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MERCURYplus Console ATP

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1. seqlib shapelib jre tel tmp aa text root fonts tun procpar font ENGE 1 devicenames nd myfids log L data2 fid rexpl m exp2 user A vnmrsys Joe DI user seq c maclib D user macros gehiniib shapelib o o F Gutotest L_ global Figure 15 VNMR Directory Structure and directories contain macros pulse sequences binary files optional VNMR software and other files that have a common usage to all users The users area contains files that are owned by that user only When VNMR is installed and user accounts are established certain directories are created in the user s home directory In some cases these directories have the same names in both the user work space in the vnmr directory When a command or instruction is executed in vnmr by auser VNMR first searches the user s vnmrsys directory for the command pulse sequence etc and then searches the global files in vnmr The System Administration manual provides more detailed explanation When creating custom macros 42 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 4 4 Managing Disk Space pulse sequences menus etc it is good practice to give these files different names from the similar files in vnmr If you want the customized macros pulse sequences etc to be available to all users place them in the appropriate directory in vn
2. The probe must be tuned to the appropriate frequency 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 can cause vortexing in samples severely degrading the resolution 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 e g rtp vnmr tests H1sn To see the parameter sets available for the standard tests enter 1s vnmr tests Other sets come from vnmr stdpar Many of the probe parameters and performance specifications will be determined automatically and the corresponding manual tests will NOT be run by the installer Certain tests such as signal to noise and lineshape will be run manually Tests corresponding to the automatic performance tests are provided should you want to run them at a later time 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 and nucleus 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 360 pulse The 360 pulse is the first non zero pulse that gives minimum intensity of the spectrum The 360 pulse is us
3. Reviewing the Probe Calibration Probe calibrations executed by vnmr1 are written to probe files one of two places Ifthe probe was created as a system probe and the probe name is unique it does not exist in export home vnmri vnmrsys probe it is written to vnmr probes probe name Ifthe probe was not created as a system probe or the probe name is not unique it does exist in export home vnmril vnmrsys probe it is written to export home vnmr1i vnmrsys probes probe name You can read or edit the file with a text editor e g vi or you can use the setup EXP pane Figure 7 Probe Administration from Setup EXP 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 25 Chapter 2 Console and Magnet Test Procedures 1 Login as vnmr1 and start VNMR 2 Click on the Setup EXP tab 3 Inthe Probe Administration part of the Setup EXP pane select the probe calibration you want to edit see Figure 7 4 Click on a field to review data Probe hen Eg a Probe Parameters The current values are shown in parentheses next gradient r mE to the probe parameter To change a parameter ee ap tn value enter the new value in the blank imap n A hsmap n sd If you are a user other then vnmri the system tunefg m rfsize 16 E probe calibrations are displayed in the TEXT Ed pa pane The calibrations cannot be changed Save Clear Exit 2 2 Automated
4. WARNING Warnings are used when failure to observe instructions or precautions could result in injury or death to humans or animals or significant property damage CAUTION Cautions are used when failure to observe instructions could result in serious damage to equipment or loss of data Warning Notices Observe the following precautions during installation operation maintenance and repair of the instrument Failure to comply with these warnings or with specific warnings elsewhere in Varian manuals violates safety standards of design manufacturing and intended use of the instrument Varian assumes no liability for customer failure to comply with these precautions WARNING Persons with implanted or attached medical devices such as pacemakers and prosthetic parts must remain outside the 5 gauss perimeter from the centerline of the magnet The superconducting magnet system generates strong magnetic fields that can affect operation of some cardiac pacemakers or harm implanted or attached devices such as prosthetic parts and metal blood vessel clips and clamps Pacemaker wearers should consult the user manual provided by the pacemaker manufacturer or contact the pacemaker manufacturer to determine the effect on a specific pacemaker Pacemaker wearers should also always notify their physician and discuss the health risks of being in proximity to magnetic fields Wearers of metal prosthetics and implants should contact their physician to de
5. 5 gauss warning signs Figure 2 Post along the 5 gauss perimeter of the magnet so that a sign can be easily seen by any person about to enter the 5 gauss field from any direction Refer to the manuals supplied with the magnet for the size of a typical 5 gauss stray field Check this gauss level after the magnet is installed Note that the stray field may extend vertically to adjacent floors and additional signs may be needed there MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 3 1 6 Posting Requirements for Magnetic Field Warning Signs Magnet area danger signs Figure 3 Post at each entrance to the magnet area Be sure each sign is outside the 5 gauss perimeter A A10 GAUSS A UAINE STRONG MAGNETIC FIELD Tools and Equipment Strong magnetic fields are present that can make magnetic items suddenly fly towards the magnet which could cause personal injury or serious damage Do not take tools equipment or personal items containing steel iron or other magnetic materials closer to the magnet than this sign Dewars The stray field of the magnet can pull a magnetic dewar into the magnet body causing serious damage Use only nonmagnetic stainless steel dewars Do not use iron or steel dewars during servicing ae aw Fun Na 87 280902 00 80694 10 Gauss VARIAN Sen STRONG MAGNETIC FIELD Pacemaker Metallic Implant Hazard Strong magnetic and rf f
6. 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 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 VNMR version Operating system Information on computer of e g 3 of 3 Manufacturer Model no Computer S N Purchased from Memory Mbytes Screen size in 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 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 62 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 5 2 Installation Customer Training Checklist 5 2 Installation Customer Training Checklist Customer Information Company University Address Principal User Phone Spectrometer type Fax Console S N Sales Order No Magn
7. 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 55 Chapter 4 Customer Training 4 7 Magnet Maintenance Magnet maintenance is described in Chapter 22 of the System Administration manual Magnet maintenance consists of three basic elements Periodic checks of the cryogen levels and boil off rates Liquid nitrogen fill Liquid helium fill WARNING The extremely low temperature of liquefied helium and nitrogen can cause skin damage similar to high temperature burns Contact with the cold gas evolving from the liquid may produce the same effect Delicate body tissues such as the eyes are easily damaged by exposure to cold gas or liquid Skin can stick to metal that is refrigerated by liquid helium and can tear when pulled away Immediately flood with large quantities of unheated water any area of the body that is burned by liquid or cold gas and then apply cold compresses If the skin is blistered or there is any chance the eyes are affected immediately seek medical treatment WARNING Wear goggles and loose fitting protective gloves while working with cyrogens Periodic checks A record or log book should be kept with dates flow rates cryogen levels and notes on changes made to or observed in the magnet A typical schedule of checks would be Weekly 1 Check air line traps for dirt or condensed water 2 Record the following readings note that the flow rates of nitrogen and helium depends on a
8. Data Acquisition 26 The automated data acquisition consists of several 1D and 2D experiments using the indanone sample listed in Table 3 Table 3 Sample for Automated Data Acquisition Sample Size Sample Part Sample mm Number 2 2 ethyl 1 indanone in chloroform d 5 01 901855 03 The system console and probe configuration determines the experiment selection as follows Tests Gradient Nongradient Systems Systems Four 1 D experiments Acquisition of a proton spectrum v Vv Acquisition of a proton decoupled carbon observe spectrum v Vv DEPT distortionless enhancement by polarization transfer v Vv APT attached proton test v Vv Nongradient 2D experiments TOCSY total correlation spectroscopY v Vv NOESY nuclear overhauser spectroscopY v Gradient 2D experiments requires PFG option and gradient probe gCOSY gradient correlation spectroscopY Vv gHSQC gradient heteronuclear single quantum correlation v gHMBC gradient heteronuclear multiple bond correlation Vv Nongradient COSY correlation spectroscopY v These experiments demonstrate the capabilities of the MERCUR Yplus spectrometer the correct calibration of the instrument and validate the correct functioning of the instrument MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 2 2 Automated Data Acquisition You will be setting up two sets of experiments You will be clicking on the Setup icon on the GLIDE
9. Experiment Selection windows appears The window that appears is determined by the value of the gradient field in the probe definition file If you have a gradient probe and the gradient field in the probe definition file is set to Y the Experiment Selection window shown in Figure 8 is displayed If you have a non gradient probe or the gradient field in the probe definition file is set to N the Experiment Selection window shown in Figure 9 is displayed If gradients are installed on your system and you do not see gradient experiments listed the gradient field in the probe file is incorrect or an entry has not been made The correct entry in the gradient field of the probe file is either y yes there are gradients or n there are no gradients Use the proton 1D default acquisition parameters displayed in the Experiment Selection window Select the following experiments in the order listed Experiments are executed following the proton 1D experiment in the order that they are selected Gradient equipped systems with gradient probe select 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 27 Chapter 2 Console and Magnet Test Procedures Figure 8 Experiment Selection Window for Gradient Experiments Figure 9 Experiment Selection Window for Nongradient Experiments gCOSY click OK to accept the default parameters gHMBC click OK to accept the default parameters gHSQC click OK to acce
10. Parameter Reference VNMR User Programming System Administration Probes and Accessories Probes amp Accessories Help File List Installation Customer Training Checklist installation Planning Quick Installation and Release Notes VNMR and Solaris Software Installation Acceptance Test Procedures Specifications Sample Management Systems VAST Technical References System Overview Hardware Technical Reference System Schematics ap VARIAN gt lt Figure 14 MERCURYplus Online Manual Menu To access the online manuals in Solaris 2 7 and later select VNMR from the CDE menu then select Online Manuals 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 39 Chapter 4 Customer Training 40 Operation Manuals After the installation has been finished you will find many of your routine questions answered in the following manuals VNMR Command and Parameter Reference Provides an alphabetical listing of the VNMR commands parameters and macros Refer to this manual when you are working at the command line and you need to review a specific command Walkup NMR Provides information about the walkup NMR interfaces available in VNMR Step by step instruction on setting up experiments using GLIDE and three Tcl Tk interfaces Detailed system calibration and administration instructions are provided in this manual Getting Started Provides an overview of VNMR and instrument ope
11. 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 unavailable 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 VT probe is used Procedure 1 Inthe config window make sure VT Controller is set to Present Alternatively enter vttype to check that vt type is set to 2 2 Set N2 gas flow to 9 5 to 10 0 LPM for temperatures below 100 C increase N2 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 temperature 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 Maximum minimum and midpoint of the allowed temperature 95 80 60 if air is used 120 30 20 if dry nitrogen is used or 120 100 40 if a heat exchanger is used Ambient temperature The software limits the ramp rate to 12 C per minute up or down Wait for the temperature to equilibrate 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 33 Chapt
