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Varian UNITY INOVA NMR Hardware Installation

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INOVA
UNITY
Solids Hardware
Installation
UNITY
INOVA NMR Spectrometer Systems
Pub. No. 01-999044-00, Rev. C0501

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Summary of Contents for Varian UNITY INOVA NMR

  • Page 1 INOVA UNITY Solids Hardware Installation UNITY INOVA NMR Spectrometer Systems Pub. No. 01-999044-00, Rev. C0501...
  • Page 2 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 This document is provided as a courtesy but is no longer kept current and thus will contain historical references to Varian.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 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 changes in any products herein to improve reliability, function, or design. Varian does not assume any liability arising out of the application or use of any product or circuit described herein;...

  • Page 4: Table Of Contents

    Table of Contents Safety Precautions..................... 7 Introduction ...................... 11 Chapter 1. Getting Started................13 Solids Modules Installation Guide ................14 CP/MAS Module ....................14 Wideline Module ....................14 CRAMPS/Multipulse Module ................14 Complete Solids Module ................... 14 Solid-State Variable Temperature System ............
  • Page 5 Table of Contents Measuring 90° Pulse and System Sensitivity ............ 33 Sodium 90° Pulse and Sensitivity Measurement ..........35 System Recovery Time ..................36 Wideline Spectral Appearance ................37 Chapter 6. CRAMPS/Multipulse Module Tests ..........43 Tuning the High-Power (Cavity) Amplifier ............... 44 Initial Tuning of the Cavity Amplifier (CW Mode) ...........
  • Page 6 List of Figures UNITY Figure 1. INOVA NMR Console with Solids Cabinet ............. 13 Decoupler Field γ B Figure 2......................24 Figure 3. Solids Cabinet Open Front View ..................26 UNITY Figure 4. INOVA Spectrometer, Front and Back Views ............28 Figure 5.
  • Page 7 List of Figures List of Tables Maximum γ B Table 1. Values ...................... 25 UNITY Table 2. Dimensions of Complete Solids Cabinet and INOVA Cabinet ......... 27 UNITY Table 3. Minimum Distances of INOVA Console from Magnet Centerline ......29 Table 4.

  • Page 8: Safety Precautions

    Safety Precautions The following warning and caution notices illustrate the style used in Varian manuals for safety precaution notices and explain when each type is used: WARNING: Warnings are used when failure to observe instructions or precautions could result in injury or death to humans or animals, or significant property damage.
  • Page 9 Any unauthorized modification could injure personnel or damage equipment and potentially terminate the warranty agreements and/or service contract. Written authorization approved by a Varian, Inc. product manager is required to implement any changes to the hardware of a Varian NMR spectrometer.
  • Page 10 Failure to comply with these cautions, or with specific cautions elsewhere in Varian manuals, violates safety standards of design, manufacturing, and intended use of the instrument. Varian assumes no liability for customer failure to comply with these precautions.
  • Page 11 SAFETY PRECAUTIONS Caution Notices ( continued ) CAUTION: Keep the PCs, (including the LC STAR workstation) beyond the 5- gauss perimeter of the magnet. Avoid equipment damage or data loss by keeping PCs (including the LC workstation PC) well away from the magnet. Generally, keep the PC beyond the 5-gauss perimeter of the magnet.

  • Page 12: Introduction

    Introduction This manual describes the procedures used for installing and testing the following solids modules on UNITY INOVA NMR spectrometers: • CP/MAS Solids Module • Wideline Solids Module • CRAMPS/Multipulse Solids Module Other Applicable Manuals NMR Probes Installation manual. Pneumatics/Tachometer Box Installation manual for installing the pneumatics/tachometer box, rotor speed control, rotor synchronization, and pneumatics/tachometer box upgrade for rotor speed control, are provided in .
  • Page 13 Introduction UNITY INOVA Solids Hardware Installation 01-999044-00 C0501...

  • Page 14: Chapter 1. Getting Started

    Getting Started Chapter 1. This manual describes the procedures used for installing and testing the following solids modules on UNITY INOVA NMR spectrometers: • CP/MAS Solids Module • Wideline Solids Module • CRAMPS/Multipulse Solids Module Figure 1 shows the UNITY INOVA NMR console next to the solids cabinet.

  • Page 15: Solids Modules Installation Guide

    Chapter 1. Getting Started 1.1 Solids Modules Installation Guide Listed below are the chapters in this manual that guide you in installing the different solids modules. Work through the chapters, in the order listed, under the solids module you want to install.

