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01-999044-00  C0501

UNITY

INOVA Solids Hardware Installation

61

Index

Index

Numerics

1H wideline

, 

51

1H wideline test

, 

56

5-MHz ADC board installation

, 

17

90° pulse measurement

, 

33

A

acquisition console card cages

, 

28

adipic acid

, 

56

amplifier tests

, 

48

AMT amplifier mains supply

, 

30

automatic teller machine (ATM) cards caution

, 

9

B

benzene

, 

51

Bird through-line wattmeter

, 

44

br-24 sequence

, 

57

broadband amplifier

, 

32

C

cautions defined

, 

7

cavity amplifier

, 

44

adjustments

, 

44

fine tuning procedure

, 

45

initial tuning procedure

, 

44

input/output match

, 

46

routine tuning procedure

, 

46

tuning

, 

44

center spike

, 

37

Class A/AB rf amplifiers

, 

25

configuring software

, 

15

CPMAS module

, 

21

adjusting decoupler field strength

, 

23

amplifier power outputs

, 

22

checking the AMT decoupler amplifier

, 

23

fine attenuators

, 

22

hardware installation

, 

21

maximum drive to the AMT

, 

23

maximum droop

, 

23

minimum power

, 

23

pulse droop measurement

, 

22

samples

, 

22

testing the system

, 

22

Cr(acac)3

, 

51

CRAMPS

installations

, 

51

module

, 

17

new ADC installation

, 

17

probe

, 

56

CRAMPS/Multipulse module

CRAMPS probe test

, 

43

experiments

, 

43

NMR tests

, 

43

RF transmitter performance tests

, 

43

system tests

, 

43

testing basic NMR

, 

51

testing CRAMPS NMR

, 

51

testing multipulse NMR

, 

51

credit cards caution

, 

9

D

data acquisition

, 

35

decoupler field gamma-H2

, 

24

decoupler field strength adjustment

, 

49

decoupler field strength gamma-B2

, 

50

decoupler transmitter

, 

32

, 

48

df command

, 

58

E

echo maximum

, 

38

F

facility voltage

, 

30

FIDs

FLIPFLIP

, 

55

FLIPFLIP real channel pattern

, 

54

FLIPFLOP

, 

53

receiver recovery

, 

53

sodium solid standard sample

, 

38

SSECHO

, 

37

system recovery time

, 

36

fine control parameters

, 

22

flammable gases warning

, 

8

FLIPFLIP pulse sequence use

, 

53

FLIPFLOP pulse sequence use

, 

53

further reading

, 

11

G

gate logic

, 

32

gating test

, 

48

getting started

, 

13

H

helium contact with body

, 

8

helium gas flowmeters caution

, 

10

high-power (cavity) amplifier

, 

44

High-Power Amplifier Control Panel

, 

47

high-power amplifiers cautions

, 

10

hollow rotor

, 

22

horns in spectral appearance

, 

37

I

installing the ADC board

, 

17

L

liquids observe

, 

31

M

magic angle

, 

22

magnet quench warning

, 

8

magnetic media caution

, 

9

mains supply

AMT amplifier

, 

30

malonic acid-d4

, 

37

Summary of Contents for UNITY INOVA NMR

Page 1: ...UNITY INOVA Solids Hardware Installation UNITY INOVA NMR Spectrometer Systems Pub No 01 999044 00 Rev C0501 ...

Page 2: ...stems Pub No 01 999044 00 Rev C0501 NOTICE Varian Inc was acquired by Agilent Technologies in May 2010 This document is provided as a courtesy but is no longer kept current and thus will contain historical references to Varian For more information go to www agilent com chem ...

Page 3: ...rmation in this document has been carefully checked and is believed to be entirely reliable However no responsibility is assumed for inaccuracies Statements in this document are not intended to create any warranty expressed or implied Specifications and performance characteristics of the software described in this manual may be changed at any time without notice Varian reserves the right to make c...