12. and floppy disks disable the information stored on the magnetic strip of automated teller machine ATM and credit cards and damage some watches To warn of the presence and hazard of strong magnetic fields the customer is responsible for posting clearly visible signs warning of magnetic field hazards This responsibility includes measuring stray fields with a gaussmeter Radio frequency emissions may also pose a danger to some individuals The rf emission levels from Varian NMR equipment have been measured and compared to the IEEE ANSI C95 1 1991 standard For further information refer to the RF Environment section of the Installation Planning Guide Warning Signs Varian provides signs to help customers meet this posting responsibility These signs must be posted according to the following requirements before the magnet is energized 1 10 gauss warning signs Figure 1 Post along the 10 gauss perimeter of the magnet so that a sign can be easily seen by any person about to enter the 10 gauss field from any direction Refer to the manuals supplied with the magnet for the size of a typical 10 gauss stray field Check this gauss level after the magnet is installed Note that the stray field may extend vertically to adjacent floors and additional signs may be needed there A sign is not required if the 10 gauss field extends less than 30 cm 12 in beyond a permanent wall or less than 61 cm 24 in beyond the floor above the magnet 2
13. arrow pointing down to a short bar Press and hold the left mouse button and drag the bottom boarder down until the text entry box is full visible 7 Click the Confirm button i At the end of the setup Z A Hal operation the Custom and Go buttons are no longer shaded asi ann and the GLIDE Acquire button appears 8 Click the Acquire button to open the Acquisition Setup window see Figure 6 9 For the purposes of the ATP ATS select all the calibration routines appropriate for the current probe 24 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 2 1 AutoCalibration and GLIDE Operation Demonstration Figure 6 Acquisition Setup Window No matter what order you select the calibration order is always the following HI observe C13 decouple gradient H1 C13 gradient ratio C13 observe H1 decouple If you do not select one of these calibrations it is skipped If you do not have gradients the gradient related calibrations are skipped 10 Enter the H1 and C13 pulse specifications of your probe s for H1 and C13 observe pw90 and decoupler pulses If you do not enter a value the calibration routine defaults to 15 usec for all pulses 11 Plot Results select Yes 12 Click the Do button to start the calibration routine At the end of the calibration routine the power and pulse width values are automatically incorporated into the probe file and the calibration spectra are plotted
14. contains the following specifications 3 1 Homonuclear Decoupling this page 3 2 Variable Temperature Operation this page 3 3 Magnet Drift page 38 3 4 Temperature Accuracy for VT Accessories page 38 3 5 Stability Calibration for High Stability VT Accessory page 38 3 1 Homonuclear Decoupling The quartet shows a single peak with no remaining evidence of splitting 3 2 Variable Temperature Operation For basic variable temperature VT accessories Varian Part No 00 992957 00 demonstrate that the VT unit and probe go to the desired temperature as registered on the window of the VT controller If the system is equipped with a VT unit the system user should read through the VT operation instructions before the demonstration Dry nitrogen is required as the VT gas if the requested temperature is over 100 C or below 10 C Otherwise air can be used For temperatures below 40 C dry nitrogen gas is recommended for cooling the bearing spinner and decoupler This prevents moisture condensation in the probe and spinner housing CAUTION The use of air as the VT gas for temperatures above 100 C is not recommended Such use destructively oxidizes the heater element and the thermocouple CAUTION Extreme temperatures can damage the probe The high and low temperature must be within the specified range of the probe Demonstration Limitations If dry nitrogen gas and liquid nitrogen are not availabl
15. is arrayed to produce the spectra shown in Figure 23 From these spectra the first estimate of the proton decouple pw90 is made Using the relationship between the pulse width and the decoupler field strength YH gt shown in the equation below the decoupler pw90 is determined 1 a pA EE E Y 4 pw90 The sequence is now set to ppcal and the proton decoupler 90 pulse pp is determined These spectra shown in Figure 24 are saved as Hdec dept 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 47 Chapter 4 Customer Training dd NA Mal onal 5 10 15 20 25 30 35 40 45 ppm Figure 21 Proton Coupled 13c Spectrum of 3C_Methyl Iodide hd pk Li Figure 22 1 C Observe pw Array of Proton Coupled Spectra These parameters and calibrations are used to setup WALTZ decoupling This completes the calibrations During the calibration procedure spectra and the array values are plotted to provide a permanent record of the calibrations 48 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 4 6 Data Acquisition Calibration and Indanone Spectra inner dun ras Figure 23 Proton Decoupler dof Array LILLE Figure 24 Calibration of the Decoupler 90 Pulse Width pp 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 49 Chapter 4 Customer Tr
16. 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 is a registered trademark of Varian Inc GLIDE is a trademark of Varian Inc VxWORKS and VxWORKS POWERED are registered trademarks of WindRiver Systems Inc Sun is a registered trademark of Sun Microsystems Inc Ultra SPARC and SPARC station are registered trademarks of SPARC International Inc Ethernet is a registered trademark of Xerox Corporation Other product names are trademarks of their respective holders Table of Contents Chapter 1 INIFOLICHION ns iricacesaiseae nis cand ca nsiasenauenennsanstaceesucnacndeacssanucsanars 11 1 1 Overview of the Acceptance Testing Process mrmrrnrvervravvrrnneneevverrerversrevrarvrrerssvseenr 11 Aoceptince TE oeri neredne iein in ein Enes ra E aE E SEERE 12 Accepiance STEAM uken 12 Computer AT 5 2 intense detente ea eree Tie EE o iiao 12 Installation Checklist oiiire eea ea Eea EEEE EE 12 System Documentation REVIEW lt sscicnc ccvicustcesesssesivotiesnesicbsussebesiivecssaea soneseevenses 12 Basie System Demonstraton susuoennnnisstinvnunvnsitgernmsunsjetiei 13 1 2 General Acceptance Testing Requirements menerevrrnvrrnvrvnvevenvveevrnrnervrnvrarvrrersvnsernr 14 1 3 Samples Required for Acceptance Tests rrrernrnervrrrnvrnvnrvvrnvnrnenvnervrervervrnvrarvrrersevsernr 14 1 4 General Testing and Specification Re
17. no greater then the specified value but not more then 0 5 us less than this value The spectra from a successful calibration are saved as H1pw90 The carbon pwx90 calibration is the next experiment The pulse sequence changes from s2pul to PWXCAL The specification for the carbon pw90 and tpwr are used as the target values If no values were specified the default values of 15 us at power in this case pwxlv1 T da i amp of 51 are used as the target values Just as with the proton pw90 calibration the autocalibration makes two attempts to achieve the specification and exits the autocalibration if the target specification is not reached after the second attempt Figure 18 C pwx Array The data from the PWXCAL are saved as C13pwx and shown in Figure 18 46 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 4 6 Data Acquisition Calibration and Indanone Spectra The next two experiments are run only if you have gradients The first experiment calibrates the Z gradient strength produces the profile shown in Figure 19 and stores this information in the parameter gcal The next experiment calculates the ratios of the gradients to be used in various indirect detection experiments and stores this information in the parameter Cgrad Figure 20 Figure 19 Gradient Profile The next calibration is carbon observe pulse width and the pulse sequence i
18. of 2 Ethyl 1 Indanone 53 Figure 31 TOCSY of 2 Ethyl 1 Indanone shows Correlations Among All Protons 00 4 54 Figure 32 TOCSY of 2 Ethyl 1 Indanone Correlations of Protons on C11 C10 C3 54 Figure 33 NOESY Spectrum of 2 Ethyl 1 Indanone esorenonnvernrevrnvvrnvrrvvrreravvrrrvsrversvervvervesvsevneer 55 Figure 34 HSQC Spectrum of 2 Ethyl 1 Indanone ss 55 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 5 Table 1 Table 2 Table 3 Table 4 Table 5 Table 6 Table 7 Table 8 Table 9 List of Tables Samples Required for Console Acceptance Tests rrrnrnvnnrnvnvrnvvervrnvnrvvrarnrrservrnvrarvsrerever 14 Samples for System Calibration ss 21 Sample for Automated Data Acquisition ss 26 Samples for Homonuclear Decoupling Test eee eee ceesse cee ceseeeeceeeeeeeeeeeseeseaeeeaes 31 Sample dor Magnet Drift Test 2 58 ind telle yestadiscsssnesedesasnessbedees 32 Samples for Optional VT Accuracy Test mmmnenereverrarrrvvrrrvrreververvvrsvervversrernervrnvrarvsrersrer 34 Samples for Optional High Stability VT Test 36 Magnet Drift Specifications ss 38 Who to Call for Assistance iii 58 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 SAFETY PRECAUTIONS The following warning and caution notices illustrate the style used in Varian manuals for safety precaution notices and explain when each type is used
19. parameters pw 2 gain 5 or some value that doesn t overload the receiver sw 10000 at 2 nt 1 in n In the acqi window set the lock to Off Disconnect the lock cable and set alock mn The test is run unlocked because the sample has no deuterated solvent to lock on Enter su and check the probe tuning for the ethylene glycol sample Enter ga to acquire the spectrum Place the cursor between the two peaks and enter movetof to move the transmitter offset 4 Click the mouse on the Box menu button to call up right and left cursors Position the right and left cursors on the right and left peaks Enter tempcal glycol 5 Record the temperature reading from the VT controller displayed face of the VT controller and the computer calculated temperature based on the chemical shift frequencies of the two peaks CAUTION Extreme temperatures can damage the probe The high and low temperatues must be within the specified range of the probe 6 Enter temp 50 su to change the temperature to 50 C Allow the sample to stabilize at 50 C for at least 10 minutes after the VT controller has reached the final temperature and regulated Enter ga to acquire a spectrum Repeat steps 4 and 5 7 Make sure that the VT gas flow and cooling air flow levels are between 9 5 to 10 LPM and gas flow to the probe is not restricted in any way Enter temp 100 su to change the temperature to 100 C 34 MERCURYplus Console Acceptance Tests amp Specifications 01 9
20. room temperature Plot a graph of the VT controller reading horizontal axis as compared with the calculated VT reading from the chemical shift differences between the two peaks vertical axis Draw a straight line through the points 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 35 Chapter 2 Console and Magnet Test Procedures 2 7 Stability Calibration for High Stability VT Optional Test This optional test is for high stability VT units only Part No 00 992953 00 The test demonstrates that the VT unit can hold the temperature with 0 1 C The test requires preconditioning of the laboratory air and restricts on the room temperature fluctuations 36 Table 7 Samples for Optional High Stability VT Test Test Sample Nucleus Sample Tube Part Number mm Doped 2 Hz H O0 D 0 0 1 mg ml GdCl H 5 01 901855 01 in 1 H O in D30 Alternatively the customer can request using a 10 mM DSS in D O sample volume of 0 6 ml in a 5 mm NMR tube DSS 3 trimethylsilyl 1 propane sulfonic acid The customer must make this sample using DSS and deuterium oxide 99 8 or 99 9 atom D Upon request Varian can make this sample if DSS is not available at the customer site Probe and Hardware Requirements High stability variable temperature accessory and a 5 mm probe capable of H direct observe are required Test Procedure 1 Enter rtp vnmr tests shmd2o to retrieve the test parameter se
21. to lock and shim automatically In the Text box enter the name of the sample in this case 2 ethyl 1 indanone If the Text box is not visible resize the Setup window until the text entry box is fully visible The Setup window in Figure 5 has been expanded to show the text box Enter an appropriate directory name e g 2 ethyl 1 indanone_C13spectra on the Save As line A directory is created using the name you entered on the Save As line with the current date and time to the name As each experiment finishes the experiment is saved in this directory The individual FIDs have the experiment names e g APT data named APT fid and the DEPT data named DEPT fid etc Click on the Setup button The Setup window closes the CUSTOM icon becomes active and the Acquire icon drops down Click on the Acquire icon and set up the proton decoupled carbon observe experiment by selecting 1000 scans the DO NOT TEST option for CARBON S N TEST and accept the defaults for the remaining options see Figure 12 Click on the following experiments in the order listed 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 29 Chapter 2 Console and Magnet Test Procedures Figure 12 Experiment Window for 13C and 13C Detected Experiments APT click OK to accept the default parameters DEPT click OK to accept the default parameters Each time the OK button is clicked an experiment is added to the list of experiments si