  • Page 16: Saving The Current Experiment

    1.5 When the Installation is Finished All replaced items from the system and all unused items from the hardware installation kit must be packaged and returned to Varian. UNITY 01-999044-00 C0501 INOVA Solids Hardware Installation...
  • Page 17 Chapter 1. Getting Started UNITY INOVA Solids Hardware Installation 01-999044-00 C0501...

  • Page 18: Chapter 2. Wideband Nmr Module

    Wideband NMR Module Chapter 2. Install the Wideband NMR Module (01-903007-00) according to the following procedure. The Wideband NMR Module is a board that includes two 5-MHz 12-bit ADCs and 2 MB of onboard memory. CAUTION: The following installation involves handling static sensitive equipment—PROMs and printed circuit boards.

  • Page 19: Testing The Wideband Nmr Module

    Chapter 2. Wideband NMR Module Double click on the loadpatch icon. Read the instructions associated with the installation. The installation may take several minutes. An alternative to using File Manager is to use a Shell Tool. Open a Shell Tool, change to the /cdrom directory and enter ./loadpath.

  • Page 20: Pulse Sequences Proton Multipulse Nmr

    2.3 Pulse Sequences Proton Multipulse NMR d1(s) >0, acqi, 2D, or array >0, acqi, 2D, or array 0.05 Operation with a shorter d1 may cause an error (fifo underflow) and halt the acquisition. If an underflow error occurs, decrease np or increase d1. Run with bs='n' if possible. Once a fifo underflow error has been generated it is sometimes necessary to run one scan successfully with a small number of points (say 2k) before continuing.
  • Page 21 Chapter 2. Wideband NMR Module UNITY INOVA Solids Hardware Installation 01-999044-00 C0501...

  • Page 22: Chapter 3. Cp/Mas Solids Module Installation

    CP/MAS Solids Module Installation Chapter 3. The CP/MAS solids module enables Varian NMR spectrometers to run CP/MAS and MAS experiments. This chapter covers the installation of the CP/MAS amplifier on the NMR spectrometer. The two sections of this chapter are the following: •...

  • Page 23: Testing The Cp/Mas Solids System

    3.2 Testing the CP/MAS Solids System The CP/MAS Solids Module for Varian NMR spectrometers is used to acquire NMR data from solid samples. The sample, usually a powder, is packed into a hollow rotor. The rotor is placed in the probe at the “magic angle”...

  • Page 24: Adjusting Decoupler Field Strength

    3.2 Testing the CP/MAS Solids System Set the decoupler to OFF by entering dm='nnn' tpwr=63 tpwrf=4095 go; then measure the power and droop of observe pulse amplifier. It should meet the following values: • Minimum power: 300 W, 220 Vpp, +54 dBm (6.3 Vpp, when measured through a 30-dB attenuator).

  • Page 25: Figure 2. Decoupler Field Γb

    Figure Measure the residual splitting of the dioxane triplet. Use h2cal to calculate γB Minimum values are shown in Table Table 1. Maximum γB Values Varian RT Probe, Varian VT Probe, Doty Probe, 7mm Magnet Other Probes 200 MHz 75 kHz —...

  • Page 26: Chapter 4. Solids Cabinet Preparation And Installation

    Spectrum analyzer • Complete Varian field service engineer tool kit Check the items in the shipping kit against the parts list. If all the parts on the list are included in the kit, proceed to the next step. If anything is missing, obtain it before proceeding.

  • Page 27: Figure 3. Solids Cabinet Open Front View

    Chapter 4. Solids Cabinet Preparation and Installation WARNING: Remember that during the installation the magnet is up to field. Equipment and tools used by the moving crew must be evaluated for safety. Install a plastic chain (or chain of other nonmagnetic material) at about 42 in.

  • Page 28: Installing The Solids Relay Driver Board

    4.2 Installing the Solids Relay Driver Board If the distance is less than the distance indicated above, determine how much distance must be added to accommodate the solids cabinet: – distance from above actual distance additional distance table needed Place the acquisition console at the correct distance. Disconnect all cables from the magnet leg and move the cables away from the right side of the console.

  • Page 29: Figure 4. Unity Inova Spectrometer, Front And Back Views

    Chapter 4. Solids Cabinet Preparation and Installation Front View PFG amplifier RF card cage RF control card cage PTS frequency synthesizers Digital card cage Linear amplifiers Shim power Power supply supply Back View panel panel Cable tray Solids Relay Driver Breakout board (00-992962-01) panel...

