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UNITYINOVA Acceptance Tests & Specifications

1. Console Acceptance Tests amp Specifications 0800 ap as VARIAN Console Acceptance Tests amp Specifications UNITYTNOVA NMR Spectrometer Systems Pub No 01 999120 00 Rev B0800 Applicability of manual UNITYTNOVA NMR Spectrometer Systems consoles Revision history A0699 Initial release E R 2751 B0200 Update autotest and phone list updated AutoTest for VNMR 6 1C Technical contributors George Gray Everett Schreiber Lisa Deuring Technical writers Dan Steele Mike Miller Copyright 2000 by Varian Inc 3120 Hansen Way Palo Alto California 94304 http www varianinc com All rights reserved Printed in the United States The information 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 Inc reserves the right to make changes in any products herein to improve reliability function or design Varian Inc does not assume any liability arising out of the application or use of any product or circuit described herein neither does it convey any license under its patent rights nor the rights of others Inclusion in this document does not imply that any particular feature is standard on the inst
2. 5 Using two cursors measure the distance in Hz between the center peak and one of the outer peak Use the same outer peak either the one on the right or the one on the left for the measurements for both spectra The two measurements in Hz are used as input for the h2cal command which calculates the yH for a given decoupler power level 6 Enter h2cal to calculate YH Record the result 7 Set dmf to 4 yH value Set dmm ccp dseq waltz16 dres 90 lb 1 and enter array dof 9 2000 500 to setup the experiment using the first decoupler If it is the second decoupler that is capable of programmable decoupling using the waveform generator set dmm2 ccp dseq2 waltz16 dres2 90 Enter ga to acquire the data Enter ds 1 aphO dssh to phase and display the spectra To plot the spectra and acquisition parameters enter pap pl al1l page 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 47 Chapter 2 Console and Magnet Test Procedures 2 3 Procedures for Contracted Custom Console Specifications The following procedures are described in this section Temperature Accuracy for VT Systems this page e Stability Calibration for High Stability VT Accessory page 50 Homospoil Demonstration page 51 e Sucrose Anomeric 1H Signal to Noise Ratio page 52 Aqueous Phenylalanine Water Suppression page 54 These procedures are not required as part of the acceptance testing but
3. VNMR version Internal hard disk Mbytes External hard disk Mbytes Tape drive size CD ROM drive model Printer model Plotter model Terminal model Other peripheral NMR host Workstation running VNMR of e g 3 of 3 Model no Purchased from Screen size in Serial no Serial no Serial no Serial no Serial no Serial no Serial no Workstation running other NMR software Workstation running VNMR and other NMR software Operating system on site or off site on site or off site on site or off site 74 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 4 2 System Installation Checklist 4 2 System Installation Checklist Company University Address Principal User Phone Spectrometer type Fax Console S N Sales Order No Magnet S N Shipment Damage Preinstallation Preparation Line voltage measured Vac console accessory Line pressure air No Air conditioning Cryogens liters LHe LN Testing and Customer Familiarization 1 Acceptance tests and computer audit Acceptance tests procedures finished Test results form completed and signed Computer audit completed and signed 2 System documentation review Software Object Code License Agreement acceptance of product constitutes acceptance Of object code license regardless of whether agreem
4. AutoTest procedure and is fixed at the time the Begin Test button is selected The format is one line per macro with each line containing the name of a macro in the order of acquisition As AutoTest proceeds each line is deleted as the specified macro finishes its activity Thus completion of the AutoTest run is defined as when this file is empty The single exception is the case of automatic repeating of AutoTest as specified by the Repeat Until Stopped checkbox in the Configuration display and as indicated by the value of the global parameter at cycletest y Inthis case at the completion of the AutoTest run the contents of the file at_cycled_tests are copied into at selected tests and the process then continues at cycled tests The at cycled tests file is updated when the Begin Test button is selected If the Repeat Until Stopped checkbox is selected in the Configuration display the global parameter at cycletestsissetto y andthefileat selected tests is copied to at_cycled_tests If no test cycling is requested this file is emptied UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing at spec table Theat spec table file is written out when the vnmrsys autotest directory is created and is spectrometer dependent The appropriate file is copied from the directory vnmr autotest depending on spectrometer frequency It contains a list of macros used in AutoT
5. Puts name of test in global variable Sets up pulse width array Specifies what to do every FID Specifies what to do at end of experiment Disables wnt processing if in repeat mode Begins acquisition and specifies wnt wexp processing to occur This part executes at end of experiment If parameter printout requested Fits to straight line and displays plots data Determines turn on time and correlation coefficients Limits number of decimal places Writes out results to history file Writes results to report Plots regression fit endif ATsvf Removes old data set and stores FID under name in at currenttest ATnext Starts next macro in at selected tests file if present endif Closes elseif part 22 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing Automated Tests with Shaped RF Gaussian 90 stability channel 1 and channel 2 Gaussian phase stability test channel 1 and channel 2 Gaussian SLP phase stability test channel 1 and channel 2 Automated Decoupling Performance Tests Be phase modulation decoupling profiles IC GARP decoupling profile 13C WALTZ 16 decoupling profile 13C XY 32 decoupling profile 13C MLEV 16 decoupling profile 13C adiabatic decoupling profiles if waveform generator present on decoupling channel 13C STUD decoupling profile PC WURST decoupling profile Sample heating during 13C broadband decoup
6. The data are fitted to a straight line using a linear regression analysis and plotted Pulse Shape Test DANTE Experiment The rf amplitude is set for a 20 us 90 pulse and the result is compared to that for a single scan spectrum e 10 pulses 2 us each e 20 pulses 1 us each e 25 pulses 800 us each e 50 pulses 400 us each 100 pulses 200 us each For all except the first 20 us pulse a 1 us delay is inserted between each pulse The data are plotted in a horizontal stack to permit comparison of amplitudes The amplitudes are measured and printed Purpose A DANTE type test is performed in which the signal response following a 20 us pulse is measured This is compared with a series of experiments in which the pulse is increasingly divided into series of pulses spaced by us The sum of the pulses is held constant at 20 us If the pulse shape is ideal and the total time of the pulse train is short compared to 75 the rotation of magnetization should be identical As the pulse length shortens any non ideality of pulse shape is revealed as a reduction in intensity Phase Switch Settling Time Experiment Parameters p1 and pw are set to the same value 1 us and 30 spectra are acquired using a 2 pulse sequence with the first and second pulses separated by a delay of 20 us The phase of the second pulse is shifted 180 from the first pulse at a variable time prior to the second pulse A single pulse spectrum is also acq
7. measurement is compared to an identical experiment in which the gradient amplitudes are UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing set to zero or mismatched by 1 More rapid diffusion at higher temperature will cause the gradient no gradient comparison to worsen Therefore performance over time should be compared for the same temperature Measurements done at 4 C have showen no difference in measured T2 for the gradient no gradient cases indicating that diffusion is responsible for the difference in these cases at higher temperatures Other Tests Heating During Spin Lock Test Experiment The same test as in the variable temperature test is performed using a 70 ms IH pulse at an rf field strength of 10 kHz with a total recycle time of 1 5 seconds including acquisition The data are plotted in the same way as in the VT test Purpose Many modern experiments use spin locks or decoupling within their pulse sequences Often rf fields can cause significant sample heating Depending on the nature of the probe this heating can be a problem causing baseline artifacts and t noise It is important to quantify the amount of sample heating the speed in attaining a new equilibrium temperature the homogeneity of temperature throughout the sample during the heating period and the final change in temperature This test imposes a rather strong 10 kHz rf field
8. 2 contains the corresponding acceptance test procedures 3 1 Specifications for AutoTest All AutoTest data is stored and plots and statistical analyses are provided as part of the acceptance testing Plots and statistical analyses are made concurrently with acquisition Sample The AutoTest sample is 0 1 13C enriched methanol in 1 H 0 99 D5O The sample is doped with gadolinium chloride at a concentration of 0 30 mg ml which produces a IH T relaxation time of about 50 to 75 ms The resulting linewidth is between 6 and 10 Hz Hardware Requirements The rf system transmitters linear modulators rf attenuators amplifiers receivers and probes must be in the standard configuration when AutoTest is run If the system configuration has been changed it must be returned to the standard configuration before running AutoTest for acceptance testing Basic Specifications Table 5 lists the specifications and demonstrations generated by AutoTest Gradient pulses are rectangular except where noted Oversampling and or digital filtering is disabled except when doing the frequency shifted image and receiver gain tests Note 1 Specifications for 90 pulse stability and 30 amplitude stability are given in instability which is 100 minus the standard deviation of the intensity in 96 Note 2 Phase cycle cancellation and gradient phase cycle cancellation specifications depend on floor vibrations not exceeding the levels specifie
9. If desired the test can be made to repeat until aborted to acquire multiple runs After several runs have been completed histograms showing all previous values of a parameter can be viewed for example all previous z axis gradient calibrations along with the average of all the results and their standard deviations Of particular interest is any parameter exhibiting a sudden change in value or a steady increase or decrease These results can give an early indication for a hardware problem AutoTest Directory Structure AutoTest uses the vnmrsys autotest directories listed in Table 1 Table 1 AutoTest Directories Directory Contents data FIDs from the recent AutoTest run s data failed FIDs from any failed Auto Test experiments history History files for the various tests reports Copies of the report generated each time AutoTest is run parameters Parameter files default entry is standard par texts Copies of the text files attached to the AutoTest experiments atdb AutoTest database data Directory The vnmrsys autotest data directory contains FIDs collected in previous AutoTest experiments As each experiment finishes the macro specified by the wexp parameter executes and as part of that macro a sv f command is performed that saves the FID under a file name specified by the parameter at currenttest if it contains a name The macro first removes any file by the same name the results of the test from the last time
10. Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing following a single 90 pulse The statistical analysis produces an rms deviation in percent of the average peak height Purpose of 30 Pulse Stability The sinusoidal nature of the excitation profile makes the signal generated following a 90 pulse less sensitive to error than signal following a much smaller flip angle pulse the top of a sine wave is broad and changes in amplitude less for small changes in flip angle than for a smaller pulse A 0 flip angle would have the highest sensitivity to flip angle but would give no signal of course A compromise between the extremes of large signal following a 90 pulse and no signal following a 0 pulse is to use a 30 pulse The rms deviation is measured from an array of spectra obtained using 30 pulses Purpose of 1 usec Pulse Stability This test emphasizes the turnon characteristics of the pulse Any instability of the pulse rise should give a corresponding reduction of measured stability Since the flip angle is much less than a 90 or 30 pulse the measured stability may be lower The rms deviation is measured from an array of spectra obtained using 1 usec pulses Cancellation Test Experiment Four single scan 4 two scan and 4 four scan 90 pulse spectra are acquired in which the transmitter phase is held fixed and the receiver is phase cycled 0 2 1 3 Data are plotted in a horizonta
11. T are measured Scope of Test Various hardware aspects are checked including Lock performance measured by phase cycle cancellation efficiency mage cancellation Built in phase modulator decoupling MLEV 16 WALTZ 16 XY 32 and GARP 1 Waveform generation WFG based decoupling WURST and STUD Heating under 13C decoupling and IH spinlocks Variable temperature response Functionality of receiver gain small angle phase shifters pulse turn on attenuators modulators and pulse shaping is measured The lock channel power and gain control is checked and quantified 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 15 Chapter 1 Installation Tests and Demonstrations Gradient performance is checked on all active axes specified by the pfgon parameter The tests include signal amplitude stability following a pulse done 100 us after a gradient pulse or a pulse followed by a bipolar gradient pair generating a gradient echo Field recovery is measured by doing a gradient followed by a variable delay and an rf pulse Gradient DAC values to generate 10 G cm strengths are determined Gradient stability is measured by measuring a CPMGT2 experiment with and without gradients within the spin echoes Test Output AutoTest results are plotted if specified FIDs are stored and results are logged in appropriate text files At the end of the test a single page report is printed summarizing the test results
12. Testing page 15 e 1 8 Varian Sales Offices page 34 1 9 Posting Requirements for Magnetic Field Warning Signs page 35 Following each installation of a Varian NTYTNOVA NMR spectrometer system an installation engineer tests and demonstrates the instrument s operation Chapter 4 Acceptance Test Results outlines the procedures for the acceptance tests The forms for recording test results in that chapter follow the same sequence as the tests 1 1 Acceptance Testing The objectives of the acceptance tests procedures are twofold To identify the tests to be performed during system installation To identify the precise methods by which these tests are performed The procedures are ordered in a sequence designed to efficiently and logically evaluate the performance of the instrument These procedures cover the basic specifications of the instrument that is signal to noise S N resolution and lineshape and are not intended to reflect the full range of operating capabilities or features of a research NMR spectrometer Note Performance of any additional tests beyond those described herein must be agreed upon in writing as part of the customer contract Test samples for these contracted tests are not supplied by Varian 1 2 Computer Audit Computer Audit page 73 includes a computer audit form The information from this form will help Varian personnel assist you better in making future software upgrades and avoiding h
13. and on plotting and CPU speed As AutoTest runs FIDs are stored in the data directory and the results from the tests are stored in the history directory 6 After AutoTest finishes inspect the reports and compare the results to the specifications Saving Data and FID Files from Previous Runs As AutoTest executes data and FID files are written into the history and data directories which are located in the autotest directory The autotest directory is usually located in the directory vnmrsys of a user s home directory The contents of the data directory are progressively overwritten as AutoTest continues Before starting a new AutoTest run do the following to save the data from a previous run 1 Open a UNIX window and enter cd vnmrsys autotest 2 Change the name of the history directory by entering for example mv history history old 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 39 Chapter 2 Console and Magnet Test Procedures 3 Change the name of the data directory by entering for example mv data data old Creating Probe Specific Files If you run AutoTest with different probes you might want to keep separate autotest directories Use the following steps to create probe specific files 1 After you have run AutoTest using a specific probe change the name of the autotest directory by using the mv command for example cd vnmrsys mv autotest autotest_probe_1 Where probe
14. be about 100 Hz off resonance from the water peak Array the homospoil parameter by entering hs nn ny Enter ga to acquire the arrayed spectra Enter ds 1 to display the first spectrum Phase the spectrum by entering aphO Display both spectra by entering dssh 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 51 Chapter 2 Console and Magnet Test Procedures 52 The second spectrum should be considerable smaller than the first spectrum Measure the amplitude of the first spectrum by moving the cursor on top of the peak and entering n1 The height of the peak in mm and the frequency are displayed in the status window Record the height of the peak for the first spectrum Measure the amplitude of the second spectrum by displaying the second spectrum using ds 2 Make sure the first and second spectra are displayed using the same values of vs vertical scale Move the cursor on top of the peak and enter n1 Record the height of the peak for the second spectrum Calculate the residual signal amplitude of the second spectrum as follows h x 100 h Percentage of residual signal amplitude Where hs is the height of the second spectrum and h is the height of the first spectrum Test Procedure Part 2 I Enter rtp vnmr tests shmd20 p1 0 hst 0 005 sw 6000 d1 60 d2 0 055 then set pw to the IH 90 pulse width value and enter su Check that the appropriate quarter wavelength cable f