22. 26 C13 and C13 Detected experiments 29 H1 and H1 detected experiments 27 sample required 26 automatic teller machine ATM cards caution 9 B basic system operation 13 broadband operation 13 C calibrate H C Ind Det amp Grad CH3I 24 LOCK gmap and z0 22 ZO and Make LOCK gmap 22 Calibration training 44 adding a probe 44 45 calibration process 45 calibrations 48 cautions defined 7 Command and Parameter Reference 40 computer audit form 12 61 console demonstration 13 console test procedures 21 CP MAS experiments 40 credit cards caution 9 cryogenics handling procedures 13 D decoupling 13 demonstration of system 13 DEPT demonstration 26 Distortionless Enhancement by Polarization Transfer 26 dpwr parameter 31 01 999186 00 B0902 Index E ethylene glycol 34 experiment setup 13 F Filling Cryogens 57 Liquid Helium 57 Liquid Nitrogen 57 flammable gases warning 8 flow rates of nitrogen and helium 56 flowmeters 13 G gamma H2 pw90 relationship 47 Getting Started manual 40 GLIDE AutoCalibration 21 26 probe and system calibration 24 25 reviewing probe and system calibrations 25 ZO and Make LOCK gmap 22 23 H hlsn file 31 helium contact with body 8 helium flowmeter 56 helium gas flowmeters caution 10 high power amplifiers cautions 10 high stability VT units optional test 36 High Temperature Calibrations Test optional 34 homogeneity se
23. 99186 00 B0902 8 2 6 Temperature Accuracy for VT Systems Optional Test Allow the sample to stabilize at 100 C for at least 10 minutes after the VT controller has reached the final temperature and regulated Enter ga to acquire a spectrum Repeat steps 4 and 5 Low Temperature Calibrations Test CAUTION For low temperature calibrations fill the VT dewar with liquid nitrogen 10 11 If a chemical mixture is used instead of liquid nitrogen for low temperature calibrations choose the chemical slurry carefully A mixture of crushed dry ice and acetone is not recommended because it will dissolve the polystyrene VT dewar Tune the probe Use a 99 8 DO sample for shimming the probe Enter rtp vnmr tests shmd20 to retrieve the test parameter set to the current experiment Acquire a normal spectrum and shim the water signal to about 3 to 4 Hz linewidth at 50 Replace the 99 8 DO sample with the 100 methanol sample Part No 00 968 120 80 Set the following parameters pw 2 gain 5 or some value that doesn t overload the receiver sw 10000 at 2 nt 1 in n In the acqi window set the lock to Off Disconnect the lock cable and set alock mn The test is run unlocked the sample lacks deuterated solvent Enter su and check the probe tuning for the methanol sample Enter ga to acquire the spectrum Place the cursor between the two peaks and enter movetof to move the transmitter offset Click on the Box menu button
24. Area Danger Sign Stray magnetic fields can reach beyond the published distances when two or more magnetic fields intersect or when the field extends over large ferromagnetic masses or structures steel doors steel construction beams etc In this case the customer must measure the stray field using a gaussmeter to determine how the 5 and 10 gauss fields are altered contact a scientific instrumentation supplier for information on acquiring a gaussmeter You can request additional signs from Varian by telephoning 1 800 356 4437 in the United States or by contacting your local Varian office in other countries 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications Chapter 1 Introduction 20 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 Chapter 2 Console and Magnet Test Procedures Sections in this chapter 2 1 AutoCalibration and GLIDE Operation Demonstration page 21 2 2 Automated Data Acquisition page 26 2 3 Homonuclear Decoupling page 31 2 4 Magnet Drift Test page 32 2 5 Variable Temperature Operation Optional Hardware page 33 2 6 Temperature Accuracy for VT Systems Optional Test page 34 2 7 Stability Calibration for High Stability VT Optional Test page 36 This chapter contains the procedures required to demonstrate the specifications for MERCURYplus consoles and magnets Chapter 5 Acceptance Test Res
25. Console Acceptance Tests amp Specifications 0902 VARIAN Console Acceptance Tests amp Specifications MERCURYplus NMR Spectrometer Systems Pub No 01 999186 00 Rev BO902 ave TAY Console Acceptance Tests amp Specifications MERCURYplus NMR Spectrometer Systems Pub No 01 999186 00 Rev B0902 Applicability of manual MERCURYplus NMR spectrometer systems Technical contributors Frits Vosman Steve Cheatham Everett Schreiber Technical writer Everett Schreiber Dan Steele Technical editor Dan Steele Revision history A0402 Initial release E R B0902 Changed magnet drift test sample from IH lineshape to doped 1 H O in D 0 Copyright 2001 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 circuit described herein neither does it convey any
26. ERCURYplus Console Acceptance Tests amp Specifications 21 Chapter 2 Console and Magnet Test Procedures Run the lineshape tests described in the probe manual before running AutoCalibration Run the AutoCalibration as described in this section Run the signal to noise test described in the probe manual Use the pw90 determined by the AutoCalibration routine Setting Up Probe Calibration Files Before you calibrate a probe for the first time you must set up the probe calibration file with the addprobe command as described below l 2 Log in as vnmr1 Enter one of the following command addprobe probe_name The probe calibrations are written to the probe file in vnmr1 vnmrsys probe probe name and are available only to the user vnmr1 _OR addprobe probe name system The calibrations are written to vnmr probe probe name and are available to all users Some probes like the Autoswitchable and 4 nucleus probes require additional calibrations not covered in this manual For information on using GLIDE to compleat the calibration of these probes see the Walkup NMR manual and installation testing and specifications manual the Probe Calibrating ZO and Make LOCK gmap Before preceding any further the lock and gradients must be calibrated for the autoshim and autolock procedures to function efficiently This procedure calibrates ZO and makes a gradient map for gradient shimming l 2 Insert the doped 2 Hz D20 s
27. If no calibration file exists for the probe or if the probe is new add the probe using the addprobe command At this point you are ready to begin the calibration process Upon completion of the calibration 1D and 2D spectra of the test sample can be obtained using GLIDE After the 1D and 2D spectra are obtained continue with the Automated Data Acquisition described in 2 2 Automated Data Acquisition page 26 A series of spectra is acquired The first of the spectra shown in Figure 16 is a H observe with CDCI as the lock solvent This data is saved as Hiref This spectrum contains three BCHI resonances centered at about 2 2 ppm The center resonance is from the protons attached to carbon 12 and the two outer resonances are from the protons attached to carbon 13 The other resonances in the sample are from trimethylphosphite that has reacted with the methyl iodide which was initially 100 C enriched eal ie een Se A 5 5 5 0 4 5 4 0 3 5 3 0 2 5 2 0 1 5 1 0 0 5 ppm Figure 16 IH Spectrum of 13C Methy1 Iodide All trimethylphosphite has reacted to form a phosponate ester CH3 P OXOCHx3 This phosponate ester has a doublet at about 1 5 ppm methyl group attached directly to SIP and a triplet of doublets centered around 4 ppm that arise from UG outer pair of doublets and 12C inner doublet of the methyl ester The analysis of this sample is fully discussed in an article by Paul Keifer in Magneti
28. aining 50 2 Ethyl 1 Indanone Spectra The proton NMR shows several distinct features First there are some impurities in the sample These impurities shown in Figure 25 are at the 2 level and some crosspeaks will show up in the 2D The very large triplet for the methyl group has BC satellites at J 125 Hz The CHClg singlet at 7 24 ppm is the Ia i i Li residual CHCI in the ps CDCI solvent ao ve The protons are assigned Figure 25 Proton Spectrum of 2 Ethyl 1 Indanone in the two expansions The assignments are based upon the 2D data for the compound The protons of the two CH groups in the molecule shown in Figure 26 are magnetically nonequivalent and show up as individual multiplets The signals at 1 9 ppm and 1 55 ppm belong to protons on carbon 10 The two double doublets at 2 8 ppm and 3 26 ppm belong to protons on carbon 3 A complex multiplet at 2 6 ppm is the single proton on carbon 2 3 4 3 2 3 0 2 8 2 6 2 4 2 2 2 0 1 8 1 6 1 4 1 2 1 0 ppm Figure 26 Aliphatic Region of the 2 Ethyl 1 Indanone Spectrum The protons of the aromatic ring shown in Figure 27 are assigned based on the gHMBC and gCOSY data Some minor impurities can be seen as well as the residual CHCl signal If the sample is shimmed very well there may be some truncation artifact on the CHCl signal MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 4 6 Data Acquisiti
29. al that is supplied with the magnet should be consulted for the exact interval between liquid helium fills and specific details on routine liquid helium fills Depending upon the type of dewar the exact details and procedures for liquid helium filing will vary consult the Oxford Magnet Manual supplied with your magnet CAUTION Failure to maintain the correct liquid helium levels may lead to a quench of the magnet WARNING Wear goggles and loose fitting protective gloves while working with cyrogens 4 8 30 Day System Maintenance The following procedures must be performed while logged in as vnmr1 1 Updating Solvent Shims Reshim lineshape and then save shims to vnmr shims acetone Refer to the Acceptance Test Procedures amp Specifications for the specific probe and to Getting Started Section 6 9 Saving and Retrieving Shim Values 2 Check Calibration of pw90 and tpwr as described in 2 1 AutoCalibration and GLIDE Operation Demonstration page 21 3 Update the lock frequency as described in the Software Installation manual Appendix B 4 Check magnet drift as described in 2 4 Magnet Drift Test page 32 5 Perform hard drive maintenance delete unused files directories old FIDs macros shims or users 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 57 Chapter 4 Customer Training 4 9 Warranty and Who to Call for Assistance The installation engineer will explain the standa
30. ample see Table 2 Open the acqi window by pressing the acqi button on the VNMR menu Lock onto the D20 resonance The lock must be set on resonance Adjust Z0 as necessary Adjust Lock Gain and Lock Power and set the lock level at 80 Exit acqi Open GLIDE by clicking on the GLIDE button in the VNMR menu and click the Setup icon in GLIDE 22 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 Running AutoCalibration 1 2 1 AutoCalibration and GLIDE Operation Demonstration Click on the GLIDE Setup button in the GLIDE interface The Experiment and Calibration Setup window Figure 4A is displayed Right mouse click the button next to Experiment to display the experiment and calibration menu A Experiment Setup Window Right mouse click on Generate Ik gmap amp calibrate z0 D20 selection from the menu Figure 4B Right mouse click the button next to Solvent to display the solvent menu Figure 4C Right mouse click on D20 Set Autoshim and Autolock to NO Click on Setup B Select Calibration from Experiment Menu Standard proton parameters are recalled and the sample confirmation window appears The message Set z0 exactly on resonance before starting acquisition displays in the VNMR window Open the lock display and set the lock as directed Click on the GO button in GLIDE to run the calibration When the calibration is completed the p
31. atter of good laboratory practice to check the calibration All calibration spectra are saved in export home vnmri vnmrsys data probe_ calibs probename_calib date Probe calibrations executed by vnmr1 are written to probe files one of two places Ifthe probe name was created as a system probe and the probe name is unique it does not exist in export home vnmri vnmrsys probe it is written to vnmr probes probe name If the probe name was not created as a system probe or the probe name is not unique it does exist in export home vnmr1 vnmrsys probe it is written to export home vnmr1 vnmrsys probes probe name Before you begin the calibration procedure check the probe parameter This parameter should be set to the probe that is currently installed in the magnet If this is not true set the parameter to the name of the probe that is currently installed The names of the installed user level and system level probes can be obtained as shown in the following example Open a terminal window User level probes gt cd vnmrsys probes gt lf gt hen HFCN System level probes 44 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 4 6 Data Acquisition Calibration and Indanone Spectra gt cd vnmr probes gt lf gt GHX BB10mm probe tmplt The actual probe directory names on your system might be different The probe parameter must match one of the these directory names
