aE i double pulse hneach List box DE SIr a 2D 163 4c 16r 464 s mT RS 2 FEB 2004 16 11 46 2 FEB 2004 16 08 28 spin echo pfg 5 Data information display box Fig 2 4 Open Data for Processing window 2 8 NMECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 Click the data file in the filename list box In the data information display box the data information of the newest version is displayed as shown below Note that the format of the data obtained by the array measurement is displayed as 2D Time domain r Frequency domain unit S Time domain data FID data n PPM Frequency domain data Fourier transformed data Field intensity 1D 2D nD Row of data A number of data points i i oO OT l 2 2D 16384 16r 4M1 s mT R Revision_time FEB 2004 16 11 48 2 FEB 2004 16 08 28 spin echo ptg 3 Comment Creation time 3 Looking at the data information display box and select the version of stored FID from the version display box If the newest version of the data displayed in step 2 is the time domain data FID data selection of a version is unnecessary 4 Click on the Ok button The nD Processor window opens is x 4 aabe nD Processor cpse_manual 1 jdf File PreTransform Window Tran
30. e LF MATCH dial to the 10 mark and turn the LF TUNE dial to minimize the deflection F2 of LEVEL METER Compare the deflection F2 of LEVEL METER at this time with F1 Repeat the above steps until the deflection of LEVEL METER becomes the mini mum 4 10 NMECA ECX USA 3 4 MEASUREMENT OF SR MA 4 5 TEMPERATURE CONTROL For the SR MAS probe the temperature can be controlled in the range from room temperature to 50 C The temperature control can be carried out in the same way in the usual solution NMR measurement However perform temperature control with the air for sample spinning flowing In any case CAUTION If a variable temperature experiment is performed while sample air is not flowing the probe may be damaged NMECA ECX USA 3 5 4 11 4 MEASUREMENT OF SR MAS 4 66 SPINNING SPEED AND RESOLUTION In some sample systems the resolution changes when the spinning speed changes For such asample system adjust the spinning speed to optimize the resolution 4 12 NMECA ECX USA 3 INDE X A AIUTO TININ wishenenchaceierheceen slices 4 6 Adjustment of resolution 4 4 A pproximate calculation equation 1 18 C Curve Analysis window 1 12 2 14 D PS ssissainssears eerste 3 1 DOSY measurement ncns 3 2 E Extracting In pick Mode 2 16 Extracting BGar cehaernemmeneioemins 2 16 Extracting peak in peak mode 2 18 I Inversion FECOVETY ccccceeeeeesereeete
31. ed For the values of x_pulse and gradient_max shown in below the default value in the probe file is automatically called Input value when the values you found in step 3 differs from the value in the probe file x_pulse 90 pulse width which you obtained in step 3 3 2 NMECA ECX USA 3 3 DOSY MEASUREMENT a gradient_max The maximum applicable magnetic field strength in the system currently used in T m For the maximum magnetic field strength to input into gradient_max measure the value for every different combination of the probe and the maximum output of the FG power supply referring to section 2 2 How to measure PFG strength 8 Input values for the parameter of measurement of the diffusion coefficient The following three parameters are necessary for measuring the diffusion coeffi cient diffusion time Time interval of two FG pulses diffusion time A grad 1 Duration of magnetic field gradient pulse grad 1 amp M agnetic field gradient strength G T m 4S The duration of magnetic field gradient pulse for DOSY processing is not equivalent to the parameter grad_1 in some types of sequence DOSY proc essing of Delta program refers to parameter delta automatically for duration of the magnetic field gradient pulse 6 hl aabe Experiment Tool cpse_ diffusion pfg ex2 gt File Tools View Options J i 2o z i L i ie fa I 1 gt J T 5 a j 3 iA ro yr E rr ta ry ah oy ov
32. ent and you want to print all those T values the Peak mode is useful The peaks to be used in the Peak mode must be listed in the peak picking list The Pick mode can be used to obtain T at any position of a spectrum The top of the peak is not required for T calculation in the Pick mode making it different from the Peak mode To select a peak in the Pick mode 1 Click on the Pick button in the Curve Analysis window The cursor tool bar in the spectral display area changes to the Pick mode 4 aabe Curve Analysis gibberellic_acid_t1_analysis 2 jdf File Options fale lal olol J Ja 14 37166 s g a x 12 0 110 100 90 80 70 60 50 40 30 20 10 0 10 20 X parts per Million 1H Mode Weighted Linear Inv Recovery Peak Height 1 14 NMECA ECX USA 3 1 RELAXATION TIME MEASUREMENT emee ela 2 Click on the i Pick position button in the cursor tool Pick mode 3 Move the mouse pointer onto the X ruler in the spectral display area and press and hold the left mouse button The cursor is displayed 4 With the mouse button pressed move the cursor to the top of the peak whose relaxation time you want to obtain and release it The pick position marker is displayed at the position at which you released the mouse button To select a peak in the Peak mode 1 Click on the Peak button in the Curve Analysis window ea aabe Curve Analysis gibberellic_acid_t1_analysis 2 jdf
33. ential Points hase 5 Click on the Set Value button Close the array parameter window and input the settings into Experiment T ool window NMECA ECX USA 3 3 5 3 DOSY MEASUREMENT aay A abe Experiment Tool cpse_ diffusion pig ex2 Fite Tools View oes x_pulse x atn O 3 T m z gradient J W Do not exceed gradient max value for gra she ape yec nm jeal t m jeol co jp cojp Totat Collection Timez 02013 00 20 13 6 Click on the Submit button M easurement starts NM ECA ECX USA 3 3 DOSY MEASUREMENT I a 3 3 PROCESSING DOSY DATA A fter measurement process the data in the nD Processor window First measurement data are loaded into the nD Processor window as in two dimensional measurement data processing In addition when the measurement data is transmitted from the spectrometer immediately after the end of DOSY measurement and the nD Processor window is already open the operation of section 3 3 1 is not necessary 3 3 1 Reading DOSY Measurement Data In order to load the data FID of DOSY measurement into the nD Processor window perform the following procedure 1 Click on the Data Processor button in the Delta Console window 44 faabe Delta ile Procesors Viewers Tools Anayss Anqision I O Delta NMR Processing and Control Software Copyright 1990 2003 by JEOL USA Inc Version 4 3 Beta 10 16 03 21 55 Linux 21 CFE part 11 technical features are ena