15. cancellation 2 scans see Note 2 Phase cycle cancellation 4 scans see Note 2 Quadrature images and spurious signals 1 scan Quadrature images and spurious signals 4 scans Frequency shifted quadrature image 1 scan Frequency shifted quadrature image 4 scans 30 amplitude stability channels 1 and 2 see Note 1 Pulse turnon time for channel 1 Pulse turnon time for channel 2 Attenuator linearity tests channels 1 and 2 full power 400 MHz systems and above 200 and 300 MHz systems Attenuator linearity test channels 1 and 2 reduced power 400 MHz systems and above 200 and 300 MHz systems 58 UNTYINOVA Acceptance Tests Procedures and Specifications demonstration demonstration demonstration demonstration demonstration demonstration demonstration demonstration 2 99 9 measure lt 0 2590 lt 0 490 lt 0 04 0 05 0 05 2 99 9 lt 0 05 us lt 0 05 us corr coef 0 95 0 03 std dev 0 007 corr coef 0 92 0 05 std dev 0 01 corr coef 0 98 0 03 std dev 0 007 corr coef 0 92 0 05 std dev 0 02 01 999120 00 B0800 3 1 Specifications for AutoTest Table 5 AutoTest Specifications and Demonstrations continued Test Modulator linearity channel 1 tpwr 40 Modulator linearity channel 2 tpwr 40 Modulator linearity channel 1 tpwr 16 Modulator linearity channel 2 dpwr 16 13 phase error channels 1 and 2 Gradient level for 10 G c
16. direct observe is recommended This test also requires a Lock Module on the spectrometer Test Procedure 1 Check that the H quarter wavelength cable is installed 200 300 and 400 MHz systems the probe is tuned H linewidth shimmed to within 2 5 to 3 5 Hz at the 50 level and the 90 pulse width determined for the 1 H50 9996 D O sample Set pw to the 90 pulse width value 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 43 Chapter 2 Console and Magnet Test Procedures 44 2 Enter rtp vnmr tests shmd2o to retrieve the test parameter set to the current experiment Acquire a normal spectrum and shim the water signal to less than 3 Hz linewidth at 5096 3 Place the cursor close to the water signal and enter movetof to move the transmitter offset to within 50 Hz of the water peak 4 Set the following parameters hom2dj ph sw 2000 1b 1 0 spin n d2 1 000 ni 0 sb n fn 32k nt 1 ss 0 at 1 5 Set pw to the 90 pulse width value p1 to the 180 pulse width value 6 Create an array of 20 d1 values by entering array d1 20 60 0 7 Enter ga to acquire the spectrum Phase the first spectrum by entering ds 1 to display the first spectrum of the array and by entering aphO to apply a first order phase correction to the spectrum 8 Enter ai to scale all of the spectra to the same vertical scale and enter dssh to display the arrayed spectra horizontally 9 Enter analyz to use the analyz
17. dissolves the polystyrene VT dewar Basic Custom Specifications The temperature reading displayed on the VT unit display panel should be within 1 C of the actual temperature reading as measured from the chemical shift UNTYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 3 3 Contracted Custom Console Specifications Stability Calibration for High Stability VT Accessory Sample Doped 2 Hz H50 D50 0 1 mg ml GdCl in 1 H O in D O Part No 01 901855 01 for 5 mm samples Alternatively the customer can request 10 mM DSS in D O sample volume of 0 6 ml in a 5 mm NMR tube DSS 3 trimethylsilyl 1 propane sulfonic acid The customer must make this sample using DSS and deuterium oxide 99 8 or 99 9 atom D Upon request Varian can make the sample if DSS is not available at the customer site Probe and Hardware Requirements The high stability VT Accessory and a 5 mm probe capable of H direct observe are required The high stability VT tests have the following customer site prerequisites 1 Room temperature regulation to within 1 C as described in the manual UN YINOVA Installation Planning 2 Dry nitrogen for the air supply for temperatures below 10 C per the guidelines in the manual NTYTNOVA Installation Planning 3 A preconditioned VT air supply with the VT air cooled to 10 C below the desired sample temperature 4 The air flow to the probe for VT regulation in accord with the Varian pr
18. humans or animals or significant property damage CAUTION Cautions are used when failure to observe instructions could result in serious damage to equipment or loss of data Warning Notices Observe the following precautions during installation operation maintenance and repair of the instrument Failure to comply with these warnings or with specific warnings 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 WARNING Persons with implanted or attached medical devices such as pacemakers and prosthetic parts must remain outside the 5 gauss perimeter from the centerline of the magnet The superconducting magnet system generates strong magnetic fields that can affect operation of some cardiac pacemakers or harm implanted or attached devices such as prosthetic 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 implants should contact their physician to determine if a danger exists Refer to the manuals supplied with the magnet for the size of a typical 5 gauss str
19. of power Purpose Overall power control is accomplished using PIN diode controlled rf attenuators These attenuators are precision devices that should have negligible phase change throughout their full range The amplitude response should also be logarithmic A log regression analysis should show the extent of fit to the ideal The phase change as a function of power is examined Raw uncorrected output should be examined without software adjustment of phase and amplitude This test does not permit a full assessment of the cause of the phase error because the amplifier might be in compression at the maximum power output Attenuator Linearity at Reduced Power Experiment The attenuator linearity test is repeated but with output of the transmitter reduced by the linear modulator This is done to isolate the effect of the rf amplifier Purpose The attenuator linearity test is performed but with reduced power input to the attenuator using the linear modulator to reduce the output power from the transmitter Raw uncorrected output should be examined without software adjustment of phase and amplitude corrections Linear Modulator Linearity Tests Experiment With the coarse rf amplitude set at a value 23 dB down from maximum the rf power is varied using the linear modulator The linear modulator is used for fine power control and shaped rf excitation The rf amplitude is varied over a range of 60 dB in 100 equally spaced steps
20. or custom contracted tests refer to Procedures for Contracted Custom Console Specifications page 48 Homonuclear Decoupling Sample 0 1 ethylbenzene 0 01 TMS 99 89 deuterochloroform CDC15 Part No Sample Tube 00 968 120 70 5mm 00 968123 70 10 mm Probe and Hardware Requirements A 5 mm probe capable of H direct observe is recommended Test Procedure 1 Enter rtp vnmr tests H1sn su to retrieve the test parameter set to the current experiment Check that the IH quarter wavelength cable is installed 200 MHz 300 MHz and 400 MHz systems and the probe is tuned 2 Enter nt 1 dm n and ga to acquire a normal spectrum without decoupling 3 Move the cursor to the central line of the triplet and enter sd to move the decoupler to that frequency 4 Enter dm2 n y dpwr 20 homo y and ga to acquire two spectra the first spectrum is without decoupling and the second is with homodecoupling The best values of dpwr must be found by experiment Start with the dpwr 20 Too much power can show increased noise too little fails to decouple the quartet Lock Frequency Stability The stability of the lock is judged by the phase response of a Hahn echo Run 20 small single scan echo experiments at 1 minute intervals and record the phase variations Sample Doped 2 Hz H50 D50 0 1 mg ml GdCl in 1 H50 in D50 Part No 01 901855 01 for 5 mm samples Probe and Hardware Requirements A 5 mm probe capable of IH
21. over the whole range This should produce a linear ramp of signal response following a small flip angle pulse Spectra are plotted in a horizontal stack of spectra in phased mode with the highest signal full scale The width of the plotted region around the water is set narrow enough to clearly show the base of the water peak The data are fitted to a straight line using a linear regression analysis and plotted Purpose Further power control is possible using the linear modulator present on the NMR transmitter board This test produces a series of experiments in which the pulse power is changed over the full range of the modulator The linear nature is tested by a linear least squares fit of the data Predictable power control is essential for delivering accurate shaped pulses and for precise power level control in Hartmann Hahn experiments in both solids and liquids Raw uncorrected output should be examined without software adjustment of phase or amplitude Linear Modulator Linearity Tests with Attenuators Set to Full Attenuation Experiment The linear modulator linearity test is repeated with the coarse rf amplitude control set for minimum power resulting in a maximum attenuation of 139 dB The pulse width is increased correspondingly to obtain comparable signal to noise as in the linear UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing modulator linearity test
22. than YNTYINOVA For probes purchased for use in systems other than Varian UN TYINOVA systems no guarantee is given that these probes meet current specifications Testing Policy for Indirect Detection Probes for Direct Observe Broadband Performance Probes designed for indirect detection applications are tested for indirect detection performance only Sample Tubes Policy Tests are performed with the following sample tubes 3 mm probes 3 mm tubes with 0 30 mm wall Wilmad 327 PP or equivalent 5 mm probes 5 mm tubes with 0 38 mm wall Wilmad 528 PP or equivalent 8 mm probes 8 mm tubes with 0 51 mm wall Wilmad 513A 7PP or equivalent 10 mm probes 10 mm tubes with 0 46 mm wall Wilmad 513 7PP or equivalent Using sample tubes with thinner wall thickness e g Wilmad 5 mm 545 PPT or equivalent Wilmad 10 mm 513 7PPT or equivalent increases signal to noise 14 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing 1 7 AutoTest Automated Instrument Testing AutoTest is a test suite designed as an instrument performance tracking tool for NTYTNOVA NMR spectrometers Automated Test Procedures Running AutoTest page 37 describes how to install AutoTest and how to use it for automated instrument testing After AutoTest is installed the user can establish benchmark values for a spectrometer and use these values to track the system s performance cha
23. 0 968120 91 5 mm 00 968123 91 10 mm Probe and Hardware Requirements A 5 mm or 10 mm broadband observe H decouple probe is recommended i e 5 mm or 10 mm broadband probes 5 mm switchable probes or 4 nucleus probes This test requires the results from the yH calibration that gives a dpwr of 1 watt at the probe Basic Specifications All of the spectra in the array show a single peak With the exception of the first and last spectrum the remaining spectra do not vary in amplitude by more than 10 of the average amplitude 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 65 Chapter 3 Consoles and Magnets Specifications WALTZ H Decoupling Using High Performance Waveform Generators This test is performed by generating shaped pulses using the waveform generators Sample Doped 40 p dioxane in benzene dg Part No Sample Tube 00 968120 91 5 mm 00 968 123 91 10 mm Probe and Hardware Requirements A 5 mm or 10 mm broadband observe H decouple probe is recommended i e 5 mm or 10 mm broadband probes 5 mm switchable probes or 4 nucleus probes This test requires the presence of waveform generator boards This test also requires the results from the YH calibration that gives a dpwr of 1 watt at the probe Basic Specifications All of the spectra in the array show a single peak With the exception of the first and last spectrum the remaining spectra do not vary in amplitude by more th
24. 0 mM NaOAc 10 mM TSP 90 H50 1096 D5O 600 ul sample volume Wilmad 535 PP for 500 600 750 and 800 MHz systems This sample can be made up by the customer can be specially prepared by Varian and sent for the test Probe and Hardware Requirements Water suppression tests should be run using a 5 mm probe capable of H direct observe The tests are designed to be performed at a power level giving rise to a 10 us 90 pulse width This test requires excellent By homogeneity As a prerequisite the probe should be shimmed well enough to meet IH nonspin lineshape specifications Test Use the following procedure 1 Check that the probe is tuned and the 90 pulse width determined for a doped 2 Hz D5O sample The 90 pulse width determined from the doped D4 O sample for example 10 us at tpwr 58 is used for the pw value for the water suppression test 2 Obtain the correct frequency for the presaturation of the water peak as follows a Enter rtp vnmr tests shmd2o to retrieve the test parameter set into the current experiment b Enternt 4 sw 7500 at 0 8 tpwr 10 gain 20 Change pw to the 90 value and enter ga to acquire the spectrum If the receiver or the ADC overloads reduce gain and reacquire the spectrum c Phase the spectrum using manual phasing and place the cursor near the water signal Enter n1 r1 4 8p movetof dof tof d Enterpresat d1 0 01 ss 2 nt 4 gain 20 lb 1 satfrq tof presat 2 satpwr 4 or the t
25. 1isthe name of the probe that was tested for example 5mmTriplePFG or 5mmID Any new AutoTest run automatically creates a new autotest directory in the user s vnmrsys directory The only file that needs to be updated would be vnmrsys autotest parameters standard par This can either be copied from the saved autotest file or the parameter set may be retrieved using rt or rtp the parameters updated and then saved replacing the standard par file This should be safe for any parameters displayed in the dg window but there are several parameters dealing with gradients and indirect detection that must also be checked It is safest to do an All Tests run the first time a new probe is used Once a calibrated standard par parameter set is present autotest directories may be renamed whenever a probe is changed In this way history files may be kept specific to a probe To change the file name back to probe_1 or the name you have chosen enter for example cd vnmrsys mv autotest autotest_probe_2 Where probe 2isthe name you have chosen for the probe last tested mv autotest probe 1 autotest Where probe 1isthe name you have chosen for the probe you now want to test If you need to repeat any individual test you can do so by recalling the appropriate FID from the data directory The experiment can then be started with the go command without overwriting the previous data Or the test may be selected from the Test Library after using the auto
26. Performance RF Waveform Generator 47 2 3 Procedures for Contracted Custom Console Specifications 48 Temperature Accuracy for V T SyStes iu ederet tet eere 48 Stability Calibration for High Stability VT Accessory eese 50 H omospol Demonstration Luar dee re een tte rer ege erts 51 Sucrose Anomeric H Signal to Noise Ratio 52 Aqueous Phenylalanine Water Suppression eese 54 Chapter 3 Consoles and Magnets Specifications 57 3 1 Specifications for Auto Test 4 rrr rtt REPE RIA ER 57 3 2 Specifications for Manual Console Tests sss 60 Lock Frequency Sta Diy uet aeo t rr Den rr ret es 61 Homonuclear Decoupling 2 2 oer tr a e nera secs 62 Nasiable Temperature OPETAN esros ei eerte petens 63 Magnet Dott Specll Gallon uuu eerte re eee eene ets 64 WALTZ H Decoupling Using Preprogrammed Phase Modulation 65 WALTZ H Decoupling Using High Performance Waveform Generators 66 3 3 Contracted Custom Console Specifications sese 67 Temperature Accuracy for VT Accessories 68 Stability Calibration for High Stability VT Accessory eese 69 Horniospoi Demonstration i2 ee n e tr ette tet senansa 70 Chapter 4 Acceptance Test Results eere 71 AM Compu terAUdt iie pe x e eere exse dea weeny ous vin dr ave Vise 73 4 2 System Install
27. Tests Procedures and Specifications 01 999120 00 B0800 4 1 Computer Audit 4 1 Computer Audit Information about your site please print Company University Address Principal User Phone Spectrometer type Fax Console S N Sales Order No Delivery month day Information on each computer additional forms are on the back of this page Include computers directly attached to the spectrometer computers networked or non networked on site or off site used to process NMR data using Varian s VNMR software and computers on site and off site used to process data collected on this spectrometer with software from other vendors Information on computer of e g 1 Of 3 Manufacturer Model no Computer S N Purchased from Memory Mbytes Screen size in Peripherals Internal hard disk Mbytes External hard disk Mbytes Serial no Tape drive size Serial no CD ROM drive model Serial no Printer model Serial no Plotter model Serial no Terminal model Serial no Other peripheral Serial no Computer function NMR host Workstation running VNMR on site or off site Workstation running other NMR software on site or off site Workstation running VNMR and other NMR software on site or off site VNMR version Operating system The above computer audit was performed during installation of the system Varian Representative Date I certify t
28. a expanded 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 27 Chapter 1 Installation Tests and Demonstrations 28 to show only the 3C bound protons side by side to permit measurement of X coil rf homogeneity The results are plotted and displayed in magnitude mode showing one of the lines of the methanol doublet Purpose This test checks the homogeneity of the rf field strength throughout the active region of the sample In an ideal case for nuclei having reasonable T values the signal generated following a 360 0 pulse should match that following a 0 pulse The signal strength as a function of flip angle should be sinusoidal The amount of drop off is related to the inhomogeneity of the rf field High rf homogeneity is important because many important pulse sequences use a large number of pulses The signal losses accumulate with each pulse such that in worst cases all the desired signal is lost Most heteronuclear indirect detection experiments on large molecules use HSQC pulse sequence components These contain 6 to 10 IH pulses including 4 to 8 X nucleus 180 pulses High rf homogeneity is especially important in these cases Receiver Test Experiment Single scan spectra are collected that span the range of receiver gain and divide that range into at least 25 evenly spaced values of gain including the highest and lowest gain values The data are plotted with the highest signal on scale s