Page 4: ...ransfer Test 18 2 3 Pulse Sequences Proton Multipulse NMR 19 Chapter 3 CP MAS Solids Module Installation 21 3 1 Installing the CP MAS Solids Module 21 3 2 Testing the CP MAS Solids System 22 Testing the Amplifier 22 Adjusting Decoupler Field Strength 23 Chapter 4 Solids Cabinet Preparation and Installation 25 4 1 Preparing to Install the Solids Cabinet 25 4 2 Installing the Solids Relay Driver Boa...

Page 5: ...e Tuning the Cavity Amplifier Pulsed Mode 45 Tuning the Cavity Amplifier During Normal Operation 46 Adjusting the Overdrive Interlock 46 6 2 Testing RF Transmitter Performance 47 Testing the Gating 48 Checking Decoupler Transmitter Performance 48 Testing the Amplifier 48 Adjusting Decoupler Field Strength 49 6 3 Testing CRAMPS NMR 51 Testing Multipulse NMR 51 Testing Basic NMR 51 Running the FLIPF...

Page 6: ...8 Figure 14 23Na FID of Sodium Standard NaNO3 Starting at Top of Echo 38 Figure 13 Wideline Spectrum With compul y 39 Figure 15 Wideline Spectrum With Sodium Solid Standard 40 Figure 16 Sample Spectrum From a Probe With Acoustical Ringing 41 Figure 17 Sample Spectrum With Sodium Background 41 Figure 18 Sample Spectrum With Sodium And Aluminium Background 42 Figure 19 High Power Cavity Amplifier 44...

Page 7: ...999044 00 C0501 List of Tables Table 1 Maximum γB2 Values 25 Table 2 Dimensions of Complete Solids Cabinet and UNITYINOVA Cabinet 27 Table 3 Minimum Distances of UNITY INOVA Console from Magnet Centerline 29 Table 4 90 Pulse and Signal to Noise Specifications 39 ...

Page 8: ...rosthetic parts and metal blood vessel clips and clamps Pacemaker wearers should consult the user manual provided by the pacemaker manufacturer or contact the pacemaker manufacturer to determine the effect on a specific pacemaker Pacemaker wearers should also always notify their physician and discuss the health risks of being in proximity to magnetic fields Wearers of metal prosthetics and implant...

Page 9: ...fumes explosion or fire WARNING Leave area immediately in the event of a magnet quench If the magnet dewar should quench sudden appearance of gasses from the top of the dewar leave the area immediately Sudden release of helium or nitrogen gases can rapidly displace oxygen in an enclosed space creating a possibility of asphyxiation Do not return until the oxygen level returns to normal WARNING Avoi...

Page 10: ... includes removable helium vent tubes If the magnet dewar should quench sudden appearance of gases from the top of the dewar and the vent tubes are not in place the helium gas would be partially vented sideways possibly injuring the skin and eyes of personnel beside the magnet During helium servicing when the tubes must be removed carefully follow the instructions and safety precautions given in t...

Page 11: ...ifiers with liquids probes On systems with solids high power amplifiers never operate the amplifiers with a liquids probe The high power available from these amplifiers will destroy liquids probes Use the appropriate high power probe with the high power amplifier CAUTION Take electrostatic discharge ESD precautions to avoid damage to sensitive electronic components Wear a grounded antistatic wrist...

Page 12: ...cters in courier typewriter like characters are used for UNIX or VNMR commands parameters directories and file names in the text of the manual for example The shutdown command is in the etc directory Characters in courier are also used to show screen output for example Self test completed successfully Italic characters are used for text displayed on the screen that is not the same every time for e...

Page 13: ...Introduction 12 UNITYINOVA Solids Hardware Installation 01 999044 00 C0501 ...

Page 14: ... CP MAS Solids Module Wideline Solids Module CRAMPS Multipulse Solids Module Figure 1 shows the UNITYINOVA NMR console next to the solids cabinet This chapter provides information about how to proceed through this manual for different combinations of solids hardware Also in this chapter is information about what to do before the installation is started 320 620 620 Figure 1 UNITYINOVA NMR Console w...

Page 15: ... of the pneumatics tachometer box rotor synchronization and rotor speed control options as specified in the Pneumatics Tachometer Box Installation manual Complete all of Chapter 2 Wideband NMR Module on page 17 Complete all of Chapter 4 Solids Cabinet Preparation and Installation on page 25 Complete all of Chapter 6 CRAMPS Multipulse Module Tests on page 43 Complete Solids Module Complete the inst...