34. eometry in Select mode and click on DOSY data display area on the screen The DOSY data display range is selected 2 Right click in the data display area A pop up menu appears NMECA ECX USA 3 3 13 3 DOSY MEASUREMENT 3 14 me Ne 3 Select the bases of the logarithm from Logarithm Base Y Ruler of the pop up menu The base can be selected from 2 and 10 for common logarithms and e for natural logarithm F Level Toot fy Options D Logarithm Base X Buler pens Display Units 6 YBRulero E m Contour 1 F Mesh 2 wv F Surface 3 F Stack 4 F mage f5 F Spatial Contour 6 Draw Components D Datadex 1D D Datadex 2D D Save Current View V Restore Saved View Sh V _ wbtedbedtserente PYSPYEe CET UNECE E TST USES ECS EVE TUEE TSE CST TST TEt tet tat tet tet te ttst Yet oem 4 Right click in the data display area again A pop up menu appears e 5 Select Options Ruler Logarithmic Y Ruler from the pop up menu F Level Toot fy 7 Options Annotations Alt A logarithm Base p Cursors JAlt C Display Units Wh Measures Sh Alt H W Contour 1 F PIP Windows Alt W E Mesh fa W Regions fAH RJ F Surface 3 integrali b F Stack 4 Peak i E mage 5 Molecule E Spatial Contour 6 Data D Draw Components b Display b Datadex 1D E File information gt 1 Datadex 2D b Ruler b A X Buter fAlt X Save Current View P ST P Y Ruler AHY Restore Saved
35. equation 3 1 and inverse Laplace transformation is used for a signal like equation 3 2 NMECA ECX USA 3 3 1 3 DOSY MEASUREMENT b ee 3 2 DOSY MEASUREMENT A DOSY measurement is basically the same as the diffusion coefficient measurement discussed in previous chapter The only difference between DOSY and diffusion coefficient measurement is that the target of measurement is a multicomponent system or a system having a distribution of molecular weight E To obtain measurement conditions 1 Measure the maximum magnetic field gradient intensity of PFG FG pulse used measurement Refer to Section 2 2 How to measure PFG strength for measuring FG pulse strength 2 Stop the sample spinning and tune the probe 3 Check the 90 pulse width 4S In order to improve the accuracy of a diffusion coefficient measurement we recommend you to check 90 pulse width of the sample to measure In order to check 90 pulse perform an array measurement using the measurement mode of single_pulse ex2 or single pulse dec ex2 4 Click on the Expmnt button in the Spectrometer Control window The Open Experiment window opens 5 Click on diffusion Pcosy ex2 Li eosy_pfz ex2 dept ex2 difference noe Idex2 F daf _cosy ex2 a ldqf cosy_pfg ex2 a Lo dgf cosy phaseex2 6 Selecta sequence to use from the File name list box The Experiment T ool window for setting parameters opens 7 Input the following values if need
36. has some backlash Therefore adjust it by turning the dial for fine tuning in only one direction Tecate 50 0 40 0 30 0 200 100 0 10 0 20 0 30 0 40 0 am a it or Current Time Expected Finish Delta Time Integral Value m Current a Expected Finish Delta Time Integral Value Fig4 1 Freelnduction Decay left and spectrum right after magic angle adjustment 4 2 NMECA ECX USA 3 4 MEASUREMENT OF SR MAS 9 After completing magic angle adjustment select the current measurement in the Spectrometer Control window and click on the STOP button 4S If a measurement is stopped while it is in progress the data file is stored automatically and the version of the data file increases In order to keep space free on the hard disk delete the file at any time 10 Remove the stick for adjustment Adjustment of the magic angle may change the resolution Be sure to check the resolution according to section 4 3 Adjustment of resolution and adjust the shim values if needed NMECA ECX USA 3 4 3 4 MEASUREMENT OF SR MAS e la 4 3 ADJUSTMENT OF RESOLUTION 1 Insert the chloroform CHCI sample It is not necessary to perform spinning 2 Select Config Shim on FID in the pull down menu of the Spectrometer Control window 3 Click on the Start button The spectrum is updated continuously 4 Adjust the phase 5 Expand near the peak and check the resolution 4 4 NMECA ECX USA 3 4 MEASUREME
37. he phase of measurement data cannot be corrected Power processing replaces phase correction in step 5 Perform the following operational procedure a Click on the amp Append button in the 1D Processor window b Select Post Transform Abs in the menu bar The abs function for power processing is entered into the process list 4 aabe 1D Processor cpse_manual 1 jdf ea x File Options PreTransform Window Transform PostTransform dat Preferences ala aa aeaea mod r HENSE Pea 32fm TA __ 5 fft 1 TRUE TRUE 6 ppm abundance 8 display phase 01 02 03 04 05 06 0 7 08 09 10 11 12 13 14 15 16 17 q X seconds 1H Y 32 mT m A v m P EAE LTTE reer 5 10 90 12 0 11 0 10 0 90 80 70 60 50 40 30 20 10 0 10 20 lA X parts per Million 1H PP sor azi A C Go to step 6 abundance NMECA ECX USA 3 2 13 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 4 26 Extraction of peaks and creation of peak intensity table Step 2 This operation calls the diffusion coefficient measurement data that performed Fourier transform processing to the Curve Analysis window and change the M ode to Diffusion Analysis E Open the Curve Analysis window and change the Mode 1 Select Viewers Analysis Curve Analysis in the menu bar of for Delta Console window The Curve Analysis window opens A A aabe Curve Analysis IE Fig 2 7 Curve Analysis window 2 Change the Mode to