32. bes On systems with solids high power amplifiers never operate the amplifiers with a liquids probe The high power available from these amplifiers will destroy liquids probes Use the appropriate high power probe with the high power amplifier Take electrostatic discharge ESD precautions to avoid damage to sensitive electronic components Wear a grounded antistatic wristband or equivalent before touching any parts inside the doors and covers of the spectrometer system Also take ESD precautions when working near the exposed cable connectors on the back of the console Radio Frequency Emission Regulations The covers on the instrument form a barrier to radio frequency rf energy Removing any of the covers or modifying the instrument may lead to increased susceptibility to rf interference within the instrument and may increase the rf energy transmitted by the instrument in violation of regulations covering rf emissions It is the operator s responsibility to maintain the instrument in a condition that does not violate rf emission requirements 10 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 Chapter 1 Introduction Sections in this chapter 1 1 Overview of the Acceptance Testing Process this page 1 2 General Acceptance Testing Requirements page 14 1 3 Samples Required for Acceptance Tests page 14 1 4 General Testing and Specification Requirements page 14 1 5 Var
33. c Moments Keifer P A Magnetic Moments 1996 8 2 18 20 The reaction results in a sample is partially enriched to give approximately 60 abundance of carbon 13 in methyl iodide The natural abundance of carbon 13 is 1 1 so this level of enrichment is more then adequate for the purposes of calibration 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 45 Chapter 4 Customer Training The next spectrum shown in Figure 17 is an array of increasing IH pulse widths based on the H pulse you specified in the Acquire window If you did not enter a value for the pulse width it is set to the default targets pw90 is set to 15 us and tpwr of 51 UU r Ly n Figure 17 IH pw Array The observe transmitter power is set to the value you specified and reduce by 3 for the first test If the resulting pw90 is shorter then the value you specified or the default if you did not specify a pw90 target the next test is started If the pw90 is longer then the target the observe power is increased Two attempts are made If the calibration fails to achieve a pw90 that is less than the specified pw90 the autocalibration exits If either attempt yields a pw90 that is less then the specified value the autocalibration routine adjusts the observe power the remaining tests are aborted If the pw90 is less then the specified value the autocalibration then adjusts the power until the measured pw90 is
34. ct Code License Agreement Varian and OEM manuals Warranty coverage and where to telephone for information MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 1 1 Overview of the Acceptance Testing Process 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 The following are demonstrated Posting requirements for magnetic field warning signs Cryogenics handling procedures and safety precautions Magnet refilling Flowmeters Homogeneity disturbances Console and Probe Demonstration The following are demonstrated Loading programs VNMR Optional VNMR packages Solaris Experiment setup including installing the probe in the magnet Basic instrument operation to obtain typical spectra including probe tuning magnet homogeneity shimming and printer plotter operation Note that Varian installation engineers are not responsible for or trained to run any spectra not described in this manual Auto calibration using the GLIDE or Tc1 dg interface of key probe parameters such as H pw90 13C pwx90 decoupler field gradi
35. d in detail in the Getting Started manual The vnmr directory and file structure is set up with the global or system files and directories that are have read and execute permission for all users and a group of user files and directories that the user has read write and execute permissions The global or system files and directories are administrated by the user vnmr1 These files and directories are located in export home vnmr which is also accessed via the symbolic link in root vnmr Only the user vnmr1 and root have read write and execute permissions while others have read and execute permission for files and directories in this area If you must make changes to VNMR files and directories make them as vnmrl not as root The global or system files 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 41 Chapter 4 Customer Training acq KEY file acqbin autotest glide Symbolic link help manual dialoglib kermit log acrobat bin fidid fid fidlib fid2d fid psg d Q m app defaults asm nuctables boot message 3 D a Le ex vnmrmenu menulib vnmrrev el ia H og devicetable Le a 2 H user templates usr
36. during system installation To identify the precise methods by which these tests are performed To leave the instrument in a calibrated ready to use state 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 11 Chapter 1 Introduction 12 Acceptance Tests Acceptance test procedures are arranged by the type of specification These procedures cover the basic specifications of the instrument signal to noise resolution and lineshape and are not intended to reflect the full range of operating capabilities or features of a MERCURYplus NMR spectrometer The order in which the tests are performed is determined by the installation engineer although the order does not matter except that some procedures use results from other procedures Performance of 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 for 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 MERCURYplus No guarantee is gi
37. e MERCURYplus spectrometer system and hardware User Programming Provides details about the VNMR macro programming language Magical II and pulse sequence statements This manual contains the information necessary to write custom macros edit existing macro write new pulse sequences and edit existing pulse sequences 4 2 Host Computer Setup and Software Installation Host computer setup and software installation is covered in detail in the VNMR and Solaris Software Installation manual NMR data is processed and displayed using the Sun host computer which is connected to the MERCURYplus NMR spectrometer with an Ethernet cable Setting up the host computer involves the following general steps Unpacking the Sun computer Connecting peripheral devices Connecting the Sun computer to the MERCURYplus console Installing the Solaris operating system software including UNIX Installing the VNMR software Configuring system hardware Setting up user accounts Setting printers and plotters During this process the Sun hard disk is laid out specifically for the needs of the VNMR software and NMR operation VNMR is installed in the directory export home and a link called vnmr is placed at the root level User accounts are also installed in export home Software is installed from CD ROMs 4 3 VNMR Directory Structure An overview of the VNMR directory and file structure is shown in Figure 15 This file structure is discusse
38. e S N Sales Order No Magnet S N Shipment Damage Preinstallation Preparation Line voltage measured Vac console accessory Line pressure air No Air conditioning Cryogens liters LHe LN Testing 1 Acceptance tests and computer audit Acceptance tests procedures finished ___ Test results form completed and signed _ Computer audit completed and signed 2 System documentation review Software Object Code License Agreement acceptance of product constitutes acceptance of ___ object code license regardless of whether agreement is signed or not ___ Varian and OEM manuals ___ Explanation of warranty and where to telephone for information 3 Installation Training 4 Installation Customer Training Check list 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 65 Chapter 5 Acceptance Test Results Notes 66 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 5 4 Supercon Shim Values 5 4 Supercon Shim Values Fill in the following information Magnet Frequency and Serial Number Magnet Frequency Serial Number Measurement in Helipot Amps Measurements Measurement X2 Y2 Drift Spacers Main Field Current Customer Signature Varian Representative Signature 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 67 Chapter 5 Acceptance Te
39. e at the time of installation the range of VT demonstration is limited to temperatures between 30 C and 100 C Basic Specifications The specifications for variable temperature ranges are listed with each probe 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 37 Chapter 3 Consoles and Magnets Specifications 3 3 Magnet Drift Table 8 lists the drift specifications for magnets Specifications for nominal field decay rate are less than or equal to the values listed in the table Table 8 Magnet Drift Specifications System Field Strength Nominal Field Decay Rate MHz mm T Hz hr 200 54 4 70 2 300 54 7 05 3 400 54 9 40 8 3 4 Temperature Accuracy for VT Accessories The temperature reading displayed on the VT unit display panel should be within 1 C of the actual temperature reading as measured from the chemical shift 3 5 Stability Calibration for High Stability VT Accessory The high stability VT accessory holds the set temperature to within 0 1 C 0 19C 0 001 ppm or in field dependent terms 0 2 Hz at 200 MHz 0 3 Hz at 300 MHz and 0 4 Hz at 400 MHz 38 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 Chapter 4 Customer Training Sections in this chapter 4 1 Where to Look for Answers this page 4 2 Host Computer Setup and Software Installation page 41 43 VNMR Directory Structure page 41 4 4 Managing Di
40. ecifications 01 999186 00 B0902 Chapters Acceptance Test Results This chapter contains the following forms for recording system information and acceptance test results 5 1 Computer Audit page 61 e 5 2 Installation Customer Training Checklist page 63 5 3 System Installation Checklist page 65 5 4 Supercon Shim Values page 67 5 5 Console and Magnet Test Results page 69 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 59 Chapter 5 Acceptance Test Results Notes 60 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 5 1 Computer Audit 5 1 Computer Audit Information about your site please print Company University Address Principal User Phone Spectrometer type Fax Console S N Sales Order No Delivery month day Information on each computer additional forms are on the back of this page Include computers directly attached to the spectrometer computers networked or non networked on site or off site used to process NMR data using Varian s VNMR software and computers on site and off site used to process data collected on this spectrometer with software from other vendors Information on computer of e g 1 Of 3 Manufacturer Model no Computer S N Purchased from Memory Mbytes Screen size in Peripherals Internal hard disk Mbytes Exter
41. enmark Herlev 42 84 6166 France Orsay 1 69 86 38 38 Germany Darmstadt 6151 70 30 Italy Milan 2 921351 Japan Tokyo 3 5232 1211 Korea Seoul 2 3452 2452 Mexico Mexico City 5 523 9465 Netherlands Houten 0118 61 71 56 Norway Oslo 9 86 74 70 Russian Federation Moscow 95 241 7014 Spain Madrid 91 472 7612 Sweden Solna 8 445 1601 Switzerland Zug 41 749 88 44 Taiwan Taipei 2 2698 9555 United Kingdom Walton on Thames England 1932 898 000 United States Palo Alto California Varian Inc NMR Systems Customer Sales Support 650 424 5434 Service Support Palo Alto California 1 800 356 4437 E mail custserv Q varianinc com North American Service Manager 9017 Mendenhall Ct Ste D Columbia MD 21045 410 381 7229 Venezuela Valencia 41 257608 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 17 Chapter 1 Introduction 1 6 Posting Requirements for Magnetic Field Warning Signs 18 The strong magnetic fields that surround a superconducting magnet are capable of causing death or serious injury to individuals with implanted or attached medical devices such as pacemakers or prosthetic parts Such fields can also suddenly pull nearby magnetic tools equipment and dewars into the magnet body with considerable force which could cause personal injury or serious damage Moreover strong magnetic fields can erase magnetic media such as tapes
42. ent grade 25 to 100 5 00 968120 79 High The samples required for acceptance testing of any individual probe are supplied with the probe Typical samples required for probe acceptance tests are chloroform in acetone dg ethyl benzene in chloroform d and ASTM 40 p dioxane in 60 benzene d6 Other samples might be required depending upon the type of probe The specific sample requirements and test procedures are specified in the manual for each probe 1 4 General Testing and Specification Requirements 14 The MERCURYplus 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 except autoswitchable probes operated in 4 nucleus mode The 136 quarter wavelength cable is used in this case MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 1 4 General Testing and Specification Requirements 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 svs sw5res These values can then be used as a starting point when adjusting the homogeneity on unknown samples by the command rts sw5res