Page 16: ...e The rotor synchronization wideline CRAMPS multipulse and complete solids modules require you to configure the NMR system as described below 1 When bootup is finished log in as vnmr1 you may need to request a password from the user login vnmr1 password 2 After VNMR has started enter the VNMR command config 3 Use the VNMR CONFIG window to configure the system VNMR configuration including details o...

Page 17: ...Chapter 1 Getting Started 16 UNITYINOVA Solids Hardware Installation 01 999044 00 C0501 ...

Page 18: ...e slot to the right of the 500 kHz ADC board Use the usual antistatic precautions and be careful that the small surface mount components on the solder side of the board do not catch on 500 kHz ADC board front panel 3 Route the two BNC cables 00 958298 10 provided in the kit through the cable path on the left of the rf card cage and through the right of the digital card cage Connect the cables as f...

Page 19: ...enter If errors occur check the cable connections If no errors or spurious signals occur the installation is complete Data Transfer Test The wideband module makes it possible to acquire data faster than the computer can store it A fifo underflow will then occur VNMR 5 3 and later software warns when this might happen and suggests a d0 or d1 value that will avoid the problem For a 1D acquisition wi...

Page 20: ...2 3 Pulse Sequences Proton Multipulse NMR The pulse sequence source files flipflop c br24 c cylbr24 c mrev8 c and cylmrev8 c must be modified to function with UNITY INOVA and VNMR 5 2F For UNITY INOVA the receiver is off by default it is on for UNITYplus When using explicit acquisition the receiver is turned on with the beginning of the acquire statement For CRAMPS this is too late the receiver mu...

Page 21: ...Chapter 2 Wideband NMR Module 20 UNITYINOVA Solids Hardware Installation 01 999044 00 C0501 ...

Page 22: ...6 for the location 5 Disconnect all cables two coax input cables two N type output cables the 25 pin D type connector and the power cord If coaxial attenuators are connected to the input of the amplifier leave them attached to the cables 6 Remove the 4 screws from the front of the top AMT linear amplifier and slide the amplifier out of the cabinet Be careful because the amplifier is heavy 7 Instal...

Page 23: ...d samples typically 20 kHz to about 1 ppm CAUTION Read this before doing any tests 1 Run all tests with the XPOLAR pulse sequence and dm nny to provide some protection to the probe from excessive decoupler duty cycle 2 Do not turn on the 100 W amplifier unless the output is connected to a properly tuned probe with a high pass filter at J6003 to a large 50 ohm load or to a large 30 dB attenuator te...

Page 24: ... of end cap will dissolve in the dioxane WARNING The 1 4 dioxane sample 00 957734 01 is a cancer suspect agent containing flammable liquid oxidizers See the enclosed MSDS for additional information and handling precautions 2 Spin the sample slowly 200 300 Hz 3 Enter rtp vnmr tests hmb seqlib xpolar Use XPOLAR with xpol n CAUTION High spinning speeds can cause the rotor to shatter creating a potent...

Page 25: ...il n tn C13 file exp sb not used toss n at 0 100 DECOUPLING gf not used pdp n np 6016 dn H1 awc not used dp y sw 3000 0 dof arrayed lsfid not used SPECIAL xpol n dm nny phfid not used srate 415 tpwr 55 dmm c wtfile temp not used tpwrf 51 dpwr 63 proc ft pw 8 0 level1 57 fn 32768 p1 0 level1f 200 d1 10 000 level2 63 tof 0 level2f 4095 werr nt 1 wexp ct 1 wbs wnt FLAGS ai no ph Gamma H2 calculation ...

Page 26: ...edicated line separate from the 20 A power line used by the UNITYINOVA console Figure 3 illustrates the solids cabinet with the front panel removed 2 The following tools and equipment are needed to perform the upgrade and performance testing Collect these before starting Dual trace oscilloscope capable of accurate voltage measurements from dc to 400 MHz 500 W 30 dB attenuator 2 W rotary attenuator...