38. here the Fourier transformed diffusion coefficient measurement data is displayed and click it The selected diffusion coefficient measurement data is recalled into the Curve Analysis window E For extracting peak There are two methods of extracting method of a peak Pick mode and Peak mode If you are using a large number of peaks to calculate the diffusion coefficient then when printing those diffusion coefficient values collectively the Peak mode is convenient The candidate peaks of the Peak mode should be listed by peak picking beforehand Using the Pick mode yuo can measure the diffusion coefficient of an arbitrary peak ina Spectrum It differs from the Peak mode and it is not necessary that the point for calculating the diffusion coefficient is the top of the peak Method of extracting in Pick mode When extracting the peaks in the Pick mode the procedure for creating the peak intensity table is as explained below 1 Click on the Pick button in the Curve Analysis window The cursor tool in the spectrum display range changes to the Pick mode 4 aabe Curve Analysis cpse_manual 3 jdf alela eld r i Y vial 5 8 5 7 5 6 5 5 5 4 5 3 5 2 5 1 5 0 4 9 4 8 4 7 4 6 4 5 4 4 4 3 4 2 4 1 4 0 39 3 8 3 7 3 6 3 E X parts per Million 1H Mode Diffusion Analysis a e Peak Heigh JE O megal fessis O 67515E 8 aa T 2 16 NM ECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT a 2 Selec
39. ine tune E When the sample is changed Although the tuning and matching of the observation system hardly change for an ordinary sample unless VT measurement is performed the tuning of the irradiation system changes a little For a sample with a high dielectric constant or a semiconductor sample tuning and matching of the irradiation and observation system change sharply Be sure to tune the probe 4 4 2 Howto Tune After inserting the sample and setting the sample spinning speed tune according to the following procedure Here as an example the case ic which the measurement method is single pulse dec the observed nucleus is Carbon13 and the irradiation nucleus is Proton will be introduced 1 Click on the Expmnt button in the Delta Console window The Open Experiment window opens 4 aabe Open Experiment Path usr delta global experiments 4 6 NMECA ECX USA 3 4 MEASUREMENT OF SR MAS 2 Click on the GJ button The contents of the Global Experiment directory appear a Click on the measurement mode single pulse _dec exp and highlighting it b Click on the OK button The Experiment T ool window opens nH fi 4 SE ws 5 S i 7 pe ee pe 5 P 3 p A a E Sic Sas Sag Se NS corte ae BERG Be Oe 1 ee i A k E f S ia f y rT i d f 4 H fg L A H r Vv E E d 4 c p Total Collection Time 00 47 27 3 Enter the measurement conditions in the order of Heade
40. lion 1H PE s i pph Fig 3 5 1D Processor window 4 Changing the window function and parameter value set up suitable window function conditions The operation of changing the window function is the same as that of usual 1D data The height information of a peak is required for inverse Laplace transformation of DOSY Therefore in order to reduce the contribution of noise it is more effective to use a larger window function conditions than usual data processing 5 Correcta phase manually and obtain suitable phase correction values The phase correction is the same as that of the usual 1D data 4S Be sure to perform phase correction manually without using automatic phase correction 4S A phase may not correct at the peak having J coupling due to J modulation If that happens refer to section 2 4 2 Reference When the phase of measure ment data can not be corrected 6 Close the 1D Processor window The window function conditions and phase correction value which were obtained in steps 4 and 5 are automatically entered in the process list in the nD Processor window 7 Select Post Transform Math Real from the menu bar Real processing is sentered in the process list of windows 4S In inverse Laplace transformation processing of DOSY only real data is need NMECA ECX USA 3 3 11 3 DOSY MEASUREMENT 3 3 26 Processing for y axis of DOSY measurement data Step 2 Carry out inverse Laplace transformation of the Y axis for the
41. n Step 1 sss sssssesssrrssrrrenrrnenrrnerrrnnrrrerrrreerrreens 2 11 2 4 2b Extraction of peaks and creation of peak intensity table Step 2 2 14 2 4 2c Method of obtaining diffusion coefficient by approximate ee iela nE E iia een enna E E 2 21 24 3 Piloting Calculation FOS NG soca rececesscxcssnssnnvecincnsecateeesestenncnebeacnestaistacannis 2 22 NM ECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 1 METHOD OF EVALUATING DIFFUSION COEFFICIENT Generally diffusion is a process by which the concentration of solution or temperature of a sample approaches uniformity However here diffusion means self diffusion in which a molecule changes the position in solution or in solid state Therefore the diffusion coefficient is a measure of transfer of the molecule E Method of evaluating diffusion coefficient by NMR Although the translational motion of molecule is 3 dimensional motions the translational motion actually observed by NMR is only the motion parallel to the z axis because a magnetic field gradient is applied along the z axis If the translational molecular motion is a random walk the probability of the molecule moving a distance Az from its Initial position during time t is the following Gaussian function P Az t 4zDt exp Az 4 Dt where D is the diffusion coefficient of the molecule In this function the Az distributes wide range with increasing t In PFG NMR the transverse m
42. neens 1 1 L Loading diffusion coefficient measurement data 2 8 Loading relaxation time measurement data 1 5 M Hage ai oan ee eee ree 4 2 Measurement of diffusion coenen D Joaiaonansinsman 2 4 M ethod of evaluating diffusion CoE e 2 1 N Nonlinear ee 1 18 Null DOIN cecesceeeeeeeeeeeeeseeetaeseneess 1 2 NM ECA ECX USA 3 P AELS E A TT 2 2 Plotting calculation results 1 20 2 22 Procedure for processing diffusion coefficient measurement data 2 10 Procedure for processing DOSY measurement data ienee 3 9 Processing diffusion measurement al E A E EE TE E 2 8 Processing DOSY data aaae 3 7 Processing relaxation time measurement data iceren 1 7 R Reading DOSY measurement data 3 7 Relaxation time T evaluation 1 1 Relaxation time measurement 1 1 S Spinning speed and resolution 4 12 SR MAS measurement 4 1 T Temperature control 4 11 To select a peak ccccceeeeceeeserseeeeens 1 14 To select a peak in the peak mode 1 15 To select a peak in the pick mode 1 14 Tuning precisely for carbonl13 4 10 U Unweighted Linear 68 1 18 W Weighted Linear ccc 0e 1 18