29. an Taipei 2 2698 9555 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 9 Posting Requirements for Magnetic Field Warning Signs United Kingdom Walton on Thames England 1932 898 000 United States Palo Alto California Varian Inc NMR Systems Customer Sales Support 650 424 5145 Service Support Palo Alto California 1 800 356 4437 E mail customer support nmr varian com North American Service Manager 6440 Dobbin Rd Ste D Columbia MD 21045 410 964 3065 Venezuela Valencia 41 257608 1 9 Posting Requirements for Magnetic Field Warning Signs The strong magnetic fields that surround a superconducting magnet are capable of causing death or serious injury to individuals with implanted or attached medical devices such as pacemakers or prosthetic parts Such fields can also suddenly pull nearby magnetic tools equipment and dewars into the magnet body with considerable force which could cause personal injury or serious damage Moreover strong magnetic fields can erase magnetic media such as tapes and floppy disks disable the information stored on the magnetic strip of automated teller machine ATM and credit cards and damage some watches To warn of the presence and hazard of strong magnetic fields the customer is responsible for posting clearly visible signs warning of magnetic field hazards This responsibility includes measuring stray fields with a gaussmeter Radio frequenc
30. an 10 of the average amplitude WALTZ decoupling using programmable decoupling should be comparable to the non programmable hardware WALTZ Compare the results obtained in this test to those obtained from the test WALTZ 1H Decoupling Using Preprogrammed Phase Modulation page 65 Note that files with other modes of decoupling can be found in the vnmr shapelib directory as pulseshape DEC 66 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 3 3 Contracted Custom Console Specifications 3 3 Contracted Custom Console Specifications This section contains the following specifications Temperature Accuracy for VT Accessories this page Stability Calibration for High Stability VT Accessory page 69 Homospoil Demonstration page 70 Before testing to specifications in this section refer to Consoles and Magnets Custom Specifications Form page 81 for any custom acceptance test specifications Note Specifications on a Custom Specifications Form are done only by prior contract agreement and supersede the specifications shown in this manual 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 67 Chapter 3 Consoles and Magnets Specifications 68 Temperature Accuracy for VT Accessories Sample For high temperature work 100 ethylene glycol reagent grade Part No 00 968120 79 for 5 mm sample tubes For low temperature work 100946 methanol reag
31. arameter set to the current experiment Acquire a normal spectrum and shim the water signal to about 3 to 4 Hz linewidth at 5096 3 Replace the 99 8 D5O sample with the 100 methanol sample Part No 00 968 120 80 Set the following parameters pw 2 gain 5 or some value that doesn t overload the receiver sw 10000 at 2 nt 1 in n In the acqi window set the lock to Off The test is run unlocked because the sample lacks deuterated solvent to lock on 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 49 Chapter 2 Console and Magnet Test Procedures 50 Enter su and check the probe tuning for the methanol sample Enter ga to acquire the spectrum Place the cursor between the two peaks and enter movetof to move the transmitter offset 4 Click on the Box menu button to call up right and left cursors Position the right and left cursors on the right and left peaks and enter tempcal methanol 5 Record the temperature reading from the VT controller displayed on the remote status module or on the front face of the VT controller Record also the computer calculated temperature based on the chemical shift frequencies of the two peaks If low temperature calibrations are performed immediately following high temperature calibrations allow the probe to cool to room temperature before continuing with the rest of the procedure 6 Enter temp 20 su to change the temperature to 20 C Allow the sample to
32. ardware compatibility problems You will be asked for information about all computers directly connected to the spectrometer or used to process NMR data 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 11 Chapter 1 Installation Tests and Demonstrations 1 3 Installation Checklist System Installation Checklist page 75 includes an installation checklist form 1 4 System Documentation Review Following the completion of the acceptance tests and computer audit the following system documentation will be reviewed with the customer Software Object Code License Agreement e Varian and OEM manuals e Warranty coverage and where to telephone for information 1 5 Basic System Demonstration 12 The basic operation of the system is demonstrated to the primary user The objective of the demonstration is to familiarize the customer with system features and safety requirements as well as to assure that all mechanical and electrical functions are operating properly Detailed specifications and circuit descriptions will not be covered Note Varian installation engineers are not responsible for nor trained to run any spectra not described in the acceptance tests procedures Magnet Demonstration The magnet demonstration includes the following items Posting requirements for magnetic field warning signs Cryogenics handling procedures and safety precautions Magnet refilling Flowmeters Homogeneity di
33. ation Checklist eese ere 75 4 3 Supercon Shim Values essere eerte eren ener TI 4 4 Console and Magnet Test Results sese 79 4 5 Consoles and Magnets Custom Specifications Form sese 81 Custom SPECICATION i ere teet the toro eerte b e bebe te Pea be a e 81 Sample Requiretments sisisi deri Ee e HR HERE Ie HERO ERE Ree 81 Name of Procedure Required for Custom Specification 81 M 83 4 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 List of Figures Figure 1 I0 Gauss Warning S190 iie bre hr ea LE hihi sete sep van ese reb see duos o dg repe reddo 36 Fipure 2 5 Gauss Warning Sign tino the t p Fee E ae et er Ee ec a cu rai ebd e 36 Fisure 3 Magnet Ared Danger SIgn 1 2 ee es erred esde eree EEEN redeat bn drea seeds 36 Figures Auto Vest Pro grainy siririn eee riti teet i erre teuren toe e ie e Eee ee SER e ieii 39 5 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 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
34. ay field This gauss level should be checked after the magnet is installed WARNING Keep metal objects outside the 10 gauss perimeter from the centerline of the magnet The strong magnetic field surrounding the magnet attracts objects containing steel iron or other ferromagnetic materials which includes most ordinary tools electronic equipment compressed gas cylinders steel chairs and steel carts Unless restrained such objects can suddenly fly towards the magnet causing possible personal injury and extensive damage to the probe dewar and superconducting solenoid The greater the mass of the object the more the magnet attracts the object Only nonferromagnetic materials plastics aluminum wood nonmagnetic stainless steel etc should be used in the area around the magnet If an object is stuck to the magnet surface and cannot easily be removed by hand contact Varian service for assistance 01 999120 00 B0800 UNITYINOVA Acceptance Tests Procedures and Specifications 7 SAFETY PRECAUTIONS Warning Notices continued Refer to the manuals supplied with the magnet for the size of a typical 10 gauss stray field This gauss level should be checked after the magnet is installed WARNING Only qualified maintenance personnel shall remove equipment covers or make internal adjustments Dangerous high voltages that can kill or injure exist inside the instrument Before working inside a cabinet turn off the main system power swit
35. ble quench tubes warning 9 RF homogeneity tests 23 rtp command 13 rts command 13 running AutoTest 38 S safety precautions 7 9 sensitivity tests pw parameter 13 set up of AutoTest 38 shaped pulse test descriptions channels 1 and 2 29 shaped rf demonstrations 24 shim parameters 13 shipment damage 75 signal to noise 13 Software Object Code License Agreement 12 solids high power amplifiers caution 10 spinning speed 13 streaming magnetic tape unit 12 svs command 13 system demonstration 12 system documentation review 12 system installation checklist 75 T temperature accuracy for VT systems 48 test conditions 13 test parameters 13 tests library 13 tpwr value for AutoTest 38 training seminars 12 84 UNITY NOVA Acceptance Tests Procedures and Specifications warnings defined 7 warranty coverage 12 01 999120 00 B0800
36. ceptance Tests Procedures and Specifications 01 999120 00 B0800 4 4 Console and Magnet Test Results 4 4 Console and Magnet Test Results Fill in the following information Homonuclear Decoupling Lock Frequency Stability Basic Variable Temperature Operation Magnet Drift WALTZ H Decoupling Preprogrammed Phase Modulation WALTZ H Decoupling High Performance RF Waveform Generator Varian Representative Date Customer Representative Date 01 999120 00 B0800 UNITYINOVA Acceptance Tests Procedures and Specifications 79 Chapter 4 Acceptance Test Results Notes 80 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 4 5 Consoles and Magnets Custom Specifications Form 4 5 Consoles and Magnets Custom Specifications Form Fill in the following information Custom Specification Sample Requirements Name of Procedure Required for Custom Specification If there is atest in this manual that can be modified for this custom specification attach the necessary procedure to this form 01 999120 00 B0800 UNITYINOVA Acceptance Tests Procedures and Specifications 81 Chapter 4 Acceptance Test Results 82 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 Numerics 180 pulse 13 90 degree pulse width calibrations PW90 23 90 pulse value for pw 13 A acceptance
37. ch located on the back of the console then disconnect the ac power cord WARNING Do not substitute parts or modify the instrument 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 Maintain safety features by referring system service to a Varian service office WARNING Do not operate in the presence of flammable gases or fumes Operation with flammable gases or fumes present creates the risk of injury or death from toxic 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 Avoid liquid helium or nitrogen contact with any part of the body In contact with the body liquid helium and nitrogen can cause an injury similar to a burn Never place your head over the helium and nitrogen exit tubes on top of the magnet If liquid helium or nitrogen contacts the body seek immediate medical attention especially if the skin is blistered or the eyes are affe
38. coupling performance tests 41 high power amplifiers cautions 10 high stability VT units 50 homogeneity disturbances 12 homogeneity settings 13 homonuclear decoupling test 43 homospoil demonstration 51 I installation checklist 12 installation engineer duties 11 installation of AutoTest 37 installation planning guide 13 L lineshape measurements 14 linewidth measurement 14 liquid nitrogen 44 63 loading programs 12 lock stability manual test procedures 43 M magnet acceptance tests 37 magnet demonstration 12 magnet quench warning 8 magnet refilling 12 magnetic media caution 9 metal objects warning 7 methanol 48 modifying the instrument 8 N 90 pulse 13 nitrogen contact with body 8 nitrogen gas 44 63 nitrogen gas flowmeters caution 10 UNITY NOVA Acceptance Tests Procedures and Specifications 83 Index noise region 14 U upper barrel warning 8 O objectives of acceptance tests 11 V OEM manuals 12 180 pulse 13 variable temperature VT units 44 Varian manuals 12 vortexing 13 P VT controller 44 VT experiment warning 8 pacemaker warning 7 parameters for tests 13 phase stability 29 W preinstallation checklist 75 probe demonstration 12 probe performance tests 41 prosthetic parts warning 7 H1sn test file 43 pw parameter 13 Q quarter wavelength cable 13 R radio frequency emission regulations 10 relief valves warning 9 remova
39. cted WARNING Do not look down the upper barrel Unless the probe is removed from the magnet never look down the upper barrel You could be injured by the sample tube as it ejects pneumatically from the probe WARNING Do not exceed the boiling or freezing point of a sample during variable temperature experiments A sample tube subjected to a change in temperature can build up excessive pressure which can break the sample tube glass and cause injury by flying glass and toxic materials To avoid this hazard establish the freezing and boiling point of a sample before doing a variable temperature experiment 8 UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 SAFETY PRECAUTIONS Warning Notices continued WARNING Support the magnet and prevent it from tipping over The magnet dewar has a high center of gravity and could tip over in an earthquake or after being struck by a large object injuring personnel and causing sudden dangerous release of nitrogen and helium gasses from the dewar Therefore the magnet must be supported by at least one of two methods with ropes suspended from the ceiling or with the antivibration legs bolted to the floor Refer to the Installation Planning Manual for details WARNING Do not remove the relief valves on the vent tubes The relief valves prevent air from entering the nitrogen and helium vent tubes Air that enters the magnet contains moisture that can freeze causi
40. d in the UNTYTNOVA Installation Planning manual 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 57 Chapter 3 Consoles and Magnets Specifications For attenuator linearity tests the standard deviation std dev value is provided as a reference but is not a specification for the test Table 5 AutoTest Specifications and Demonstrations Test AutoTest Specification RF homogeneity test lH RF homogeneity test Re Water resonance frequency Ti H PW90 determination for channels 1 and 2 13C PW90 determination High band amplifier compression Low band amplifier compression Temperature rise in decoupler heating test AutoGain test for 90 pulse Signal to noise normal and oversampled Folded noise reduction with large SW Average signal to noise 20 trials IH rf homogeneity spec for probe 13C rf homogeneity spec for probe value reported value reported IH PW90 spec for probe 13C PW90 spec for probe measure measure demonstration demonstration demonstration demonstration demonstration Po phase modulation decoupling profile using phase modulator GARP 1 modulation WALTZ 16 modulation XY 32 modulation MLEV 16 modulation 5C adiabatic decoupling profiles using waveform generator STUD modulation WURST modulation Receiver gain tests normal and oversampled Small angle phase test channels 1 and 2 90 pulse stability channels 1 and 2 see Note 1 Phase cycle
41. diabatic decoupling schemes Gradient Tests Gradient Profile Experiment A spectrum with a 100 kHz spectral width is acquired using a gradient echo collect echo during a Z axis gradient This acquisition is repeated for both positive and negative gradients that are sufficient to spread the pattern greater than 50 kHz at the base Gradient strength and duration as well as the size of the active length of the coil are noted The experiment is repeated for both the X axis and Y axis gradients if available Purpose This test uses pulsed field gradients PFGs to quantitate the gradient field strength The width of the pattern is directly proportional to the gradient strength The width at 20 of maximum is used to calculate the gradient strength Both positive and negative gradients are used This should be done for all orthogonal axes available Field Recovery Stability Experiment The 90 pulse stability test is performed but preceding the rf pulse is a 1 ms 30 G cm Z axis gradient pulse which is then followed by a 100 4 field stabilization 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 31 Chapter 1 Installation Tests and Demonstrations 32 delay This test is repeated with a 10 G cm gradient pulse If X and Y gradients are available the test is repeated with a 10 G cm gradient pulse for each gradient Purpose A gradient is applied prior to a measuring pulse The stability of the signa
42. e gaussian pulse is used for a single transient one pulse spectrum The linear modulator is used to scale down the amplitude of the pulse in 100 steps over a range of 60 dB Plot widths are set small enough to show the base of the water and plot all spectra in a horizontal stack in phased mode with the maximum signal spectrum at full scale Purpose The linear nature of the system is graphically tested by measuring NMR response when the amplitude is under full control both by the rf attenuator and by the linear modulator 13C Test X coil rf homogeneity can be determined using an indirect detection pulse sequence Sensitivity in many indirect detection experiments is markedly affected by X coil performance because of the large number of 180 pulses used X decoupling is tested for various modulation schemes at constant amplitude WALTZ 16 GARP 1 etc as well as more powerful adiabatic pulse techniques Efficiency is measured by varying the PO decoupling frequency while observing the proton spectrum under broadband decoupling UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing 13C 90 Pulse Width Calibration The power level for a 90 flip of approximately 15 us on the X coil of the probe is determined Amplifier compression is determined by lowering power by 12 dB and redetermining the 90 pulse width Both results are reported X Phase Modulation Decoupling Pro
43. e should also be logarithmic A log regression analysis should show the extent of fit to the ideal Spectral Purity Test Experiment Four single scan 100 kHz spectral width spectra are acquired with no pulse Each spectrum is plotted with a few millimeters of noise Purpose RF purity of the transmitter and receiver can be tested by recording data without any excitation pulse The spectrum reveals any artifactual signals Variable Temperature Test Experiment Single scan spectra are acquired during an increase of 5 C in sample temperature Spectra are recorded sequentially Spectra are taken every 2 seconds until the 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 33 Chapter 1 Installation Tests and Demonstrations sample reaches equilibrium as reflected in a stable chemical shift of a methyl proton Spectra are plotted in a stacked manner to permit examination of the rate of change of temperature the homogeneity of temperature and the length of time necessary to reach equilibrium Purpose The sample temperature is increased by 5 C while recording spectra every 2 seconds Most methyl resonances show a chemical shift of s rq 100 Hz C and this shift therefore indicates the actual temperature distribution within the sample The methyl resonance should move quickly and homogeneously to its new equilibrium position The rate of change and homogeneity of change demonstrate the VT performance
