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MERCURY Acceptance Test Procedures and Specifications

1. A LS RE E EE T EE er 3800 3600 3400 3200 3000 2800 2600 2400 2200 2000 Hz Benzene peak Quartet Figure 8 H sensitivity measurement 44 MERCURY Acceptance Test Procedures and Specifications 67 192327 00 E0997 2 5 Sensitivity Procedures 19F Sensitivity Sample Sample Tube Test Sample Sample Part No mm 5 0 05 trifluorotoluene in benzene de 00 968120 82 Procedure 1 Ifyou just finished the 90 pulse width calibration enter pw pw90 f full nm and skip to step 5 2 Enter rtp vnmr tests F19sn su 3 If you completed the 90 pulse width calibration usingGLIDE enter the following getparam tpwr tpwr getparam pw90 pw 4 Tune the probe 5 Enter 1b 1 6 ga to acquire the spectrum The spectrum is a single line 6 Choose a 200 Hz noise region with the cursors then enter the command dsn to determine the signal to noise ratio 7 Retune the probe to H for the next test 8 Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 45 Chapter 2 Liquids Probes Test Procedures 46 31P Sensitivity Samples Sample Tube Test Sample Sample Part No mm 5 0 0485 M triphenylphosphate in CDCl 00 968120 87 10 0 0485 M triphenylphosphate in CDC 00 968123 87 Procedure 1 Make sure the appropriate quarter wavelength cable is installed 2 If you just
2. MERCURY Acceptance Test Procedures and Specifications 0997 ap ms VARIAN MERCURY Acceptance Test Procedures and Specifications MERCURY NMR Spectrometer Systems Pub No 87 192327 00 Rev E0997 Revision history A1196 Initial release A1296 Minor update B0397 Added ECO 7670 3 13 97 C0497 Added ECO 70394 4 16 97 D0697 Added ECO 70468 6 3 97 D0797 Added svs commands to save solvent shims clarified procedures E0997 Updated for VNMR 6 1 Applicability of manual Acceptance Test Procedures and Specifications for MERCURY NMR Spectrometer Systems Technical contributors Frits Vosman Rob Rice Technical writer Dan Steele Technical editor James Welch Copyright 1997 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 reserves the right to make changes in any products herein to improve reliability function or design Varian does not assume any liability arising out of the application or use of any product or circ
3. 105 1 4 mm 40 uL IH Nano Available by request 68 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 4 4 Variable Temperature Range Specifications 4 4 Variable Temperature Range Specifications Table 15 broadband systems and Table 16 4 nucleus systems list the variable temperature VT acceptance tests specifications for Varian liquids probes Probes are categorized by frequency and specifications are listed under the appropriate nucleus About VT Range Specifications Acceptance test specifications are achieved using the procedure in Variable Temperature Operation Optional on page 57 To achieve the VT range specifications the probe is tested empty Table 15 VT range specifications for broadband systems Probes VT Range C 200 MHz 5 mm N 3 P Broadband 150 to 200 10 mm N 3 P Broadband 150 to 200 5 mm H 9F N 3 P Switchable 150 to 200 300 MHz 5 mm H F 3C P AutoSwitchable PFG 20 to 80 10 mm N 3 P Broadband 150 to 200 5 mm H 5N 3 P Indirect Detection 100 to 100 5 mm H N 3 P Indirect Detection PFG 0 to 50 4 mm 40 uL Nano Room temperature 5 mm H 9F N 3 P Switchable Broadband 100 to 160 400 MHz 5 mm H F 3C 7 P AutoSwitchable PFG Available by request 10 mm N 3 P Broadband 150 to 200 5 mm H N 3 P Indirect Detection 100 to 100 5 mm 1H 15N 31P Indirect Detection PFG 0 to 50 4 mm 40 uL Nano Ro
4. D lines are fully relaxed wait at least 8 minutes between acquisitions 6 The signal of interest is the highest line of the CgDg triplet left side of display as shown in Figure 9 Use the cursors to select a 1400 Hz wide noise region between the CgD and dioxane peaks 7 Enter dsn The computer calculates the signal to noise ratio 8 Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 9 After the specifications are met do the following e Write down the values for z0 Lockpower and lockgain as they appear in the Acqi window Use the forms provided in Liquids Probes Test Results on page 83 Save the shims by entering the following command in the VNMR input window svs c6d6 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 47 Chapter 2 Liquids Probes Test Procedures Benzene dg Dioxane cee ee he Le ot I ee et ee a 14000 13000 12000 11000 10000 9000 8000 7000 Hz Figure 9 1 C Sensitivity 48 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 5 Sensitivity Procedures 29Si Sensitivity Only 4 Nucleus Probes with 2 Si This test is for broadband systems only Sample Sample Tube mm Test Sample Sample Part No 5 25 hexamethyldisiloxane in benzene d 00 968 120 98 Procedure 1 Make sure the appropriate quarter wavelength cable is installed Enter rtp vnmr tests Si2
5. Variable Temperature Operation Optional Magnet Drift Test Varian Representative Date Customer Representative Date 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 87 Chapter 5 Acceptance Test Results 88 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 Numerics 13C observe 90 pulse width test 29 13C resolution test 24 Bo sensitivity test 47 ISN sensitivity test 50 180 pulse 14 IH lineshape test 21 H observe 90 pulse width test 26 TH spinning sidebands test 23 31p sensitivity test 46 90 pulse 14 A acceptance test specifications overview 11 acceptance tests documentation 14 acceptance tests objectives 11 acetone shim file 51 APT demonstration 55 Attached Proton Test 55 Autolock 52 Autoshim 52 B basic system operation 13 broadband operation 13 C Cl3res file 24 c6d6 shim file 51 cdcl3 shim file 51 computer audit form 12 77 console demonstration 12 cryogenics handling procedures 12 D decoupling 13 demonstration of system 12 DEPT demonstration 55 Distortionless Enhancement by Polarization Transfer 55 dpwr parameter 56 drift specifications for magnets 71 E experiment setup 13 F floor vibration 21 flowmeters 12 G YH2 specifications 65 yH2 spectra 29 YH2 test procedure 29 GLIDE 51 52 87 192327 00 E0997 Index GLIDE operation demonstration 54 H Hl1lshp test file 2
6. 5 mm probes is typically 3 6 spinning and is not demonstrated at installation Samples for Resolution and Lineshape Tests Table 3 lists the samples used to achieve the H resolution and lineshape specifications Table 4 lists the samples used to achieve 13C resolution and lineshape specifications The 4 mm sample tube has a 4 mm outside diameter O D and a 40 uL sample volume Table 3 Samples for H resolution lineshape and spinning sidebands tests Sample Tube Sample Part Amplitude Level mm Test Sample No 50 0 0 55 0 11 5 20 chloroform in acetone d 00 968 120 76 50 0 0 55 0 11 5 5 chloroform in acetone d 00 968 120 99 50 0 0 55 0 11 4 5 chloroform in acetone d4 00 993 143 99 50 0 0 55 0 11 5 1 chloroform in acetone dg 00 968 120 89 Table 4 Samples for 13C resolution lineshape and spinning sidebands tests Sample Tube Sample Part Amplitude Level mm Test Sample No 50 0 0 55 0 11 5 40 p dioxane in benzene d4 ASTM 00 968 120 69 50 0 0 55 0 11 10 40 p dioxane in benzene dg ASTM 00 968 123 69 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 4 1 Resolution Lineshape Spinning Sidebands Specifications Table 5 Resolution and lineshape specifications for broadband systems Resolution and Linewidth Probe Hz 200 MHz 1H Spinning 13C Spinning 5 mm N 3 P Broadband 0 2 10 mm N P Broadband 0 2 5 mm H F 5N 3 P S
7. No Shipment Damage Spectrometer type Console S N Magnet S N Preinstallation Preparation Line voltage measured Vac console Line pressure air Air conditioning accessory No Cryogens liters LHe 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 LN Software Object Code License Agreement acceptance of product constitutes acceptance ___ of object code license regardless of whether agreement 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 using GLIDE _ Using GLIDE for basic operation to obtain typical H and C spectra ___ Demonstration of APT and DEPT spectra ___ Demonstration of optional homonuclear and heteronuclear decoupling 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Speci
8. Procedure To perform the SN or X nucleus 90 pulse width calibration in the indirect mode use the HMQC pulse sequence 1 Make sure the appropriate quarter wavelength cable and probe tuning rod are installed 2 Insert the sample Tune the probe on this sample 3 Enter rtp vnmr tests H1sn to retrieve the parameters from the IH sensitivity measurement 4 Set pw and tpwr to the values determined for the H sensitivity procedure you can get these values from the probe calibration file by entering getparam tpwr tpwr getparam pw90 pw 5 Set gain 10 dn N15 d1 5 and enter ga 6 Place two cursors around the region with the peaks Enter move sw to narrow the spectral width 7 Determine the 90 pulse width by arraying pw to 2360 pulse width The the macro array to set up the array As the macro displays the following prompts type in the response shown in bold parameter to be arrayed pw number of steps in the array 25 starting increment 2 array increment 2 In the above example the experiment is set up to array the pw from 2 pis to 52 us in 2 us increments If the 90 pulse width is 10us the 450 pulse width corresponds to pw 50 us 5 pw90 8 Enter ga to start the acquisition After the last spectrum is finished type ds 5 vp 50 to display the fifth spectrum Type aph to phase the spectrum then type ai dssh to display the arrayed spectra 9 Set pw equal to the 90 pulse width you have determined Ether
9. Specifications 61 Chapter 4 Liquids Probes Specifications 4 1 Resolution Lineshape Spinning Sidebands 62 Specifications Resolution and lineshape specifications are listed in Table 5 for broadband systems or in Table 6 for 4 nucleus systems Probes are categorized by frequency and specifications are listed under the appropriate nucleus Table 7 broadband systems and Table 8 4 nucleus systems list the spinning sidebands acceptance test specifications for Varian liquids probes Probes are categorized by frequency and specifications are listed under the appropriate nucleus About Resolution and Lineshape Specifications All resolution lineshape and spinning sidebands values of Varian probes should be less than or equal to the values listed in the table Acceptance test specifications are achieved using the procedures in Resolution Lineshape and Spinning Sidebands Procedures on page 20 Blank spaces shown as in the specifications column indicate that Varian does not specify a value or that it is not applicable to specify a value Linewidths for resolution and lineshape are in units of Hz at the 50 0 55 and 0 11 amplitude levels The H natural lineshape and linewidth of chloroform at high field have a contribution from the spread in chemical shift of 35C1 and CI isotopomers see Anet and Kopelevich J Am Chem Soc 109 5870 1987 Lineshape for 5C at the 0 55 and 0 11 amplitude levels with
10. as registered on the window of the VT controller If the system is equipped with a VT unit you should read through the VT operation instructions before this 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 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 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 No sample is used Probe and Hardware Requirements Any variable temperature probe is used Basic Specifications The specifications for variable temperature ranges are listed with each probe in the liquids probes chapter of the NMR Probes Installation Manual Procedure 1 Inthe CONFIG window make sure VT Controller is set to Present Alternatively enter vtt ype to check that vtt ype 2 2 Set N gas flow to 9 5 to 10 0 LPM for temperatures below 100 C increase N flow to 12 LPM 3 Enter a value for temp then enter su For values below room temperature the heat exchanger must be in place Maintain the tempera
11. as the H lineshape test Use the spectra and parameter set from the lineshape test Plot the spectrum again using a large enough value of wp to show all the spinning sidebands Measure spinning sideband amplitudes as a percentage of the main peak Spinning sidebands occur at frequency intervals on either side of the central peak equal to the spinning rate The sidebands might not be split The standard test requires nt 4 If the sidebands meet specifications at nt 4 repeating the test at nt 16 is not necessary Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 23 Chapter 2 Liquids Probes Test Procedures 24 13C Resolution Test Samples Amplitude Level Sample Test Sample Part No mplitude Lev Tube mm e p art No 50 0 0 55 0 11 5 40 p dioxane in benzene dg 00 968 120 69 ASTM 50 0 0 55 0 11 10 40 p dioxane in benzene d 00 968 123 69 ASTM Procedure 1 Enter rtp vnmr tests Cl3res su 2 Tune the probe 3 Set nt 4 and 1b n Set the decoupler modulation to dmm c and d1 60 4 Set the sample spinning rate at 20 5 Hz 5 Enter ga to acquire the spectrum Plot the spectrum using wp 50 and use dres to determine the linewidth at 50 of the decoupled peak 6 If decoupling is not complete run a proton spectrum and set the cursor at the center of the single peak Ente