43. ent provides temporary storage of the data The data in the experiment work space remains intact until an acquisition is started in that experiment a previously saved data set is loaded into the current experiment or the current experiment is deleted see the Getting Started manual for details on creating and deleting experiments in VNMR The amount of disk space consumed by an experiment depends upon the type of NMR experiment To manage this users should save their data and either remove the experiment delete the experiment workspace execute a simple experiment that uses little disk space s2pul with np 8k for example or load a previously saved data set that has a small number of data points defining the FID Saving the data to a directory that is on the same slice or partition as the user s vnmrsys will not improve matters The saved data should be placed in a directory on a different slice a different physical hard disk a network server disk or copied to some archive such as a tape The contents of directories such as maclib seqlib etc do not tend to fill up with old files that quickly except for users that are developing pulse sequences macros etc Old shim files tend to accumulate and can be cleared out from time to time Periodic archiving of important spectra to tape central file servers etc and removal of these files from the disk is necessary Small data files can be copied to floppy disks The use of tapes and floppy disks i
44. ent strength if gradients are present and other probe specific parameters Demonstration of automated data acquisition via GLIDE interface Using the 2 Ethyl 1 indanone sample provided with the console the following experiments will be run 1D Experiments IH Be lg APT and DEPT 2D Non gradient experiments NOESY and TOCSY for non gradient system or probe COSY is also run 2D Gradient experiments gCOSY gHSQC gHMBC will be demonstrated if gradients are present Walk through the demonstration spectra and the Data Acquisition Calibration and Indanone Spectra page 44 Demonstration of gradient shimming using PFG gradients if present or homospoil Review how to use the manuals online and hard copy and where to find information Review the post installation 30 day check list Detailed specifications and circuit descriptions are not covered Formal training in the operation and maintenance of the spectrometer is conducted by Varian at periodically scheduled training seminars held in most Varian Application Laboratories Installation engineers are responsible for guiding you through the acquisition of the spectra as provided in the manual The installation engineer is not responsible for interpretation of the results beyond what is provided in this manual On site training is 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 13 Chapter 1 Introduction available in some geog
45. er 2 Console and Magnet Test Procedures 2 6 Temperature Accuracy for VT Systems Optional Test The optional tests in this section check temperature accuracy calibrations for high and low temperatures using ethylene glycol and or methanol respectively Table 6 lists the samples for low temperature and high temperature tests Table 6 Samples for Optional VT Accuracy Test Temperature Range Sample Tube Sample Part sample C mm Number 100 methanol reagent grade 50 to 25 Low 5 00 968120 80 100 ethylene glycol reagent grade 25 to 100 High 5 00 968120 79 Probe and Hardware Requirements The variable temperature accessory and a VT probe are required Run VT tests with a 5 mm probe capable of IH direct observe from 150 C to 200 C For probes that have a more limited temperature range particularly PFG probes run the test at two or three temperatures that fall within the VT range of the probe These tests can also be run using the H decoupling coil of the 5 mm broadband probe as H direct observe High Temperature Calibrations Test 1 Tune the probe Use a 99 8 D20 sample not supplied by Varian for shimming 2 Enter rtp vnmr tests shmd2o to retrieve the test parameter set to the current experiment Acquire a normal spectrum and shim the water signal to about 3 to 4 Hz linewidth at 50 3 Replace the 99 8 DO sample with the 100 ethylene glycol sample Part No 00 968 120 79 Set the following
46. et S N Magnet Familiarization Done Topic Reference Overall magnet familiarization LHe and LN top off procedures Use of flow meters Antivibration system operation Posting of magnetic field warning signs Oxford Magnet Reference Manual Oxford Magnet Reference Manual and Lhe refill video Oxford Magnet Reference Manual Antivibration Accessory Installation Manual Installation Planning Guide Probes Done Topic Reference Eu Probe installation removal tuning and filter setup for ID and TR experiments VT system installation VT system operation Choose a specific probe manual AutoSwitchable probes Broadband probes Indirect Detection probes Nano probes Switchable probes Flow probes Variable Temperature Unit Installation User Guide Liquids NMR Chapter 8 Console Done Topic Reference Major component overview Shut down procedures Host console connection and overview System Overview System Administration manual 3 1 3 2 3 3 System Administration manual 3 1 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 63 Chapter 5 Acceptance Test Results Host Computer Done Topic Reference Host computer setup Solaris and VNMR software installation Directory structure overview Using acqproc and makeuser commands Shutdown and startup of UNIX S
47. fications for the MERCURYplus spectrometer and magnet Included in this manual is the information used by the installation engineer in the introductory training at the end of the installation This manual does not cover the probe test procedures VNMR and Solaris Software Installation Details the installation of the Sun host computer hardware and the Solaris and VNMR software Detailed instructions on system configuration are included here Also included in this manual are instructions for setting up various plotters and printers and other administration tasks MERCURYplus CP MAS Accessory Installation Describes how to install and test the CP MAS accessory Probe installation testing and specifications manuals Each type of probe has its own installation test and specifications manual In these manuals are the detailed instructions for installing tuning testing the probe Accessory manuals Each accessory is covered in an independent manual which contains installation testing and sometimes operation instructions MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 4 2 Host Computer Setup and Software Installation Technical References System Schematics Provides schematic and technical drawings for MERCURYplus NMR spectrometer systems Technical Reference Provides technical details of the spectrometer systems and electronics System Description Provides an overview of th
48. helium or nitrogen contacts the body seek immediate medical attention especially if the skin is blistered or the eyes are affected 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 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 Warning Notices continued WARNING Support the magnet and prevent it from tipping over The magnet dewar has a high center of gravity and could tip over in an earthquake or after being struck by a large object injuring personnel and causing sudden dangerous release of nitrogen and helium gasses from the dewar Therefore the magnet must be supported by at least one of two methods with ropes suspended from the ceiling or with the antivibration legs bolted to the floor Refer to the Installation Planning Manual for details WARNING Do not remove the relief valves on the vent tubes The relief valves prevent air from entering the nitrogen and
49. helium vent tubes Air that enters the magnet contains moisture that can freeze causing blockage of the vent tubes and possibly extensive damage to the magnet It could also cause a sudden dangerous release of nitrogen and helium gases from the dewar Except when transferring nitrogen or helium be certain that the relief valves are secured on the vent tubes WARNING On magnets with removable quench tubes keep the tubes in place except during helium servicing On Varian 200 and 300 MHz 54 mm magnets only the dewar includes removable helium vent tubes If the magnet dewar should quench sudden appearance of gases from the top of the dewar and the vent tubes are not in place the helium gas would be partially vented sideways possibly injuring the skin and eyes of personnel beside the magnet During helium servicing when the tubes must be removed carefully follow the instructions and safety precautions given in the manual supplied with the magnet Caution Notices Observe the following precautions during installation operation maintenance and repair of the instrument Failure to comply with these cautions or with specific cautions elsewhere in Varian manuals violates safety standards of design manufacturing and intended use of the instrument Varian assumes no liability for customer failure to comply with these precautions CAUTION Keep magnetic media ATM and credit cards and watches outside the 5 gauss perimeter from the centerl
50. ian Sales Offices page 17 1 6 Posting Requirements for Magnetic Field Warning Signs page 18 Following each installation of a Varian Inc MERCURYplus NMR spectrometer system an installation engineer tests and demonstrates the instrument s operation using the procedures in this manual This manual contains the acceptance test procedures and specifications for MERCURYplus NMR spectrometers The following is an overview of the chapters in this manual Chapter 2 Console and Magnet Test Procedures provides the acceptance test procedures Chapter 3 Consoles and Magnets Specifications provides the acceptance test specifications Chapter 4 Customer Training provides basic spectrometer maintenance and operation training Chapter 5 Acceptance Test Results contains forms for recording test results The acceptance test procedures and specifications for each probe are contained in a separate probe family manual for example procedures and specifications for AutoSwitchable probes are contained in the AutoSwitchable NMR Probes manual Only the lineshape and signal to noise tests are preformed manually All other probe calibrations are performed by the instrument during the auto calibration procedures The manual tests are provided as a reference 1 1 Overview of the Acceptance Testing Process The objectives of the acceptance tests procedures are threefold To identify the tests to be performed
51. ields are present that can cause serious injury or death to persons with implanted or attached medical devices such as pacemakers and prosthetic parts Such persons must not go closer to the magnet than this sign until safety at a closer distance is identified by a physician or device Magnetic Media ATM Credit Cards Strong magnetic fields are present that can erase magnetic media disable ATM and credit cards and damage some watches Do not take such objects closer to the magnet than this sign r IAN a ave Pub No 87 250300 00 B0694 5 Gauss Waring Sign VA Figure 1 10 Gauss Warning Sign Figure 2 5 Gauss Warning Sign Pub No 87 250801 00 80694 Magnet Area Entrance Danger Sign Amma STRONG MAGNETIC AND RADIO FREQUENCY FIELDS ARE PRESENT Tools and Equipment Magnetic Media and ATM Credit Cards Strong magnetic fields are present that could erase magnetic media such as floppies and tapes disable ATM towards the magnet body which and credit cards and damage some watches Do not take such objects closer to the magnet than the 5 GAUSS WARNING signs Strong magnetic fields are present that could make some magnetic items suddenly fly could cause personal injury or serious damage Do not take tools equipment or personal items containing steel iron or other magnetic materials closer to the magnet than the 10 GAUSS WARNING signs aw VARIAN Figure 3 Magnet
52. ine of the magnet The strong magnetic field surrounding a superconducting magnet can erase magnetic media such as floppy disks and tapes The field can also damage the strip of magnetic media found on credit cards automatic teller machine ATM cards and similar plastic cards Many wrist and pocket watches are also susceptible to damage from intense magnetism Refer to the manuals supplied with the magnet for the size of a typical 5 gauss stray field This gauss level should be checked after the magnet is installed 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 9 Caution Notices continued CAUTION CAUTION CAUTION CAUTION Keep the PCs including the LC STAR workstation beyond the 5 gauss perimeter of the magnet Avoid equipment damage or data loss by keeping PCs including the LC workstation PC well away from the magnet Generally keep the PC beyond the 5 gauss perimeter of the magnet Refer to the Installation Planning Guide for magnet field plots Check helium and nitrogen gas flowmeters daily Record the readings to establish the operating level The readings will vary somewhat because of changes in barometric pressure from weather fronts If the readings for either gas should change abruptly contact qualified maintenance personnel Failure to correct the cause of abnormal readings could result in extensive equipment damage Never operate solids high power amplifiers with liquids pro