44. ecified in AutoTest display 90 pw at reduced power Power level at reduced power 90 pw on channel 2 Bc pw90 determined at at pwx901vl 13c power level for approximately 15 us pwx90 13C pw90 at reduced power Tops power level at reduced power y or n for VT test Current temperature Current value of global parameter vt t ype Value reflects usage of temp t c1 tk panel y or n for gradient tests Current value of pfgon y or n for gradient mapping shimming Value of G cm per DAC unit for z axis gradient Value of G cm per DAC unit for x axis gradient Value of G cm per DAC unit for y axis gradient 20 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing and executes the macro specified by at cur smacro Iftheat selected tests file is empty ATnext either finishes the AutoTest run or calls the ATrestart macro which copies the at cycled tests filetoat selected tests permitting repeated AutoTest runs until manually aborted by the user ATnext is usually found at the bottom of each macro defining a particular test This permits the linking of one test to another in a general fashion ATxxx Macros Specific tests usually have the designation of AT followed by a number or group of letters Each macro is self contained having the ability of setting up parameters performing acquisition processing the acquired data possibly setting up new experiments and
45. ecommended Test Procedure 1 Enter rtp vnmr tests Hllshp to retrieve the test parameter set to the current experiment 2 Check that the H quarter wavelength cable is installed 200 MHz 300 MHz and 400 MHz systems and the probe is tuned Acquire a normal spectrum and shim the chloroform signal to less than 1 Hz linewidth at 50 3 Connect to the acqi window turn the lock off turn the spinner off and set the spinner speed to 0 Make sure the lock signal is on resonance the lock signal display should be flat Disconnect the acqi window 4 Enterin n spin n nt 1larray d1 11 3600 0 d1 1 60 This sets up an array of d1 values with the first spectrum to be collected after 1 minute and subsequent spectra to be collected at one hour intervals 5 Enter ga to acquire the spectra The test takes about 10 to 11 hours to finish 6 After the spectra are acquired phase the first spectrum by entering ds 1 to display the first spectrum of the array and by entering aphO to apply a first order phase correction to the spectrum 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 45 Chapter 2 Console and Magnet Test Procedures 46 Enter ai to scale all of the spectra to the same vertical scale and enter dssa to display the arrayed spectra stacked vertically Compare the frequency shift of the chloroform peak of the arrayed spectra to the frequency of the first spectrum in the array WALTZ H Deco
46. ent grade Part No 00 968120 80 for 5 mm sample tubes Table 7 lists which sample to use with a temperature range for VT calibration curve Table 7 Samples for VT Calibration Curve Temperature Range Sample Tube CC init Test Sample Sample Part No 50 to 25 Low 5 methanol 00 968120 80 25 to 100 High 5 ethylene glycol 00 968120 79 Probe and Hardware Requirements A V T Unit and a VT probe are required fore these tests For best results run the VT tests using a 5 mm probe that is capable of H direct observe over the temperature range of 150 C to 200 C For probes that have a more limited temperature range particularly PFG probes run the test at two or three temperatures that fall within the VT range of the probe These tests can also be run using the IH decoupling coil of the 5 mm broadband probe as IH direct observe CAUTION Before performing variable temperature calibrations check that theVT unitis correctly installed according to the instructions in the installation manual Dry nitrogen gas should be used for the gas flow to the probe and upper barrel for both the high and low temperature calibrations CAUTION For the low temperature calibrations fill the VT dewar with liquid nitrogen If a chemical mixture is used instead of liquid nitrogen for the low temperature calibrations be careful about the choice of the chemical slurry A mixture of crushed dry ice and acetone is not recommended because it
47. ent is signed or not Varian and OEM manuals ___ Explanation of warranty and where to telephone for information 3 Magnet demonstration ___ Posting requirements for magnetic field warning signs ___ Warning signs posted ___ Cryogenics handling and safety Magnet refilling ___ Flowmeters ___ Homogeneity disturbances 4 Console and probe demonstration CAUTION To avoid possible preamplifier damage make sure the probe is connected and tuned to resonance ___ Loading programs operating the streaming tape unit ___ Experiment setup ___ Basic operation to obtain typical spectra ___ Demonstration of broadband operation Demonstration of homonuclear and heteronuclear decoupling 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 75 Chapter 4 Acceptance Test Results Notes 76 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 4 3 Supercon Shim Values 4 3 Supercon Shim Values Fill in the following information Magnet Frequency and Serial Number Magnet Frequency Serial Number Measurement in Helipot Amps Measurement Y ZX ZY XY X2 Y2 Drift Spacers Main Field Current Customer Signature Varian Representative Signature 01 999120 00 B0800 UNITYINOVA Acceptance Tests Procedures and Specifications 77 Chapter 4 Acceptance Test Results Notes 78 UNITY NOVA Ac
48. ermination of lineshape from a plot a Usealarge enough plot width to allow accurate determination of the baseline The baseline should be drawn through the center of the noise in a region of the spectrum with no peaks b The 0 55 and 0 11 levels are then measured from the baseline and calculated from the height of the peak and the value of vs For example if a peak is 9 0 cm high with vs 200 the 0 55 level on a 100 fold vertical expansion vs 20000 is 9 0 x 0 55 or 4 95 cm from the baseline If the noise is significant at the 0 55 and 0 11 levels the linewidth should be measured horizontally to the center of the noise Forall sensitivity tests a noise region free of any anomalous features should be chosen with the cursors Neither cursor should be placed any closer to an edge of the spectrum than 10 percent of the value of sw This should produce the best possible signal to noise that is representative of the spectrum The results of all tests should be plotted as a permanent record Include a descriptive label and a list of parameters These plots can then be saved as part of the acceptance tests documentation Probe Installation Policies The following policies are in effect at installation Custom Specifications Policy For custom specifications that have been purchased record test results in Consoles and Magnets Custom Specifications Form page 81 Specifications Policy for Probes Used in Systems other
49. est For each macro the following is specified The history file affected by the macro The column number not counting date containing the result The lower limit for the result The upper limit for the result Atext description of the result This text description is used for the graphical displays and plots A comment line above each macro serves to describe the test All results specified in this manual have upper and lower limits specified numerically in this file Those not having Varian specifications have asterisks as entries for upper and lower limits and these results will have no indication of pass or fail in their history files or colored indication of failure in the graphical displays of the history files Users may wish to set their own upper and lower limits for many if not all of the results They may do so by replacing the asterisks with numbers Of course this should only be done after a good statistical base is obtained such as more than 20 complete AutoTest runs Once this base is obtained the numbers put into the at spec table file should have a reasonable margin of error built in It is a good idea to make a copy of the file at specs table file prior to changing it as well as the modified file because deletion or renaming of the autotest directory will result in a default at spec table being copied from vnmr autotest atdb AutoTest Macros To help users who may want to add tests or modify te
50. etween 30 C and 100 C Sample An empty sample tube with spinner Probe and Hardware Requirements Any variable temperature probe UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 2 2 Manual Test Procedures Required to Demonstrate Console Operation Test Procedure 1 Set N3 gas flow to 9 5 to 10 0 LPM For temperatures below 100 C set N flow to 12 LPM 2 Entera value for temp then enter su For values below room temperature the heat exchanger must be in place Maintain the requested temperature for 5 minutes 3 Operate the VT unit within the specifications of the probe Test the temperature at set points that correspond to the following Maximum minimum and midpoint of the allowed temperature For example probes with a VT range of 150 to 200 could be tested as follows 95 80 60 if air is used 120 30 20 if dry nitrogen is used 120 100 40 if a heat exchanger is used Ambient temperature Adjust the temperature by no more than 50 C enter su and wait for the temperature to equilibrate Magnet Drift The magnet drift test is an overnight test Sample For 200 and 300 MHz systems use IH lineshape sample 20 CHCI in 80 deuteroacetone CD3 5CO Part No 00 968120 76 For 400 500 600 750 and 800 MHz systems use 1 CHCl in 99 deuteroacetone CD3 CO Part No 00 968120 89 Probe and Hardware Requirements A 5 mm probe capable of H direct observe is r
51. f the autotest directory at user Name of the user running autotest printed in report at coilsize length in mm of active window in coil typically 16 or w 9 w m 9 op mo o 9 o Qo o o vo o wo mo Qo wo o wo o Qo o o vo o wo mo o o o vo o wo WM D t consoletype t consolesn t probetype t wntproc t cycletest t printparams t plotauto t graphhist t locktests t TT t gain L tor t fsq t dsp t ampl compr t LBampl compr t decHeating t linewidth t pw90 t tpwr t pw90Lowpower t tpwrLowpower t pw90 ch2 t pwx90 t pwx90lvl t pwx90Lowpower t pwx90Lowpowerlvl t vttest t temp t vttype t tempcontrol t gradtests t pfgon t gmap t gzcal t gxcal t gycal 18 mm Name of console entered in AutoTest window Number of console entered in AutoTest window Name entered for probe used in AutoTest window y or n for processing display after each FID y or n for automatic repeating of AutoTest y or n for parameter list pulse sequence printouts y or n for automatic plotting y or n for history graphs plotting y or n for lock power gain tests Value of last determined T Value of gain determined by autogain Value of tof for water Value of sq parameter Current value of dsp at start of run Value of high band amplifier compression Value of low band amplifier compression Temperature increase from decoupling Linewidth of water resonance 90 pw at power specified in AutoTest display Power sp
52. files 13C power level is reduced 20 dB from the level used to obtain a 15 us 90 approximately 1 8 kHz and the 3c decoupling efficiency is determined for the following phase modulated constant amplitude broadband decoupling sequences WALTZ 16 e GARP 1 e XY 32 MLEV 16 The PC decoupling frequency is varied over a range of 80 ppm in a series of single scan proton observe experiments Only the 13C bound protons are shown in the expanded spectrum which is plotted with spectra side by side in absolute intensity mode to illustrate decoupling efficiency X Adiabatic Decoupling Profiles The decoupling profile experiment is repeated with the following adiabatic decoupling schemes STUD modulation and WURST modulation Decoupler Heating The same test as in the variable temperature test is performed but this time using a 75 ms T decoupling period prior to acquisition within a total recycle time of 1 5 seconds including acquisition One hundred single scan spectra are collected with 13C decoupling followed by 100 identical spectra with no decoupling The spectra are plotted in a stacked manner to permit examination of the rate of change of temperature the homogeneity of temperature and the length of time necessary to reach equilibrium The rf field strength should be sufficient to decouple over a 160 ppm range using garp 1 Note that decoupling over 160 ppm at IH frequencies over 750 MHz 200 MHz 130 require efficient broadband a
53. for a period of time often used in TOCSY experiments using a recycle time of 1 5 seconds including acquisition Single transients are acquired at a rate of one per 1 5 seconds The data show any temperature change at the expected 0 01 ppm degree The intensity and or linewidth can be used to measure temperature homogeneity The number of transients needed to attain a new equilibrium temperature measures the ability of the probe to stabilize the effects of internal sample heating The final shift value indicates the total temperature change This can be used to reduce the requested temperature value so as to obtain the desired equilibrium Of course the amount of heating is a function of the sample itself primarily its salt content The same approach may be used to follow the actual temperature in the sample under the influence of X nucleus decoupling Lock Tests Experiment Lock power is varied over a 30 dB range and the lock level recorded The experiment is repeated for the lock gain A log regression analysis is performed to confirm the relationship between the lock signal and power gain Purpose of Lock Gain Test Lock gain is selectable in a logarithmic manner in dB In an ideal case variation of receiver gain should produce a logarithmic dependence of signal strength Purpose of Lock Power Control Using an RF Attenuator Overall lock power control is accomplished using computer controlled rf attenuators The amplitude respons
54. g up the probe prior to the VT calibrations e Doped 2 Hz H50 D50 0 1 mg ml GdCl in 1 H O in D5O Part No 01 901855 01 for 5 mm samples 2 Enter rtp vnmr tests shmd2o to retrieve the test parameter set to the current experiment Acquire a normal spectrum and shim the water signal to about 3 to 4 Hz linewidth at 5096 48 UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 2 3 Procedures for Contracted Custom Console Specifications 3 Replace the 99 8 DO sample with the 100 ethylene glycol sample Part No 00 968120 79 Set the following parameters pw 2 gain 5 or some value that doesn t overload the receiver sw 10000 atz2 nt 1 in n In the acqi window set the lock to Off The test is run unlocked because the sample has no deuterated solvent to lock on Enter su and check the probe tuning for the ethylene glycol sample Enter ga to acquire the spectrum Place the cursor between the two peaks and enter movetof to move the transmitter offset 4 Click the mouse on the Box menu button to call up right and left cursors Position the right and left cursors on the right and left peaks Enter tempcal glycol 5 Record the temperature reading from the VT controller displayed on the remote status module or on the front face of the VT controller and the computer calculated temperature based on the chemical shift frequencies of the two peaks CAUTION Extreme temperatures can damage the probe The hi
55. gh and low temperatues must be within the specified range of the probe 6 Enter temp 50 su to change the temperature to 50 C Allow the sample to stabilize at 50 C for atleast 10 minutes after the VT controller has reached the final temperature and regulated Enter ga to acquire a spectrum Repeat step 3 above and record the two temperatures 7 Make sure that the VT gas flow and cooling air flow levels are between 9 5 to 10 LPM and gas flow to the probe is not restricted in any way Enter temp 100 su to change the temperature to 100 C 8 Allow the sample to stabilize at 100 C for at least 10 minutes after the VT controller has reached the final temperature and regulated Enter ga to acquire a spectrum Repeat step 3 above and record the two temperatures Test Procedure for Low Temperature Calibrations CAUTION For low temperature calibrations fill the VT dewar with liquid nitrogen If a chemical mixture is used instead of liquid nitrogen for low temperature calibrations choose the chemical slurry carefully A mixture of crushed dry ice and acetone is not recommended because it will dissolve the polystyrene VT dewar 1 Check that the H quarter wavelength cable is installed and the probe is tuned Use the following sample for shimming up the probe prior to the VT calibrations Doped 2 Hz H50 D50 0 1 mg ml GdCl in 1 H O in DO Part No 01 901855 01 for 5 mm samples 2 Enter rtp vnmr tests shmd2o to retrieve the test p
56. gradient probes X axis for triax probes Y axis for triax probes Gradient echo stability for the following Z axis at 30 G cm X axis at 10 G cm Y axis at 10 G cm Z axis at 10 G cm Gradient recovery stability for the following X axis at 10 G cm Y axis at 10 G cm Z axis at 10 G cm Gradient recovery for the following X axis at 10 G cm Y axis at 10 G cm Z axis at 10 G cm Cancellation after gradient Automated Console Acceptance Demonstration Tests AutoTest performs the following console demonstration tests High band amplifier compression Low band amplifier compression Temperature rise in decoupler heating test AutoGain result for 90 pulse Receiver gain normal sampling 10 kHz sweep width Receiver gain oversampling 100 kHz sweep width Folded noise reduction with large spectral width Phase switch settling time 2 2 Manual Test Procedures Required to Demonstrate Console Operation This section contains the required manual test procedures Homonuclear Decoupling this page Lock Frequency Stability page 43 Basic Variable Temperature Operation page 44 Magnet Drift page 45 WALTZ 1H Decoupling Preprogrammed Phase Modulation page 46 WALTZ 1H Decoupling High Performance RF Waveform Generator page 47 42 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 2 2 Manual Test Procedures Required to Demonstrate Console Operation For optional
57. hat the information on this form is accurate and that all computers to be used to run VNMR software including variants VnmrS VnmrX VnmrI VnmrSGI and VnmrV or to run other software to process data obtained on this spectrometer have been included in the audit including those previously registered as part of purchases of other Varian NMR spectrometers Customer Representative Date 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 73 Chapter 4 Acceptance Test Results Use these forms for additional computers If more forms are needed copy this page Attach all copies to the Computer Audit Manufacturer Computer S N Memory Mbytes Peripherals Computer function VNMR version Information on computer Internal hard disk Mbytes External hard disk Mbytes Tape drive size CD ROM drive model Printer model Plotter model Terminal model Other peripheral NMR host Workstation running VNMR Workstation running other NMR software Workstation running VNMR and other NMR software Operating system of e g 2 of 3 Model no Purchased from Screen size in Serial no Serial no Serial no Serial no Serial no Serial no Serial no on site or off site on site or off site on site or off site Manufacturer Computer S N Memory Mbytes Peripherals Computer function Information on computer