12. comply with these precautions The following warning and caution illustrate the style used in Varian manuals for safety precaution notices and explain when each type is used WARNING Warningsare used when failure to observe instructions or precautions could result in injury or death to humans or animals or significant property damage CAUTION Cautions are used when failure to observe instructions could result in permanent damage to equipment or data WARNINGS Cardiac pacemaker and metal prosthetics wearers must remain more than 2 8 meters 9 feet from the magnet system until safety is clearly established The MERCURY magnet system generates strong magnetic and electromagnetic fields that can affect operation of some cardiac pacemakers or harm a metal prosthesis 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 always notify their physician and discuss the health risks of being in proximity to magnetic fields Wearers of metal prosthetics should contact their physician to determine if a danger exists The following table may help determine the effect of a system on pacemakers or a metal prosthesis The table shows the radial 1 e horizontal and axial vertical extent of the 5 gauss level stray magnetic field as measured from the magnet center Proton Frequency Bore Radial Extent Axia
13. finished the 90 pulse width calibration enter pw pw90 f full nm and skip to step 5 Enter rtp vnmr tests P31sn su 4 Ifyou completed the 90 pulse width calibration usingGLIDE enter the following getparam tpwr tpwr getparam pw90 pw 5 Tune the probe 6 Enter ga to acquire the spectrum The spectrum is a single line 7 Set vp 50 and adjust vs so that the peak covers about half the screen 8 For noise measurement locate the cursor in a representative 2000 Hz region 9 Enter dsn The computer measures the signal to noise ratio 10 Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 5 Sensitivity Procedures 13 Sensitivity Samples Sample Lube Test Sample Sample Part No mm 5 40 p dioxane in benzene dg ASTM 00 968 120 69 10 40 p dioxane in benzene dg ASTM 00 968 123 69 Procedure The specification for the FE lineshape test must be met before performing this test For this test you must recall parameters because the SE pw90 test leaves pp calibration parameters 1 Make sure the appropriate quarter wavelength cable is installed 2 Enter rtp vnmr tests C13sn su 3 If you completed the 90 pulse width calibration usingGLIDE enter the following getparam tpwr tpwr getparam pw90 pw 4 Tune the probe 5 Enter nt 1 ga to acquire the spectrum To ensure that C
14. for each probe in the forms provided in Liquids Probes Test Results on page 83 8 After the specifications are met do the following e Write down the values for z0 Llockpower and lockgain as they appear in the Acqi window Use the forms provided in Liquids Probes Test Results on page 83 Save the shims by entering the following command in the VNMR input window svs acetone CHCl peak 18C satellite 18C satellite e 0 55 j lt lt 0 11 140 120 100 80 60 40 20 0 20 40 60 80 100 120 Hz Figure 1 H lineshape spinning measurement 22 MERCURY Acceptance Test Procedures and Specifications 67 192327 00 E0997 2 3 Resolution Lineshape and Spinning Sidebands Procedures 1H Spinning Sidebands of CHCl Samples Amplitude Level 50 0 0 55 0 11 50 0 0 55 0 11 50 0 0 55 0 11 50 0 0 55 0 11 50 0 0 55 0 11 Sample Tube mm Test Sample 5 20 chloroform in acetone d6e 3 5 chloroform in acetone d 4 5 chloroform in acetone d4 5 1 chloroform in acetone dg 10 1 chloroform in acetone d Part No 00 968 120 76 00 968 120 99 00 993 143 99 00 968 120 89 00 968 123 89 Procedure The H spinning sidebands test this test and the IH lineshape test the previous test must be passed simultaneously and both tests plotted together 1 Using the appropriate CHCl sample measure the ig spinning sidebands on the same spectrum
15. ga to acquire the spectrum Enter f ds to display the spectrum 10 To perform the ISN X nucleus 90 pulse width calibration in the indirect mode using HMQC enter hmqc in the same experiment or move the parameters to a 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 39 Chapter 2 Liquids Probes Test Procedures different experiment by entering mp x y where x is the current experiment and y is the experiment to which the parameter set is to be moved 11 Set the following parameters fn 8192 ni 1 phase 1 nt 1 ss 0 spin 0 use acqi to turn the spinner off if the optional spinner hardware is not installed d1 2 and set pw to the 1H 90 pulse width determined from the previous steps tpwr to the tpwr level to give the H 90 pulse width determined from the previous steps nul1 0 j 90 tof to the tof determined from the H spectrum of the 2 benzamide N in step 6 above tn N15 dm nnn and dof from the following table 1H frequency MHz lie I5N 31p Hz Hz Hz 400 965 12000 9000 300 9000 9200 7000 12 To determine the N X nucleus 90 pulse width and rf homogeneity using the HMQC pulse sequence pwx is arrayed for a particular pwxlv1 The spectrum corresponding to the N X nucleus 90 pulse width using the HMQC pulse sequence is the maximum amplitude spectrum An array of spectra appears as shown in Figure 7 In HMQC nu11 occurs at 45 135 maximum at 90 and n ative at 180 Set
16. information Basic System Demonstration The installation engineer will also demonstrate the basic operation of the system to the laboratory staff 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 The system demonstration includes the following items Magnet Demonstration e Posting requirements for magnetic field warning signs Cryogenics handling procedures and safety precautions e Magnet refilling Flowmeters e Homogeneity disturbances Console and Probe Demonstration e Loading programs MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 1 2 General Acceptance Testing Requirements Experiment setup including installing the probe in the magnet e Basic instrument operation to obtain typical spectra including probe tuning magnet homogeneity shimming and printer plotter operation Note that Varian installation engineers are neither responsible for nor trained to run any spectra not described in the Acceptance Tests Procedures Demonstration of GLIDE H and C operation e Demonstration of GLIDE APT and DEPT experiments Demonstration of optional homonuclear decoupling Detailed specifications and circuit descriptions are not covered Formal training in the operation and maintenance of the spectrometer is conducted by Varian at peri
17. nitrogen and helium vent tubes Air that enters the magnet will contain moisture that can freeze causing blockage of the vent tubes and possibly extensive damage to the magnet Except when transferring nitrogen or helium be certain that the relief valves are secured on the vent tubes 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 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 Chapter 1 Introduction Following each installation of a Varian MERCURY NMR spectrometer system an installation engineer tests and demonstrates the instrument s operation 1 1 Overview The procedures for the acceptance tests as well as specifications are provided in this manual The forms for entering the test results are provided in Chapter 5 Acceptance Test Results beginning on page 75 The forms follow the same sequence as the tests Acceptance Tests The objectives of the acceptance tests procedures are threefold e To identify the tests to be performed during system installation e To i
18. or in Table 11 for 4 nucleus systems Probes are categorized by frequency and specifications are listed under the appropriate nucleus About 90 Pulse Width andyH Specifications All 90 pulse width and yH values of Varian probes should be less than or equal to the values listed in the table Acceptance test specifications are achieved using the procedures in the section 90 Pulse Wdth Procedures on page 25 Blank spaces shown as in the specifications column indicate that Varian does not specify a value or that it is not applicable to specify a value Asterisks in the specifications column indicate that the 90 pulse width was determined using the indirect method Refer to the probe installation manuals for the power handling capability of Varian probes About Test Samples Table 9 lists the samples used to achieve the 90 pulse width andyH specifications Note that the 4 mm sample tube is used only for Nano probes The 4 mm sample tube has a 4 mm outside diameter O D and a 40 uL sample volume Doped D 0 can be used for the H pulse width test instead of the sample specified in Table 9 Table 9 Samples for 90 pulse width andyH tests Nucleus ne le Tube Test Sample vany n ber IH 5 0 1 ethylbenzene 0 01 TMS 00 968120 70 99 89 deuterochloroform CDC13 IH 4 0 1 ethylbenzene 0 01 TMS 00 993 143 99 99 89 deuterochloroform CDCl 19 5 0 05 trifluorotoluene in benzene ds 00 968120 82 31p 5 0 0485 M tr
19. window Select Calibrate Carbon from the Experiment drop down menu You do not need to select a solvent Click the Setup button at the bottom of the Setup window Tune the probe Click on the Acquire button under Custom If you have already locked and shimmed the sample turn off autolock and autoshim Enter an appropriate value for pwmax which is listed in Table 10 and Table 11 on page 66 Click on Close at the bottom of the Acquire window Click the Go icon in the GLIDE window You should get a plot of arrayed spectra for 90 pulse width andyHp as well as arrayed spectra for pp Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 29 Chapter 2 Liquids Probes Test Procedures 29Si Observe 90 Pulse Width Oni 4 Nucleus Probes with 29Si This test is only for 4 nucleus probes with si Sample Sample Tube Sample mm Test Sample Part Number 5 25 hexamethyldisiloxane in benzene d 00 968120 98 Procedure 1 Make sure the appropriate quarter wavelength cable is installed 2 Insert the sample into the magnet 3 Enter rtp vnmr tests Si29sn su 4 Tune the probe observe channel without using the filter 5 Enter addnucleus Si29 to add an entry for 29Si to the probe calibration file 6 Setd1l 200 at 6 fn 8k sw 2k dm y dmm w 7 If you already calibrated Bg you can retr
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21. 1 hisn file 56 homogeneity settings 13 homonuclear decoupling test 56 I installation engineer 11 installation planning guide 13 L lineshape measurements 14 lineshape test 21 linewidth measurement 14 liquid nitrogen 57 loading programs 12 M magnet demonstration 12 magnet drift specifications 71 magnet drift test procedure 58 magnet refilling 12 N N15sn file 31 nitrogen gas 57 noise region 14 O observe 90 pulse width test 26 29 OEM manuals 12 P policies for acceptance test specifications 11 pp calibration spectra 29 preinstallation checklist 79 probe demonstration 12 pw parameter 14 Q quarter wavelength cable 13 R resolution test 24 rts command 13 S setlk 51 MERCURY Acceptance Test Procedures and Specifications 89 Index shim files 51 shim files moving 51 shim parameters 13 shims directory 51 shipment damage 79 Si29sn file 30 signal to noise 14 Software Object Code License Agreement 12 solvent based shims 51 spectral editing 55 spinning sidebands test 23 spinning speed 13 streaming magnetic tape unit 12 svs command 13 system demonstration 12 system documentation review 12 system installation checklist 79 T test conditions 13 test parameters 14 training seminars 13 V Varian manuals 12 vortexing 13 Ww warranty coverage 12 90 MERCURY Acceptance Test Procedures and Specifications 87 192327