43. nsnmniinnnnnnaninuwen 3 7 3 3 2 Procedure for Processing DOSY M easurement Data 3 9 3 3 2a Processing for x axis of DOSY measurement data Step 1 3 10 3 3 26 Processing for y axis of DOSY measurement data Step 2 e 3 12 NM ECA ECX USA 3 3 DOSY MEASUREMENT 3 1 OUTLINE OF DOSY The DOSY Diffusion Ordered NMR SpectroscopY method evolves the diffusion coefficient of a sample on one axis in the two dimensional spectrum by inverse Laplace transformation or curve fillings E Principle of DOSY As described in Chapter 2 M easurement of Diffusion Coefficient and Data Processing when the phase coherence of the spin is lost due to the first FG pulse and the phase coherence is restored by a second FG pulse the signal intensity is as follows if interval of two FG pulsesis A I G A I 0 A exp D 7Gd A 6 3 Therefore when two or more NMR signals overlap in the same chemical shift since the echo intensity becomes a linear combination of the signals the echo is given as follows G A 1 0 A exp D G8 A 5 3 3 1 Moreover for a sample which has a continuous molecular weight distribution like a polymer the echo intensity is given as follows G A Gt D exp D 7G6 A 8 3 dD 3 2 where G D is the distribution function of D Such overlapping signals evolve along with one axis by the diffusion coefficient using the peak intensity Curve fitting is used for a signal like
44. p 2 is the time domain data selection of the version is unnecessary 4 Click on the Ok button nD Processor window opens 44 aabe nD Processor cpse_manual 1 jdf eiii File PreTransform Window Transform PostTransform Display Preferences m aaao aaa a 2 sexp OAL Hz 0 0 s 3 trapezoids O 80 100 4 zerofill 1 5 fft 1 TRUE TRUE 6 ppm 7 transpose Fig 3 4 nD Processor window 3 8 NMECA ECX USA 3 3 DOSY MEASUREMENT Z 3 3 2 Procedure for Processing DOSY Measurement Data The processing of the DOSY measurement data consists of the following two steps Step 1 Fourier transformation the X axis of DOSY measurement data set under same conditions for the 1 to n th measurement data set as shown in the following sche matic diagram l at Step 2 For the processing of the Y axis of DOSY measurement data Inverse Laplace Transformation is carried out on every data point that is Fourier transformed along the X axis as shown in the following schematic diagram a eee ee ILT Q O i um2 s ppm The procedures are explained in the order of these steps below NMECA ECX USA 3 3 9 3 DOSY MEASUREMENT 3 3 2a Processing for x axis of DOSY measurement data Step 1 Display one data of DOSY measurement data in the 1D Processor window as 1D slice data and search a suitable window function and phase correction values 1 Click on
45. r Instrument Acquisition and Pulse in the Experiment Tool window 4 Click on force_tune in the Header Err J Bis ee a es Aa F View ponio e A TNE E nr 7 i i s gt T Jia E 7 7 P mi i P 7 E a i j 47 x o Ef f y x x z E E 5 f Ean E ey 1 we Get Acq View filename single _pulse_dee single pulse decoupled gated NOE active_global std_carhon_autophaselist Edit c D J 3 Browse J il i Total Collection Time 00 47 27 NM ECA ECX USA 3 4 7 4 MEASUREMENT OF SR MAS ae one ae 5 Click on the Submit button A tuning message appears The message of Proton appears first At this time the NMR system is already prepared for tuning Please tune coil HFI to 1H and click GO when complete 6 Adjust the sensitivity of the indicator for Proton tuning If LEVEL METER of the head amplifier chassis is out of range or does not move far adjust the button and knob of METER GAIN RF POWER SAMPLE HF 1 HF2 LF1 LF2 C Loa EMPTY O O O O O O LEVEL METER CHECK SWR SELECT METER GAIN HF1 HF2 LF1 LF2 Ox1 0Ox10 Button and knob of METER GAIN 7 Adjust HF high frequency TUNE knob of the probe to minimize LEVEL METER display first and next adjust the HF MATCH knob Finally adjust the HF TUNE knob again HF MATCH knob HF TUNE knob Fig 4 3 Bottom view of the probe 4 8 NMECA ECX USA 3 4 MEASUREMENT OF SR MAS
46. ring in the selection state by pressing the Apply button the display changes to Auto When changing the peak which obtains the diffusion coefficient or when changing the parameter value an approximate calculation is performed automatically NMECA ECX USA 3 2 21 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 4 3 Plotting Calculation Results 1 Click on the Plot Data File button in the Curve Analysis window The Plot Option window opens Plot Options Options per Slice Slice Point X I X value table 1 value table Curve fit equation _ Standard deviation c _ Chi square 32 Number of points Plots Page 1 2 Place a check mark in the box of each item that you want to plot W hen two or more peaks are selected in the Peak mode and you wont to print the diffusion coefficient values of those peaks collectively turn on All Slices 4S In order to put check mark on an item to plot click its button from Curves amp Info Peaks amp Equations or Vectors amp Equations or the check button of an item to plot directly 3 Click on the Plot data with current state icon The items selected in step 2 are plotted 2 22 NMECA ECX USA 3 DOSY MEASUREMENT AND DATA PROCESSING ee ee OFU T rA 3 1 22 DOST MEASUREMENT es eres aise ieee 3 2 3 3 PROCESSING DOSY DA A nctentetascnrencaracenscsintecnncsnsprdecenarindiasensstrdetnainpnnantend 3 7 3 3 1 Reading DOSY Measurement D de iistiiinnnn