58. hould be saved outside vnmrsys autotest since this file can be deleted later parameters Directory The vnmrsys autotest parameters directory contains any parameter set used by AutoTest macros including any put there by the user Normally only standard par is present This parameter set has all parameters necessary for the AutoTest macros Values of parameters may be displayed by using dg in the text window Some parameters are only displayed when certain variables are nonzero or y if a string parameter however these parameters are printed and displayed if used in an experiment The AutoTest macro At rt p is used to recall a parameter set from this directory reports Directory The vnmrsys autotest reports directory contains text files from previous AutoTest runs by date Each run produces a report whether plotting is requested or not The report file for a currently proceeding AutoTest run is vnmrsys autotest REPORT At the end of an AutoTest run this file is copied to the reports directory under a title that includes the date and time If AutoTest is repeated automatically a new report is written out for each complete AutoTest run The existing vnmrsys autotest REPORT file is renamed as vnmrsys autotest LASTREPORT whenever an AutoTest run begins Similar actions are executed for the atrecord report trexts Directory The vnmrsys autotest texts directory contains mainly text files that are printed on some spec
59. ic instrumentation supplier for information on acquiring a gaussmeter You can request additional signs from Varian by telephoning 1 800 356 4437 in the United States or by contacting your local Varian office in other countries UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 Chapter 2 Console and Magnet Test Procedures Sections in this chapter 2 Automated Test Procedures Running AutoTest this page e 22 Manual Test Procedures Required to Demonstrate Console Operation page 42 2 3 Procedures for Contracted Custom Console Specifications page 48 This chapter contains the procedures for testing NTYTNOVA NMR consoles and magnets These procedures are required to demonstrate the specifications listed in Chapter 3 Consoles and Magnets Specifications for WTIYTNOVA NMR consoles and magnets 2 1 Automated Test Procedures Running AutoTest The AutoTest automated test procedures software features a series of automated tests for both the console and the probe These tests demonstrate the console performance and its compliance with the acceptance test specifications as well as some of the probe acceptance tests and its compliance with the specifications listed in Chapter 3 AutoTest tests only channels 1 and 2 The automated tests write the results to a text file and plot the resulting spectra Although plotting is optional plotting should be activated for acceptance testing and customer rev
60. iew A hard copy of the AutoTest report should be attached to the appropriate acceptance test results in Chapter 4 Refer to Details of AutoTest Experiments page 24 for detailed descriptions of the tests performed by AutoTest Installing Autotest AutoTest is available beginning with the VNMR 6 1B AutoTest can be installed at any time but it is most convenient to install it when VNMR is installed If AutoTest is not already installed use these steps to install it now CAUTION Remove any files used for previous versions of AutoTest from your vnmrsys directories particularly any vnmrsys seqlib AT or vnmrsys maclib AT files Remove AT DEC gauss32 RF gauss RF and eburpl RF from vnmrsys shapel1ib if present Make sure that vnmrsys maclib autotest is not present 1l Mount the VNMR CD ROM change to the CD ROM directory and enter 1oad nmr The VNMR installation menu appears 2 Select the NTYTNOVA system at the top of the menu The VNMR installation menu for NTYTNOVA appears 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 37 Chapter 2 Console and Magnet Test Procedures 3 Select the AutoTest checkbox Click on install Refer the manual VNMR and Solaris Software Installation for further details Sample for AutoTest As the sample AutoTest uses 0 1 3C enriched methanol in 1 H 0 99 D20 The sample is doped with gadolinium chloride at a concentration of 0 30 mg ml which p
61. inearity channel 1 and channel 2 tpwr 40 standard deviation tpwr 16 standard deviation Temperature increase in spinlock test Lock power test correlation coefficient Lock gain test correlation coefficient Variable temperature test 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 21 Chapter 1 Installation Tests and Demonstrations Table 3 Source Code for AT16 Macro Example Code Comment if 320 ATrtp standard then text Pulse Turnon Test at_currenttest turnon_chl tpwr tpwr 6 ph array pw 37 0 1 025 Ss 2 wnt ATwft select celem wexp AT16 PART1 aph0 vsadj dssh dtext ATcycle au write line3 Pulse Turnon Test channel 1 dps elseif 1 PART1 then if at_plotauto y then if at printparams y then pap ATpltext pps 120 0 wcmax 120 90 page endif endif select arraydim apho f peak ht cr rl 0 sp 1p wp 2p vsadj dssh dtext ATreg6 ATp13 turnon corrcoef Sturnon trunc turnon corrcoef trunc 1000 Scorrcoef 1000 ATrecord TURNONch1 Pulse Turnon Time channel 1 time turnon corr coef corrcoef nsec write file autotestdir REPORT Pulse Turnon Time channel 1 2 0f nsec Corr Coef 1 3f turnon corrcoef IE then at_plotauto y ATpltext 100 wc2max 5 full wc 50 pexpl page First time AT16 is run it has no arguments Recalls standard parameter set
62. it was run and then executes svf Thus the data directory may contain FIDs obtained during different AutoTest runs if those runs were not full runs Any data files stored in the data directory can be recalled by normal VNMR commands such as rt The data may then be transformed and displayed The wexp parameter will contain the name of the macro normally used for data processing so that the wexp command can be used to duplicate the actions normally done in an automatic manner CAUTION If file vnmrsys autotest atdb at selected tests S empty only processing and no further acquisition is done 16 UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing This result is normally the case if the last AutoTest run came to a normal completion However if the last AutoTest run was aborted and no new entry into the AutoTest Program was done this file will contain entries and an acquisition may start up following the wexp command If so just abort the acquisition data failed Directory The vnmrsys autotest data failed directory contains any data from any failed experiment Failure results when a calculated result falls outside limits defined in the vnmrsys autotest atdb at spec table file Varian specifications are indicated in the vnmrsys autotest atdb at spec table file Users can modify this file by supplying upper and lower limits Any user modified at spec table file s
63. l response is used to measure the ability and reproducibility of the system to recover from the gradient pulse Field Recovery Experiment The gradient 90 pulse stability test is repeated with the field recovery delay varied from 0 to 1000 us using a positive 10 G cm Z axis gradient pulse The spectra are plotted in a horizontal stack with the 1000 Lis data at full scale The test is repeated using a negative 10 G cm gradient and if available for both the X and Y gradients Rectangular and half sine gradients are used Recovery is defined as the time it takes to recover to 9596 or more of the amplitude Purpose A gradient is applied prior to a measuring pulse and the time before the pulse is varied The rate of recovery determines how soon a pulse may be applied Gradient Echo Stability Experiment The 90 pulse stability test is run this time with a positive gradient for 1 ms a 500 us delay and a negative gradient for 1 ms following the rf pulse The following gradient strengths and axes are used e 30 G cm Z axis only 10 G cm Z axis and if present X and Y axes Purpose Following a single pulse a pair of opposite signed gradients is applied The stability of the resulting refocused signal measures any instability in the gradient amplitude as well as the accuracy of the gradient level control This should be done for all orthogonal axes available Gradient Effect on Cancellation Test Experiment Four 1
64. l stack with the single scan spectra on scale The vertical scale is increased by 100 times and plotted in the same manner Average residual signal for 2 scan and 4 scan cancellation are determined Purpose Modern experiments HMQC HSQC NOE difference etc often rely on phase cycling to achieve desired results This test compares single transient response versus two and four transient response in which the phase cycling is set to achieve cancellation Phase Stability 13 Phase Error Test Experiment The 90 pulse stability test is repeated but uses a 90 pulse 1 ms 90 pulse train with the carrier positioned 37 Hz off resonance from the water Purpose Phase stability is essential for high performance modern experiments Poor phase stability would produce poorer water suppression and increase T noise in 2D NMR The most robust tests of phase stability are solids tune up sequences used for verifying performance for line narrowing sequences such as WAHUHA or MREV 8 because these sequences are fairly independent of amplitude stability Another test is the 13 test in which two 90 pulses separated by 1 ms are applied with the transmitter placed 37 Hz off resonance The resulting NMR response stability is a product of both rf amplitude stability and phase stability because variations in phase between the pulses induce an amplitude change The observed amplitude error should be divided by a factor of 7 1 to obtain a measure of pha
65. lation Planning Guide are met Varian cannot warrant that the NMR spectrometer system will meet the published specifications General Requirements The UNTYTNOVA performance specifications in effect at the time the system is ordered are used to evaluate the system The appropriate quarter wavelength cable must be used for each nucleus Homogeneity settings must be optimized for each sample manual shimming may be required in any or all cases The shim parameters for resolution tests on each probe should be recorded in a log book and in a separate file in the vnmr shims directory for each probe For example for a 5 mm switchable probe the shim parameters can be saved with the command svs vnmr shims sw5res These values can then be used as a starting point when adjusting the homogeneity on unknown samples by using rts sw5res The probe must be tuned to the appropriate frequency The spinning speed used is the following Sample mm Nuclei Speed Hz 5 all 20 26 10 all 15 Note Making 10 mm tubes spin faster than 15 Hz may cause vortexing in samples severely degrading the resolution All test parameters are stored in the disk library vnmr tests and can be recalled by entering rtp vnmr tests xxx where xxx is the name of the test for example rtp vnmr tests H1sn To see the parameter sets available for the standard tests enter 1s vnmr tests For all sensitivity tests the value of pw m
66. lb 1 0 4 Enter ga to acquire the spectrum If the receiver or the ADC overloads reduce gain and reacquire the spectrum 5 Phasethe spectrum using manual phasing and place the cursor on the water signal 6 Enternl r1 4 8p movetof satfrq tof andreaquire the spectrum Then adjust gain to the highest level without ADC overload The sucrose anomeric proton peak will be at 5 3 ppm Determine the IH 90 pulse width for the sample by arraying pw to determine the optimum pw 7 Expand the spectral region between 5 to 7 ppm The IH signal to noise of the anomeric proton of sucrose is measured using a 200 Hz noise region between 5 4 to 7 0 ppm 8 Write the results on the forms provided in Consoles and Magnets Custom Specifications Form page 81 9 Insertsample B into the probe tune the probe and adjust the homogeneity using the lock signal 10 Determine the H 90 pulse width for the sample by arraying pw Use the same tpwr value as used for the no salt test 11 Repeat the procedure for sample C 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 53 Chapter 2 Console and Magnet Test Procedures The H 90 pulse width for sample B is increased 20 to 25 over the sucrose with no salt sample 12 Write the results for each probe in the forms provided in Consoles and Magnets Custom Specifications Form page 81 Aqueous Phenylalanine Water Suppression Sample 1 mM phenylalanine 1
67. le ATM and credit cards and damage some watches Do not take such objects closer to the magnet than this sign ix aS Pub No 87 25030300 B0694 5 Gauss Waring Sign VARIAN Figure 1 10 Gauss Warning Sign Figure 2 5 Gauss Warning Sign Amm A STRONG MAGNETIC AND RADIO FREQUENCY FIELDS ARE PRESENT LUET DOES Eel Ceo LE W Tale ATM Credit Cards Strong magnetic fields are present that could erase magnetic media such as floppies and tapes disable ATM Elite Ee Cr e CA UT e ETET G3 some watches Do not take such objects closer to the magnet than the 5 GAUSS WARNING signs Pub No 87 250801 00 B0694 Magnet Area Entrance Danger Sign Tools and Equipment Strong magnetic fields are present that could make some magnetic items suddenly fly towards the magnet body which could cause personal injury or serious damage Do not take tools equipment or personal items containing steel iron or other magnetic materials closer to the magnet than the 10 GAUSS WARNING signs a VARIAN Figure 3 Magnet Area Danger Sign Stray magnetic fields can reach beyond the published distances when two or more magnetic fields intersect or when the field extends over large ferromagnetic masses or structures steel doors steel construction beams etc In this case the customer must measure the stray field using a gaussmeter to determine how the 5 and 10 gauss fields are altered contact a scientif
68. ling 90 Pulse Width Calibrations PW90 H 90 pulse width calibrations on channels 1 and 2 13C 90 pulse width calibrations PW90 RF Homogeneity Tests IH rf homogeneity test 13C rf homogeneity test Gradient Calibrations and Performance Tests Gradient level for 10 G cm along the following Z axis for all gradient probes X axis for triax probes Y axis for triax probes Gradient echo stability for the following Z axis at 30 G cm X axis at 10 G cm Y axis at 10 G cm Z axis at 10 G cm Gradient recovery stability for the following X axis at 10 G cm Y axis at 10 G cm Z axis at 10 G cm Gradient recovery for the following X axis at 10 G cm Y axis at 10 G cm Z axis at 10 G cm Cancellation after gradient 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 23 Chapter 1 Installation Tests and Demonstrations 24 Console Demonstration Tests High band amplifier compression e usec pulse amplitude stability channel 1 and channel 2 Low band amplifier compression Temperature rise in decoupler heating test e AutoGain result for 90 pulse Receiver gain normal sampling 10 kHz sweep width e Receiver gain oversampling 100 kHz sweep width Folded noise reduction with large spectral width Phase switch settling time CPMG T result for the following Gradient level 10 G cm Without gradients 1 gradient mismatch Shaped RF Demonstrations Shaped pulse acc
69. m along Z Gradient level for 10 G cm along X Gradient level for 10 G cm along Y Z gradient echo stability 30 G cm X gradient echo stability 10 G cm Y gradient echo stability 10 G cm Z gradient echo stability 10 G cm CPMG T calculation gradients on mismatched and off Z gradient recovery stability 10 G cm X gradient recovery stability 10 G cm Y gradient recovery stability 10 G cm Z axis signal recovery rect Z axis signal recovery sine X axis signal recovery rect X axis signal recovery sine Y axis signal recovery rect Y axis signal recovery sine Gradient phase cycle cancellation 4 scans see note 2 Gaussian 90 stability channels 1 and 2 Gaussian 13 phase error channels 1 and 2 GaussianSLP 13 phase error channels 1 and 2 Temperature rise in spinlock test Lock power test corr coef Lock gain test corr coef AutoTest Specification std dev 0 25 std dev 0 25 std dev 0 50 std dev 0 50 lt 0 09 value reported value reported value reported 2 99 9 2 99 9 2 99 9 2 99 9 demonstration 2 99 9 2 99 9 299 9 lt 50 us lt 50 us lt 30 us lt 30 us lt 30 us lt 30 us lt 0 596 2 99 9 lt 0 09 lt 0 09 demonstration 2 0 85 20 9 standard deviation std dev provided as reference but is not a specification for the test 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 59 Cha
70. macro to process the 20 spectra for average height phase deviation and frequency shift The lock frequency stability is displayed as the standard deviation degrees When the prompt Plot Results n y appears answer y to print the results Basic Variable Temperature Operation For the basic variable temperature VT accessory Varian Part No 00 992957 00 this test demonstrates that the VT accessory and probe go to the desired temperature as registered on the window of the VT controller VT accessory operation is described in detail in the VNMR manuals For the high stability VT accessory refer to Stability Calibration for High Stability VT Accessory page 50 Dry nitrogen is required as the VT gas if the requested temperature is over 100 C or below 10 C Otherwise air can be used For temperatures below 40 C dry nitrogen gas is recommended for cooling the bearing spinner and decoupler This gas prevents moisture condensation in the probe and spinner housing CAUTION The use of air as the VT gas for temperatures above 100 C is not recommended Such use destructively oxidizes the heater element and the thermocouple Demonstration Limitations The VT range varies from probe to probe VT will be demonstrated only at temperatures within the specified range of the probe in use If dry nitrogen gas and liquid nitrogen are not available at the time of installation the range of VT demonstration is limited to temperatures b
71. may be performed during the installation of the Varian NMR spectrometer system if mutually agreed to before the installation Users are encouraged to perform these procedures on their own as further familiarization and evaluation of the instrument performance Temperature Accuracy for VT Systems The tests in this section check temperature accuracy calibrations for high and low temperatures using ethylene glycol and or methanol respectively Sample Table 4 lists the samples for low temperature and high temperature tests Table 4 Samples for VT Calibration Curve Temperature Range Sample Tube i Sample Part C roni Test Sample Number 50 to 25 Low 5 100 methanol reagent grade 00 968120 80 25 to 100 High 5 100 ethylene glycol reagent grade 00 968120 79 Probe and Hardware Requirements The variable temperature accessory and a VT probe are required VT tests should be run using a 5 mm probe that is capable of H direct observe over the temperature range of 150 C to 200 C For probes that have a more limited temperature range particularly PFG probes run the test at two or three temperatures that fall within the VT range of the probe These tests can also be run using the IH decoupling coil of the 5 mm broadband probe as H direct observe Test Procedure for High Temperature Calibrations 1 Check that the H quarter wavelength cable is installed and the probe is tuned Use the following sample e for shimmin