22. 3 Acceptance Test Procedures Chapter 2 Liquids Probes Test Procedures ns 17 21 Howto Testa Probe ini nn R MR sonst E E OA 18 2 2 Probe Calibration Files cs cscccssccsccesccvaccvscestevscsetecvaccvacvscavaccvacevdcctecvacevacevacdvecsaeevas 19 2 3 Resolution Lineshape and Spinning Sidebands Procedures eee 20 IH Spinning Resolution and Lineshape 50 0 55 0 11 of CHCl 21 IH Spinning Sidebands of CHOC nt nn ini 23 CG ti A E E ones 24 2 4 90 Pulse Width Procedures semiseri sensenti eean ai iaia 25 IH Observe 90 Pulse Wdth en 26 19E Observe 90 Pulse With 27 31D Observe 90 Pulse Wdth cssssssssssssssssssseessseessssseeeeeeeeeeeeesessnsseseeeset 28 13C Observe 90 Pulse Wdth and YHy se 29 29Si Observe 90 Pulse Wdth Only 4 Nucleus Probes with 2 Si 30 SN Observe 90 Pulse Wdth Only 400 MHz or 4 Nuc Probes with ISN 31 13C pwx90 Pulse Width sen 32 31P pwx90 Pulse Width acts iociassacosesscissastveoocdeoseseubvedeonesioteoicsnaviotenveskowsicooots 36 DN pwx90 Pulse Width Only 400 MHz with Indirect Detection Probes 39 2 3 Sensitivity PTOCEQUTES cssccsscctscciccviccviccvaccvesvacevaccvacsstcviectacsvassvacsbesvaeevacsvaecteavaesvie 42 IH Sensitivity nn 43 VOR Sensitivity mens 45 BTP Sensitivity crise 46 OESS AA RP 47 Si Sensitivity Only 4 Nucleus Probes with FOOT ccciscvsnisivsivesseibioasiavinivies 49 IN Sensitivity Only 400 MHz or 4 Nucleus Probes with PD E 50 2 6 Configuring Solvent Based Shims and
23. 9sn su Tune the probe fe st Set dmf and dpwr from the C calibration by entering getparam dmf H1 dmf getparam dpwr H1 dpwr 5 Set tpwr and pw from the Si calibration by entering getparam tpwr tpwr getparam pw90 pw 6 Enter su 7 Enter fn 16384 dm nny ga to acquire a spectrum The spectrum is a single line 8 For noise measurement locate the cursor in a representative 500 Hz region 9 Enter dsn The computer calculates the signal to noise ratio 10 Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 49 Chapter 2 Liquids Probes Test Procedures 15N Sensitivity Only 400 MHz or 4 Nucleus Probes with N This test is performed at installation only on 400 MHz systems and broadband systems with 5 mm H 9F 3c 5N 4 nucleus probes unless explicitly agreed upon in writing as part of the customer contract Samples Sample Tube mm Test Sample Sample Part No 5 90 formamide in DMSO d6 00 968120 83 10 90 formamide in DMSO d6 00 968123 83 Procedure 1 Make sure the appropriate quarter wavelength cable and probe tuning rod are installed 2 If you just finished the 90 pulse width calibration enter pw pw90 f full and skip to step 5 Enter rtp vnmr tests N15sn su 4 Ifyou completed the 90 pulse width calibration and entered the wlues into
24. EPT experiment performs an automated DEPT analysis ADEPT which produces four spectra 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 55 Chapter 3 Console and Magnet Test Procedures 56 Homonuclear Decoupling Optional This test is only performed on systems with the homonuclear decoupling accessory installed We recommend using a 5 mm probe capable of H direct observe Samples Sample Tube Sample mm RSR Part Number 5 0 1 ethylbenzene 0 01 TMS 00 968120 70 99 89 deuterochloroform CDC1 10 0 1 ethylbenzene 0 01 TMS 00 968123 70 99 89 deuterochloroform CDCl Procedure 1 Enter rtp vnmr tests Hisn 2 Tune the probe Set nt 1 Run a normal spectrum without decoupling 3 Set dm yyy Use the cursor and sd to set the decoupler on the central line of the triplet and then run a decoupled spectrum The best values of dpwr must be found by experiment Too much power might show increased noise too little might not decouple the quartet Setting dpwr 25 is a good starting point Possible dpwr values are 0 to 49 49 is maximum power in steps of 1 0 dB 4 Observe that the quartet collapses to a single peak with no remaining evidence of splitting MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 Variable Temperature Operation Optional This optional test demonstrates that the basic variable temperature VT unit and probe changes to the desired temperature
25. IDE button in the VNMR menu Click on the Setup icon Insert the sample in the magnet using either the manual button on the magnet leg or the Insert button in the Setup window Select Calibrate Florine from the Experiment drop down menu You do not need to select a solvent Click the Setup button at the bottom of the Setup window Tune the probe Click on the Acquire button under Custom If you have already locked and shimmed the sample turn off autolock and autoshim Enter an appropriate value for pwmax which is listed in Table 10 and Table 11 on page 66 Click on Close at the bottom of the Acquire window Click the Go icon in the GLIDE window You should get a plot of arrayed spectra Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 27 Chapter 2 Liquids Probes Test Procedures 31P Observe 90 Pulse Width Samples Sample Tube Sample mm Test Sample Part Number 5 0 0485 M triphenylphosphate in CDCI3 00 968120 87 10 0 0485 M triphenylphosphate in CDCl 00 968123 87 Procedure This procedure calibrates tpwr and the 90 pulse width for P 1 2 3 4 wn 1 an 11 12 13 Make sure the appropriate quarter wavelength cable is installed Open GLIDE by clicking the GLIDE button in the VNMR menu Click on the Setup icon Insert the sample in the magnet using either the ma
26. Sensitivity Samples Sample Tube imm Test Sample Sample Part No 5 0 1 ethylbenzene 0 01 TMS 00 968120 70 99 89 deuterochloroform CDCI3 10 0 1 ethylbenzene 0 01 TMS 00 968 123 70 99 89 deuterochloroform CDCI3 4 0 1 ethylbenzene 0 01 TMS 00 993143 99 99 89 deuterochloroform CDC13 Procedure 1 If you just finished the 90 pulse width calibration enter pw pw90 f full nm and skip to step 5 2 Enter rtp vnmr tests Hisn su 3 If you completed the 90 pulse width calibration usingGLIDE enter the following getparam tpwr tpwr getparam pw90 pw 4 Tune the probe Enter nt 1 ga to acquire the spectrum 6 When the spectrum is displayed phase it and enter wp 500 to display the quartet 7 Use the cursors to locate a 200 Hz noise region to the left downfield of the quartet as shown in Figure 8 8 Enter dsn The computer calculates the signal to noise ratio 9 Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 10 After the specifications are met do the following e Write down the values for z0 Llockpower and lockgain as they appear in the Acqi window Use the forms provided in Liquids Probes Test Results on page 83 e Save the shims by entering the following command in the VNMR input window svs cdcl3 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 43 Chapter 2 Liquids Probes Test Procedures
27. Sidebands Procedures The procedures in this section demonstrate the resolution lineshape and spinning sidebands SSB specifications listed in Resolution Lineshape Spinning Sidebands Specifications on page 62 1H Spinning Resolution and Lineshape 50 0 55 0 11 of CHCI3 1H Spinning Sidebands of CHCI3 13C Resolution Test 20 MERCURY Acceptance Test Procedures and Specifications amp 7 192327 00 E0997 2 3 Resolution Lineshape and Spinning Sidebands Procedures 1H Spinning Resolution and Lineshape 50 0 55 0 11 of CHCI Samples Amplitude Level Sample Test Sample Part No mplitude Lev Tube mm K mp rt No 50 0 0 55 0 11 5 20 chloroform in acetone d 00 968120 76 50 0 0 55 0 11 5 5 chloroform in acetone d 00 968 120 99 50 0 0 55 0 11 4 5 chloroform in acetone d 00 993 143 99 50 0 0 55 0 11 5 1 chloroform in acetone d 00 968 120 89 50 0 0 55 0 11 10 1 chloroform in acetone dg 00 968 123 89 Procedure The H lineshape test this test and the ly spinning sidebands test the next test must be passed simultaneously and both tests plotted together 1 Insert the appropriate CHCl sample in the magnet and spin it 2 Enterrtp vnmr tests Hllshp nmandsetnt 1 vs 100 Enter su to set up the system hardware Tune the probe 4 Enter a value for pw appropriate for your sample If your sample is Then use the value for a 1 CHCl 00 968120 89 90 pu
28. ative signal The 90 pulse width is one half the 180 pulse Signal to noise S N is measured by the computer as follows SIN maximum amplitude of peak 2 x root mean square of noise region Lineshape should be measured digitally with the aid of the system software The properly scaled spectra should also be plotted and the plot retained Digital determination of lineshape 1 Display and expand the desired peak 2 Enter nm then dc for drift correction to ensure a flat baseline Set vs 10000 Click the menu button labeled Th to display the horizontal threshold cursor Set th 55 the 0 55 level 3 Click the menu button labeled Cursor or Box until two vertical cursors are displayed and align them on the intersections of the horizontal cursor and the peak Type delta to see the difference in Hz between the cursors 4 Set th 11 the 0 11 level and repeat Determination of lineshape from a plot 1 Use a large 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 2 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 then 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 lev
29. coupling calibration as well as how to measure yH for indirect detection 1 2 Set pwx equal to the value determined in step 14 in the previous procedure Enter ga to acquire a spectrum The spectrum should look like the second spectrum in Figure 4 with the outer two peaks of the three line pattern up and the center peak down Set dmm ccc dm nny dpwr 30 dof dof 2000 dof 2000 Then enter ga Enter ds 1 place a cursor on each of the positive peaks and write down the delta Enter ds 2 place a cursor on each of the positive peaks and write down the delta Enter h2ca1 and enter the delta values for the high field and low field coupling 34 MERCURY Acceptance Test Procedures and Specifications 67 192327 00 E0997 2 4 90 Pulse Width Procedures HMQC NT 1 PWX 0 90 DEGREES Figure 4 HMQC with and without X nucleus pulses 7 When prompted enter 151 for the coupling constant A YH of 5000 is necessary for decoupling in indirect detection If the value is not 5000 increase dpwr by 3 dB until yH is 5000 8 To store the values in the probe calibrations file enter the following commands setparams dpwr 43 C13 setparams dmf 20000 C13 Be sure to enclose the values in single quotes because they are treated as strings 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 35 Chapter 2 Liquids Probes Test Procedures 31P pwx90 Pulse Width This test is only for systems w
30. dentify the precise methods by which these tests are performed e To leave the instrument in a calibrated ready to use state The procedures are arranged by the type of specification The arrangement of the procedures does not matter although some procedures use results from other procedures and is determined by the installation engineer These procedures cover the basic specifications of the instrument signal to noise S N resolution and lineshape and are not intended to reflect the full range of operating capabilities or features of a MERCURY NMR spectrometer Performance of any additional tests beyond those described in this manual must be agreed upon in writing as part of the customer contract Acceptance Specifications All specifications are subject to change without notice The specifications published in this manual shall prevail unless negotiation or customer contract determines otherwise Refer to the text in each chapter for other conditions Request of any additional specifications beyond those listed in this manual must be agreed upon in writing as part of the customer contract The following policies are in effect at installation Specifications Policy for Probes Used in Systems other than MERCURY No guarantee is given that probes purchased for use in systems other than MERCURY will meet current specifications Testing Policy for Indirect Detection Probes used for Direct Observe Broadband Performance Probes de
31. dures GLIDE Operation Demonstration Samples Sample Tube PERN Sample imm Nucleus Test Sample Part Number 5 IH 0 1 ethylbenzene in CDCl 00 968120 70 5 IH 0 1 3 heptanone in CDCl 00 968120 93 5 BC 40 p dioxane in benzene dg ASTM 00 968120 69 5 He 10 menthol in CDCI 00 968120 94 Procedure 1 With the 3 heptanone or the ethylbenzene sample run fully automated GLIDE which should take about 5 minutes Insert the sample Click the Setup icon In the dialog box that appears select Proton 1D from the Experiment menu and then select CDCI3 from the Solvent menu Insert the sample If the Insert Eject selections are available in the Setup window click on Insert Otherwise use the button on the magnet leg Enter the relevant text in the Text field e g standard proton 1D Click the Setup button Click the Go icon in the GLIDE window You should get one spectrum displayed and plotted 2 With the menthol sample run a carbon spectrum using Customize to reset the number of scans to 16 e pu m9 me Click the Setup icon In the dialog box that appears select Carbon 1D from the Experiment menu and CDCI3 from the Solvent menu Insert the sample If the Insert Eject selections are available in the Setup window click on Insert Otherwise use the button on the magnet leg Enter the relevant text in the Text field e g custom proton 1D Click the Setup button Click the Customize icon in GLIDE Clic