53. interface once for H1 and H1 detected experiments and once of the C13 and C13 detected experiments H1 and H1 Detected Experiments l 10 11 Open GLIDE by clicking on the GLIDE button in the VNMR menu Click the Setup icon Insert the indanone sample Table 3 use the Eject and Insert buttons see Figure 5 From the Experiment menu select H1 and H1 detected Expt Right click the Experiment menu and left click H1 and H1 detected Expt From the Solvent menu select CDCI3 Set Autoshim and Autolock Click the No button if your sample is already locked and shimmed Click the YES button to lock and shim automatically Enter the sample name 2 ethy1 1 indanone in the text box If the Text box is not visible resize the Setup window until the text entry box is fully visible The Setup window in Figure 5 has been expanded to show the text box Enter an appropriate directory name e g 2 ethyl 1 indanone_H1spectra on the Save As line A directory is created using the name you entered on the Save As line with the current date and time to the name As each experiment finishes the experiment is saved in this directory The individual FIDs have the experiment names e g cosy fid tocsy fid etc Click the Setup button The Setup window closes the Custom icons become active and the Acquire icon drops down Click the Acquire icon to select the experiments After you click on the Acquire icon one of two possible
54. milar to Figure 13 displays in the VNMR Text pane see Figure 13 in the order they will be run Experiment 1 CARBON Experiment 2 APT Experiment 3 DEPT Figure 13 13C and 13C Detected Experiment List 10 Click the Do button to begin acquisition 30 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 2 3 Homonuclear Decoupling 2 3 Homonuclear Decoupling Use this procedure to calibrate homonuclear decoupling power values Samples Table 4 Samples for Homonuclear Decoupling Test Sample Tube Sample Part Test Sample mij Number 0 1 ethylbenzene 0 01 TMS gt 00 968 120 70 99 89 deuterochloroform CDCI3 0 1 ethylbenzene 0 01 TMS 10 00 968 123 70 99 89 deuterochloroform CDCI3 Hardware A 5 mm probe capable of H direct observe should be used for this test Procedure 1 Enter rtp vnmr tests Hisn 2 Tune the probe Set nt 1 Run a normal spectrum without decoupling 3 Set dm nny Use the cursor and sd to set the decoupler on the central line of the triplet and then run a decoupled spectrum Possible dpwr values are 0 to 49 49 is maximum power in steps of 1 0 dB 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 isa good starting point 4 Observe that the quartet collapses to a single peak with no remaining evidence of splitting 5 Write the results on the f
55. mr 4 4 Managing Disk Space The primary tool used by the system administrator to manage disk space is the UNIX command df k see the System Administration manual for more details This command may be executed from any terminal window by any user The output from this command may look like this In this example user accounts are placed in export home lt user gt in the root File system kbytes used avail capacity Mounted on dev dsk cot0d0s0 2467482 1818540 599593 76 proc 0 0 0 0 proc fd 0 0 0 0 dev fd swap 243472 496 242976 1 tmp dev dsk c0t0d0s1 1372362 477485 839983 37 space directory In some installations export home lt user gt maybe a separate slice or partition There are two user accessible slices or partitions on this disk dev dsk c0t0d0s0 mounted on dev dsk c0t0d0s1 mounted on space When a partition or slice has reached 90 of its capacity it is time to do some maintenance UNIX will in some cases allow the capacity to exceed 100 but this is not a good condition In the worst case if the file system or slice containing the user s vnmrsys directory becomes full the system may stop during a go or VNMR will not load or process a data set This situation can lead to data being lost Each user account has a vnmrsys directory contain maclib seqlib and other needed VNMR directories Also within the user s vnmrsys directory is a directory for each experiment work space Each work space or experim
56. nal adjustments Dangerous high voltages that can kill or injure exist inside the instrument Before working inside a cabinet turn off the main system power switch located on the back of the console then disconnect the ac power cord Do not substitute parts or modify the instrument Any unauthorized modification could injure personnel or damage equipment and potentially terminate the warranty agreements and or service contract Written authorization approved by a Varian Inc product manager is required to implement any changes to the hardware of a Varian NMR spectrometer Maintain safety features by referring system service to a Varian service office 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 liquid helium or nitrogen contact with any part of the body In contact with the body liquid helium and nitrogen can cause an injury similar to a burn Never place your head over the helium and nitrogen exit tubes on top of the magnet If liquid
57. nal 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 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 61 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 of ____ e g 2 Of 3 Manufacturer Model no Computer S N Purchased from Memory Mbytes Screen size in Peripherals Internal hard disk Mbytes External hard disk Mbytes Tape drive size
58. nce suisses 56 P TIOUIG CHEEKS 5 din EE 56 PHARE CE OR sn nude Annie nan aes 57 4 8 30 Day System Maintenance iii 57 4 9 Warranty and Who to Call for Assistance rrerrnerrarvererrnvrrrvrrnrrrvernvnnneeververrrervererere 58 Chapter 5 Acceptance Test Results nn 59 3 A Computer Audit ax ccccssicc sceetssevescdcecetvadebscecdsedenssbelseusdssschabesscotsasuevssibet dobwaddvesdetensenescav 61 5 2 Installation Customer Training Checklist 0 eee cece ceeceeeeeceseeseceecseenaesneeeaeerens 63 5 3 System Installation Checklist ss 65 5 4 Supercon Shim Values sise 67 5 5 Console and Magnet Test Results ss 69 4 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 List of Figures Figure 1 10 Gauss Warning Sign ss 19 Figure 2 5 Gauss Warning Sign ses 19 Figure 3 Magnet Area Danger Sign ss 19 Figure 4 GLIDE Calibrate LOCK ere 23 Figure 5 GLIDE Setup Window and Drop Down Experiment Menu 24 Figure 6 Acquisition Setup Window sise 25 Figure 7 Probe Administration from Setup EXP 25 Figure 8 Experiment Selection Window for Gradient Experiments esnvrnvrrvvavvvrvvnvnrvvravravvrrerarnn 28 Figure 9 Experiment Selection Window for Nongradient Experiments 28 Figure 10 NOESY Acquisition Parameter Window 28 Figure 11 1H and 1H Detected Experiment List 29 Figure 12 Experiment Window for 13C and 13C Detected Experiments usornvrrnv
59. nnnnnnnner 37 3 1 Homonuclear Decoupling sisi 37 3 2 Variable Temperature Operation ss ss 37 Mapnet Drift 2 san an A keen 38 3 4 Temperature Accuracy for VT Accessories mmrmverrvereerrevrervrrrrarerrerrrnsrrverveenverseevnee 38 3 5 Stability Calibration for High Stability VT Accessory oo cee eeseseeseeeeeeeceeeeeeeeeeeees 38 Chapter 4 Customer Training esrnrnnnnnnnnnnnvnnnnnnnnnnnnnnvnnnnnennnnnnnnnnnnnnnnnnnnnnnnnnvenen 39 4 1 Where to Look for Answers iii 39 Operation Manualg enmneetsnednandiiegnnenintvbdteieinseiiein 40 InStallat10ns sm scivscoscezssend dvedatcadeasecsnesdedesvengevenevees ienvetsdeysneubtonsegetenseadesabenaenvecse 40 Techical Referenc s sank ie dennes 41 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 3 Table of Contents 4 2 Host Computer Setup and Software Installation mererrvrrnrornrvvrnvranvrnnennverneevrarvarvrere 41 4 3 VNMR Directory Structure iii 41 4 4 Managing Disk Space merovernernrevrarvrrernenrrevesnrrsnervvevvensenvunsvreevavvravvssvrasvavevesvvenvensensner 43 45 Tunmg Probes es sepeceesceusessvenseoesselenbevaetsveesnsvorhte ERA RETER NEOR Reet 44 4 6 Data Acquisition Calibration and Indanone Spectra sernrernervrnvravvrnvravververrrevrervrere 44 The Calibration Process i cs ci c505 aseienesscvabv ssnccnevsenienvecedesartvatedveletessesestebessevueess 44 JE led Indanone Specifa eirese aee eaei Rene EAO SEEE a EOE 50 4 7 Magnet Maintena
60. nrnrvvrnvravvrverarnr 30 Figure 13 13C and 13C Detected Experiment List 30 Figure 14 MERCURYplus Online Manual Menu 39 Figure 15 VNMR Directory Structure nesinori reog e a EE raa E Eras 42 Figure 16 IH Spectrum of 13C Methyl I 01001 nt Martinet 45 Figure 17 IH DW AA ne bec rein AE E a EE nee Ne Morel ion dien ee da ttes 46 Figure 18 me PWX ATTAY nr dip ccivssaceesecnscavecsdcad ches codsteibeedepaneeteevevenconds durselsscevecesten sossaeedebbeaviccys 46 Figure 19 Gradient Profl ussssnns eneste scasesscnsceiacvssnevotsceusnaia tei EE EREE sets ba E E Ea NEES 47 Figure 20 Gradient Calibrations EE NEEE EEEREN EEEN E EEE 47 Figure 21 Proton Coupled e Spectrum of 13C Methyl Iodide ssssssssesnsmiatsdid 48 Figure 22 13C Observe pw Array of Proton Coupled Spectra ce eceeeseeceseeerceeeeeeseeeeeeenes 48 Figure 23 Proton Decoupler dof Array sise 49 Figure 24 Calibration of the Decoupler 90 Pulse Width pp 49 Figure 25 Proton Spectrum of 2 Ethyl 1 Indanone sserervorenrrnorvvvnverrvvrnvevnvevserveersnevsrerevrservserven 50 Figure 26 Aliphatic Region of the 2 Ethyl 1 Indanone Spectrum 50 Figure 27 Aromatic Region of the 2 Ethyl 1 Indanone Spectrum 51 Figure 28 Gradient COSY of 2 Ethyl 1 Indanone ss 52 Figure 29 Gradient COSY gCOSY of Aliphatic Region of 2 Ethyl 1 Indanone 53 Figure 30 Gradient COSY gCOSY of the Aromatic Region
61. o to Call for Assistance 58 Z ZO and Make LOCK gmap calibration 22 23 01 999186 00 B0902
62. on Calibration and Indanone Spectra Protons High Ll 7 9 7 8 7 3 7 32 ppm Figure 27 Aromatic Region of the 2 Ethyl 1 Indanone Spectrum The gradient COSY shows cross peaks describing the coupling pathways Some smaller cross peaks are also present in the spectrum which actually arise from the impurities shown in Figure 28 An example of this is the cross peak at 3 5 ppm The methyl triplet in Figure 29 shows major cross peaks to the H10 protons The multiplicity of the H10 and H2 protons cross peaks show that they are weakly coupled the J value is small Assignment of the aliphatic region begins with H7 the most deshielded proton Figure 30 From H7 direct connectivity is apparent to H6 The rest of the assignment is H6 to HS the other triplet and then to H4 The assignment of H7 to the signal at 7 72ppm is confirmed by the gHMBC data TOCSY is a phase sensitive experiment The cross peaks are narrower than in the COSY giving higher resolution Correlations among all protons in a spin system are observed in the TOCSY spectrum see Figure 31 The critical parameter is mix In this case mix is 0 08 seconds which is sufficient to show correlations throughout the entire spin system Shorter mix times will reveal fewer correlations The expansion shows the completely defined spin system starting with the CH3 group and ending with protons on C10 Figure 32 A total of 5 crosspeaks are seen in the ro
63. orm in Chapter 5 5 Console and Magnet Test Results 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 31 Chapter 2 Console and Magnet Test Procedures 2 4 Magnet Drift Test The magnet drift test is an overnight test Samples Depending upon the probe the concentration of H 0 The H O concentrations are 1 for the 01 and autotest samples and 2 for the 02 sample Use the sample that provides a signal with good a good signal to noise ratio in most cases the 1 H O 99 D 0 samples will a good signal Table 5 Sample for Magnet Drift Test Sample Sample Tube mm Sample Part Number Doped 2 Hz H 0 D 0 0 1 mg ml 5 01 901855 01 GdCl in 1 HO in D20 Doped 2 Hz H 0 D 0 0 1 mg ml 5 01 901855 02 GdCl in 2 H 0 in D20 autotest sample 0 1 BC enriched 9 01 96812068 xx methanol in 1 H 0 99 D30 Probe and Hardware Requirements A 5 mm probe capable of IH direct observe is recommended Test Procedure 1 Enter rtp vnmr tests shmd2o0 to retrieve the test parameter set to the current experiment 2 Tune the probe 3 Acquire a normal spectrum and shim the HDO signal to 2 to 3 Hz linewidth at 50 4 Connect to the acqi window turn the lock off turn the spinner off and set the spinner speed to 0 Make sure the lock signal is on resonance the lock signal display should be flat Disconnect the acqi window Then disconnect the lock cable from the probe 5 Enterin n
64. pt the default parameters Non Gradient systems or non Gradient Probe select COSY click OK to accept the default parameters Both Gradient and Non Gradient systems or non Gradient Probe select NOESY Change the following acquisition parameters 4 Scans per increment mixing time 1 sec then click OK see Figure 10 Figure 10 NOESY Acquisition Parameter Window TOCSY click OK to accept the default parameters 28 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 2 2 Automated Data Acquisition Each time the OK button is clicked an experiment is added to the list of experiments displayed in the VNMR TEXT pane in the order they are run as shown in Figure 11 Experiment Experiment 1 PROTON ay Acq amp Obs Experiment 2 gCOSY Experiment 3 gHMBC Decouplers Experiment 4 gHSQC sequence Experiment 5 NOESY STE 6 TOCSY Figure 11 1H and 1H Detected Experiment List 12 Click Do to start data acquisition C13 and C13 Detected Experiments All systems and broadband capable probes can run these experiments 1 Open GLIDE and click the Setup icon The indanone sample Table 3 should already be inserted If not insert it now From the Experiment menu select C13 and C13 detected Expt From the Solvent menu select CDCI3 Set Autoshim and Autolock Click the No button if your sample is already locked and shimmed Click the YES button if you would prefer