47. roe E iB i F p Ae ce Tey L i k S T AY 3T lz gradient max n pg a Ret er Le rin per ae a Cees TEE ah aapa Ne A Do not exceed gradient max value for grad 1 amp E i al l a LLE Fa a tata d fj ae Tu Ta gran _ Shape SOUARE T Total Collection Time 00 01 49 F i MM M Taai pemer b waa y Fig 3 1 Experiment Tool window 9 Input about 10 times the value of T into relaxation delay 10 Perform an array measurement at the minimum and maximum value of the variable magnetic field gradient strength which are used in the actual measurement For example when changing magnetic field from 3 mT m to 0 27 T m perform an array measurement at 3 mT m and 0 27 T m A magnetic field strength greater than gradient_max cannot be output NMECA ECX USA 3 3 3 3 DOSY MEASUREMENT i I fy acq 3 mT m 270 mT m Fig 3 2 Array parameter window 11 Process the data in the nD processor window and check the decay of the signal Be careful of the following points when two or more kinds of molecules are in cluded e When the maximum magnetic field gradient to use is applied adjust measurement conditions so that a signal can be observed also for the molecule with the largest diffusion coefficient e Also for the molecule with the smallest diffusion coefficient select the measure ment conditions to make at the decay of the signal intensity about 1 2 When the measurement s
48. s necessary to measure the strength of magnetic field gradient G Therefore the maximum magnetic field gradient strength of the system being used should be measured before carrying out an actual measurement E Simple way to measure PFG strength 1 Prepare a water sample with the liquid height adjusted to about 5 mm 4S A sample tube such as a micro cell in which the height of liquid is clearly known is needed 2 Click on the Expmnt button in the Spectrometer Control window The Open Experiment window opens 3 Click on diffusion K Open Experiment 0 a e Path sr delta global experiments Fig 2 1 Open Experiment window 4 Select the fg_power_check ex2 sequence from the File name list box The Experiment Tool window for setting parameters opens 5 Set the parameter grad amp Since a long magnetic field gradient pulse will be used in the fg power_check ex2 sequence do not use a large magnetic field gradient Use a value of 1 to 5 for the value of grad_amp 6 Click on the Submit button A measurement is performed 7 Process the data in the 1D processor window and display the absolute value of the spectrum In order to display the absolute value perform abs processing 8 Measure the frequency at the both ends of the obtained rectangular spectrum in Hz 2 2 NMECA ECX USA 3 9 10 NMECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT Select Tools Math Gradient Strength from the menu bar
49. s the same as that of usual 1D data W hen calculating the diffusion coefficient only the height information of a peak is required Therefore in order to reduce the contribution of noise it is more effective to use a wider window function than usual Correcting the phase manually obtain suitable phase correction value The operation of phase correction is the same as that of the usual 1D data 4S Be sure to correct phase manually without using automatic phase correction 4S The phase of a peak having J coupling may not be corrected due to J modula tion If that happens refer to the following procedure Reference When the phase of measurement data can not be corrected Close the 1D Processor window The window function conditions and phase correction values which were obtained in steps 4 and 5 are automatically entered in the process list of the nD Processor window Click on one of the following icon Usually select Ey Process File And Put In Data Slate button or gu Process File And Put In Data Viewer button If you click the Cy button the after performing the data processing specified by the process list to the 1 to n th measurement data set the Data Slate window appears NMECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT If you click the l button the after performing the data processing specified the process list to the 1 to n th measurement data sets the Data Viewer window ap pears Reference When t
50. sform PostTransform Display Preferences Ci ws ea a J a 1 de_balance 0 FALSE rm 1 transpose _ 2 sexp 0 2 Hz 0 0 s 3 trapezoid3 0 80 100 4 zerofill 1 5 fft 1 TRUE TRUE 6 ppm 7 transpose Fig 2 5 nD Processor window NMECA ECX USA 3 2 9 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 4 2 Procedure for Processing Diffusion Coefficient Measurement Data The processing of the diffusion coefficient measurement data consists of the following three steps Step 1 Fourier transform the diffusion measurement data sets under the same conditions for the 1 to n th measurement data set as shown in the following schematic figure FET mM iil Step 2 Transmit the processed data to the C urve Analysis window Then select the peaks to use to perform the diffusion coefficient calculation by picking the peaks Step 3 Obtain the diffusion coefficient using the approximate calculation The procedure is explained in the order of these step 2 10 NM ECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT ae one 2 4 2a Fourier transformation Step 1 Displaying one diffusion coefficient measurement data set in the 1D Processor window as 1 dimensional slice data search a suitable window function and phase correction value 1 Click on the X button in the nD Processor window 4 faabe nD Processor double_pulse 1 jdf File PreTransform Window
51. sion _ None 5 Click on the Set Value button Close the array parameter window and input the set values into the Experiment Tool window W A aabe Experiment Tool cpse diffusion pfg ex2 E x File Tools View Options 3 5 dB oe o i l _ D a a z_gradient_max IES 3 T m Do not exceed gradient MAX value for grad 1 amp 6 Click on the Submit button M easurement starts NMECA ECX USA 3 2 7 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 4 PROCESSING DIFFUSION MEASUREMENT DATA After measurement process the data in nD Processor window and use the Curve Analysis window for calculation of the diffusion coefficient The procedure is explained below First recall the measurement data into the nD Processor window as in two dimensional measurement data processing In addition the operation of section 2 4 1 is not necessary when the nD Processor window is already displayed when measurement data is transmitted from the spectrometer immediately after the end of diffusion coefficient measurement 2 4 1 Loading Diffusion Coefficient Measurement Data In order to load the diffusion coefficient measurement data FID into the nD Processor window perform the following procedure l Click on the iel Data Processor button in the Delta Console window ia aabe Delta File Processors Viewers Tools Analysis Acquisition Delta NMR Processing and Control Softwar