32. e lock signal display should be flat Disconnect the acqi window Then disconnect the lock cable from the probe Enter in n spin n nt 1array dl 11 3600 0 a1 1 60 This will set 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 Enter ga to acquire the spectra The test takes approximately 10 to 11 hours to finish 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 Compare the frequency shift of the chloroform peak of the arrayed spectra to the frequency of the first spectrum in the array MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 ran Acceptance Test Specifications Chapter 4 Liquids Probes Specifications Chapter 4 Liquids Probes Specifications This chapter contains the following specifications for liquids probes e 4 1 Resolution Lineshape Spinning Sidebands Specifications page 62 e 4 2 90 Pulse Wdth and gH2 Specifications page 65 e 4 3 Sensitivity Specifications page 67 e 4 4 Variable Temperature Range Specifications page 69 e 4 5 Magnet Drift page 71 87 192327 00 E0997 MERCURY Acceptance Test Procedures and
33. e of the magnet and firmly attached to the upper part of the magnet The ropes must not be under tension since this could transfer building vibrations to the magnet and affect NMR spectra To calculate rope size and ceiling attachment points refer to the site installation plan for the weight and height of the magnet On 80 day hold 200 54 and 300 54 magnets ALOX only an alternative is to bolt the magnet to the floor however floor mounting can be used only if it is first confirmed that floor vibration will not interfere with the operation of the spectrometer 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 9 10 CAUTIONS Keep magnetic tapes credit cards and watches away from the magnet dewar Most personal plastic cards such as automated teller ATM and credit cards contain a strip of magnetic media that can damaged by a strong magnetic field Many wrist and pocket watches are also susceptible to damage from intense magnetism 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 Do not remove the relief valves on the vent tubes The relief valves prevent air from entering the
34. eeseeseeeseeeeeeeee 64 Spinning sidebands specifications for 4 nucleus systems 64 Samples for 90 pulse width andyH tests 0 0 eee sseeeeeeeeee sees cecee cases sessaeesarseaeeees 65 90 pulse width and yH specifications for broadband systems ou eeeeeeseeeeeeeeeeeeee 66 90 pulse width and yH specifications for 4 nucleus systems 00 eeeseeeeeeeeeeeeeeeeeee 66 Samples OF sensitivity tests ccccisscsszsessnscevscezesesndscdbelaniesssaensensosdssssnseinuecdeapsbacsedbesbaaevaane 67 Sensitivity S N specifications for broadband systems 68 Sensitivity S N specifications for 4 nucleus systems 68 VT range specifications for broadband systems ceseeeceseseessesecseceteeceseceeeeceeesaeeees 69 VT range specifications for 4 nucleus systems 2 00 0 ee eeeeeeseeseeseeseceeeeeeseeaeeeeeeesaeseeeeeee 70 Magnet Drift Sp cifications iets rires etant i than na a aE aie 71 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 SAFETY PRECAUTIONS Observe the following safety precautions during installation operation maintenance and repair of this instrument Failure to comply with these precautions or with specific warnings and cautions elsewhere violates safety standards of design manufacture and intended use of the instrument Varian assumes no liability for customer failure to
35. els the linewidth should be measured horizontally to the center of the noise For all 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 to create 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 14 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 ran Acceptance Test Procedures Chapter 2 Liquids Probes Test Procedures Chapter 3 Console and Magnet Test Procedures Chapter 2 Liquids Probes Test Procedures This chapter contains procedures for both required and optional liquids probes tests Specifications to be demonstrated are contained in Part 2 of this manual Write the results of each probe test on the forms provided in Liquids Probes Test Results on page 83 The following is a list of the sections in this chapter 2 1 How to Test a Probe page 18 e 2 2 Probe Calibration Files page 19 e 2 3 Resolution Lineshape and Spinning Sidebands Procedures page 20 e 2 4 90 Pulse Wdth Procedures page 25 e 2 5 Sensitivity Procedures page 42 e 2 6 Configuring Solvent Based Shims and set
36. em is installed or the first time a probe is used Create or change the probe calibration file as follows To Create a Probe Calibration File Do these steps for each probe that is tested 1 Loginas vnmrl 2 Enter the following command in the VNMR input window addprobe probe_name system Where probe_name is a descriptive name for the probe For example sw5mm for a 5 mm switchable probe or 4nucPFG for a 4 nucleus PFG probe The system argument makes the probe calibration files for this probe avaible to all users by placing the files in vnmr probes Without the argument the files are placed in the vnmrsys directory of the user who entered the command e g vnmrl vnmrsys probes and are only available to that user The values for power pw90 dmf and pp are initially set to O and filled in later by running the calibration procedures for H 19F 31P and BC using GLIDE To Change to a Different Probe Calibration File After the probes are tested and calibrated use this procedure to switch to the appropriate calibration file when a different probe is installed 1 Loginas vnmrl 2 Enter the following command in the VNMR input window probe probe_name Where probe_nameis the name of the directory in vnmr probes named for the new probe e g sw5mm 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 1 9 Chapter 2 Liquids Probes Test Procedures 2 3 Resolution Lineshape and Spinning
37. en saved for a 400 MHz system or with a probe with ISN Other solvents that GLIDE supports by default are D20 and CD3OD The steps below describe how to add other solvent based shims and how to move the shim files to the vnmr shims directory You must still be logged in as vnmr1 Note that starting with VNMR 6 1 the names for shim files should be all lower case 1 If you primarily use only the solvents used in the ATP Acetone CDCl3 and C6D6 skip to step 2 below If you normally use D20 or CD30D or DMSO and it wasn t used in the ATP in addition to the solvents used in the ATP set up the shim files for these solvents as follows Lock and shim on each solvent Write down the values for z0 lockpower and lockgain for each solvent These values are displayed in the Acqi window Save the shims with the svs command in the VNMR input window Use the following commands svs d2o if the solvent is DO svs cd3od if the solvent is CD30D svs dmso if the solvent is DMSO 2 Ina shell tool or a Terminal window still logged in as vnmr1 move the shim files from vnmrsys shims to vnmr shims Change to the vnmr shims directory and use the mv command to move the shim files Don t forget the dot at the end of each mv command cd vnmr shims mv vnmrsys shims acetone mv vnmrsys shims cdc13 mv vnmrsys shims c6d6 And if present mv vnmrsys shims dmso mv vnmrsys shims d2o mv vnmrsys CD30D Now go t
38. en you locked and shimmed on other solvents The example below shows some of the entries with the ZO value entered The ZO value represents the value of ZO shown in the lock display in acqi if Ssolv cdcl3 then z0 512 lockpower 37 lockgain 41 else if Ssolv d2o0 then z0 521 lockpower 37 lockgain 48 else if Ssolv acetone then z0 512 lockpower 21 lockgain 39 else if S solv dmso then lockpower 33 lockgain 36 else if Ssolv c6d6 then lockpower 20 lockgain 39 else if Ssolv cd30d then lockpower 25 lockgain 35 else lockpower 30 lockgain 40 ndif endif endif endif endif endif Note that you should have one endif for each if in the entries 4 Save the file and exit the text editor Clean up the VNMR file system as necessary 52 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 Chapter 3 Console and Magnet Test Procedures This chapter contains the procedures required to demonstrate the specifications for MERCURY consoles and magnets Below is an outline of the tests in this section e GLIDE Operation Demonstration APT and DEPT Demonstration e Homonuclear Decoupling Optional e Variable Temperature Operation Optional e Magnet Drift Test Write the results of the tests in the appropriate forms provided in Console and Magnet Test Results on page 87 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 53 Chapter 3 Console and Magnet Test Proce
39. er model Plotter model Terminal model Other peripheral Computer function NMR host Workstation running VNMR 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 Workstation running other NMR software Workstation running VNMR and other NMR software VNMR version Operating system on site or off site on site or off site Information on computer Manufacturer Computer S N Memory Mbytes of e g 3 of 3 Model no Purchased from Screen size in 78 Peripherals Internal hard disk Mbytes External hard disk Mbytes Tape drive size CD ROM drive model Printer model Plotter model Terminal model Other peripheral Computer function NMR host Workstation running VNMR Workstation running other NMR software Workstation running VNMR and other NMR software VNMR version Operating system Mercury Acceptance Test Procedures and Specifications 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 87 192327 00 E0997 5 2 System Installation Checklist Company University 5 2 System Installation Checklist Address Principal User Phone Fax Sales Order
40. erals 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 that the information on this form is accurate and that all computers to be used to run VNMR software including variants VnmrS VnmrX Vnmrl 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 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 77 Chapter 5 Acceptance Test Results Use these forms for additional computers If more forms are needed copy this page Attach all copies to the Computer Audit Information on computer Manufacturer Computer S N Memory Mbytes Peripherals Internal hard disk Mbytes External hard disk Mbytes Tape drive size CD ROM drive model Print
41. erssrsrsresrsrrrrresrsresese 69 About VT Range Specifications isisisi assasi seniisisossskse seinri 69 AI Magnet Drift brises sirinin ee oei Ea enis 71 About Magnet Drift SpeGHCANONS sssr iiis aesa 71 Acceptance Test Results Chapter 5 Acceptance Test Results 75 3 1 Computer Audit is nine intestinale iiaa 77 5 2 System Installation Checklist cece eeeeesseesseseceseceseeeeeeeeeeeeeeeeeeeeeeneeesees 79 4 35 S perc n Shim Valles sions litres iege iie siian 81 5 4 Liquids Probes Test Results ss 83 Resolution and Lineshape 50 0 55 0 11 HZ esseeseesseesseeseeeseeeeeeeees 84 Spinning SIT DANUS ccsactavisecaatcsdecazessdisdeceavsstedensnswseatevadscnstascesedoussus adhe segvesvs 84 OO Pulse MAUR scleccscscicdiestiecasustvisadesaectaecedeacezascetneatsaceadedassbbosdesensssasanenaus 84 Sensitviiy CSV IM ceits ccahodsasisessasacdecsbesnsieacceadsdeshasebodeaeiusssosotastesodonesed ease stueney 84 WRG CRIED ne Ne Et seeseestesecues 85 WT BARGE E E N 85 B EN E EA E A ne E anse 85 5 5 Console and Magnet Test Results ss 87 MONON isc neat asin RER Rene 89 4 MERCURY Acceptance Test Procedures and Specifications 67 192327 00 E0997 List of Figures Figure 1 IH lineshape spinning measurement esssessesseeseeseseetestesttersteesersesserstresresstesressesseesset 22 Figure 2 Normal IH spectrum of GBCHI E E EEE sucsosnesvecgontesucedeie eeceasesssncvsss T 33 Figure 3 pwx calibration coarse left and fine right ees