65. ptance testing 14 sensitivity tests 15 shim parameters 15 shipment damage 65 signal to noise measurement 15 skin damage from helium and nitrogen 56 Software Installation 40 Software Object Code License Agreement 12 solids high power amplifiers caution 10 spectra 5C observe pw array 48 spinning speed 15 streaming magnetic tape unit 13 svs command 15 System Administration manual 40 72 MERCURYplus Console Acceptance Tests amp Specifications System Demonstration 13 system demonstration 13 system documentation review 12 system installation checklist 65 System Maintenance 30 day check list 57 T Technical References System Description 41 System Schematics 41 Technical Reference 41 User Programming 41 temperature accuracy for VT systems 34 test conditions 14 test parameters 15 training 2 ethyl 1 indanone spectra 50 52 training seminars 13 tuning probes 44 U updated 23 User Guide Solids NMR 40 User Guide Liquids NMR manual 40 V variable temperature control demonstration 33 temperature accuracy optional 34 Varian manuals 12 Varian Sales Offices 17 VNMR directory and file structure 41 vortexing 15 VT experiment warning 8 W Walkup NMR manual 40 warnings defined 7 warranty coverage 12 weekly maintenance 56 where to look for answers 39 Installations 40 Operations 40 Technical References 41 Varian Sales Offices 17 Who to Call for Assistance 58 Wh
66. quirements mrnorrnvrnvrnnvnvveevrnrnervrevrarvrrersvvrernr 14 15 Varan Sales OffICes susuvaselninnmrieddnitasvintddtiatuutkistdsald 17 1 6 Posting Requirements for Magnetic Field Warning Signs 18 Warning SIENS ikelmsinninssnsrinsibelnlis oE Eas ECEE SEE ESEE EEEE REES 18 Chapter 2 Console and Magnet Test Procedures 21 2 1 AutoCalibration and GLIDE Operation Demonstration mrererrvrvrvornervrnvrrvvrrersvnvernr 21 Setting Up Probe Calibration Files 242248 22 Calibrating 20 and Make LOCK MAD suisiertrebnesimitisriisisistniss ini 22 Running AutoCali tation ses nease sinais n ere esistere resani 23 Calibrating Probe and System Files unges ietnetnsaendeste 24 Reviewing the Probe Calibration 32252 r fenetres tot eseinies uses 25 2 2 Automated Data Acquisition iii serrer 26 HT and HI Detected Experiments ini i n e AS 27 C13 and C13 Detected Experiments 1 444 440 etienne 29 2 3 Homonuclear Decoupling siennes 31 24 Magnet Drift Test 2 85 cies sibesceees VRE EEEE E ERE EERE RE SKEE EEEE E 32 2 5 Variable Temperature Operation Optional Hardware srsnrenrrnnnvnvnrnervrnvravvrrensvvvernr 33 2 6 Temperature Accuracy for VT Systems Optional Test mrnernrrrornervrnvrarvrrevrvnvernr 34 2 7 Stability Calibration for High Stability VT Optional Test oo eee eee 36 Chapter 3 Consoles and Magnets Specifications vrrnvrnnnrnnrnnnnnnnnn
67. r is a single contour below the plane By contrast to the gHSQC experiment the gHMBC and HMBC experiment shows long range mostly 2 and 3 bond IH PC correlations This shows connectivity between the non protonated carbonyl and the protons on C 2 52 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 4 6 Data Acquisition Calibration and Indanone Spectra na ao 9 ae oe 4 h F1 ppm Figure 31 TOCSY s an 1 Indanone shows Correlations nto All Protons 0 2 6 2 2 F1 ppm Figure 29 Gradient COSY gCOSY of Aliphatic Region of 2 Ethyl 1 Indanone T T T T T T T T T 8 0 7 9 7 8 17 7 17 6 7 5 7 4 17 3 7 2 7 1 F1 ppm Figure 30 Gradient COSY gCOSY of the Aromatic Region of 2 Ethyl 1 Indanone 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 53 Chapter 4 Customer Training na to 9 F1 ppm Figure 31 TOCSY of 2 Ethyl 1 Indanone shows Correlations Among All Protons 54 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 4 6 Data Acquisition Calibration and Indanone Spectra Lu e Figure 33 NOESY Spectrum of 2 Ethyl 1 Indanone TTT kiddi idid haidi bidid idid TT TT hihid iid idi 130 110 90 80 70 60 50 40 30 20 F1 ppm Figure 34 HSQC Spectrum of 2 Ethyl 1 Indanone 01 999186
68. raphic 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 manuals before viewing the demonstration 1 2 General Acceptance Testing Requirements Each MERCURYplus spectrometer is designed to provide high resolution performance when operated in an environment as specified in the Installation Planning Guide Unless both the specific requirements of this manual and the general requirements specified in the MERCURYplus Installation Planning Guide are met Varian cannot warrant that the NMR spectrometer system will meet the published specifications 1 3 Samples Required for Acceptance Tests The MERCURYplus spectrometer is supplied with the samples listed in Table 1 Table 1 Samples Required for Console Acceptance Tests Sample Tube Sample Test sample mm Nucleus Part Number UG enriched 1 methyl iodide 1 Trimethyl 5 BE 00 968120 96 phosphite and 0 2 Cr AcAc in Chloroform d Doped 2 Hz H 0 D 0 0 1 mg ml GdCl in 5 IH 01 901855 01 2 2 ethyl 1 indanone in Chloroform d 5 IH and C 01 901855 03 0 1 ethylbenzene 0 01 TMS 5 00 968120 70 99 89 deuterochloroform CDCI3 0 1 ethylbenzene 0 01 TMS 10 00 968123 70 99 89 deuterochloroform CDCI chloroform in acetone d lineshape 5 00 968120 xx 100 methanol reagent grade 50 to 25 Low 5 00 968120 80 100 ethylene glycol reag
69. rations This manual covers the VNMR menu systems in detail as well as command line operations locking and shimming data acquisition parameters probe tuning digital signal processing and data processing display and plotting Data management storage retrieval and archival is also addressed in this manual User Guide Liquids NMR Lists and explains how to set up all the standard experiments provided with VNMR Not every experiment listed can be run on every system The type and configuration of the instrument will determine which experiments can be run This is the manual to go to when you have very specialized experimental requirements and will most likely be running the experiments from the command line You will also want to refer to this manual for a general overview of the experiments that are automatically set up through the GLIDE and VNMR menu systems User Guide Solids NMR Explains how the run CP MAS experiments and describes the XPOLARI pulse sequences System Administration Provides detailed information on both the UNIX operating system and VNMR software for the system administer is presented Also included are magnet maintenance and other administrative items Installations MERCURYplus Installation Planning Guide Provides site planning information for MERCURYplus NMR spectrometer systems MERCURYplus Acceptance Test Procedures and Specifications Covers the console installation test procedures and speci
70. rd warranty terms Non standard warranty terms if included as a condition of sale are detailed in the sales contract and will not be covered by the installation engineer Table 9 Who to Call for Assistance Online Customer Support and Information Webb Addresses Service and Technical Support http Avww varianinc com nmr service Applications Support http Avww varianinc com nmr apps Sales Support http Avww varianinc com nmr contact Product Information http www varianinc com nmr products In warranty Service United States and North America Europe Other International Technical Support United States and North America Europe Other International Post Warranty Support United States and North America Europe Other International Applications Support United States and North America Europe Japan Other International Location Palo Alto California Local Sales Office Local Sales Office Location Palo Alto California Oxford UK Local Sales Office Location Palo Alto California Local Sales Office Local Sales Office Location Palo Alto California Columbia Maryland Darmstadt Germany Tokyo Japan Local Sales Office Phone Number 1 800 356 4437 See page 17 See page 17 Phone Number 1 800 356 4437 44 1865 388 800 See page 17 Phone Number 1 800 356 4437 See page 17 See page 17 Phone Number 650 424 4526 410 381 7229 49 6152 703 253 81 3 5232 1211 See page 17 58 MERCURYplus Console Acceptance Tests amp Sp
71. robe calibration file is updated C Solvent Menu Figure 4 GLIDE Calibrate LOCK 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 23 Chapter 2 Console and Magnet Test Procedures Calibrating Probe and System Files 1 Open GLIDE by clicking on the GLIDE button in the VNMR menu and click the Setup icon in GLIDE Right click 2 Use the Sample Eject Insert buttons Figure 5 to eject the 2 Hz D20 sample and insert the chloroform sample Table 2 Tune the probe if needed 3 Right click on the Experiment select button using the right mouse button Left click on Calibrate H C Ind Det amp Grad CH3D in the drop down experiment menu see Figure 5 place the mouse pointer on the experiment selection Calibrate H C Ind Det amp Grad CH3I and click with the left mouse button Make this selection for pfg and non pfg systems 4 From the Solvent menu select CDCI3 Left click 5 Set Autoshim and Autolock Calibrate H C Ind Det amp Grad CH31 Click the No button if your sample is already locked and shimmed Figure 5 GLIDE Setup Window and Drop Down Experiment Menu Click the YES button to lock and shim automatically 6 Enter a relevant text in the Text field e g calibration of ASWprobe and click the Setup button If the text box is not visible place the mouse pointer on the bottom of the Setup Window boarder The mouse pointer will change to an
72. s 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 2 00 then the 0 55 level on a 100 fold vertical expansion vS 20000 is 9x 0 55 or 4 95 cm from the baseline If the noise is significant at the 0 55 and 0 11 levels the linewidth should be measured horizontally to the center of the noise Usethe dsnmax macro to determine signal to noise sensitivity You can also choose a noise region free of any anomalous features 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 16 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 1 5 Varian Sales Offices 1 5 Varian Sales Offices For product sales and service information contact one of the Varian sales offices Argentina Buenos Aires 114 783 5306 Australia Mulgrave Victoria 3 9566 1138 Austria V sendorf 1 699 96 69 Belgium Brussels 02 721 51 51 Brazil Sao Paulo 11 829 5444 Canada Ottawa Ontario 613 260 0331 China Beijing 10 6846 3640 D
73. s changed to s2pul for direct observation of the carbon The calibration will follow the same pattern as the calibration of the proton pw90 and the carbon pwx90 using default values for target values if no target specification is given A reference carbon spectrum is Il ll till I m mi obtained first The full reference spectrum contains three sets of Figure 20 Gradient Calibrations resonances at the far right approximately 22 ppm is the UG resonance from methyl iodide the doublet at 10 ppm is from the 16 resonance from the phosponate methylester and the 1 1 1 triplet far left at 78ppm is the UG resonance of chloroform d HCCI The carbon pw90 calibration is analogous to the proton calibration The reference carbon spectrum shown in Figure 21 is saved as C13ref The carbon observe pw90 is determined using a pw array see Figure 22 and saved as C13pw90 The final calibration is of the proton decoupler The first calibration step determines the value of yH at a decoupler power of 40 the default value This measurement is made using continuous wave cw decoupling The pulse sequence is the same as in the previous experiment carbon observe with proton decoupling except pw is now set to a fixed value decoupler modulation mode dmm is set to c decoupler mode dm is set to yyy and the decoupler offset dof
74. s discussed in detail in the System Administration manual 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 43 Chapter 4 Customer Training 4 5 Tuning Probes Probe tuning is covered in Chapter 6 of the Getting Started manual Tuning operations and tuning ranges specific to each probe are covered in the manual provided with the probe 4 6 Data Acquisition Calibration and Indanone Spectra This section covers the calibration of the spectrometer and the acquisition of several 1D and 2D data sets using the 2 2 ethyl 1 indanone sample a typical small molecule with a formula weight of 160 g mole Step by step instructions for calibration and acquiring spectra of the 2 ethyl 1 indanone sample are given in 2 1 AutoCalibration and GLIDE Operation Demonstration page 21 and 2 2 Automated Data Acquisition page 26 of this manual and will not be repeated here This section examines the order in which the calibration data is acquired and resulting spectra The Calibration Process Before acquiring spectra of a sample the spectrometer must first be calibrated Calibration is necessary if one of the following is true The probe has been changed The experiments are to be run at a different temperature than the last calibrations Solvent changes significantly i e an organic lock solvent vs deuterium oxide lock solvent The calibration has not been run for several weeks in this case it is simply a m
75. sk Space page 43 4 5 Tuning Probes page 44 4 6 Data Acquisition Calibration and Indanone Spectra page 44 4 7 Magnet Maintenance page 56 4 9 Warranty and Who to Call for Assistance page 58 4 8 30 Day System Maintenance page 57 This chapter describes training provided by the installer This training is intended as a general overview of the instrument basic maintenance requirements software features data acquisition and storage file maintenance and other routine tasks Comprehensive training classes are offered at various Varian Inc Applications Laboratories around the world Call your sales representative or contact the Varian Inc NMR systems office nearest you for class offerings schedules and cost 4 1 Where to Look for Answers Knowing where to look is the first step to answering a question All manuals are available in hard copy and can also be installed online Figure 14 shows the menu for the MERCUR Yplus online manuals The online manuals are accessed from the Workspace menu To access the Workspace menu in Solaris 2 5 and newer place the mouse pointer on the background and click with the right mouse button To access the online manuals in Solaris 2 6 click on Online manuals on the Workspace menu Server i NMR Spectrometer Systems Online Manuals Menu Operation Getting Started User Guide Liquids NMR Walkup NMR Using GLIDE VNMR Command and