Page 27: ...that there is enough room to accommodate the solids cabinet on the floor plan of the laboratory by following the guidelines below a Measure the distance between the edge of the UNITYINOVA console and the centerline of the magnet If this distance is greater than the distance indicated in Table 3 for the specific system go on to step 5 Figure 3 Solids Cabinet Open Front View Status panel Sorensen VT...

Page 28: ... the solids cabinet up towards the right side of the UNITYINOVA console looking from the front so that there is 6 in 15 cm between them and both front panels face the same directions The minimum distance between the edge of the solids cabinet and the magnet must be at least 42 in 107 cm for 300 MHz magnets and 48 in 122 cm for a 400 MHz or any widebore 89 mm magnet 4 2 Installing the Solids Relay ...

Page 29: ... 5 J8212 J8213 U S E R A P U S E R A P CLKSTB ACK 5V ATTEN EMERG J232 ACK J232 STB J233 ACK J233 STB Figure 4 UNITYINOVA Spectrometer Front and Back Views PFG amplifier PTS frequency synthesizers Digital card cage Shim power RF card cage RF control card cage Linear amplifiers Power supply supply Fan Cable tray Solids Relay Driver AMT amplifier vent outlets Shim power Fan VT controller Breakout Pow...

Page 30: ...Bxx and GND rail lower labeled TB2x on the control card cage 4 3 Installing the Solids Cabinet The following steps describe how to install the solids cabinet Figure 5 illustrates the open back of the solids cabinet and the relay panel The table shows which steps to follow for each solids module When Installing Do These Steps Wideline 1 through 5 CRAMPS Multipulse 5 through 10 Complete solids 1 thr...

Page 31: ...onnected between J4073 liquidsAMT channelA out and K5004 3 preamplifier housing Remove this cable 8 Locate the cable 00 990626 16 connected to K7201 C in the solids cabinet Connect the other end to J4073 liquids AMT channel A out 9 Locate the cable 00 990626 17 connected to K7203 C in the solids cabinet Connect the other end to K5004 3 in the preamplifier housing 10 Connect the solids cabinet to t...

Page 32: ...nated in appropriate 50 ohm loads at all times The high power available from the amplifier in the solids cabinet is intended only for solids experiments Applying this power to a liquids probe will destroy the probe Before turning on the amplifier in the solids cabinet check that the appropriate solids probe has been put in place Always disable all high power solids amplifiers before installing any...

Page 33: ...ier at the front panel and check that all interlocks go out Only the light labeled POWER should be lit If the status lights labeled PULSE WIDTH and or DUTY CYCLE are lit move jumper J2 on the Solids Relay Driver board to short the middle and bottom pins 4 Confirm that the minimum full power output in the pulsed mode is 1 kW 60 dBm This should not require adjustment of the amplifier gain 5 Observe ...

Page 34: ...following NMR performance using the 1 M NaCl 2 D2O 98 H2O standard sample Part No 00 969104 03 Measuring 90 Pulse and System Sensitivity 1 Enter rtp vnmr stdpar H2 to recall parameters 2 Set up the spectrometer for data acquisition as follows nt 1 dm n dp y lb 50 gain 0 rof1 30 alfa 0 sw 1e5 np max fn 65536 3 Enter su 4 Tune the probe to the deuterium resonance frequency refer to the NMR Probes In...

Page 35: ...kHz 800 700 600 500 400 300 200 100 0 S N 249 6 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 61 395 date Apr 1 lb 50 00 il n tn H2 solvent none sb not used in n at 0 008 file vnmr gf not used dp y np 16384 stdpar H2 awc not used hs nn sw 1e 06 DECOUPLING lsfid not used fb 1e6 dn H1 phfid 90 0 bs not used dof 0 wtfile ss 0 dm n proc ft SPECIAL tpwr 57 dmm c fn 65536 temp not used pw 2 2 dmf 4000 math f...