  • Page 30: Installing The Solids Cabinet

    4.3 Installing the Solids Cabinet Install the Solids Relay Driver board (00-992962-01) by inserting the four screws removed step Connect the ribbon cable at J7001 and connect the power cable at J7004. Reconnect the tune relay cable at J7301. Connect one end of the second power cable (00-993140-00) to J7003 on the Solids Relay Driver board.

  • Page 31: Setting The Amt Amplifier Main Supply

    Chapter 4. Solids Cabinet Preparation and Installation Locate the cable connected between J4072 (liquids AMT channel B out) and K5004- 2 (preamplifier housing). Remove this cable. Locate the cable (00-990626-16) connected to K7200-C in the solids cabinet. Connect the other end to J4072 (liquids AMT channel B out). Locate the cable (00-990626-17) connected to K7202-C in the solids cabinet Connect the other end to K5004-2 in the preamplifier housing.

  • Page 32: Chapter 5. Wideline Module Tests

    Wideline Module Tests Chapter 5. This chapter contains test procedures for the wideline module. The tests are broken into two groups as follows: RF transmitter performance tests: • Liquids observe transmitter rf signal path • Solids observe transmitter rf signal path •...

  • Page 33: Testing The Solids Observe Transmitter Rf Signal Path

    Chapter 5. Wideline Module Tests Enter the following parameters to observe the transmitter pulse along the transmitter pathway: nt=1e5 pw=100 dm='n' rof1=30 rof2=0.2 alfa=0 sw=1e5 at=0.001 tpwr=63. On the solids cabinet control panel (see Figure 7), set the LO BAND switch to HI POWER.

  • Page 34: Solids Cabinet Status Light And Safety Switch Performance

    5.2 Wideline NMR Tests in a normal, liquids-only NMR spectrometer and should be under the control of dpwr as usual. Some parameters in the acquisition group may not be displayed in dg if they are set to zero. Be aware of power parameters like tpwr, dpwr, and pulse lengths. Check their values at experiment setup! Solids Cabinet Status Light and Safety Switch Performance Make sure that there is no observe or decoupler output to the probe with the amplifier...

  • Page 35: Figure 8. Sample Spectrum, S/N = 249.6, 300-Mhz System

    Chapter 5. Wideline Module Tests absolute value mode, with vs=1000, normalized, nm. Confirm that the quadrature image is less than 1% by height as compared to the main resonance. Set tof to 1 kHz off-resonance. Measure H sensitivity. Use a spectral noise region of 20 kHz, centered approximately 10 kHz off-resonance.

  • Page 36: Sodium 90° Pulse And Sensitivity Measurement

    5.2 Wideline NMR Tests Sodium 90° Pulse and Sensitivity Measurement Use the standard liquid sample(00-969104-03), the same as for Enter rtp('/vnmr/tests/Na23wl') to recall parameters. Set up the spectrometer for data acquisition as follows: seqfil='s2pul' nt=1 sw=1e5 np=max dm='n' dp='y' lb=50 gain=0 rof1=30 alfa=0 fn=65536.

  • Page 37: System Recovery Time

    Chapter 5. Wideline Module Tests System Recovery Time This test is run with no sample in the probe. Remove the sample and retune the probe. Set the spectrometer as follows: rof2=0 sw=2e6 np=16384 nt=1 alfa=0. Set pw to the value of pw90. Enter go.

  • Page 38: Wideline Spectral Appearance

    5.2 Wideline NMR Tests Wideline Spectral Appearance Insert wideline solids sample (Part No. 00-969104-00). Tune the probe carefully for H frequency. If you need to, refer to the NMR Probes Installation manual for tuning instructions. Acquire a quadrupolar signal of the malonic acid-d sample using the SSECHO pulse sequence and following the instructions in the User Guide: Solid-State NMR.

  • Page 39: Figure 12. Wideline Sspectrum Of Malonic Acid-D With Compul='N

    Chapter 5. Wideline Module Tests 1600 kHz 1200 1000 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 61.395 date Apr 1 1000.00 solvent none not used 0.082 file /vnmr/~ not used 16384 tests/H2wl not used 2e+06 DECOUPLING lsfid compul 1e+06 phfid 90.0 wtfile tpwr proc SPECIAL...

  • Page 40: Figure 13. Wideline Spectrum With Compul='Y

    5.2 Wideline NMR Tests 1600 kHz 1200 1000 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 61.395 date Apr 1 1000.00 solvent none not used 0.082 file /vnmr/~ not used 16384 tests/H2wl not used 2e+06 DECOUPLING lsfid compul 1e+06 phfid 90.0 wtfile tpwr proc SPECIAL 65536...