52. sion coefficient by approximate calculation Step 3 This method calculates the diffusion coefficient approximately E Input parameters used for measurement Select the parameters used as variables for the array measurement in the Y Value Type check boxes Enter a check mark into the check box of a variable to selected it Input the gyromagnetic ratio of the nucleus used for calculation and the other parameters which were not used as array variables into the parameter input boxes When the following parameters are used in the used sequence these default values are read J x_ domain Gyromagnetic ratio of an observed nucleus G grad 1 amp Amplitude of magnetic field gradient pulse 0 delta Duration of magnetic field gradient pulse A diffusion time Diffusion time E To obtain diffusion coefficient by approximate calculation Click on the Apply button An approximate calculation is performed and the result of the calculation of a diffusion coefficient and the approximation curve in yellow appear A A aabe Curve Analysis cpse_manual 3 jdf 5 54 53 52 51 50 49 48 4 7 46 45 4443 42 41 40 39 38 37 AX parts per Million 1H Mode Diffusion Analysis Peak Height Integral ao Type GimT m fms Afms j N y 267515E 8 rad sT i e 1 0 abundance 2 0 01 02 03 O4 05 O06 07 08 OFF 10 11 12 13 y X Gsm 2 4S When ente
53. sor window 1 Click on the Data Processor button in the Delta Console window a amp i H aabe Delta File Processors Viewers Tools Analysis Acquisition DMD p S E Delta NMR Processing and Control Software Copyright 1990 2003 by JEOL USA Inc Yersion 4 3 Beta 01 06 04 11 16 Linux 21 CFR part 11 technical features are enabled The Open Data for Processing window is displayed 4 aabe Open Data for Processing x Path usr people aabe files data Format JEOL Delta Filter Jaj Directory Filename Version Favorites any Al double pulse hncach Version display box single_pulse List box Data information display box Fig 1 4 Open Data for Processing window NMECA ECX USA 3 1 5 1 RELAXATION TIME MEASUREMENT 2 Click on the data file you want to load from the list box The following data information with the latest version is displayed in the data information display box The T data obtained in the array measurement is represented as having 2D format 3 If the Time domain Frequency domain display in the data information display box is not s time domain data select the version number from the version display box so as to display the time domain data If the Time domain Frequency domain display in the data information display box displayed in Step 2 is Time domain that is the latest version is time domain data FID data the selection of the version can be omit
54. t the Pick Pick position by cursor tool 3 Move the mouse pointer onto the X ruler in the spectrum display area and press and hold down the left mouse button A cursor appears 4 While continuing to hold down the left mouse button move the cursor so that E X parts per Million 1H a 14 aabe Curve Analysis cpse_manual 3 jdf ea ej ea oll el alr IE m 32 mT m 0 2 abundance 01 5 8 5 7 5 6 5 5 5 4 5 3 5 2 51504948 47464544 43424140 39 3 8 3 7 3 6 3 5 3 Mode Diffusion Analysis __ Peak Height Peak Heigh t m O megal e 2 67515E 8 O O raast T OO w T abundance 0 04 006 O08 Q1 012 O14 O16 018 02 022 O24 0 26 A X Tm 1 it intersects the top of a peak that you want to use to calculate the diffusion coefficient then release the mouse button A pick position marker is displayed at the position where you released the mouse 5 When displaying the peak intensity table select File Point List in the pull NM ECA ECX USA 3 fel opto ooo O e Ly down menu of the Curve Analysis Tool faabe Curve Analysis cpse_manual 3 jdf gt ee Plot Uw ves ap Set Scale Close Q 5 8 5 7 5 6 5 5 5 4 5 3 5 2 5 1 5 0 4 9 4 8 4 7 4 6 4 5 4 4 4 3 4 2 4 1 4 0 39 38 3 7 3 6 3 5 3 Wo X parts per Million 1H Mode ee e Peak Heigh nt Integral Integral 2 17 2 MEASUREMENT OF DIFFUSION COEFFICIEN
55. ted 4 Click on the Ok button The nD Processor window opens M A jaabe nD Processor double_pulse 1 jdf File PreTransform Window Transform PostTransform Display Preferences 2 sexp 0 2 Hz 0 0 s 3 trapezoida USS 80 100 d zerofill 1 5 fft 1 TRUE TRUE Fig 1 5 nD Processor window 1 6 NMECA ECX USA 3 1 RELAXATION TIME MEASUREMENT 1 2 2 Processing Relaxation Time Measurement Data Processing of relaxation time measurement data is performed in the following three steps Step 1 All sets of measurement data from the first to the nth are transformed together under the same condition HL iil Step 2 The processed data sets are transferred to the C urve analysis window Then the peak for T calculation is selected from any numbered data set by peak picking Step 3 The relaxation times are obtained by approximate calculation The procedures are next explained in the order of the above steps NM ECA ECX USA 3 1 7 1 RELAXATION TIME MEASUREMENT 1 2 2a Fourier transforming Step 1 if an appropriate window function and phase correction values are already known and are saved in the processing list 1 Load the desired processing list in the nD Processor window 4 faabe nD Processor double_pulse 1 jdf File PreTransform Window Transform PostTransform Display Preferences be y i _ x Lde_balance 0 FALSE PN 1 transpose _ 2 sexp 0 2 Hz