72. n erase magnetic media such as floppy disks and tapes The field can also damage the strip of magnetic media found on credit cards automatic teller machine ATM cards and similar plastic cards Many wrist and pocket watches are also susceptible to damage from intense magnetism Refer to the manuals supplied with the magnet for the size of a typical 5 gauss stray field This gauss level should be checked after the magnet is installed 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 9 SAFETY PRECAUTIONS Caution Notices continued CAUTION CAUTION CAUTION 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 Refer to the Installation Planning Guide for magnet field plots Check helium and nitrogen gas flowmeters daily Record the readings to establish the operating level The readings will vary somewhat because of changes in barometric pressure from weather fronts If the readings for either gas should change abruptly contact qualified maintenance personnel Failure to correct the cause of abnormal readings could result in extensive equipment damage Never operate solids high power amplifiers with liquids probes On systems with solids high power amplifiers never
73. ng blockage of the vent tubes and possibly extensive damage to the magnet It could also cause a sudden dangerous release of nitrogen and helium gases from the dewar Except when transferring nitrogen or helium be certain that the relief valves are secured on the vent tubes WARNING On magnets with removable quench tubes keep the tubes in place except during helium servicing On Varian 200 and 300 MHz 54 mm magnets only the dewar 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 the manual supplied with the magnet Caution Notices Observe the following precautions during installation operation maintenance and repair of the instrument 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 CAUTION Keep magnetic media ATM and credit cards and watches outside the 5 gauss perimeter from the centerline of the magnet The strong magnetic field surrounding a superconducting magnet ca
74. not changed during the pulse sequence and acquisition and digital filtering is not used The test is repeated using frequency shifted quadrature detection FSQD with single scans FSQD is described FSQD is described with the digital filtering information in the Getting Started manual Purpose This test checks the inherent balance in the two quadrature channels and the ability of phase cycling to eliminate any quadrature image Four single transient and 4 four transient responses are collected and compared Quadrature images can also be eliminated using digital filtering techniques The FSQD test measures image rejection under these conditions UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 7 AutoTest Automated Instrument Testing Shaped Pulse Test Channels 1 and 2 Gaussian Shaped Pulse Excitation Experiment A gaussian shaped pulse with excitation bandwidth at 50 amplitude about 200 Hz is applied e g a 12 ms 90 pulse length Single scan spectra are taken with the transmitter stepped over the range 250 Hz from resonance in 5 Hz steps The data are plotted in a horizontal stack with the on resonance spectrum at full scale to illustrate the gaussian shape of excitation The vertical scale is increased by x10 and plotted again to show the wings Purpose The most demanding test of shaped pulse accuracy is the ideality of the NMR data following a shaped pulse This test determine
75. nto the probe Probe and Hardware Requirements Any variable temperature probe is used Basic Specifications The specifications for variable temperature ranges are listed with each probe 01 999120 00 B0800 UNITYINOVA Acceptance Tests Procedures and Specifications 63 Chapter 3 Consoles and Magnets Specifications 64 Magnet Drift Specifications Sample For 200 and 300 MHz systems use IH lineshape sample 20 CHCl in 80 deuteroacetone CD3 5CO Part No 00 968120 76 For 400 500 600 and 750 MHz systems use 1 CHCl in 99 deuteroacetone CD4 CO Part No 00 968120 89 Probe and Hardware Requirements A 5 mm probe capable of H direct observe is recommended Basic Specifications Table 6 lists the drift specifications for magnets Specifications for nominal field decay rate are less than or equal to the values listed in the table Table 6 Magnet Drift Specifications System Field Strength Nominal Field Decay Rate MHz mm T Hz hr 200 54 200 89 4 70 2 300 54 300 89 7 05 3 400 54 9 40 8 400 89 9 40 10 500 51 11 75 10 600 51 14 10 10 750 51 17 60 15 UNITY INOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 3 2 Specifications for Manual Console Tests WALTZ H Decoupling Using Preprogrammed Phase Modulation This test is performed using the phase modulator and not the waveform generators Sample Doped 40 p dioxane in benzene dg Part No Sample Tube 0
76. o that the heights can be easily compared The results are fitted to a straight line using linear regression and the fitted data are plotted Next the data are normalized and plotted with the water signal held to a constant height so that the noise levels are easily compared a few mm of noise in the baseline are provided The signal to noise ratios for the water line in all spectra are measured with a spectral width of 10000 Hz and no oversampling Channel 1 is used for the acquisition With oversampling X10 the experiment is repeated Processing plotting and quantization of the oversampled data are the same as for the data from the 10000 Hz experiment Purpose Receiver gain is selectable in a logarithmic manner in dB In an ideal case variation of receiver gain should produce a logarithmic dependence of signal strength As the gain is lowered the noise becomes dominated by noise generated in the ADCs not in the preamplifier and probe Regardless of the signal strength operation in this range of gain will produce poorer signal to noise Image Rejection Test Experiment Plot the data from the following tests first in a horizontal stack with the single scan data on scale and then with the vertical scale increased 100 times Quantitate the average image and center glitch e Four single scan and four 4 scan 90 pulse spectra are acquired in which the carrier frequency is shifted 1000 Hz from the water The carrier position is
77. obe manuals Specifications for High Stability VT Units The high stability VT accessory holds the set temperature to within 0 1 C 0 1 C 0 001 ppm 600 MHz 0 6 Hz 500 MHz 0 5 Hz 400 MHz 0 4 Hz 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 69 Chapter 3 Consoles and Magnets Specifications 70 Homospoil Demonstration Sample Doped 2 Hz H50 D5O 0 1 mg ml GdCl in 1 H O in D5O Part No 01 901855 01 for 5 mm samples Probe and Hardware Requirements Use a 5 mm probe capable of H direct observe Specifications Part 1 The residual signal amplitude of the second spectrum is less than 5 of the signal amplitude of the first spectrum Part 2 The residual signal amplitude of the second spectrum is greater than or equal to 95 of the signal amplitude of the first spectrum UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 Chapter 4 Acceptance Test Results Sections in this chapter 4 1 Computer Audit page 73 4 System Installation Checklist page 75 4 3 Supercon Shim Values page 77 4 4 Console and Magnet Test Results page 79 4 5 Consoles and Magnets Custom Specifications Form page 81 This chapter contains forms for recording system information and acceptance test results 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 71 Chapter 4 Acceptance Test Results Notes 72 UNITY NOVA Acceptance
78. of the probe and regulation hardware Small Angle Phase Shift Test Experiment Single scan spectra are acquired in which the phase of the pulse is incremented by 10 in each spectrum through a full 360 at constant receiver phase Spectra are plotted in a horizontal stack to show a smooth phase rotation of the spectrum The test is repeated using pulses generated from channel 2 Purpose Small angle phase adjustment is used in multiple quantum selection q 2 phase modulated pulses and a variety of complex pulse sequences This test exercises the phase shift hardware by varying the pulse phase in small increments over 360 1 8 Varian Sales Offices For product sales and service information contact one of the Varian sales offices Argentina Buenos Aires 114 783 5306 Australia Mulgrave Victoria 3 9566 1138 Austria V sendorf 1 699 96 69 Belgium Brussels 2 721 48 50 Brazil Sao Paulo 11 829 5444 Canada Ottawa Ontario 613 260 0331 China Beijing 10 6846 3640 Denmark Herlev 42 84 6166 France Orsay 1 69 86 38 38 Germany Darmstadt 6151 70 30 taly Milan 2 921351 Japan Tokyo 3 5232 1211 Korea Seoul 2 3452 2452 Mexico Mexico City 5 523 9465 Netherlands Houten 30 635 0909 Norway Oslo 9 86 74 70 Russian Federation Moscow 95 241 7014 Spain Madrid 91 472 7612 Sweden Solna 8 445 1601 Switzerland Zug 41 749 88 44 Taiw
79. 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 Take electrostatic discharge ESD precautions to avoid damage to sensitive electronic components Wear a grounded antistatic wristband or equivalent before touching any parts inside the doors and covers of the spectrometer system Also take ESD precautions when working near the exposed cable connectors on the back of the console Radio Frequency Emission Regulations The covers on the instrument form a barrier to radio frequency rf energy Removing any of the covers or modifying the instrument may lead to increased susceptibility to rf interference within the instrument and may increase the rf energy transmitted by the instrument in violation of regulations covering rf emissions It is the operator s responsibility to maintain the instrument in a condition that does not violate rf emission requirements 10 UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 Chapter 1 Installation Tests and Demonstrations Sections in this chapter 1 1 Acceptance Testing this page e 1 2 Computer Audit this page 1 3 Installation Checklist page 12 e 1 4 System Documentation Review page 12 1 5 Basic System Demonstration page 12 1 6 General Acceptance Testing Requirements page 13 e 1 7 AutoTest Automated Instrument
80. or H is installed 200 300 and 400 MHz systems and the probe is tuned Enter ga to acquire a normal spectrum Shim the water signal to about 3 Hz or less linewidth at 50 Set the t of to be about 100 Hz off resonance from the water peak Array the homospoil parameter by entering hs nn ny Enter ga to acquire the arrayed spectra Enter ds 1 to display the first spectrum Phase the spectrum by entering aphO Display both spectra by entering dssh The second spectrum should be considerably smaller than the first spectrum Measure the amplitude of the first spectrum by moving the cursor on top of the peak and entering n1 The height of the peak in mm and the frequency are displayed in the status window Record the height of the peak for the first spectrum Measure the amplitude of the second spectrum by displaying the second spectrum using ds 2 Make sure the first and second spectra are displayed using the same values of vs vertical scale Move the cursor on top of the peak and enter n1 Record the height of the peak for the second spectrum Calculate the residual signal amplitude of the second spectrum as follows h x 100 7 Percentage of residual signal amplitude 1 Where hs is the height of the second spectrum and h is the height of the first spectrum Sucrose Anomeric H Signal to Noise Ratio This test measures signal to noise ratio for anomeric proton of 1 46 mM sucrose in DO with and without 250 mM NaCl fo
81. ors and additional signs may be needed there 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 35 Chapter 1 Installation Tests and Demonstrations 36 3 Magnet area danger signs Figure 3 Post at each entrance to the magnet area Be sure each sign is outside the 5 gauss perimeter A10 GAUSS 3l WAG Wes 7 STRONG MAGNETIC FIELD Tools and Equipment Strong magnetic fields are present that can make magnetic items suddenly fly towards the magnet which could cause personal injury or serious damage Do not take tools equipment or personal items containing steel iron or other magnetic materials closer to the magnet than this sign Dewars The stray field of the magnet can pull a magnetic dewar into the magnet body causing serious damage Use only nonmagnetic stainless steel dewars Do not use iron or steel dewars during servicing av aw Pub No 87 250302 00 B0694 10 Gauss Warning Sign VARIAN A STRONG MAGNETIC FIELD Pacemaker Metallic Implant Hazard Strong magnetic and rf fields are present that can cause serious injury or death to persons with implanted or attached medical devices such as pacemakers and prosthetic parts Such persons must not go closer to the magnet than this sign until safety at a closer distance is identified by a physician or device Magnetic Media ATM Credit Cards Strong magnetic fields are present that can erase magnetic media disab
82. ours before the next step Enter in2 n spin n nt landarray d1 73 600 0 d1 1 0 This sets up an array of d1 values with the first spectrum to be collected at time 0 minutes and subsequent spectra to be collected at 10 minute intervals for up to 12 hours Enter ga to acquire the spectra The test takes 10 to 11 hours to complete After the spectra are acquired phase the first spectrum by entering ds 1 to display the first spectrum of the array and by entering aphO to apply a first order phase correction to the spectrum Enter ai to scale all of the spectra to the same vertical scale and enter dssa to display the arrayed spectra stacked vertically Measure the difference between the left most peak and the right most peak in Hz Homospoil Demonstration Sample Doped 2 Hz H50 D50 0 1 mg ml GdCl in 1 H O in D4O Part No 01 901855 01 for 5 mm samples Probe and Hardware Requirements A 5 mm probe capable of IH direct observe is recommended Test Procedure Part 1 1 Enter rtp vnmr tests shmd20 to retrieve the test parameter set to the current experiment Enter solvent d2o0 pw 0 hst 0 005 sw 6000 d1 60 d2 0 055 then set p1 to the H 90 pulse width value and enter su Check that the appropriate quarter wavelength cable for H is installed 200 300 and 400 MHz systems and the probe is tuned Enter ga to acquire a normal spectrum Shim the water signal to about 3 Hz or less linewidth at 50 Set tof to
83. ped rf Gaussian 90 stability channel 1 and channel 2 Gaussian phase stability test channel 1 and channel 2 Gaussian SLP phase stability test channel 1 and channel 2 Automated Heteronuclear Decoupling Performance Tests AutoTest performs the following automated decoupling performance tests Bc phase modulation decoupling profiles 13C GARP decoupling profile 13C WALTZ 16 decoupling profile e BCXyY32 decoupling profile 13C MLEV 16 decoupling profile e 13C adiabatic decoupling profiles if waveform generator is present on the decoupling channel BC STUD decoupling profile PC WURST decoupling profile e Sample heating during 5C broadband decoupling Automated Probe Performance Tests Note Individual probe acceptance test procedures and specifications specify probe acceptance tests and specifications The automated tests do not form the basis of a probe s acceptance or rejection AutoTest performs the following 90 pulse width calibrations PW90 e lH 90 pulse width calibrations on channels 1 and 2 e 13C 90 pulse width calibrations PW90 AutoTest performs the following rf homogeneity tests e Hef homogeneity test Pes homogeneity test 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 41 Chapter 2 Console and Magnet Test Procedures AutoTest performs the following gradient calibrations and performance tests Gradient level for 10 G cm along the following Z axis for all
84. processing the data acquired from those experiments creating plots parameter printouts archiving the raw data performing statistical analyses of the data and writing results to history files and reports A new MAGICAL capability is used that makes the macro easier to read and write the elseif statement This removes the need for multiple endif statements if multiple calls to the same macro are used To better illustrate the structure of these macros Table 3 gives the source code for macro AT16 the turn on test channel 1 A column of descriptive comments has been added to clarify the statements The AutoTest macros can be run as independent macros if a specific test is desired This is done by entering the macro in the VNMR command line Again if the file at selected tests is not empty the ATnext macro will start a new acquisition Standard Tests Performed by AutoTest Automated Console Tests 90 pulse stability channel 1 and channel 2 30 amplitude stability channel 1 and channel 2 Pulse turnon time channel 1 and channel 2 Phase cycle cancellation 2 scan test is run as demonstration no specification is set Quadrature image 1 scan and 4 scans Frequency shifted quadrature image 1 scan Phase stability test 13 test channel 1 and channel 2 Attenuator test channel 1 and channel 2 Full power correlation coefficient and standard deviation Reduced power correlation coefficient and standard deviation Modulator l
85. pter 3 Consoles and Magnets Specifications 3 2 Specifications for Manual Console Tests This section contains the following specifications Lock Frequency Stability this page Homonuclear Decoupling this page Variable Temperature Operation page 63 Magnet Drift Specifications page 64 WALTZ 1H Decoupling Using Preprogrammed Phase Modulation page 65 WALTZ 1H Decoupling Using High Performance Waveform Generators page 66 60 UNITY TNOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 3 2 Specifications for Manual Console Tests Lock Frequency Stability Sample 99 D450 196 H50 in a 5 mm sample tube 0 7 ul volume Probe and Hardware Requirements A 5 mm probe capable of H direct observe is recommended This test also requires a Lock Module on the spectrometer Basic Specifications The lock is stable to within 0 01 Hz as judged by the phase response of a Hahn echo in 99 D O 1 H30 with 500 ms echo interval 0 1 Hz 36 zero order phase change The maximum phase variation in the twenty experiments must not exceed 3 6 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 61 Chapter 3 Consoles and Magnets Specifications Homonuclear Decoupling Sample 0 1 ethylbenzene 0 01 TMS 99 89 deuterochloroform CDC14 Part No Sample Tube 00 968 120 70 5mm 00 968123 70 10 mm Probe and Hardware Requirements A 5 mm probe capable of H direc
86. pwr type power level provides a 50 Hz field on the transmitter see step 3 for the calibration procedure tpwr 63 pw 8 or whatever is the tpwr and pw values meet the H 90 pulse width calibration specification for the probe e Enter ga to acquire the spectrum The spectrum should show that the water peak is suppressed The water peak should be roughly the same amplitude or smaller than the acetate about 2 ppm and the TSP at 0 ppm peaks 54 UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 2 3 Procedures for Contracted Custom Console Specifications If the water peak is not suppressed the satpwr level may need to be calibrated to give a 50 Hz YH field or the t of may need to be moved so that it is directly on the water peak 3 The YH field calibration is made by calibrating the 90 pulse If the water peak is used to calibrate the 90 pulse the water signal would overload the system A better way is to apply a pulse to the TSP 0 ppm line Calibrate the yH field as follows a Place the cursor on the TSP resonance the line furthest to the right as you look at the spectrum from the previous steps b Enternl movetof c Setd1 10 nt 1 pw 5000 The relationship between the desired yH field and pw is pw 1 4 yH field For a 50 Hz YH field pw 5000 d Array tpwr over a range of values that span the desired power level a suggested array is tpwr 4 6 8 10 12 14 16 18 20 Enter wexp wft d