42. es with thinner walls Wilmad 5 mm sample tubes 545 PPT or equivalent Wilmad 10 mm sample tubes 513 7PPT or equivalent will increase signal to noise Blank spaces shown as in the specifications column indicate that Varian does not specify a value or that it is not applicable to specify a value If a pulse width is not provided but is needed to achieve a sensitivity acceptance test specification calibrate using the test results obtained in the factory About Test Samples Table 12 lists the samples used to achieve the sensitivity specifications Note that the 4 mm sample tube is used only for Nano probes The 4 mm sample tube has a 4 mm outside diameter O D and a 40 uL sample volume Table 12 Samples for sensitivity tests Nucleus m Ie Tube Test Sample pa H 5 0 1 ethylbenzene in CDCl 00 968 120 70 IH 4 0 1 ethylbenzene in CDCl 00 993 143 99 19 5 0 05 trifluorotoluene in benzene d 00 968120 82 31p 5 0 0485 M triphenylphosphate in CDCI 00 968120 87 as 10 0 0485 M triphenylphosphate in CDC 00 968123 87 Bc 5 40 p dioxane in benzene d ASTM 00 968 120 69 aC 10 40 p dioxane in benzene dg ASTM 00 968 123 69 ISN 5 90 formamide in DMSO d 00 968 120 83 ISN 10 90 formamide in DMSO d 00 968123 83 295 5 25 hexamethyldisiloxane in benzene d 00 968120 98 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 67 Chapter 4 Liquids Probes Specifications Table 13 Sensitivity S N specif
43. fications 79 Chapter 5 Acceptance Test Results Notes 80 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 5 3 Supercon Shim Values 5 3 Supercon Shim Values Fill in the following information for the supercon shims Magnet Frequency and Serial Number Magnet Frequency Serial Number Measurement in Helipot Amps Measurement X2 Y2 Drift Spacers Main Field Current Customer Signature Varian Representative Signature 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 81 Chapter 5 Acceptance Test Results Notes 82 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 5 4 Liquids Probes Test Results 5 4 Liquids Probes Test Results Please provide the following information about the probes and system List any special hardware or conditions below under Notes Then fill in the results on the following sheets for every test performed on each probe Probe Size Model and Serial Number Probe Size and Model Serial Number Probe 1 Probe 2 Probe 3 Probe 4 Probe 5 System Frequency 200 MHz 300 MHz 400 MHz Notes 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 83 Chapter 5 Acceptance Test Results Resolution and Lineshape 50 0 55 0 11 Hz 1H Spin 18C Spin Notes ZO lock gai
44. gnet 3 Enter rtp vnmr tests Ni5sn su 4 Tune the probe observe channel 5 Setd1l 200 at 6 fn 8k sw 2k dm y dmm w 6 If you already calibrated BC you can retrieve dpwr and dmf with the following commands getparam dpwr H1l dpwr getparam dmf H1 dmf 7 Enter ga 8 Enter ds Set vs 50 and adjust vs so that the peak occupies about half the screen 9 Seta cursor on the peak Entermovetof pw 10 20 30 40 50 60 70 80 ga 10 When the last spectrum is obtained enter dssh 11 The first null spectra is the 180 pulse therefore the 90 pulse width is one half the 180 pulse Store the tpwr used and the 90 pulse width found by entering the folloving commands in the VNMR input window setparams tpwr 58 setparams pw90 12 5 The values are treated as strings therefore they are enclosed in single quotes 12 Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 31 Chapter 2 Liquids Probes Test Procedures 13C pwx90 Pulse Width This test is only for systems with indirect detection probes Sample Sample Tube Sample mm Test Sample Part Number 5 1 iodomethane C 1 trimethylphosphite 0 2 00 968120 96 Cr acac in CDCl Procedure To perform the 13C or X nucleus 90 pulse with calibration in the indirect mode use the HMQC experiment 1 Make sure the appropriate qua
45. hloroform CDCI3 4 0 1 ethylbenzene 0 01 TMS 00 993 143 99 99 89 deuterochloroform CDCl3 Procedure This procedure calibrates t pwr and the 90 pulse width for H 1 2 3 Co ls Oy pi 10 11 12 Open GLIDE by clicking the GLIDE button in the VNMR menu Click on the Setup icon Insert the sample in the magnet using either the manual button on the magnet leg or the Insert button in the Setup window Select Calibrate Proton from the Experiment drop down menu You do not need to select a solvent Click the Setup button at the bottom of the Setup window Tune the probe Click on the Acquire button under Custom If you have already locked and shimmed the sample turn off autolock and autoshim Enter an appropriate value for pwmax which is listed in Table 10 and Table 11 on page 66 Click on Close at the bottom of the Acquire window Click the Go icon in the GLIDE window You should get a plot of arrayed spectra Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 26 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 4 90 Pulse Width Procedures 19F Observe 90 Pulse Width Sample Sample Tube Sample mm Test Sample Part Number 5 0 05 trifluorotoluene in benzene ds 00 968120 82 Procedure This procedure calibrates tpwr and the 90 pulse width for PF 1 2 3 a A MN 10 11 12 Open GLIDE by clicking the GL
46. ications for broadband systems Probe Sensitivity S N Specifications 200 MHz 1H 19F 31p RC IN 295i 5 mm N 3 P Broadband 40 1 45 1 10 mm 5N P Broadband 125 1 140 1 _ 5 mm H 9F N 3 P Switchable 40 1 40 1 40 1 40 1 300 MHz 1H 19F 3p a I5N 295i 5 mm H F 3C 7 P AutoSwitchable PFG 4 nucleus mode 105 1 105 1 70 1 80 1 switchable mode 105 1 105 1 100 1 90 1 10 mm N P Broadband 250 1 280 1 5 mm H N 3 P Indirect Detection 135 1 5 mm H 5N 3 P Indirect Detection PFG 180 1 4 mm 40 uL H Nano Available by request 5 mm H 9F N P Switchable Broadband 130 1 130 1 105 1 1051 400 MHz 1H 19F 31p tig IN 295i 5 mm H F 3C P AutoSwitchable PFG Available by request 10 mm N 3 P Broadband 350 1 450 1 45 1 5 mm H N 3 P Indirect Detection 350 1 5 mm H N P Indirect Detection PFG 350 1 4 mm 40 uL IH Nano Available by request 5 mm H 9F N 3 P Switchable 130 1 130 1 150 1 120 1 15 1 Table 14 Sensitivity S N specifications for 4 nucleus systems Probe Sensitivity S N Specifications 200 MHz 1H op 31p Be 5 mm H 3C RT Computer Switchable 30 1 35 1 5 mm H 3C VT Computer Switchable 30 1 35 1 300 MHz 1H 19F 31p e 5 mm H F 3CP P AutoSwitchable PFG 4 nucleus mode 105 1 105 1 70 1 75 1 switchable mode 105 1 105 1 100 1 90 1 5 mm H C RT Computer Switchable 60 1 70 1 5 mm H C VT Computer Switchable 130 1
47. ieve dpwr and dmf with the following commands getparan dpwr H1 dpwr getparam dmf H1 dmf 8 Enter ga 9 Enter ds Set vs 50 and adjust vs so that the peak occupies about half the screen 10 Set a cursor on the peak Enter movetof pw 10 20 30 40 50 60 70 80 ga 11 When the last spectrum is obtained enter dssh The first null spectra is the 180 pulse therefore the 90 pulse width is one half the 180 pulse 12 Store the tpwr used and the 90 pulse width found by entering the folloving commands in the VNMR input window setparams tpwr 58 setparams pw90 12 5 The values are treated as strings therefore they are enclosed in single quotes 13 Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 30 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 4 90 Pulse Width Procedures 15N Observe 90 Pulse Width Ony 400 MHz or 4 Nuc Probes with 15N This test is performed at installation on only 400 MHz systems and broadband systems with 5 mm H 9F 3C N 4 nucleus probes unless explicitly agreed upon in writing as part of the customer contract Samples Sample Tube Sample mm teats Part Number 5 90 formamide in DMSO d 00 968 120 83 10 90 formamide in DMSO d 00 968 123 83 Procedure 1 Make sure the appropriate quarter wavelength cable and probe tuning rod are installed 2 Insert the sample into the ma
48. ing magnets ALOX include removable helium vent tubes If the magnet dewar should quench sudden appearance of gasses 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 follow carefully the instructions and safety precautions given in the Oxford documentation 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 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 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 gases from the dewar To prevent tip over at least two ropes each rated at least twice the weight of a full magnet should be suspended from the ceiling on either sid
49. iphenylphosphate in CDCI 00 968120 87 ju 10 0 0485 M triphenylphosphate in CDCI 00 968123 87 BC 5 40 p dioxane in benzene d ASTM 00 968 120 69 IC indirect 5 1 iodomethane C in CDC 00 968120 96 e 10 40 p dioxane in benzene d ASTM 00 968123 69 ISN 5 90 formamide in DMSO d 00 968 120 83 ISN indirect 5 2 benzamide N in DMSO d4 00 968120 97 ISN 10 90 formamide in DMSO d 00 968 123 83 295 5 25 hexamethyldisiloxane in benzene dg 00 968120 98 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 65 Chapter 4 Liquids Probes Specifications Table 10 90 pulse width and yH specifications for broadband systems Probe 90 Pulse Width Specifications us YE 200 MHz 1H 197 3p Bc ISN 2 Hz 5 mm N 3 P Broadband 15 a 2700 10 mm N P Broadband 20 20 _ 2700 5 mm H 9F N 3 P Switchable 20 20 15 2700 300 MHz 1H 9p Hp Bc Ny si 5 mm H F 3CP P AutoSwitchable PFG 12 18 15 12 2700 10 mm 5N P Broadband _ 20 20 _ 2700 5 mm H 5N P Indirect Detection 15 18 2700 5 mm H 5N 3 P Indirect Detection PFG 10 18 2700 4 mm 40 uL H Nano Available by request 2700 5 mm H 9F N P Switchable Broadband 12 12 15 2700 400 MHz 1H 9p 3p Bc Ny si 5 mm H F 3C P AutoSwitchable PFG Available by request 10 mm N 3 P Broadband 20 _ 2700 5 mm H 5N P Indirect Detection 10 18 2700 5 mm H N 3 P Indirect Detectio
50. ipment and potentially terminate the warrantee agreements and or service contract Written authorization approved by the MERCURY product manger of Varian Inc is required to implement any changes to the hardware of the spectrometer Maintain safety features by referring service to a Varian service office 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 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 Avoid helium or nitrogen contact with any part of the body In contact with the body 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 helium or nitrogen contacts the body seek immediate medical attention especially if the skin is blistered or the eyes are affected MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 WARNINGS continued On magnets with removable quench tubes keep the tubes in place except during helium servicing Oxford 80 day hold 200 54 and 300 54 superconduct
51. ith indirect detection probes Sample Sample Tube Sample mm Te Part Number 5 1 iodomethane C 1 trimethylphosphite 00 968 120 96 0 2 Cr acac in CDCl Procedure To perform the 31P or X nucleus 90 pulse width calibration in the indirect mode use the HMQC pulse sequence 1 Make sure the appropriate quarter wavelength cable is installed 2 Insert the sample Tune the probe on this sample 3 Enter rtp vnmr tests H1sn to retrieve the parameters from the H sensitivity measurement 4 Set pwand tpwr to the values determined for the H sensitivity procedure you can get these values from the probe calibration file by entering getparam tpwr tpwr getparam pw90 pw 5 Set gain 10 dn P31 d1 5 and enter ga 6 Place two cursors around the region with the peaks Enter movesw to narrow the spectral width 7 Determine the 90 pulse width by arrayingpw to 2360 pulse width Enter the macro array to set up the array As the macro displays the prompts type in the response shown in bold parameter to be arrayed pw number of steps in the array 25 starting increment 2 array increment 2 In the above example the experiment is set up to array pw from 2 yus to 52 us in 2 us increments If the 90 pulse width is 10 us the 450 pulse width corresponds to pw 50 Us 5 pw90 8 Enter ga to start the acquisition After the last spectrum is finished enter ds 5 vp 50 to display the fifth spectrum Enter aph to phase the
52. itivity on page 46 Table 2 Test order for probes that observe 25i ISN or indirect detection Test Done 29Si Observe 90 Pulse Wdth Only 4 Nucleus Probes with 29Si on page 30 29Si Sensitivity Only 4 Nucleus Probes with 29Si on page 49 15N Observe 90 Pulse Wdth Only 400 MHz or 4 Nuc Probes with 15N on page 31 15N Sensitivity Only 400 MHz or 4 Nucleus Probes with 15N on page 50 13C pwx90 Pulse Width on page 32 31P pwx90 Pulse Width on page 36 15N pwx90 Pulse Width Only 400 MHz with Indirect Detection Probes on page 39 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 2 Probe Calibration Files 2 2 Probe Calibration Files VNMR 5 3 software includes probe calibration files in the directory vnmr probes Probe calibration files contain pw90 tpwr dmf dpwr and pwx settings for each probe used with the system GLIDE automation and manual operation using macros including h1 hcosy and dept retrieve appropriate power levels the pw90 value and the dmf value from the probe calibration file instead of using preset values in the parameters files Successful operation depends on the existence of a probe calibration file for each probe that is used with the system When the MERCURY NMR spectrometer is installed the proper probe calibration files are set up so that the system is ready to use when the installer leaves the site The probe calibration files must be created when the syst