  • Page 41: Figure 15. Wideline Spectrum With Sodium Solid Standard

    Chapter 5. Wideline Module Tests 1600 kHz 1200 1000 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 105.800 date Apr 1 1000.00 Na23 solvent none not used 0.082 file /vnmr/~ not used 16384 tests/Na23wl not used 2e+06 DECOUPLING lsfid compul 1e+06 phfid 90.0 wtfile tpwr proc...

  • Page 42: Figure 16. Sample Spectrum From A Probe With Acoustical Ringing

    5.2 Wideline NMR Tests 1600 kHz 1200 1000 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 61.395 date Apr 1 1000.00 solvent none not used 0.082 file /vnmr/~ not used 16384 tests/H2wl not used 2e+06 DECOUPLING lsfid compul 1e+06 phfid 90.0 wtfile tpwr proc SPECIAL 65536...

  • Page 43: Figure 18. Sample Spectrum With Sodium And Aluminium Background

    Chapter 5. Wideline Module Tests 2000 kHz 1600 1400 1200 1000 ACQUISITION SAMPLE PROCESSING FLAGS sfrq 105.800 date Apr 1 1000.00 Na23 solvent none not used 0.082 file /vnmr/~ not used 16384 tests/Na23wl not used 2e+06 DECOUPLING lsfid compul 1e+06 phfid 90.0 wtfile...

  • Page 44: Chapter 6. Cramps/Multipulse Module Tests

    CRAMPS/Multipulse Module Tests Chapter 6. The CRAMPS/Multipulse Solids Module enables Varian UNITY INOVA spectrometers to run CRAMPS and multipulse experiments. The CRAMPS/multipulse experiment is normally used to observe H. In CP/MAS, the H amplifier is used as a heteronuclear decoupler, while in CRAMPS the H amplifier is used as an high-power observe channel.

  • Page 45: Tuning The High-Power (Cavity) Amplifier

    Chapter 6. CRAMPS/Multipulse Module Tests 6.1 Tuning the High-Power (Cavity) Amplifier The most reliable method for tuning the cavity amplifier (shown in Figure 19) requires a Bird through-line wattmeter on the input to the cavity and some other power measuring device on the output from the cavity.

  • Page 46: Fine Tuning The Cavity Amplifier (Pulsed Mode)

    6.1 Tuning the High-Power (Cavity) Amplifier WARNING: This procedure exposes the operator to high voltages. Take all appropriate safety precautions! Exercise extreme care! Turn on the low voltage power supply to energize the tube filament. CAUTION: Do not apply rf input or high voltage supply until at least 3 minutes after turning on the low voltage power supply.

  • Page 47: Tuning The Cavity Amplifier During Normal Operation

    Chapter 6. CRAMPS/Multipulse Module Tests 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. Continue in this way (40%, 60%, .

  • Page 48: Testing Rf Transmitter Performance

    6.2 Testing RF Transmitter Performance If this is not the value, adjust the potentiometer R83 (in zone P4) on the board to obtain it. (The range is from 80 mA (4.96 V) to 160 mA (9.92 V)). Reassemble the amplifier and return it to the cabinet. 6.2 Testing RF Transmitter Performance This series of tests evaluates the third cabinet relay and attenuator operation as well as the 1 kW amplifier power output and performance.

  • Page 49: Testing The Gating

    Chapter 6. CRAMPS/Multipulse Module Tests Enter go. Check rf power of about 44 dBm. Stop the acquisition. Set tpwr=50 and set HI BAND to HI POWER. Confirm rf power of about 50 dBm at the preamplifier. Set tpwr=63. Restart and check for 900 W (59.5 dBm) or more at the preamplifier.

  • Page 50: Adjusting Decoupler Field Strength

    6.2 Testing RF Transmitter Performance Set the following parameters: level2=63 level2f=4095 nt=1e6 dm='nny' sw=1e5 np=128 d1=0.1 Enter go and add sufficient in-line attenuators so that the peak power does not exceed 2 mW (+3 dBm). Enter aa to stop the acquisition and then reconnect the AMT amplifier. At the input to the high-power decoupler amplifier, calibrate power as a function of level2 when level2f=4095.

  • Page 51: Figure 21

    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 —...

  • Page 52: Testing Cramps Nmr

    • FLIPFLOP • MREV8 • H wideline If the CRAMPS probe is supplied by Varian, two further spinning tests should be performed on adipic acid: • MREV8 • BR24 Before operating the cavity amplifier, it must be tuned as described in “Tuning the High-...