Page 36: ...nter this value for pw90 4 Set tof to 1 kHz off resonance 5 Measure 23Na sensitivity Use a spectral noise region of 20 kHz centered approximately 10 kHz off resonance Refer to Figure 9 for sample spectrum Figure 9 Sample Sodium 90 Pulse and Sensitivity Spectrum 300 MHz System 1000 kHz 500 0 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 105 800 date Apr 1 lb 50 00 il n tn Na23 solvent none sb not used i...

Page 37: ...e point in the FID where the normal noise level returns The difference between the cursors should be less than 12 µs Refer to Figure 10 for a sample FID display Figure 10 System Recovery Time Sample FID Display System recovery time 7 1 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 105 800 date Apr 1 lb 50 00 il n tn Na23 solvent none sb not used in n at 0 004 file vnmr gf not used dp y np 16384 tests N...

Page 38: ...nd not hardware malfunctions When phased properly the height of the two horns of the pattern should differ by less than 5 The sample has D2O therefore you get a center spike that will phase correctly only if np 16384 5 Set pw to the 90 pulse for 2H Figure 11 shows an example SSECHO FID using lsfid and correct phase Refer to Figure 12 for all other spectral parameters Set tof on resonance for the w...

Page 39: ...all the standard test parameter by entering rt vnmr tests Na23wl The sodium solid standard FID appears similar to the example in Figure 14 Figure 12 Wideline SSpectrum of Malonic Acid d6 With compul n 1600 kHz 1200 1000 800 600 400 200 0 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 61 395 date Apr 1 lb 1000 00 il n tn H2 solvent none sb not used in n at 0 082 file vnmr gf not used dp y np 16384 tests ...

Page 40: ... a flat noise baseline with no broad peaks Refer to Figure 16 for test parameters and results with a probe that does exhibit acoustical ringing 11 The wideline probe does exhibit 23Na and 27Al background due to the glass rods in the coil support Refer to Figure 17 and Figure 18 for an example of the expected sodium and aluminum background Figure 13 Wideline Spectrum With compul y 1200 1600 kHz 100...

Page 41: ...1 lb 1000 00 il n tn Na23 solvent none sb not used in n at 0 082 file vnmr gf not used dp y np 16384 tests Na23wl awc not used hs nn sw 2e 06 DECOUPLING lsfid 10 compul n fb 1e 06 dn H1 phfid 90 0 tof 0 dof 0 wtfile tpwr 57 dm n proc ft SPECIAL pw 2 7 fn 65536 temp not used p1 0 p180 0 d1 1 000 TRANSIENTS werr tau1 20 0 bs not used wexp tau2 15 0 ss 0 wbs nt 16 wnt ct 0 1200 1600 kHz 1000 800 600 ...

Page 42: ...roc ft SPECIAL pw 2 2 fn 65536 temp not used p1 0 p180 0 d1 1 000 TRANSIENTS werr tau1 20 0 bs not used wexp tau2 15 0 ss 0 wbs nt 16 wnt ct 0 Figure 17 Sample Spectrum With Sodium Background 1600 2000 kHz 1200 1000 600 400 200 0 1400 800 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 105 800 date Apr 1 lb 1000 00 il n tn Na23 solvent none sb not used in n at 0 082 file vnmr gf not used dp y np 16384 te...

Page 43: ...AMPLE PROCESSING FLAGS sfrq 105 800 date Apr 1 lb 1000 00 il n tn Na23 solvent none sb not used in n at 0 082 file vnmr gf not used dp y np 16384 tests Na23wl awc not used hs nn sw 2e 06 DECOUPLING lsfid 10 compul n fb 1e 06 dn H1 phfid 90 0 tof 0 dof 0 wtfile tpwr 57 dm n proc ft SPECIAL pw 2 7 fn 65536 temp not used p1 0 p180 0 d1 1 000 TRANSIENTS werr tau1 20 0 bs not used wexp tau2 15 0 ss 0 w...

Page 44: ...erformance AMT amplifier calibration 1 kW amplifier calibration gating CRAMPS Multipulse NMR tests Decoupler calibration FLIPFLIP FLIPFLOP MREV8 1 H wideline CRAMPS probe test Varian supplied probe only MREV8 narrowing at magic angle BR24 narrowing at the magic angle CAUTION Read the following cautions Make sure that all amplifiers are terminated in appropriate 50 ohm loads at all times The high p...