53. k the Acquire icon in the Custom window Scroll through the list of adjustables and enter 16 for the Number of scans Click the Close button in the Acquire dialog box Click on the up arrow under the Customize icon Click the Go icon in the GLIDE window You should get one spectrum displayed and plotted 54 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 APT and DEPT Demonstration The APT Attached Proton Test and DEPT Distortionless Enhancement by Polarization Transfer spectral editing experiments give an example of the capabilities of the MERCURY system Sample Sample Size Sample mm Pest Serine Part Number 5 30 menthol in CDCL3 00 968 120 94 Procedure 1 Open GLIDE by clicking on the GLIDE button in the VNMR menu 2 Click the Setup icon 3 Insert the sample If the Insert Eject selections are available in the Setup window click on Insert Otherwise use the button on the magnet leg 4 Select APT or DEPT as follows For APT select APT in the Experiment drop down menu For DEPT select C13 and dept spectra in the Experiment drop down menu Select CDCL3 in the Solvent drop down menu Enter the relevant text in the Text field e g APT or DEPT Click the Setup button at the bottom of the Setup window 1 n wm Click the Go icon and wait until the spectra is plotted The APT spectrum should appear with three peaks upright CH2 and seven peaks inverted CH CH3 The D
54. l Extent MHz mm m m 200 54 1 50 1 50 200 long hold 54 2 20 2 80 300 54 1 64 2 05 300 long hold 54 2 20 2 80 400 54 2 20 2 80 400 long hold 54 2 20 2 80 Refer to the MERCURY Installation Planning Guide for additional stray magnetic field plots and the effect of the stray field on electronic equipment Varian provides signs containing this warning with each system Post the signs according to the directions on the sign Additional signs are available by request 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 7 WARNINGS continued Keep metal objects at least 2 8 meters 9 feet away from the magnet The strong magnetic field of the dewar attracts objects containing steel iron or other magnetic materials such as tools electronic equipment compressed gas cylinders steel chairs and steel carts Unless restrained such objects can suddenly fly towards the magnet causing personal injury and extensive damage to the probe the dewar and the superconducting solenoid Only nonferromagnetic materials such as plastics aluminum wood and stainless steel should be used in the area around the magnet dewar Only qualified maintenance personnel shall remove equipment covers or make internal adjustments Dangerous high voltages exist inside the equipment that can kill or injure Do not substitute parts or modify the instrument Any unauthorized modification could injure personnel or damage equ
55. lk for GLIDE page 51 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 17 Chapter 2 Liquids Probes Test Procedures 2 1 How to Test a Probe This section provides the basic steps for testing a probe 18 1 Create a probe calibration file as described in Probe Calibration Files on page 19 Follow the appropriate test procedures listed in Table 1 and Table 2 for the probe If you wish you can check off each test as it is finished Table 1 lists the tests for probes that observe IH BC VF or LP Table 2 lists the test for probes that observe SN or Si and probes capable of indirect detection After the appropriate tests are completed for the probe print the corresponding probe calibration file by entering the following command in the VNMR input window ACreport Follow the instructions Section 2 6 for configuring solvent based shims and the set1k macro for proper GLIDE and automation operation Table 1 Test order for each probe that observes IH BC VF or IP Test Done 1H Spinning Resolution and Lineshape 50 0 55 0 11 of CHC13 on page 21 1H Spinning Sidebands of CHC13 on page 23 1H Observe 90 Pulse Wdth on page 26 1H Sensitivity on page 43 13C Resolution Test on page 24 13C Observe 90 Pulse Wdth and gH2 on page 29 13C Sensitivity on page 47 19F Observe 90 Pulse Wdth on page 27 19F Sensitivity on page 45 31P Observe 90 Pulse Wdth on page 28 31P Sens
56. lse 5 CHCH 00 968 120 99 30 pulse 20 CHCl 00 968 120 76 20 pulse 5 Enter ga to acquire the spectrum Phase the spectrum set wp 250 and plot using p1 Increase vs by a factor of 100 times and plot the expanded spectrum using pl pscale page If floor vibration results in excessive noise around the base of the peak nt can be set to a larger value e g nt 4 or nt 16 however if extreme vibrations are present it may be impossible to measure the lineshape accurately Measure lineshape as the linewidth of the CHCI peak at 50 0 55 and 0 11 of the main peak amplitude Refer to Figure and use the substeps below to determine the lineshape a Display and expand the desired peak Enter nm then dc for drift correction to ensure a flat baseline Set vs 10000 Place a cursor on the chloroform line and enter nl dres the 50 level c Enter nm then dc for drift correction to ensure a flat baseline Set vs 10000 Click the VNMR menu button labeled Th to display the horizontal threshold cursor Set th 55 the 0 55 level 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 21 Chapter 2 Liquids Probes Test Procedures d Click the first menu button labeled Cursor or Box 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 e Set th 11 the 0 11 level and repeat 7 Write the results
57. n lock power values for D20 and CHClg ASTM acetone shims Probe 1 Probe 2 Probe 3 Probe 4 Probe 5 Spinning Sidebands 1H 13 Notes Probe 1 Probe 2 Probe 3 Probe 4 Probe 5 90 Pulse Width s 1H SF Sp ic SN Psi Notes Probe 1 Probe 2 Probe 3 Probe 4 Probe 5 Sensitivity S N Notes ZO lock gain lock power values for CDCI3 1 19 31 13 15 29 Fi j G N Si C6D6 and DMSO shims Probe 1 Probe 2 Probe 3 Probe 4 Probe 5 84 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 5 4 Liquids Probes Test Results Ho Hz YH Specification Notes Probe 1 Probe 2 Probe 3 Probe 4 Probe 5 VT Range C Temperature Range Notes Probe 1 Probe 2 Probe 3 Probe 4 Probe 5 Other Specification Notes Probe 1 Probe 2 Probe 3 Probe 4 Probe 5 Varian Representative Date Customer Representative Date 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 85 Chapter 5 Acceptance Test Results Notes 86 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 5 5 Console and Magnet Test Results 5 5 Console and Magnet Test Results GLIDE Operation Demonstration APT and DEPT Demonstration Homonuclear Decoupling Optional
58. n PFG 10 18 _ 2700 5 mm H 9F N 3 P Switchable 20 15 15 15 15 2700 90 pulse width determined using the indirect method Table 11 90 pulse width and yH specifications for 4 nucleus systems Probe 90 Pulse Width Specifications us YE 200 MHz 1H 19F 31p BC Hz 5 mm H 3C RT Computer Switchable 18 _ 18 2700 5 mm H 3C VT Computer Switchable 18 18 2700 300 MHz 1H 19F 31p Bc 5 mm H F 3CP P PFG AutoSwitchable 18 25 15 15 2700 5 mm H C RT Computer Switchable 18 18 2700 5 mm H C VT Computer Switchable 18 18 2700 4 mm 40 uL H Nano Available by request 2700 66 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 4 3 Sensitivity Specifications 4 3 Sensitivity Specifications Table 13 broadband systems and Table 14 4 nucleus systems list the sensitivity acceptance test specifications for Varian liquids probes Probes are categorized by frequency and specifications are listed under the appropriate nucleus About Sensitivity Specifications Sensitivity values of varian probes should be greater than or equal to the values listed in the table Acceptance test specifications are achieved using the procedures in the section Sensitivity Procedures on page 42 Tests are performed in 5 mm sample tubes with 0 38 mm wall thickness Wilmad 528 PP or equivalent and 10 mm sample tubes with 0 46 mm wall thickness Wilmad 513 7PP or equivalent Use of sample tub
59. n in Figure 2 The large three line pattern at about 2 2 ppm is the signal of interest 32 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 4 90 Pulse Width Procedures Figure 2 Normal IH spectrum of BCH 10 To perform the 13C X nucleus 90 pulse width calibration in the indirect mode using HMQC enter hmqc in the same experiment or move the parameters to a different experiment by entering mp x y where x is the current experiment and y is the experiment to which the parameter set is to be moved 11 Set the following parameters fn 8192 ni 1 phase 1 nt 1 ss 0 spin 0 use acqi to turn the spinner off if the optional spinner hardware is not installed d1 5 pw to the H 90 pulse width determined from the previous steps tpwr to the tpwr level to give the H 90 pulse width determined from the previous steps nu11 0 j 151 tof to the tof determined from the IH spectrum of the 1 iodomethane 3C in step 6 above dn C13 dm nnn and dof from the following table 1H freq MHz C Hz SN Hz P Hz 400 965 12000 9000 300 9000 9200 7000 12 To determine the C X nucleus 90 pulse width and rf homogeneity using the HMQC pulse sequence pwx is arrayed for a particular pwxlv1 The spectrum corresponding to the 3C X nucleus 90 pulse width using the HMQC pulse sequence is the maximum amplitude spectrum An array of spectra appears as shown in Figure 3 The array shows only the re
60. nual button on the magnet leg or the Insert button in the Setup window Select Calibrate Phosphorus from the Experiment drop down menu You do not need to select a solvent Click the Setup button at the bottom of the Setup window Tune the probe Click on the Acquire button under Custom If you have already locked and shimmed the sample turn off autolock and autoshim Enter an appropriate value for pwmax which is listed in Table 10 and Table 11 on page 66 Click on Close at the bottom of the Acquire window Click the Go icon in the GLIDE window You should get a plot of arrayed spectra Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 28 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 4 90 Pulse Width Procedures 13C Observe 90 Pulse Width andyH Samples Sample Tube Sample mm Test Sariple Part Number 5 40 p dioxane in benzene d ASTM 00 968 120 69 10 40 p dioxane in benzene d4 ASTM 00 968 123 69 Procedure This procedure calibrates t pwr the 90 pulse width dpwr and yH for 13 C as well set dmf 1 2 3 4 m W po le O 11 12 13 pplvl and pp Make sure the appropriate quarter wavelength cable is installed Open GLIDE by clicking the GLIDE button in the VNMR menu Click on the Setup button Insert the sample in the magnet using either the manual button the magnet leg or the Insert button in the Setup
61. o the next section to configure the set 1k macro 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 51 Chapter 2 Liquids Probes Test Procedures To Configure the setlk Macro A properly configured set 1k is critical to Autolock and Autoshim performance and GLIDE performance The set 1k macro once properly configured allows the system to perform the following adjustments for each system e Explicitly set z0 lockpower and lockgain Retrieve solvent based shim sets Explicitly setting z0 Llockpower and lockgain for solvents typically used ensures the best possible results when using Autolock The reliability of Autolock is especially important for the first sample of an automation run if lock power has been low the first sample may not be run because of an Autolock failure Use the following steps to configure the set 1k macro 1 Using a text editor such as vi open the file vnmr maclib setl1k 2 To allow the system to automatically retrieve a set of shims for each solvent remove the quotes around the following lines if e gt 0 5 or e1 gt 0 5 then rts solv else exists userdirt shims cdcl3 file Se exists systemdir shims cdcl3 file Sel if Se gt 0 5 or el gt 0 5 then rts cdcl3 endif endif 3 Remove the quotes from the lines with the solvents you plan to use Replace the appropriate values of z0 lockpower lockgain using the values you wrote down during the ATP or wh