56. the X button in the nD Processor window 4 aabe nD Processor double_pulse 1 jdf File PreTransform Window Transform PostTransform Display Preferences Click on one of above buttons 2 Click on the Axes button to display the slice position setting screen and set the slice data to the number of points from the number of sets 1 n in the DOSY measurement data Usually slice the first measurement data whose phase correction is easy to per formed N A aabe nD Processor cpse_manual 1 jdf File PreTransform Window Transform PostTransform Display Preferences DEENA T r x Me Mpm eae E e iM oe Ail Slice positi i pnt Dais IL position ill d a 100 parameter input box i diipi qei o ER Points 6 N i Poms 4 het ees D l 4 Afii i pnt pl points 4 Points aim y SE al Ws 1 pnt Pl Points Points 3 o on 3 10 NMECA ECX USA 3 3 DOSY MEASUREMENT ae one ae 3 Click on the 1D Slice button The slice data at the specified position is displayed in the 1D Processor window 4 aabe 1D Processor pst_manual 1 jdf ox EA ae Jaa azl Y 32fmTim 4 zerofill 1 5 fft 1 TRUE TRUE 6 phase 109 0 50 7 ppm 8 display phase Ly 0 1 02 03 04 05 06 0 7 08 09 10 11 12 13 14 15 16 17 a ai poe ee oor PI a Jb PP 50r zA D EE See 120 11 0 10 0 90 80 70 60 50 40 30 20 10 0 10 20 Ms X parts per Mil
57. 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 In 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 JEOL Ltd 1 2 Musashino 3 chome Akishima Tokyo 196 8558 Japan Telephone 81 42 543 1111 Facsimile 81 42 546 3353 UR
58. ting Calculation Results sctcrrcncsrasnintunnimemntandenses 2 22 3 DOSY MEASUREMENT AND DATA PROCESSING L PUTERE RT TUS T a 3 1 Bee TAE ee ON arinn 3 2 Oe PROCESSING DOSE DATA urnini 3 7 3 3 1 Reading DOSY M easurement Dat s sssssssssserrsrrserrsrrrserrserrrerrrens 3 7 3 3 2 Procedure for Processing DOSY M easurement Data 3 9 3 3 2a Processing for x axis of DOSY measurement data Step 1 3 10 3 3 2b Processing for y axis of DOSY measurement data Step 2 3 12 4 MEASUREMENT OF SR MAS 4 1 OUTLINE OF SR MAS MEASUREMENT hesen 4 1 4 2 HOW TO ADJUST MAGIC ANGLE sssssssrssissrisiresrrsrrsrrinrsrrsnnnnnnns 4 2 43 ADJUSTMENT OF RESOLUTION iciimnciccitnnnienaemmnmencna 4 4 4 4 ADJUSTING TUNING vic ccecessssssssssterserssssrssssersrsvserssnevsreveersesens 4 6 4 4 1 When Tuning is NECA aly vicnscctisicrmiemeiieeun maine 4 6 NM ECA ECX USA 3 i C 1 CONTENTS ee PROT cert ieee NS 4 6 4 4 3 How to Adjust Tuning Precisely for CarbDOn13 serres 4 10 4 5 TEMPERATURE CT ROL sicstensnetisiiecneieniitienainimonea 4 11 46 SPINNING SPEED AND RESOLUTION mnsnsuwiamdinanewaiens 4 12 INDEX C 2 NMECA ECX USA 3 RELAXATION TIME MEASUREMENT AND DATA PROCESSING 1 1 RELAXATION TIME MEASUREMENT ccsiemcimnscitsenanesiiienceemnieen 1 1 1 1 1 Relaxation Time T Evaluation vi ccccccsccssccssssesessessseeesscessuneessesseenees 1 1 1 1 2 Measurement of Relaxation Times 7 1 cccccsccscccccsscssccsssseessesssseeeessessenees 1
59. tion becomes zero This delay time is called the null point and is represented by Tup Thus T 1s given by T Ty IN 1 44 X Tau To obtain an accurate value of T first obtain the null point and then perform the array measurement NM ECA ECX USA 3 1 1 1 RELAXATION TIME MEASUREMENT 1 1 2 Measurement of Relaxation Times T E To obtain the null point l Tune the probe 2 Verify the 90 pulse width 4S To enhance accuracy of T measurement verify the 90 pulse width of the Sample used to measure relaxation time To do this perform array measurement in the single pulse or single pulse dec measurement mode 3 Click on the Expmnt button in the Spectrometer Control window The Open Experiment window opens 4 Click on relaxation 4 aabe Open Experiment Path usr delta global experiments toms Psd JQ cosy ex2 AJ cosy_pfg ex2 dept ex2 difference noe 1d ex2 Fig 1 1 Open Experiment window 5 To perform T measurement for H select double_pulse ex2 from the file name list box To perform T measurement for C select double_pulse_dec ex2 4 aabe Open Experiment x Path Ausr delta global experiments relaxatio Format Fite fed Q Directory The Experiment Tool window used to set the parameters opens 1 2 NMECA ECX USA 3 1 RELAXATION TIME MEASUREMENT mar oe ae 6 Enter the following values x_ pulse 90 pulse width obtained in Step 2 tau_interval Value at most 1 10 of the expected
60. uares method Lower weights are applied to measurement points having higher tau_ interval values W eighted L inear Unweighted L inear U nweighted linear least squares method Nonlinear Nonlinear least squares method 4S The statement such as Inv Recovery Sat Recovery and Spin Lock which follows these commands shows experimental method Inv Recovery Sat Recovery and Spin Lock are meaning Inversion Recovery method Saturation Recovery method and Spin Lock method respectively 1 18 NMECA ECX USA 3 1 RELAXATION TIME MEASUREMENT M To execute an approximate calculation and obtain relaxation times Click on the Apply button The approximate calculation is executed and the calculated result of the relaxation time and the yellow approximation curve are displayed i aabe Curve Analysis gibberellic_acid_t1_analysis 2 jdf File Options Y 14 37166 s 1 0 Thousands 12 0 110 100 90 80 7 0 i AI 2 1 0 0 L i Vt PBA Atle JAAS BEB ES 2 398 Scagene Atte S26 SaF SHASARK San Hr GWAVA donaa A X parts per Million 1H Mode Weighted Linear Inv Recovery Peak Height in tegral auto f inf 6 36932E 02 Calculation results of relaxation time Approximation curve 200 0 20 0 600 90 10 0 11 0 120 130 140 7 0 8 0 4S When we enter the selection state by pressing the Apply button the display changes to Auto When changing the peak to obtain
61. ues This operation is the same as that of correcting the phase of the ordinary 1D data 4S eBesure to perform manual phase correction without using automatic phase correction e f you cannot correct the phase of the J modulated and J coupled peak during T measurement refer to the topic labeled Reference below pi Close the1D Processor window The window function condition and the phase correction values obtained in Steps 4 and 5 are automatically inserted in the processing list in the nD Processor window ie Click on the Process File And Put In Data Slate button or Process File And Put i Data Viewer button Normally click on Ly button Clicking on the monn performs the data processing specified in the process ing list for the fie to the nth measurement data sets and displays the processed data sets in the Data Slatewindow Clicking on the button performs the data processing specified in the processing list for the first to the nth measurement data sets and displays the processed data sets in the Data Viewer window 1 10 NMECA ECX USA 3 1 RELAXATION TIME MEASUREMENT Reference If you cannot correct the phase of T transverse relaxation time measurement data Repeat Step 4 using the sinbell window function Perform power processing without phase correction in Step 5 according to the following procedure a Click on the Append button in the1D Processor window b Select PostTransform Abs from the menu bar