  • Page 53: Figure 22. Standard 1 H Observe Spectrum Using The S2Pul Pulse Sequence

    Chapter 6. CRAMPS/Multipulse Module Tests 800 k 600 k 400 k 200 k -200 k -400 k -600 k -800 k ACQUISITION SAMPLE PROCESSING FLAGS sfrq 399.952 date Apr 1 not used file not used 16384 DECOUPLING not used 1e+04 not used trig lsfid...

  • Page 54: Running The Flipflip Pulse Sequence

    6.3 Testing CRAMPS NMR Figure 23. Receiver Recovery FID Running the FLIPFLIP Pulse Sequence Enter flipflop and set d1=4 pw=1.5 fb=1e6 sw=2e6 np=128 tau=7 rof1=1.5 rof2=0. Set phase1=0 phase2=0 (this sets up the “flipflip mode”) phaser=0 phfid=0 or 'n' trig='n' gain=0 nt=1 dp='y'. UNITY Note that trig='n' is needed for INOVA systems since the 500-kHz synching...

  • Page 55: Figure 24. Real Channel Fid Pattern

    Chapter 6. CRAMPS/Multipulse Module Tests ACQUISITION SAMPLE PROCESSING FLAGS sfrq 399.952 date Apr 1 not used file not used DECOUPLING not used 2e+06 not used trig 1e+06 lsfid SPECIAL phfid not used srate 1542 dpwr 4096 temp 27.0 tpwr tpwrf 3500 werr tauc...

  • Page 56: Figure 25. Flipflip Fid At Exact 90° Pulse

    6.3 Testing CRAMPS NMR Figure 25. FLIPFLIP FID at Exact 90° Pulse ACQUISITION SAMPLE PROCESSING FLAGS sfrq 399.952 date Apr 1 not used file not used DECOUPLING not used 2e+06 not used trig 1e+06 lsfid SPECIAL phfid not used srate 1542 dpwr 4096...

  • Page 57: Using Mrev8 To Demonstrate Multipulse Operation

    2 MHz wide. The upper trace is an expansion showing the shape of the line. Testing the CRAMPS Probe Follow the two procedures in this section only if you are installing a Varian probe. Preparing the Sample The final tests are performed using a solid sample of adipic acid. This compound is a white powder.

  • Page 58: Figure 28. Adipic Acid Spectrum

    6.3 Testing CRAMPS NMR Figure 28. Adipic Acid Spectrum Tamp down this sample carefully. Then add a small amount of adipic acid and tamp the acid down. Fill the rotor with more inert material and insert the cap. Replace the benzene sample with the adipic acid sample. Do not retune the probe. Put the probe in the magnet and spin the sample at 1550 Hz.

  • Page 59: Figure 29. Cramps Adipic Acid Spectrum Using The Mrev8 Pulse Sequence

    Chapter 6. CRAMPS/Multipulse Module Tests Acquire a FID. Display the FID using the df command and phase it so that the real channel has no on-resonance component. This is used later in step 5. Transform the FID and check that the result is an adipic acid spectrum. Note that a quad image and a large zero spike appear.

  • Page 60: Figure 30. Cramps Adipic Acid Spectrum Using The Br24 Pulse Sequence

    6.3 Testing CRAMPS NMR Figure 30. CRAMPS Adipic Acid Spectrum Using the BR24 Pulse Sequence UNITY 01-999044-00 C0501 INOVA Solids Hardware Installation...
  • Page 61 Chapter 6. CRAMPS/Multipulse Module Tests UNITY INOVA Solids Hardware Installation 01-999044-00 C0501...

  • Page 62: Index

    Index Index Numerics 1H wideline data acquisition 1H wideline test decoupler field gamma-H2 5-MHz ADC board installation decoupler field strength adjustment 90° pulse measurement decoupler field strength gamma-B2 decoupler transmitter df command acquisition console card cages adipic acid amplifier tests echo maximum AMT amplifier mains supply automatic teller machine (ATM) cards caution...
  • Page 63 Varian CRAMPS probe tram tracks transmitter rf signal path tune-up sequences safety precautions tuning the cavity amplifier samples adipic acid...
  • Page 64 Index VNMR voltage requirements VT experiment warning warnings defined wideband NMR module installing the Solids ADC/DTM board wideline module spectral appearance wideline probe wideline solids module NMR tests RF transmitter performance tests system recovery time test procedures test sample kit testing 1H wideline wideline spectral appearance XPOLAR pulse sequence...
  • Page 65 Index UNITY INOVA Solids Hardware Installation 01-999044-00 C0501...

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