Page 45: ...ge section Contact with a bare terminal can result in serious injury or death The high voltage section has no tuning adjustments Only qualified service personnel shall remove the cover CAUTION To prevent the cavity amplifier from failing never let the grid current exceed 160 mA pulsed or 60 mA CW continuous wave The tuning procedure is broken into three sections initial tuning and fine tuning whic...

Page 46: ...tenna do not exceed the 3 o clock position shown in Figure 19 in a counter clockwise direction The antenna is damaged when it contacts the moving load wall of the cavity Also do not over loosen the locking ring because the antenna will become loose move freely and be damaged 7 Rotate the output coupling lever to achieve maximum power output and then tighten the locking disk to hold this position 8...

Page 47: ... tn H1 sw 1e5 at 01 d1 0 nt 1e6 2 Attempt to maximize the output power while minimizing the grid current Adjust both TUNE and LOAD to maximize the output The gain should be 14 dB at 46 dBm input To find the amplifier input output match begin with the TUNE at one extreme and then adjust the LOAD for a maximum Then move the TUNE 20 towards the other extreme and readjust the LOAD for a new maximum Co...

Page 48: ...er 3 Make sure that the power to the third cabinet and the low voltage power supply are on Wait 3 minutes 4 After three minutes switch on the EHT supply and make sure of the following The EHT voltage readout is 2 2 kV or greater The EHT current is no more than 2 2 mA pulsed mode or 55 mA CW mode 5 Carefully tune the cavity amplifier See Tuning the High Power Cavity Amplifier on page 44 for the tun...

Page 49: ...signal J7024 and observe rf Determine the gating delay by measuring the time at which the rf is fully on Add 200 ns to this value The liquids amplifier should gate on in less than 2 µs 4 Repeat steps 1 through 3 with both HI BAND and LO BAND set to HI POWER The rf should gate on in less than 2 µs Checking Decoupler Transmitter Performance Confirm that the decoupler transmitter output to the probe ...

Page 50: ...tput level in watts 4 Decrease the value of level2 until this output is no more than 100 W Note that you must enter aa level2 go where is a new value for level2 each time you change the value of level2 5 When the level2 value is determined halt the acquisition and write down the value so you can refer to it later 6 Enter aa and return the system to normal configuration Note Whenever level1 63 or l...

Page 51: ...alculate γB2 Set dpwr to achieve a γB2 that is as close as possible to the minimum values listed in the following table Do not exceed this power level for any other experiment For the XPOLAR pulse sequence the maximum level1 and level2 correspond to this dpwr value Magnet Varian RT CP MAS Doty CP MAS Varian VT CP MAS 200 MHz 75 kHz Figure 21 Decoupler Field Strength γB2 ACQUISITION SAMPLE PROCESSI...

Page 52: ...lse NMR Use a CRAMPS probe if available or a wideline probe tuned to the 1 H frequency The following tests are performed using a test sample of benzene and Cr acac 3 Part No 00 958984 87 in a spherical bulb This sample provided with the kit is inserted into the coil of the probe so that it is at the center of the coil Note that is essential that the spherical portion of the sample has no air bubbl...

Page 53: ... use 12 Enter rof2 0 alfa 0 sw 2e6 go to reacquire a single FID Figure 23 shows an example of a receiver recovery FID 13 Enter df and examine the beginning of the FID Using a cursor determine the time taken for the receiver system to recover and write down the value Figure 22 Standard 1 H Observe Spectrum Using the S2PUL Pulse Sequence 800 k 600 k 400 k 200 k 0 200 k 400 k 600 k 800 k Hz ACQUISITI...

Page 54: ... the pw for a 90 pulse from the following relationship where N is the number of points in 1 cycle pw pw 4 N 6 Repeat the acquisition adjusting pw and then tpwr to get approximately a 1 5 µs 90 pulse 7 Enter gf and then connect to the acqi window Select FID and then IPA Adjust tpwrf until a pattern similar that in Figure 25 is obtained This occurs at the exact 90 pulse Running the FLIPFLOP Pulse Se...