62. ulses diffusion time A grad 1 Duration of magnetic field gradient pulse grad 1 amp M agnetic field strength G 4S The duration of magnetic field gradient pulse 6 which is used for calculation of the diffusion coefficient is not equivalent to the parameter grad_1 in some sequences Refer to the parameter delta for the duration of the mag netic field gradient pulse 6 used for the calculation of the diffusion coeffi cient 4a aabe Experiment Tool cpse_ diffusion ptg ex2 gt File Tools View ae ax 0 3 T m z gradient_max Do not exceed gradient max value for grad 1 amp grad shape scc2 nm jeol co jp totsr conection Time wor Collection Time 00 01 49 Fig 2 2 Experiment Tool window 8 Input a number about 10 times the value of T into relaxation_ delay 9 Perform an array measurement at the minimum value and maximum of the variable magnetic field strength that are used in the actual measurement For example to change magnetic field gradient from 3 mT m to 0 27 T m carry out an array measurement at 3 mT m and 0 27 T m 4S The instrument cannot output a magnetic field strength greater than gradi ent max NMECA ECX USA 3 2 5 2 MEASUREMENT OF DIFFUSION COEFFICIENT i i L None Fig 2 3 Array parameter window 10 Process the data in the nD processor window and check the decay of the signal Repeat steps 8 and 9 changing the values of diffusion time and grad_1so that the
63. ument 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 In 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 use of the information contained in this manual or the software described in this manual Some countries do not allow
64. ure ment is carried out without air flowing NM ECA ECX USA 3 4 1 4 MEASUREMENT OF SR MAS 4 2 HOWTO ADJ UST MAGIC ANGLE CAUTION Receive instruction from an experienced person when the magic angle is adjusted the first time The SR MAS probe may be damaged if un suitable adjustment is performed 1 Insert the reference sample KBr 2 Start the spinning 3 Insert the stick for magic angle adjustment through the top of the SCM 4 Change LF Lower frequency channel to Bromine79 observation Check the combination of the stick and the tuning dial for Bromine79 observation 5 Load the pulse sequence global experiments single_pulse ex2 in the Experiment Tool window and perform the following setting e Set observed nucleus to Bromine79 e Set x_sweep to 1000 ppm e Add the repeat flag to Header and turn on spinning e Set scans to 1 6 Click on the Submit button The pulse occurs and measurement starts If the Inform window appears click on the GO button 7 Adjusts a phase by the following procedure a Click on the View button The ViewTool window opens b After clicking on the View button click on the Process vector button to change the display C Select Processing Phase and Processing Phase Boxes The Phase Boxes window opens d Adjust the phase 8 Adjust the magic angle Turn the adjustment stick to maximize the spinning side band of K Br Fig 4 1 4S The gear of the magic angle adjustment mechanism
65. use button move the cursor to the top of a peak that you want to use to calculate the diffusion coefficient then release the mouse button The selected peak changes to white When printing the diffusion coefficient value of two or more peaks collectively drag the mouse cursor around the area of the peaks All the peaks listed in the peak intensity table in the dragged area are selected and their numerical markers change to white NMECA ECX USA 3 2 19 2 MEASUREMENT OF DIFFUSION COEFFICIENT 4A faabe Curve Analysis cpse_manual 3 jdf aeae el l ENE Y 32 mT m abundance 0 1 0 2 12 0 11 0 100 90 80 70 60 50 40 30 20 10 0 10 20 4 6530 E X parts per Million 1H Mode Diffusion Analysis sevens u Peak Heigh t m Integral Ty ype GimT T m e r 0 3 0 2 abundance 01 0 04 0 06 0 08 0 1 0 12 0 14 860 16 0 18 0 2 0 22 0 24 0 26 X Tm 1 6 When displaying the peak intensity table select File Point List in the pull down menu of the Curve Analysis Tool faabe Curve Analysis cpse_manual 3 jdf File Options jom Ie C Points List L Points List 4 6530 Wo X parts per Million 1H Mode Diffusion Analysis Peak Height Integral avy The Point list appears a faahe Points List a 3 2 20 NMECA ECX USA 3 2 MEASUREMENT OF DIFFUSION COEFFICIENT 2 4 2c Method of obtaining diffu
66. ween the selection of ascending and descending order as shown in Fig TZ Set the initial value of the array parameter maximum value to the approximate value of T multiplied by 10 corresponding to infinite tau in the inversion recovery between ascending and descending order S1 1 5151 5 0 8157 0 615 0 4fs 0 2Ish Set Value Fig 1 2 Array parameter window 3 Click on the Set Value button The array parameter window closes and the set values are entered into tau_interval in the E xperiment Tool window el aabe Experiment Tool double_pulse ex2 File Tools View Options ee gg me ee mses ey TA 444 544507 repeti ition me dadi Di 3 EJ Fig 1 3 Experiment Tool window 1 4 NM ECA ECX USA 3 1 RELAXATION TIME MEASUREMENT ae one ae 12 RELAXATION TIME DATA PROCESSING Data processing following measurement is performed in the nD processor window and then T calculation is performed in the Curve Analysis window Chapter 2 explains the procedure for data processing 1 2 1 Loading Relaxation Time Measurement Data First load measurement data in the nD Processor window in the same way as to perform 2D measurement data processing 4S If measurement data was transferred from the spectrometer immediately after relaxation time measurement finished and the nD Processor window is already Open you can omit the procedure of Section 1 2 1 To load relaxation time measurement data FID in the nD Proces

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