87. r 500 600 750 and 800 MHz systems UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 2 3 Procedures for Contracted Custom Console Specifications Samples The samples are the following e 300 ug sucrose in 0 6 mL of D3O e 300 ug sucrose 250 mM NaCl in 0 6 mL of DO e 0 6 mL sample volume in a standard 5 mm NMR sample tube Wilmad 535 PP These samples can be made up by the customer or specially prepared samples from Varian can be sent for the test Probe and Hardware Requirements This test requires 5 mm triple resonance indirect detection and proton probes probes capable of IH direct observe The tests are designed to be performed at a power level giving rise to a 90 pulse width less than or equal to 10 us for the no salt sample This test requires excellent By homogeneity As a prerequisite the probe should be shimmed well enough to meet IH non spin lineshape specifications The sucrose IH signal to noise test is performed with the sample not spinning Test Procedure 1 Insert sample A into the magnet tune the probe and adjust the homogeneity using the lock signal 2 Enter rtp vnmr tests shmd20 and presat to retrieve the test parameter set to the current experiment 3 Setnt 1 spin n sw 6000 at 5 0 gain 40 pw 10 H 90 pulse width tpwr 57 or whatever t pwr was used to give a H 90 pulse width of 10 usor less dm2 nnn satpwr 4 satfrq tof presat 2 0 tnsat y composit n
88. racteristics at regular intervals The test is completely automated and can be performed in about 40 to 90 minutes depending on the options chosen Significant deviations from the norm can provide an indication of a hardware failure or slow degradation each of which might be hard to identify using normal spectra Tests have been designed to test only one aspect of performance and one piece of hardware at a time as much as possible Historical trends in performance can be displayed This section contains the following topics Test Design this page e Scope of Test this page Test Output page 16 e AutoTest Directory Structure page 16 e AutoTest Macros page 19 e Standard Tests Performed by AutoTest page 21 Details of AutoTest Experiments page 24 Test Design The test is designed to quantitate instrument performance on an unbiased statistical basis The average values and standard deviations from stability and reproducibility measurements are determined Other tests produce a regular intensity output exponential or linear such as when an attenuator or modulator value is varied Correlation coefficients and standard deviations from a regression analysis are reported Calibrations are made of parameters such as H pw90 using channels 1 and 2 13C pw90 and high and low band amplifier compressions Probe rf homogeneity H 450 90 810 90 and 3C 360 0 720 0 values are determined Sensitivity T and
89. rd Tests Performed by AutoTest 21 Details or Auto Test EXDOLIDETIIS iei erect tree tette ter ore eei ind 24 1 8 Varian Sales Offices i er e rt etre ER a ERE REPE TREE RR EEA 34 1 9 Posting Requirements for Magnetic Field Warning Signs 35 MEDIIS SIEDS zie dier RP LO E De E I ege E RSS RR PE RAE 35 Chapter 2 Console and Magnet Test Procedures 37 2 1 Automated Test Procedures Running AutoTest esee 37 Installing AutGtest sere eee teret e e n retro e lesedsravesaneseteaetes 37 oantple Tor AUIOTESE 2 eget e et er reta ler eR ERR EINER ed 38 Setting DpidorANUtO Tes ente tetendit ee nte ne ope Re 38 Runnin AU OUTESL 51th peer treten rte a RE Pe ERE RUNE Gee eara ed 38 Saving Data and FID Files from Previous Runs eee 39 Creatine Probe specie Biles 2 6 irm nmt t t ge etn epentes 40 Tests Performed by AutoTest 2 ice rnnt e eta en ra reete 40 2 2 Manual Test Procedures Required to Demonstrate Console Operation 42 Homonuclear Decoupling 2 oie err tree eo ere es 43 Lock Frequency Stability 2er eet erre tee e tee tnt 43 Basic Variable Temperatiie Operation eget eee reet 44 IVIL DUE 2uehelaedeseseiee vesc oie e D RR T 45 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 3 WALTZ H Decoupling Preprogrammed Phase Modulation 46 WALTZ H Decoupling High
90. re fluctuations Sample Doped 2 Hz H50 D50 0 1 mg ml GdCl in 1 H50 in D50 Part No 01 901855 01 for 5 mm samples Alternatively the customer can use a 10 mM DSS in D5O sample volume of 0 6 ml in a 5 mm NMR tube DSS 3 trimethylsilyl 1 propane sulfonic acid The customer must make this sample using DSS and deuterium oxide 99 8 or 99 9 atom D Upon request Varian can make this sample if DSS is not available at the customer site Probe and Hardware Requirements High stability variable temperature accessory and a 5 mm probe capable of H direct observe are required UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 2 3 Procedures for Contracted Custom Console Specifications Test Procedure l Enter rtp vnmr tests shmd20 to retrieve the test parameter set to the current experiment Enter temp 40 at 10 sw 10000 Set pw to the IH 90 pulse width for the probe and then enter spinz n su Allow the VT controller to regulate to 40 C which should be about 10 higher than the room temperature Check that the IH quarter wavelength cable is installed 200 300 and 400 MHz systems and the probe is tuned Acquire a normal spectrum by entering ga Move the cursor to the DSS signal right most peak Enter movetof sw 1000 at 10 Acquire a normal spectrum and shim the DSS signal to about 0 6 Hz or less linewidth at 50 The sample of DSS in D50 should equilibrate at 40 C for at least 2 h
91. roduces a IH T relaxation time of about 50 to 75 ms The resulting line width is considerable larger than the magnet determined line width because of the paramagnetic relaxation contribution Setting Up for AutoTest To set up for autotest Make sure all units of the rf system transmitters linear modulators rf attenuators amplifiers receivers and probes are in the standard configuration 2 Ifthe system has a PFG accessory installed make sure that the gradient amplifier is on and p gon is set correctly for the number of gradients available e pfgon nny for Z axis only e pfgon yyy for triax Allow sufficient time for stabilization AutoTest calibrates the gradients 3 Insert the AutoTest sample 4 Setthe VT to 25 C Allow the temperature of the sample to regulate and equilibrate While specifications are determined at 25 C normal day to day AutoTest runs may be done at other temperatures 5 Tune the probe and lock on the D20 resonance 6 Shim the field on the sample to give a nonspinning half height that is dominated by the paramagnetic relaxation agent Because the H5O line is quite broad this should not require much time 7 Notethe tpwr value necessary to produce a IH 90 pulse width that is within specification 8 to 10 us but does not cause probe arcing AutoTest uses this t pwr value in determining the H 90 pulse width and calculates the amplifier compression at this tpwr value 8 To save the re
92. rument UNITYINOVA UNITY plus UNITY and VXR are registered trademarks of Varian Inc Sun is a registered trademark of Sun Microsystems Inc SPARC and SPARCstation are registered trademarks of SPARC International Inc Ethernet is a registered trademark of Xerox Corporation Other product names are trademarks of their respective holders Table of Contents SAFETY PRECAU IONS AT 7 Chapter 1 Installation Tests and Demonstrations 11 LI Acceptance Testing 5 eere rt re Fe RR Ree RAF XR Fr XR RR ERR UR 11 1 2 Computer Audit 1 retrieve Ebr k Ua are barro 11 1 3 Installation Checklist 5 2 noue Rh ttr mr re re EEUU 12 1 4 System Documentation Review sees neret ener nennen 12 1 5 Basic System Demonstration esses nnne ene ETE 12 Magnet Demonslratol 11 2 5 e I RR ORE ROREM FAEERE Ee ER IRE 12 Console and Probe Demons ramon 15 eene nere eren ionis 12 1 6 General Acceptance Testing Requirements esee 13 General ROquremienbs ca eee scere e er ee e iie Ies 13 Probe Installation POlGIeS genes eee ie edere ie n Peers 14 1 7 AutoTest Automated Instrument Testing sese 15 Test DUM 15 SCODE Of TeSt ioter tte rte he rn ti rho t Ro ra dee Ro E Rasen Ren 15 Test Output e 16 Auto Test Directory SUUGQUEE usd eee iet edtes 16 Auto Test Macros DE 19 Standa
93. s case the pulse length is repeatedly incremented while appropriately reducing power levels The NMR response should be identical Shaped Pulse Test Rectangular Gaussian and EBURP 1 Experiment Single scan one pulse excitation spectra are collected using rectangular gaussian and EBURP 1 pulses at the same peak amplitude note the power value and pulse lengths Constant peak amplitude is maintained therefore pulse width ratios of 1 0 2 4 16 0 for the rectangular gaussian EBURP 1 pulses respectively are used to obtain the same flip angle Spectra are plotted side by side in absolute intensity mode at full vertical scale Atany constant power the 90 pulse lengths should reflect their theoretical ratios Here the pulse lengths are set in a ratio of 1 2 4 16 The resulting NMR responses should be identical in amplitude Shaped Pulse Test Constant Bandwidth for a Variety of Shapes Experiment Single scan one pulse excitation spectra are collected using a variety of shapes that are automatically calculated using Pbox based on a single pulse calibration using a rectangular pulse for a constant 4000 Hz bandwidth The shaped pulses have different peak amplitudes and pulse widths note the power value and pulse lengths Spectra are plotted side by side in absolute intensity mode at full vertical scale The resulting NMR responses should be identical in amplitude Shaped Pulse Scalability Experiment A small flip angl
94. s the accuracy of a gaussian pulse by examination of the off resonance excitation This is done by repeating the same single pulse excitation while varying the transmitter position through a wide range A stacked array of data should show the magnitude of excitation as a function of offset from resonance In the ideal case this excitation envelope would also be gaussian Any non gaussian nature of the pulse as delivered to the probe would be represented by a convolution of excitation envelopes For example if the power were not delivered in a linear manner producing some rectangular nature the excitation envelope would have some sinx x nature producing characteristic sinc wiggles The lack of such non gaussian behavior is a direct measure of the accuracy with which the hardware can deliver an ideal shape to the nuclei Gaussian 90 Pulse Stability Experiment The rf 90 pulse stability test is repeated using a gaussian pulse at the same peak power The data are plotted in a horizontal stack with the on resonance spectrum at full scale to illustrate the gaussian shape of excitation Purpose Modern experiments require very high pulse reproducibility to minimize cancellation residuals and T noise in 2D experiments This tests amplitude reproducibility by comparing a series of spectra obtained with the signal following a single 90 pulse The statistical analysis produces an rms deviation in percent of the average peak height Ga
95. scan four 2 scan and four 4 scan 90 pulse spectra are acquired with a 10 G cm Z axis gradient pulse 100 us prior to the rf pulse and the transmitter phase held constant while the receiver is phase cycled 0 2 1 3 The spectra are plotted in a horizontal stack with the single scan spectra on scale Vertical scale is increased by 100 times and plotted in the same manner The average residual signal for the 4 scan cancellation is quantitated and the results plotted and analyzed as above Purpose The cancellation test is done with a gradient pulse applied 100 us before the rf pulse If the lock circuitry and field recovery characteristics are favorable no deterioration in cancellation efficiency should be noted CPMG T Experiment A CPMG T experiment is performed with 2 ms between 180 pulses for total echo pulse trains ranging from a few milliseconds out to at least 2 7 This experiment is repeated for the case where 500 us 10 G cm rectangular pulses are placed around the 180 pulses in each echo as well as the case in which no gradients are used The values for 7 are reported for all cases The experiment is repeated for the case of a 196 mismatch in gradient amplitude Purpose Following a single pulse pairs of same signed gradients are applied within the echoes of a CPMG T pulse echo train The measured T gives a measure of any instability in the gradient amplitudes as well as the accuracy of the gradient level control This
96. se error in degrees Pulse Turn on Time Experiment Single scan experiments are taken in which the pulse is varied from 0 to 1 2 us in minimum pulse width steps at low enough power so that the response is linear The response is fitted to a straight line and the turn on time is determined Because of differences in implementation turn on times for channel 2 are usually longer than for channel 1 even though the hardware is identical e Purpose The quality of modern rf is good enough that examination of pulse shapes using an oscilloscope is not as informative as well designed and executed NMR tests 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 25 Chapter 1 Installation Tests and Demonstrations 26 The turn on and turn off characteristics of a very short pulse are properties that can be measured sensitively by NMR The turn on test measures the amplitude of a signal following a short variable length pulse In the limit of a small flip angle this dependence is linear The data are analyzed and least squares fitted to a straight line The intercept is the pulse turn on time Attenuator Linearity Experiment For a small flip angle pulse the rf coarse power is varied from maximum to minimum in single scan mode The data are plotted in a horizontal stack to facilitate visual inspection The data are fitted to a linear regression and plotted in phased mode to show any phase change as a function
97. ssh au e Selectthe tpwr value that gives the maximum signal amplitude from the previous step f Enter setlimit pw 50000 0 0 025 to allow the software limit for pw to exceed 8192 g Array pw around the 360 pulse 4 90 pulse A suggested array is pw 16000 18000 20000 22000 24000 26000 h Select the yH value that gives the best null signal The exact yH field is 1 360 pulse width Substitute the t pwr value that gives the desired yH field for the value of sat pwr in step 2d 4 With the t pwr that gives the desired yH field substituted for the sat pwr move the cursor near the water peak andenternl r1 4 8p movetof dof tof Enter ga to acquire the spectrum Measure the width of the suppressed water peak at the height of the phenylalanine multiplet near 4 ppm 5 Write the results for each probe on the forms provided in Consoles and Magnets Custom Specifications Form page 81 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 55 Chapter 2 Console and Magnet Test Procedures 56 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 Chapter 3 Consoles and Magnets Specifications Sections in this chapter 3 Specifications for AutoTest this page 3 2 Specifications for Manual Console Tests page 60 3 3 Contracted Custom Console Specifications page 67 Each section contains the published specifications for NTYTNOVA consoles and magnets Chapter
98. st Library display after entering the macro autotest or by using a menu calling this macro The macro names are not shown in the display checkboxes are displayed next to the test description New tests may be added to the at tests file by specifying a group title use the Label keyword as the first word on the line followed by a descriptive phrase Specify a macro name and then a test description one per line at groups file The at groups file file defines test packages that have been assembled for convenience Each package has a line that gives a description in double quotes followed by a list of macros to be used in the order of acquisition There are no restrictions on the placement of these macros in the text file only the order matters When the next double quoted entry appears a new group is set The AutoTest interface display shows these packages as checkbox entries in the Configuration display Selection of one or more of these causes their execution in the order of selection once the Begin Test button is selected When this happens the at selected tests file is fixed Selection of the All Tests checkbox disables all the other selections because they will be done as part of the All Tests run Users may add new packages to the Configuration display list by adding appropriate lines totheat groups file in the same format at selected tests Theat selected tests file contains the names of the macros to be run as part of the
99. stabilize at 20 C for at least 10 minutes after the VT controller has reached the final temperature and regulated Enter ga to acquire a spectrum Repeat step 3 above and record the two temperatures 7 Enter temp 80 su to change the temperature to 80 C Allow the sample to stabilize at 80 C for at least 10 minutes after the VT controller has reached the final temperature and regulated Enter ga to acquire a spectrum Repeat step 3 above and record the two temperatures 8 After finishing the low temperature test enter temp n su to turn off the temperature regulation While keeping the dry nitrogen gas flowing to the probe and upper barrel remove the polystyrene VT dewar containing liquid nitrogen The flow of dry nitrogen gas to the probe will prevent condensation inside the probe Allow the dry nitrogen gas to flow through the probe and upper barrel for at least 15 minutes while the probe warms up to room temperature 9 Plota graph of the VT controller reading horizontal axis as compared with the calculated VT reading from the chemical shift differences between the two peaks vertical axis Draw a straight line through the points Stability Calibration for High Stability VT Accessory This test is for high stability VT units only Part No 00 992953 00 It demonstrates that the VT unit can hold the temperature within 0 1 C The test requires preconditioning of the laboratory air and applies restrictions on the room temperatu
100. sts this section describes some of the macros used by AutoTest These macros are in vnmr maclib maclib autotest ATglobal Macro The ATglobal macro is run when the AutoTest program begins The macro checks for the existence of autotest parameters in the user file vnmrsys global These parameters are used to store calibrations and results that are used by autotest macros If the parameters are not present ATglobal creates them Otherwise the parameters are left unchanged A partial list of these parameters is given in Table 2 ATstart Macro The ATstart macro is run after the Begin Test button is selected in the Configuration display The macro sets the global parameters to reflect the current state of the hardware and aborts under certain circumstances such as if requested tests are not compatible with the current hardware settings Messages are displayed indicating the source of the problem The reports are initialized with relevant information and the ATnext macro is executed ATnext Macro The ATnext macro checks the at selected tests file and copies the first entry into the global parameter at cur smacro deletes the top line in at selected tests 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 19 Chapter 1 Installation Tests and Demonstrations Table 2 Selected Parameters Created by ATglobal Parameter Contains at currenttest Name under which the FID is stored autotestdir Full path o