Page 55: ...cannot be done carefully adjust the 1 kW amplifier tune or load The desired result is shown in Figure 27 Figure 24 Real Channel FID Pattern ACQUISITION SAMPLE PROCESSING FLAGS sfrq 399 952 date Apr 1 lb not used il n tn H1 file exp sb not used in n np 128 DECOUPLING gf not used dp y sw 2e 06 dn H1 awc not used trig y fb 1e 06 dof 0 lsfid 0 SPECIAL bs 16 dm n phfid not used srate 1542 ss 0 dpwr 30 ...

Page 56: ...399 952 date Apr 1 lb not used il n tn H1 file exp sb not used in n np 128 DECOUPLING gf not used dp y sw 2e 06 dn H1 awc not used trig y fb 1e 06 dof 0 lsfid 0 SPECIAL bs 16 dm n phfid not used srate 1542 ss 0 dpwr 30 fn 4096 temp 27 0 tpwr 54 tpwrf 2794 werr tauc 10 000 pw 1 400 wexp df mp_at 0 000640 tau 10 000 wbs d1 4 000 wnt phase1 0 tof 2986 3 FLAGS phase2 0 nt 1 ai cdc ph phaser 65 7 ct 0 ...

Page 57: ... quantitative result 1 Use adipic acid as the sample If using a CRAMPS probe pack a rotor as detailed in Preparing the Sample on page 56 for the CRAMPS probe tests If using a wideline probe pack a 15 mm long piece of 5 mm NMR tube with about 3 mm in depth of adipic acid Try to arrange this so that when placed in the probe it is approximately in the center of the coil 2 Install the probe and sample...

Page 58: ...e a spectrum and check that it looks similar to the one in Figure 29 Note that the dscale values are wrong Vary tof to get the best resolution of the right hand peaks 8 Place a cursor on each peak of the doublet and enter scalesw sfrq delta to set the scale factor 9 Place the cursor on the right most peak and enter rl 2p to reference it The spectrum should now have resonances at 2 3 and about 14 p...

Page 59: ...doublet while keeping all peaks on the same side of the center spike 6 Set a cursor on each peak on the right hand pair and enter scalesw sfrq delta to scale the spectrum 7 Place the cursor on the right most peak and enter rl 2p to reference the spectrum See Figure 30 Now you can measure the resolution by measuring the width at half height of either of the right hand peaks You must use the cursors...

Page 60: ...6 3 Testing CRAMPS NMR 01 999044 00 C0501 UNITYINOVA Solids Hardware Installation 59 Figure 30 CRAMPS Adipic Acid Spectrum Using the BR24 Pulse Sequence ...

Page 61: ...Chapter 6 CRAMPS Multipulse Module Tests 60 UNITYINOVA Solids Hardware Installation 01 999044 00 C0501 ...

Page 62: ... 17 new ADC installation 17 probe 56 CRAMPS Multipulse module CRAMPS probe test 43 experiments 43 NMR tests 43 RF transmitter performance tests 43 system tests 43 testing basic NMR 51 testing CRAMPS NMR 51 testing multipulse NMR 51 credit cards caution 9 D data acquisition 35 decoupler field gamma H2 24 decoupler field strength adjustment 49 decoupler field strength gamma B2 50 decoupler transmitt...

Page 63: ...0 pulse and sensitivity spectrum 35 sodium resonance 35 software confguring VNMR 15 versions 15 solid sample preparation 56 solids cabinet before you install 25 class A AB rf amplifiers 25 dimensions 25 installation 29 main power supply 25 open front view illustration 25 preinstallation preparation 25 relay performance test 31 required tools and equipment for installation 25 space requirements 26 ...

Page 64: ...fined 7 wideband NMR module installing the Solids ADC DTM board 17 wideline module spectral appearance 37 wideline probe 56 wideline solids module NMR tests 31 RF transmitter performance tests 31 system recovery time 36 test procedures 31 test sample kit 33 testing 1H wideline 56 wideline spectral appearance 37 X XPOLAR pulse sequence 22 ...

Page 65: ...Index 64 UNITYINOVA Solids Hardware Installation 01 999044 00 C0501 ...

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