62. odically 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 To make the system demonstration most beneficial the customer should review Varian and OEM operation and reference manuals before viewing the demonstration 1 2 General Acceptance Testing Requirements Each Varian MERCURY spectrometer is designed to provide high resolution performance when operated in an environment as specified in the MERCURY Installation Planning Guide Unless both the specific requirements of this Acceptance Test Procedures manual and the general requirements specified in the MERCURY Installation Planning Guide are met Varian cannot warrant that the NMR spectrometer system will meet the published specifications General Requirements The MERCURY performance specifications in effect at the time of your order are used to evaluate the system The appropriate quarter wavelength cable must be used for each nucleus e 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 name in the directory vnmr shims for each probe For example for a 5 mm switchable probe the shim parameters can be saved with the command s
63. om temperature 5 mm H 9F N 3 P Switchable 150 to 200 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 69 Chapter 4 Liquids Probes Specifications Table 16 VT range specifications for 4 nucleus systems Probes VT Range C 200 MHz 5 mm H C RT Computer Switchable Room temperature 5 mm H 3C VT Computer Switchable 150 to 200 300 MHz 5 mm H 9F 3c P AutoSwitchable PFG 20 to 80 5 mm H 3C RT Computer Switchable Room temperature 5 mm H 3C VT Computer Switchable 100 to 160 4 mm 40 uL IH Nano Room temperature 70 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 4 5 Magnet Drift 4 5 Magnet Drift Table 17 lists the drift specifications for magnets Specifications for nominal field decay rate are less than or equal to the values listed in the table About Magnet Drift Specifications Use H lineshape sample 20 CHCl in 80 deuteroacetone CD3 CO Part No 00 968120 76 We recommend using a 5 mm probe capable of H direct observe Table 17 Magnet Drift Specifications System MHz mm 200 54 200 89 300 54 300 89 400 54 400 89 Field Strength Nominal Field Decay Rate T 4 70 7 05 9 40 9 40 Hz hr 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 71 Chapter 4 Liquids Probes Specifications 72 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 rans Acceptance Test Result
64. procedure Enter ga to acquire a spectrum Set dmm ccc dm nny dpwr 30 dof dof 2000 dof 2000 Then enter ga Enter ds 1 place a cursor on each of the positive peaks and write down the delta Enter ds 2 place a cursor on each of the positive peaks and write down the delta Enter h2ca1 and enter the delta values for the high field and low field coupling Enter 90 for the coupling constant when prompted A YH of 3000 is necessary for decoupling in indirect detection If the value is not 3000 increase dpwr in increments of 3 dB until yH is 3000 To store the values in the probe calibrations file enter the following commands setparams dpwr 42 N15 setparams dmf 12000 N15 Be sure to enclose the values in single quotes because they are treated as strings 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 41 Chapter 2 Liquids Probes Test Procedures 2 5 Sensitivity Procedures This section covers the sensitivity procedures required to demonstrate the specifications listed in Sensitivity Specifications on page 67 This section contains the following test procedures 1H Sensitivity 19F Sensitivity 31P Sensitivity 13C Sensitivity 29Si Sensitivity Only 4 Nucleus Probes with 29Si 15N Sensitivity Only 400 MHz or 4 Nucleus Probes with 15N 42 MERCURY Acceptance Test Procedures and Specifications amp 7 192327 00 E0997 2 5 Sensitivity Procedures 1H
65. pwx is arrayed for a particular pwxlv1 The spectrum corresponding to the P X nucleus 90 pulse width using the HMQC pulse sequence is the maximum amplitude spectrum An array of spectra appears as shown in Figure 6 In HMQC nu11 occurs at 45 135 maximum at 90 and neative at 180 Set pwxl1v1 to the tpwr value for normal 31P observe to get this value you can enter getparam tpwr P31 pwxlv1 Enter array to array pwx As array displays the following prompts enter in the response shown in bold parameter to be arrayed pwx number of steps in the array 20 starting increment array increment In this example the experiment is set up to array pwx from 2 us to 22 us in 1 us increments 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 37 Chapter 2 Liquids Probes Test Procedures 38 13 14 15 Figure 6 pwx calibration coarse left and fine right Enter ga to start the acquisition After the last spectrum is finished enter ds 1 to display the first spectrum Enter aph to phase the spectrum then enter ai dssh to display the arrayed spectra Determine the pwx90 from the first maximum Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 To store the values in the probe calibrations file enter the following commands setparams pwxlvl 61 0 P31 setparams pwx 14 2 P31 Be sure to enclose the values in single quote
66. pwx1v1 to the tpwr value for normal gt N observe to get this value you can enter getparam tpwr N15 pwxlv1 Enter array to array pwx As array displays the following prompts enter in the response shown in bold parameter to be arrayed pwx number of steps in the array 20 starting increment array increment In this example the experiment is set up to array pwx from 2 Us to 22 Us in 1 us increments Figure 7 pwx calibration coarse left and fine right 40 MERCURY Acceptance Test Procedures and Specifications 67 192327 00 E0997 13 14 15 2 4 90 Pulse Width Procedures Enter ga to start the acquisition After the last spectrum is finished enter ds 1 to display the first spectrum Enter aph to phase the spectrum then enter ai dssh to display the arrayed spectra Determine the pwx90 from the first maximum Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 To store the values in the probe calibrations file enter the following commands setparams pwxlvl 61 0 N15 setparams pwx 14 2 N15 Be sure to enclose the values in single quotes because they are treated as strings SN Decoupling Calibration Measuring yH for Indirect Detection This procedure describes how to perform DN decoupling calibration as well as how to measure YH for indirect detection 1 2 3 Set pwx equal to the value determined in step 14 in the previous
67. r movet of then enter tof to display the new values of tof Record the value 7 Enter jexpn where nis the experiment number of the carbon experiment e g jexp2 to join experiment 2 and set dof to the value of tof obtained in the proton spectrum 8 Repeat step 5 9 Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 4 90 Pulse Width Procedures 2 4 90 Pulse Width Pocedures This section contains the procedures required to demonstrate the specifications listed in 90 Pulse Wdth and gH2 Specifications on page 65 1H Observe 90 Pulse Width 19F Observe 90 Pulse Wdth 31P Observe 90 Pulse Width 13C Observe 90 Pulse Wdth and gH2 29Si Observe 90 Pulse Wdth Only 4 Nucleus Probes with 29Si 15N Observe 90 Pulse Width Only 400 MHz or 4 Nuc Probes with 15N 13C pwx90 Pulse Width 31P pwx90 Pulse Width 15N pwx90 Pulse Width Only 400 MHz with Indirect Detection Probes Refer to other Varian manuals for further information on pulse width determination 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 25 Chapter 2 Liquids Probes Test Procedures 1H Observe 90 Pulse Width Samples Sample Tube Sample mm Test Sample Part Number 5 0 1 ethylbenzene 0 01 TMS 00 968120 70 99 89 deuterochloroform CDCI3 10 0 1 ethylbenzene 0 01 TMS 00 968123 70 99 89 deuteroc
68. robe 200 MHz 5 mm 5N P Broadband 10 mm N P Broadband 5 mm H 9F N 3 P Switchable 300 MHz 5 mm H F 3C P AutoSwitchable PFG 10 mm N P Broadband 5 mm TAL y3 p Indirect Detection 5 mm H 5N 3 P Indirect Detection PFG 4 mm 40 uL H Nano 5 mm H 9F Proton 5 mm H 9F N 3 P Switchable Broadband 400 MHz 5 mm H 9F 3C P AutoSwitchable PFG 10 mm N 3 P Broadband 5 mm AL ISN 31P Indirect Detection 5 mm AL by lp Indirect Detection PFG 4 mm 40 uL H Nano 5 mm H 9F N 3 P Switchable Spinning Sidebands 1 H 13 C 1 1 1 1 1 H 13 C 1 1 1 1 1 1 1 Available by request 1 1 1 1 H 13 C Available by request 1 1 1 Available by request 1 1 Table 8 Spinning sidebands specifications for 4 nucleus systems Probe Spinning Sidebands 200 MHz IH BC 10 mm N 3 P Broadband 1 5 mm H C RT Computer Switchable 1 1 5 mm H C VT Computer Switchable 1 1 300 MHz IH BC 5 mm H F 3C 7 P AutoSwitchable PFG 1 1 5 mm H C RT Computer Switchable 1 1 5 mm H 3C VT Computer Switchable 1 1 4 mm 40 uL TH Nano Available by request 64 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 4 2 90 Pulse Width andyH Specifications 4 2 90 Pulse Width andyH Specifications The 90 pulse width and yH acceptance test specifications for Varian liquids probes are listed in Table 10 for broadband systems
69. rter wavelength cable is installed 2 Insert the 1 iodomethane 3C sample Part No 00 968120 96 Tune the probe on this sample 3 Enter rtp vnmr tests H1sn to retrieve the parameters from the H sensitivity measurement 4 Set pw and t pwr to the values determined for the H sensitivity procedure you can get these values from the probe calibration file by entering getparam tpwr tpwr getparam pw90 pw 5 Set gain 10 dn C13 d1 5 and enter ga 6 Place two cursors around the region with the peaks Enter movesw to narrow the spectral width 7 Determine the 90 pulse width by arrayingpw to 2360 pulse width Enter the macro array to set up the array As the macro displays the following prompts type in the response shown in bold parameter to be arrayed pw number of steps in the array 25 starting increment 2 array increment 2 In the above example the experiment is set up to array the pw parameter from 2 us to 52 us in 2 us increments If the 90 pulse width is 10 us the 450 pulse width corresponds to pw 50 us 5 pw90 8 Enter ga to start the acquisition After the last spectrum is finished enter ds 5 vp 50 to display the fifth spectrum Enter aph to phase the spectrum then enter ai dssh to display the arrayed spectra 9 Set pw equal to the 90 pulse width you have determined Ether ga to acquire the spectrum Enter f ds to display the spectrum The spectrum should appear similar to the example show
70. s Chapter 5 Acceptance Test Results Chapter 5 Acceptance Test Results This chapter contains the following forms for recording system information and acceptance test results e 5 1 Computer Audit page 77 e 5 2 System Installation Checklist page 79 5 3 Supercon Shim Values page 81 5 4 Liquids Probes Test Results page 83 e 5 5 Console and Magnet Test Results page 87 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 75 Chapter 5 Acceptance Test Results Notes 76 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 5 1 Computer Audit 5 1 Computer Audit Please provide the following information about your site please print Company University Address Principal User Phone Spectrometer type Fax Console S N Sales Order No Delivery month day Please provide the following information for 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 Periph
71. s because they are treated as strings 31P Decoupling Calibration Measuring yH for Indirect Detection 1 2 3 Set pwx equal to the value determined in step 14 in the previous procedure Enter ga to acquire a spectrum Set dmm ccc dm nny dpwr 30 dof dof 2000 dof 2000 Then enter ga Enter ds 1 place a cursor on each of the positive peaks and write down the delta Enter ds 2 place a cursor on each of the positive peaks and write down the delta Enter h2ca1 and enter the delta values for the high field and low field coupling Enter 10 5 for the coupling constant when prompted A YH of 3000 is necessary for decoupling in indirect detection If the value is not 3000 increase dpwr in increments of 3 dB until yH is 3000 To store the values in the probe calibrations file enter the following commands setparams dpwr 44 P31 setparams dmf 12000 P31 Be sure to enclose the values in single quotes because they are treated as strings MERCURY Acceptance Test Procedures and Specifications 67 192327 00 E0997 2 4 90 Pulse Width Procedures 15N pwx90 Pulse Width Only 400 MHz with Indirect Detection Probes This test is performed at installation only on 400 MHz systems with indirect detection probes unless explicitly agreed upon in writing as part of the customer contract Sample Sample Tube Sample mm Test sample Part Number 5 2 benzamide N 0 2 Cr acac in CDCI 00 968120 97