101. sturbances Console and Probe Demonstration The console and probe demonstration includes the following items Loading programs and operating the streaming magnetic tape unit Experiment setup including mounting the probe in the magnet Basic instrument operation to obtain typical spectra including probe tuning magnet homogeneity shimming and printer plotter operation Demonstration of broadband operation Demonstration of homonuclear and heteronuclear decoupling Formal training in the operation and maintenance of the spectrometer is conducted by Varian NMR Systems at periodically scheduled training seminars held in most Varian Application Laboratories On site training is available in some geographic locations Contact your sales representative for further information on availability and pricing for these courses UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 1 6 General Acceptance Testing Requirements To make the system demonstration most beneficial the customer should review Varian and OEM manuals before viewing the demonstration 1 6 General Acceptance Testing Requirements Each Varian UNTYTNOVA spectrometer is designed to provide high resolution performance when operated in an environment as specified in the NTYTVOVA NMR Spectrometer Systems Installation Planning Guide Unless both the specific requirements of this manual and the general requirements specified in the UNTYTNOVA Instal
102. sults of a previous AutoTest run rename the history and data directories For further information refer to the manual System Administration Running AutoTest To run AutoTest you enter values and make selection in the AutoTest window and then select the Begin Test button Be sure to press the Return key after entering each value 1 Enter the macro autotest The AutoTest window opens similar to Figure 4 2 Select the Configuration tab at the top of the window if not already selected 3 Fill in the fields for the Operator Name Console type etc at the top of the window In the pw90 field enter an approximate IH pw90 for the value of tpwr that you entered 10 us is recommended 38 UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 2 1 Automated Test Procedures Running AutoTest Auto Test E s E z E E 5 s z e E E E Figure 4 AutoTest Program 4 Selectthe options desired in the checkboxes in the middle and lower part of the window A full AutoTest run including all available options must be run before any single test or partial set of tests is specified Most of these tests rely on calibrations that are performed as part of the full AutoTest run This option is specified by the All Tests checkbox 5 Click the Begin Test button at bottom of the window to start the test s AutoTest begins The total time for the test s depends on the test s specified
103. t observe is recommended Basic Specifications The quartet shows a single peak with no remaining evidence of splitting 62 UNITY NOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 3 2 Specifications for Manual Console Tests Variable Temperature Operation For basic variable temperature VT accessories Varian Part No 00 992957 00 demonstrate that the VT unit and probe go to the desired temperature as registered on the window of the VT controller If the system is equipped with a VT unit the system user should read through the VT operation instructions before the demonstration Dry nitrogen is required as the VT gas if the requested temperature is over 100 C or below 10 C Otherwise air can be used For temperatures below 40 C dry nitrogen gas is recommended for cooling the bearing spinner and decoupler This prevents moisture condensation in the probe and spinner housing CAUTION The use of air as the VT gas for temperatures above 100 C is not recommended Such use destructively oxidizes the heater element and the thermocouple CAUTION Extreme temperatures can damage the probe The high and low temperature must be within the specified range of the probe Demonstration Limitations If dry nitrogen gas and liquid nitrogen are not available at the time of installation the range of VT demonstration is limited to temperatures between 30 C and 100 C Sample Insert an empty sample tube with spinner i
104. test macro or a menu calling this macro Tests Performed by AutoTest This section provides an outline of the tests run by AutoTest A full description of each test is provided in AutoTest Automated Instrument Testing page 15 Automated Console Acceptance Tests AutoTest performs the following automated console acceptance tests 90 pulse stability channel 1 and channel 2 30 amplitude stability channel 1 and channel 2 Pulse turnon time channel 1 and channel 2 Phase cycle cancellation 2 scan test is run as demonstration no specification is set Quadrature image 1 scan and 4 scans 40 UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 2 1 Automated Test Procedures Running AutoTest Frequency shifted quadrature image 1 scan Phase stability test 13 test channel 1 and channel 2 Attenuator test channel 1 and channel 2 Full power correlation coefficient and standard deviation standard deviation is provided for reference no specification is set Reduced power correlation coefficient and standard deviation Modulator linearity channel 1 and channel 2 tpwr 40 standard deviation tpwr 16 standard deviation Temperature increase in spinlock test Lock power test correlation coefficient Lock gain test correlation coefficient Variable temperature test Automated Console Acceptance Tests Using Shaped RF AutoTest performs the following automated acceptance tests with sha
105. tests documentation 14 acceptance tests objectives 11 automated console acceptance tests using shaped rf 41 automated console tests 21 automated decoupling performance tests 23 automated tests with shaped rf 23 automatic teller machine ATM cards caution 9 AutoTest 13C 90 degree Pulse Width Calibration 31 13C test descriptions 30 CPMG 12 32 creating probe specific files 40 directory structure 16 experiment details 24 gradient tests descriptions 31 macros 19 other test descriptions 33 RF performance test descriptions nonshaped channels 1 and 2 24 sample requirement 38 saving data and FID files from previous runs 39 standard tests 21 B basic system operation 12 broadband operation 12 C cautions defined 7 computer audit 11 computer audit form 73 console acceptance demonstration tests 42 console acceptance tests 37 console acceptance tests using AutoTest 40 console demonstration 12 console demonstration tests 24 credit cards caution 9 cryogenics handling procedures 12 D decoupling 12 demonstrate console operation 42 demonstration of system 12 demonstration of the system 12 01 999120 00 B0800 Index E ethylene glycol 48 experiment setup 12 F flammable gases warning 8 flowmeters 12 G gradient calibrations and performance tests 23 H H1sn test file 43 Hahn echo 43 helium contact with body 8 helium gas flowmeters caution 10 heteronuclear de
106. the data Enter ds 1 aphO dssh to phase and display the spectra To plot the spectra and acquisition parameters enter pap pl all page UNITYINOVA Acceptance Tests Procedures and Specifications 01 999120 00 B0800 2 2 Manual Test Procedures Required to Demonstrate Console Operation WALTZ H Decoupling High Performance RF Waveform Generator Sample Doped 40 p dioxane in benzene dg Part No Sample Tube 00 968120 91 5 mm 00 968123 91 10 mm Probe and Hardware Requirements A 5 mm or 10 mm broadband observe H decouple probe is recommended i e 5 mm or 10 mm broadband probes 5 mm switchable probes or 4 nucleus Autoenmr probes This test requires the presence of waveform generator boards This test also requires the results from the yH calibration that gives a dpwr of 1 watt at the probe Test Procedure If you completed the previous test WALTZ 1H Decoupling Preprogrammed Phase Modulation page 46 skip to step 5 in the following procedure 1 Enter rtp vnmr tests gamah2 su to retrieve the test parameter set to the current experiment 2 Check that the appropriate quarter wavelength cable for 5C is installed and the probe is tuned 3 Setpw to the 13C 90 pulse width and tpwr to the power used to achieve the 13c 90 pulse width 4 Set dm nny dpwr 30 d1 10 for the doped ASTM or d1 30 for the dioxane deuterobenzene sample and enter ga to acquire the spectra Each spectrum shows a triplet
107. tral plots and most parameter set printouts These files explain the purpose of the test history Directory The vnmrsys autotest history directory contains text files that record the values determined in AutoTest runs They are generated automatically by the ATrecord macro which is used in any AutoTest macro that obtains a numerical result from an NMR experiment Each result is written on a new line and is date stamped Tests that have a Varian specification listed in this manual will be denoted as having passed or failed Ifthe history file has more than one result per line any one failure will cause a fail result for the whole line When the history file is viewed using the History display after using the macro autotest failure is indicated by a red data point in graphical output and a colored entry in the text output 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 17 Chapter 1 Installation Tests and Demonstrations 18 atdb Directory The vnmrsys autotest atdb directory contains mainly the following text files used by the Auto Test program to create the AutoTest interface at tests file Theat tests file file defines all the tests that AutoTest can perform Tests are specified by a macro name and description Normally these are grouped and separated by a line starting with Label The word following will be displayed as a heading for a group of tests The test descriptions are displayed in the Te
108. uired The arrayed 2 pulse spectra and the single pulse spectrum are plotted with the single pulse spectrum last This last spectrum serves as a reference The phase shift should be accomplished in 100 ns or less Purpose This test exercises the phase shift hardware by finding the time needed to perform a 180 phase shift The pulse sequence is a version of jump and return in which two 1 Lis pulses are executed just 20 us apart Ideally because the second pulse has a 180 phase shift with respect to the first pulse there should be no excitation By varying the time before the second pulse at which the phase shift is done from 0 to 20 us an estimate of the phase switch and settling time can be made The last spectrum is that from just a single 1 us pulse and serves as a reference This phase shift should be accomplished in 100 ns or less RF Homogeneity 1H RF Homogeneity Experiment One hundred experiments are run in which the pulse width is incremented from 1 to 100 us The spectra are plotted in a horizontal stack in phased mode and sufficiently expanded so that the base of the water can be examined using the same phase settings for each spectrum use channel 1 13C RF Homogeneity Experiment In the pulse sequence delay pw90 1H delay 1 2JCH pw 13C the pw 13C is varied from 0 to a flip angle greater than 900 while observing the 13c coupled protons The 0 flip angle spectrum is adjusted to full scale and the dat
109. upling Preprogrammed Phase Modulation Sample Doped 40 p dioxane in benzene dg Part No Sample Tube 00 968120 91 5 mm 00 968123 91 10 mm Probe and Hardware Requirements A 5 mm or 10 mm broadband observe H decouple probe is recommended i e 5 mm or 10 mm broadband probes 5 mm switchable probes or 4 nucleus Autoenmr probes This test requires the results from the yH calibration that gives a dpwr of 1 watt at the probe Test Procedure 1 Enter rtp vnmr tests gamah2 su toretrieve the test parameter set to the current experiment Check that the appropriate quarter wavelength cable for a is installed and the probe is tuned Set pw to the 13C 90 pulse width value and tpwr to the power value used to achieve the C 90 pulse width Enter dmm nny dpwr 30 d1 10 for the doped ASTM or d1 30 for the dioxane deuterobenzene sample and ga to acquire the spectra Each spectrum shows a triplet Using two cursors measure the distance in Hz between the center peak and one of the outer peak Use the same outer peak either the one on the right or the one on the left for the measurements for both spectra The two measurements in Hz are used as input for the h2cal command which calculates the YH for a given decoupler power level Enter h2ca1 to calculate yH Record the result Set dmf to the 4 yH value Set dmm w 1b 1 and enter the command array dof 9 2000 500 to set up the experiment Enter ga to acquire
110. uracy waveform generator gaussian profile RFamplitude predictability using a gaussian pulse Amplitude scaling of shaped pulses using a gaussian pulse RF excitation predictability using a variety of shaped pulses Details of AutoTest Experiments This section provides descriptions of the experiments performed by AutoTest All units of the rf system transmitters linear modulators rf attenuators amplifiers receivers and probes must be in the standard configuration when AutoTest is run If the system configuration has been changed it must be returned to the standard configuration before running AutoTest for acceptance testing All data is stored and both plots and statistical analyses are provided as part of the acceptance testing Plots and statistical analyses are made concurrently with acquisition RF Performance Test Nonshaped Channels 1 and 2 Pulse Stability Experiment A single scan pulse experiment is repeated 20 times and the spectra plotted in a horizontal stack The average peak amplitude and rms deviation are measured and reported This test is run for the following 90 flip pulses e 30 flip pulses e usec pulses Purpose of 90 Pulse Stability Modern experiments require very high pulse reproducibility to minimize cancellation residuals and T noise in 2D experiments This test checks amplitude reproducibility by comparing a series of spectra obtained with the signal UNITYINOVA Acceptance Tests
111. ussian 13 Phase Error Experiment The rf 13 test is repeated using a gaussian pulse at the same peak power as in the phase stability test The data are plotted in a horizontal stack with the on resonance spectrum at full scale Purpose The rf 13 test can be done using shaped pulses In this case a gaussian pulse is used at high peak power Gaussian SLP 13 Phase Error Phase Ramped Gaussian Pulses Experiment This 13 test is repeated using a phase ramped gaussian pulses The rf carrier should be 37 Hz off resonance from water but the center of excitation of the gaussian phase ramped pulses should be 1000 Hz from the carrier The amplitude of the gaussian pulses is set high enough to exert a 90 pulse on the water Purpose The 13 test can be done using phase modulated pulses These types of pulses provide single or multiple frequency selective excitation through the use of both amplitude and phase modulation 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 29 Chapter 1 Installation Tests and Demonstrations 30 Shaped Pulse Settability Experiment Single pulse single scan spectra are collected The rf power is dropped in eight successive spectra by 3 dB each time and the pulse width increased so that a 90 flip angle is maintained The spectra are plotted in a horizontal stack for easy amplitude comparison Purpose An rf attenuator should permit accurate power control In thi
112. ust be changed to the value of the 90 pulse found in the pulse width test on the same probe For all direct observe pulse width tests an appropriate array of pw values must be entered to determine the 180 pulse The 180 pulse is the first non zero pulse that gives minimum intensity of the spectrum The 180 pulse is usually determined by interpolation between a value that gives a positive signal and a value that gives a negative signal The 90 pulse width is one half the 180 pulse Signal to noise S N is measured by the computer as follows S N maximum amplitude of peak 2 x root mean square of noise region 01 999120 00 B0800 UNITY NOVA Acceptance Tests Procedures and Specifications 13 Chapter 1 Installation Tests and Demonstrations Lineshape should be measured with the aid of the system software The properly scaled spectra should also be plotted and retained Software determination of lineshape Display and expand the desired peak b Enter nm then de for drift correction to ensure a flat baseline Set vs 10000 Press F7 until Thresh is displayed on axis 2 Press the F2 key to display the horizontal threshold cursor Set th 55 the 0 55 level c Press the F1 key to display two vertical cursors and align them on the intersections of the horizontal cursor and the peak Enter delta to see the difference in Hz between the cursors d Set th 11 the 0 11 level and repeat the first three steps Det
113. y emissions may also pose a danger to some individuals The rf emission levels from Varian NMR equipment have been measured and compared to the IEEE ANSI C95 1 1991 standard For further information refer to the RF Environment section of the Installation Planning Guide Warning Signs Varian provides signs to help customers meet this posting responsibility These signs must be posted according to the following requirements before the magnet is energized 1 10 gauss warning signs Figure 1 Post along the 10 gauss perimeter of the magnet so that a sign can be easily seen by any person about to enter the 10 gauss field from any direction Refer to the manuals supplied with the magnet for the size of a typical 10 gauss stray field Check this gauss level after the magnet is installed Note that the stray field may extend vertically to adjacent floors and additional signs may be needed there A sign is not required if the 10 gauss field extends less than 30 cm 12 in beyond a permanent wall or less than 61 cm 24 in beyond the floor above the magnet 2 5 gauss warning signs Figure 2 Post along the 5 gauss perimeter of the magnet so that a sign can be easily seen by any person about to enter the 5 gauss field from any direction Refer to the manuals supplied with the magnet for the size of a typical 5 gauss stray field Check this gauss level after the magnet is installed Note that the stray field may extend vertically to adjacent flo

UNITYINOVA Acceptance Tests & Specifications

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UNITYINOVA Acceptance Tests &amp; Specifications

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UNITYINOVA Acceptance Tests & Specifications