72. seeseesseesesssersessesesesreerreesesssersesreseseesee 34 Figure 4 HMQC with and without X nucleus pulses ss 35 Figure 5 Normal IH spectrum of BCHI gibi A AEE EEEE sets dySvenseyerbonsabbonestanssbedeotses 37 Figure 6 pwx calibration coarse left and fine right 0 0 ee eeesseeseeeceeceeeceeeeseeeeeeeeeeeeeneeeneees 38 Figure 7 pwx calibration coarse left and fine Tight 0 eececceeseesseeseeeceeeeceeesecseceeeceeeeteeerensees 40 Figure 8 IH sensitivity measurement sise 44 Figure Q 19C Sensitivity SR eian atik iiaii aii 48 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 5 Table 1 Table 2 Table 3 Table 4 Table 5 Table 6 Table 7 Table 8 Table 9 Table 10 Table 11 Table 12 Table 13 Table 14 Table 15 Table 16 Table 17 List of Tables Test order for each probe that observes IH BC IF or Pee ean ereeer 18 Test order for probes that observe 296 15 N or indirect detection ccceeeeeseeeseeeeeeees 18 Samples for H resolution lineshape and spinning sidebands tests 0 eee 62 Samples for 3C resolution lineshape and spinning sidebands tests 0 0 0 eee 62 Resolution and lineshape specifications for broadband systems eseeeeseeeeeeeeeeeeees 63 Resolution and lineshape specifications for 4 nucleus systems 20 eeeeeeeeeeeeeeeeeeeeeeee 63 Spinning sidebands specifications for broadband systems o 0 eee eeees
73. setlk for GLIDE oo eects 51 To Set Up the Solvent Based Shim Piles 4e 51 To Conieure ME SEU Magro nn nn nee ne 52 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 3 Table of Contents Chapter 3 Console and Magnet Test Procedures 53 GLIDE Operation D monstratio siisii ali tonteuedeiers abdessnecsse ga ceniene 54 APT and DEPT Demonstration unes seise de eneetayy 55 Homonuclear Decoupling Optional ss 56 Variable Temperature Operation Optional oo eee eee ese eseeeeeeeeteeeeeeeee 57 Magoet Dritt TeS wissciasdescvetbin iid esni anarias iaa araneae tetes 58 Acceptance Test Specifications Chapter 4 Liquids Probes Specifications sens 61 4 1 Resolution Lineshape Spinning Sidebands Specifications 00 eee 62 About Resolution and Lineshape Specifications ci ce eee eeeeeeeeteeeeeeees 62 Samples for Resolution and Lineshape Tests ooo eee eseeseeeeeseteeeeeeeees 62 4 2 90 Pulse Wdth and yH Specifications oo eee cece ce eeeeeeeetseteteeseeeeens 65 About 90 Pulse Width and yH Specifications oo eee eseeeeeseeeeeeees 65 About Test Samples sn Seas eceussenscaduonscdieguooned stesueussay sepeengsloanddenvolees 65 4 3 Sensitivity Specifications ss 67 About SENSILIVIEY S PECIICANOUS 6 6 5 5 iioscisaassceteanig cvosevandeacvacenpeavosssnemguasneas 67 About Test Samples iisisti iaasa aaarnas 67 4 4 Variable Temperature Range Specifications eessesseeeeseeesres
74. signed for indirect detection applications are tested for 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 11 Chapter 1 Introduction 12 indirect detection performance only Indirect detection acceptance tests are performed only if an indirect detection probe was purchased for use with the MERCURY Sample Tubes Policy Tests are performed in 5 mm sample tubes with 0 38 mm wall thickness Wilmad 528 PP or equivalent and 10 mm sample tubes with 0 46 mm wall thickness Wilmad 513 7PP or equivalent Using sample tubes with thinner walls Wilmad 5 mm 545 PPT or equivalent Wilmad 10 mm 513 7PPT or equivalent increases signal to noise Computer Audit A computer audit form is included in Computer Audit on page 77 The information from this form will help Varian assist you better in distributing future software upgrades and avoiding hardware compatibility problems You are asked for information about all computers directly connected to the spectrometer or else used to process NMR data Installation Checklist An installation checklist form is given in System Installation Checklist on page 79 System Documentation Review Following the completion of the acceptance tests and computer audit the installation engineer will review the following system documentation with the customer e Software Object Code License Agreement e Varian and OEM manuals Warranty coverage and where to telephone for
75. spectrum then enter ai dssh to display the arrayed spectra 9 Set pw equal to the 90 pulse width you have determined Enter ga to acquire the spectrum Enter f ds to display the spectrum The spectrum should appear similar to the example shown in Figure 5 The large two line pattern at about 3 75 ppm is the signal of interest 10 To perform the 31P X nucleus 90 pulse width calibration in the indirect mode using HMQC enter hmqc in the same experiment or move the parameters to a 36 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 4 90 Pulse Width Procedures Figure 5 Normal IH spectrum of BCHI different experiment by entering mp x y where x is the current experiment and y is the experiment to which the parameter set is to be moved 11 Set the following parameters fn 8192 ni 1 phase 1 nt 1 ss 0 spin 0 use acqi to turn the spinner off if the optional spinner hardware is not installed d1 2 pw to the H 90 pulse width determined from the previous steps tpwr to the tpwr level to give the H 90 pulse width determined from the previous steps nul1 0 j 10 5 tof to the tof determined from the IH spectrum of the 1 iodomethane 3C in step 6 above dn P31 dm nnn and dof from the following table 1H frequency MHz C Hz 15N Hz 31P Hz 400 965 12000 9000 300 9000 9200 7000 12 To determine the P X nucleus 90 pulse width and rf homogeneity using the HMQC pulse sequence
76. sponse of the outer line at about 2 4 ppm of the three line pattern In HMQC null occurs at 45 135 maximum at 90 and neative at 180 Set pwx1v1 to the tpwr value for normal C observe to get this value you can enter getparam tpwr C13 pwxlv1 Enter array to array pwx As array displays the following prompts enter in the responses shown in bold parameter to be arrayed pwx number of steps in the array 20 starting increment array increment 1 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 33 Chapter 2 Liquids Probes Test Procedures 13 14 15 Figure 3 pwx calibration coarse left and fine right In this example the experiment is set up to array pw from 2 us to 22 Us in 1 us increments Enter ga to start the acquisition After the last spectrum is finished enter ds 1 to display the first spectrum Enter aph to phase the spectrum then enter ai dssh to display the arrayed spectra Determine the pwx90 from the first maximum Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 To store the values in the probe calibrations file enter the following commands setparams pwxlvl 61 0 C13 setparams pwx 14 2 C13 Be sure to enclose the values in single quotes because they are treated as strings 13C Decoupling Calibration Measuring yH for Indirect Detection This procedure describes how to perform 13C de
77. the probe calibration file you can retrieve these values by entering getparam tpwr tpwr getparam pw90 pw 5 Tune the probe 6 Fora5 mm sample set nt 4 For a 10 mm sample set nt 1 7 Set dmf and dpwr from the calibration by entering getparam dmf H1 dmf getparam dpwr H1 dpwr 8 Enter 1b 0 4 fn 16384 d1 100 dm nny ga to acquire s spectrum the spectrum is a single line 9 For noise measurement locate the cursor in a representative 100 Hz region 10 Enter dsn The computer calculates the signal to noise ratio 11 Write the results for each probe in the forms provided in Liquids Probes Test Results on page 83 12 After the specifications are met do the following e Write down the values for z0 Lockpower and lockgain as they appear in the Acqi window Use the forms provided in Liquids Probes Test Results on page 83 Save the shims by entering the following command in the VNMR input window svs dmso 50 MERCURY Acceptance Test Procedures and Specifications 87 192327 00 E0997 2 6 Configuring Solvent Based Shims and setlk for GLIDE 2 6 Configuring Solvent Based Shims and setlk for GLIDE For GLIDE and automation to work properly solvent based shims must be set up and the setlk macro must be configured To Set Up the Solvent Based Shim Files During the probe acceptance tests ATP at least three solvent based shim files were saved acetone cdc13 and c6d6 dmso would have be
78. ture for 5 minutes 4 Operate the VT unit within the specifications of the probe Test the temperature at set points that correspond to the following e Maximum minimum and midpoint of the allowed temperature 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 Be sure to never ramp the temperature by more than 12 C per minute up or down For probes with small temperature ranges ramping increments will be much less than 12 C per minute To achieve the 12 C per minute change adjust the temperature by no more than 50 C enter su and wait for the temperature to equilibrate 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 57 Chapter 3 Console and Magnet Test Procedures 58 Magnet Drift Test The magnet drift test is an overnight test Sample Use H lineshape sample 20 CHCl in 80 deuteroacetone CD3 CO Part No 00 968 120 76 Probe and Hardware Requirements We recommend using a 5 mm probe capable of IH direct observe Test Procedure 1 10 11 Enter rtp vnmr tests H11shp to retrieve the test parameter set to the current experiment Tune the probe Acquire a normal spectrum and shim the chloroform signal to less than 1 Hz linewidth at 50 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 th
79. uit 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 instrument MERCURY Gemini GEMINI 2000 UNITY plus UNITY VXR XL VNMR Vnmrs VamrX Vamrl VnmrV VnmrSGI MAGICAL II AutoLock AutoShim AutoPhase limNET ASM and SMS are registered trademarks or trademarks of Varian Inc Sun Solaris CDE Suninstall Ultra SPARC SPARCstation SunCD and NFS are registered trademarks or trademarks of Sun Microsystems Inc and SPARC International Oxford is a registered trademark of Oxford Instruments LTD Ethernet is a registered trademark of Xerox Corporation Other product names in this document are registered trademarks or trademarks of their respective holders Table of Contents SAFETY PREG Oi i isaac ct emcees eee ees 7 Chapter 1 Introduction ya eecceee eet ein 11 Dell OVERVIEW aisoissa iniii i steve intestins A 11 Acceptance TESS iiinis arasina tt ein rin te lien einen tns ets 11 Acceptance SPSCUMICAIONE onnsa coasasasroacsenten i sensara esiseaventas 11 COMET AMIE eisein aasarin i aiani naanin 12 Tostallaton Chec khet siiiereciioriiriaiainacioninisanesnasesiii iakinen 12 System Documentation Review ss 12 Basie System D MONSITAMDI tsccceccseceaccsiaiecasieaionecueiivecesseasccwasyuerevaceteestans 12 1 2 General Acceptance Testing Requirements o0 ec eee cee eecneeseceeeeseteeteeeeeeaes 1
80. vs sw5res These values can then be used as a starting point when adjusting the homogeneity on unknown samples by the command rts sw5res The probe must be tuned to the appropriate frequency The spinning speed must be set to the following Sample mm Nuclei Speed Hz 5 all 20 26 10 all 15 Spinning 10 mm tubes faster than 15 Hz may cause vortexing in samples severely degrading the resolution 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 1 3 Chapter 1 Introduction Some 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 file that contains the parameters to be retrieved for example rtp vnmr tests H1sn To see the parameter sets available for the standard tests enter 1ls vnmr tests Other sets come from vnmr stdpar For all sensitivity tests the value of pw must be changed to the value of the 90 pulse found in the pulse width test on the same probe During calibration GLIDE creates an appropriate pw array to determine the 90 pulse width For manually run 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 neg
81. witchable 0 4 6 0 12 0 0 2 300 MHz 1H Spinning 13C Spinning 5 mm H 9F 3C P AutoSwitchable PFG 0 4 6 0 12 0 0 2 10 mm N P Broadband 0 2 5 mm H 5N 3 P Indirect Detection 0 4 6 0 12 0 0 2 5 mm H 5N 3 P Indirect Detection PFG 0 4 6 0 12 0 0 2 4 mm 40 uL H Nano Available by request 5 mm H 9F N P Switchable Broadband 0 4 6 0 12 0 0 2 400 MHz 1H Spinning 6 Spinning 5 mm H 9F 3 3 P AutoSwitchable PFG Available by request 10 mm N 3 P Broadband 0 2 5 mm H 5N 3 P Indirect Detection 0 45 6 0 12 0 5 mm H N P Indirect Detection PFG 0 45 6 0 12 0 0 2 4 mm 40 uL IH Nano Available by request 5 mm H 9F N 3 P Switchable 0 45 6 0 12 0 0 2 Full linewidth at half height Table 6 Resolution and lineshape specifications for 4 nucleus systems Probe 200 MHz 5 mm H C RT Computer S witchable 5 mm H C VT Computer Switchable 300 MHz 5 mm H F 3C 3 P AutoSwitchable PFG 5 mm H C RT Computer Switchable 5 mm H C VT Computer Switchable 4 mm 40 uL H Nano Resolution and Linewidth Hz 1H Spinning BE Spinning 0 4 6 0 12 0 0 2 0 4 6 0 12 0 0 2 1H Spinning BG Spinning 0 4 6 0 12 0 0 4 6 0 12 0 0 2 0 4 6 0 12 0 0 2 Available by request Full linewidth at half height 87 192327 00 E0997 MERCURY Acceptance Test Procedures and Specifications 63 Chapter 4 Liquids Probes Specifications Table 7 Spinning sidebands specifications for broadband systems P

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