76. spin n nt 1 array d1 11 3600 0 di 1 60 This sets up an array of d1 values with the first spectrum to be collected after 1 minute and subsequent spectra to be collected at 60 minute intervals 6 Enter ga to acquire the spectra The test takes approximately 10 to 11 hours to finish 7 Phase the first spectrum by entering ds 1 to display the first spectrum of the array and by entering 1p 0 aph0 to apply a first order phase correction to the spectrum 8 Enter ai to scale all of the spectra to the same vertical scale and enter dssa to display the arrayed spectra stacked vertically 9 Compare the frequency shift of the HDO peak of the arrayed spectra to the frequency of the first spectrum in the array 10 Write the results on the form in Chapter 5 5 Console and Magnet Test Results 32 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 2 5 Variable Temperature Operation Optional Hardware 2 5 Variable Temperature Operation Optional Hardware This demonstration shows that the basic variable temperature VT unit and probe changes to the desired temperature and displays on the VT controller If the system is equipped with a VT unit 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
77. st Results Notes 68 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 5 5 Console and Magnet Test Results 5 5 Console and Magnet Test Results Fill in the following information From AutoCalibration and GLIDE Operation Demonstration page 21 From Automated Data Acquisition page 26 From Homonuclear Decoupling page 31 From Magnet Drift Test page 32 From Variable Temperature Operation Optional Hardware page 33 From Temperature Accuracy for VT Systems Optional Test page 34 From Stability Calibration for High Stability VT Optional Test page 36 Varian Representative Date Customer Representative Date 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 69 Chapter 5 Acceptance Test Results Notes 70 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 Numerics 180 pulse 15 2 Ethyl 1 indanone in chloroform d automated data acquisition 26 2 ethyl 1 indanone in chloroform d sample part number 26 90 pulse 15 A Acceptance Test Procedures and Specifications 40 acceptance test specifications overview 12 acceptance tests documentation 16 acceptance tests objectives 11 Accessory Manuals 40 addprobe 22 air line traps 56 APT demonstration 26 Attached Proton Test 26 AutoCalibration 21 26 automated data acquisition
78. t to the current experiment Enter temp 40 at 10 sw 10000 Set pw to the IH 900 pulse width for the probe and then enterspin n su Allow the VT controller to regulate to 40 C which should be about 10 higher than the room temperature Check that the probe is tuned Acquire a normal spectrum by entering ga Move the cursor to the DSS signal right most peak Enter movetof sw 1000 at 10 Acquire a normal spectrum and shim the DSS signal to about 0 6 Hz or less linewidth at 50 The sample of DSS in D20 should equilibrate at 40 C for at least 2 hours before the next step Enter in n spin n nt landarray d1 73 600 0 d1i 1 0 This sets up an array of d1 values with the first spectrum to be collected at time 0 minutes and subsequent spectra to be collected at 10 minute intervals for up to 12 hours Enter ga to acquire the spectra The test takes about 12hours to complete After the spectra are acquired phase the first spectrum by entering ds 1 to display the first spectrum of the array and by entering 1p 0 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 10 Measure the difference between the left most peak and the right most peak in Hz MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 Chapter 3 Consoles and Magnets Specifications This section
79. termine if a danger exists Refer to the manuals supplied with the magnet for the size of a typical 5 gauss stray field This gauss level should be checked after the magnet is installed WARNING Keep metal objects outside the 10 gauss perimeter from the centerline of the magnet The strong magnetic field surrounding the magnet attracts objects containing steel iron or other ferromagnetic materials which includes most ordinary tools electronic equipment compressed gas cylinders steel chairs and steel carts Unless restrained such objects can suddenly fly towards the magnet causing possible personal injury and extensive damage to the probe dewar and superconducting solenoid The greater the mass of the object the more the magnet attracts the object Only nonferromagnetic materials plastics aluminum wood nonmagnetic stainless steel etc should be used in the area around the magnet If an object is stuck to the magnet surface and cannot easily be removed by hand contact Varian service for assistance 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 7 Warning Notices continued WARNING WARNING WARNING WARNING WARNING WARNING WARNING Refer to the manuals supplied with the magnet for the size of a typical 10 gauss stray field This gauss level should be checked after the magnet is installed Only qualified maintenance personnel shall remove equipment covers or make inter
80. to call up right and left cursors Position the right and left cursors on the right and left peaks and enter tempcal methanol Record the temperature reading from the VT controller displayed on the front face of the VT controller Record also the computer calculated temperature based on the chemical shift frequencies of the two peaks If low temperature calibrations are performed immediately following high temperature calibrations allow the probe to cool to room temperature before continuing with the rest of the procedure Enter temp 20 su to change the temperature to 20 C Allow the sample to stabilize at 20 C for at least 10 minutes after the VT controller has reached the final temperature and regulated Enter ga to acquire a spectrum Repeat steps 4 and 5 Enter temp 80 su to change the temperature to 80 C Allow the sample to stabilize at 80 C for at least 10 minutes after the VT controller has reached the final temperature and regulated Enter ga to acquire a spectrum Repeat steps 4 and 5 After finishing the low temperature test enter temp n su to turn off the temperature regulation While keeping the dry nitrogen gas flowing to the probe and upper barrel remove the polystyrene VT dewar containing liquid nitrogen The flow of dry nitrogen gas to the probe will prevent condensation inside the probe Allow the dry nitrogen gas to flow through the probe and upper barrel for at least 15 minutes while the probe warms up to
81. torage devices and accessories VNMR file backup and recovery Software Installation Software Installation Getting Started manual 1 4 System Administration and Software Installation System Administration 5 5 System Administration Chapter 10 System Administration Chapter 10 Spectrometer Operation Done Topic Reference Standard parameter and probe calibration setup Basic H C experiment setup using GLIDE COSY demonstration GLIDE Homonuclear and heteronuclear decoupling demonstration Manual lock and shim demonstration Basic spectral display procedures Gradient shimming demonstration CP MAS experiment information Walkup NMR Walkup NMR Chapter 2 Walkup NMR 3 8 Getting Started manual 7 2 and Acceptance Test Procedures Getting Started manual 6 10 Getting started manual 4 10 and 9 5 User Guide Liquids NMR 11 6 User Guide Solid State NMR Miscellaneous ATP signoff and Walkup NMR demo if applicable Hallmark of Quality Customer contacts for service applications etc Accessory training as required Varian Representative Date Customer Representative 64 MERCURYplus Console Acceptance Tests amp Specifications Date 01 999186 00 B0902 5 3 System Installation Checklist 5 3 System Installation Checklist Company University Address Principal User Phone Spectrometer type Fax Consol
82. ttings 15 homonuclear decoupling test 31 I installation checklist 63 65 installation engineer 11 Installation Planning Guide 40 installation planning guide 14 L lineshape determination digital 15 from a plot 16 linewidth measurement 16 liquid helium level in dewar 56 liquid nitrogen 33 37 loading programs 13 Low Temperature Calibrations Test optional 35 M magnet demonstration 13 magnet drift test procedure 32 sample and part number 32 magnet quench warning 8 magnet refilling 13 MERCURYplus Console Acceptance Tests amp Specifications 71 Index magnet test procedures 21 magnetic media caution 9 managing disk space 43 metal objects warning 7 methanol 34 N nitrogen contact with body 8 nitrogen flowmeter 56 nitrogen gas 33 37 nitrogen gas flowmeters caution 10 noise region 16 O OEM manuals 12 P pacemaker warning 7 Periodic checks 56 policies for acceptance test specifications 12 preinstallation checklist 65 Probe Acceptance Test Procedures and Specifications Manuals 40 probe and system calibrations 24 25 probe demonstration 13 probe tuning 44 prosthetic parts warning 7 pw parameter 15 Q quarter wavelength cable 14 R radio frequency emission regulations 10 relief valves warning 9 removable quench tubes warning 9 reviewing the probe calibration 25 rts command 15 S safety precautions 7 9 samples required for acce
83. ually determined by interpolation between a value that gives a positive signal and a value that gives a negative signal The 90 pulse width is one quarter the 360 pulse 360 4 Signal to noise S N is measured by the computer as follows S N maximum amplitude of peak 2 x root mean square of noise region 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 de 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 Enter delta to see the difference in Hz between the cursors 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 15 Chapter 1 Introduction 4 Set th 11 the 0 11 level and repeat 5 You can also use the macro res Place the cursor on the resonance of interest and type res on the command line 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 peak
84. ults contains forms for writing the results Lineshape and resolution tests described in the probe manual shipped with your probe must be run before these console tests are run During the console tests probe calibration files are created that are used during some of the console tests The probe calibrations written to these probe files will meet or exceed the specifications for the probe Probe performance tests and calibrations that are executed during AutoCalibration will not be repeated manually These probe calibration files are required for some of the console tests 2 1 AutoCalibration and GLIDE Operation Demonstration The AutoCalibration procedures calibrates the probe and demonstrates the performance of the probe During the AutoCalibration a probe calibration file containing the IH and PC 90 pulse widths decoupler calibration gradient calibration if present is set up as described in the probe installation manual that shipped with your probe Table 2 lists the samples used for the AutoCalibration Table 2 Samples for System Calibration Sample Sample Nucleus Tube mm Part Number UG enriched 1 methyl iodide 1 trimethyl 136 5 00 968120 96 phosphite and 0 2 Cr AcAc in Chloroform d Doped 2 Hz H 0 D 0 0 1 mg ml GdCl in IH 5 01 901855 01 1 H20 in D20 The total time for the tests and calibrations should be about 1 hour Run the tests and calibrations in the following general order 01 999186 00 B0902 M
85. variety of factors such as atmospheric pressure and a high reading is not necessarily an indication of a problem but it is worth investigating Pressure at the air valve for the magnet Liquid nitrogen level Readings on the nitrogen and helium flow meters Twice Each Month Check liquid helium level Monthly or Bimonthly Check signal to noise and lineshape using the standard proton sample the BC 90 pulse width and the decoupler field strength Keep the resulting spectra and parameter in a secure place for future reference 56 MERCURYplus Console Acceptance Tests amp Specifications 01 999186 00 B0902 4 8 30 Day System Maintenance Filling Cryogens All cryogens should be delivered in nonmagnetic dewars Consult the manual supplied by Oxford complete instructions and for more detailed information on cyrogen fill intervals and capacities Liquid Nitrogen The interval between liquid nitrogen fills it nominally 2 weeks The Oxford manual that is supplied with the magnet should be consulted for the exact interval between nitrogen fills CAUTION Failure to maintain the correct liquid nitrogen levels will lead to excessive liquid helium boil off which in turn may lead to a quench of the magnet Liquid Helium The interval between liquid helium fills is dependent upon the type of dewar There are standard and long hold Dewars available for some magnets The recommended refill interval is specified in the Oxford manu
86. ven that probes purchased for use in systems other than MERCURYplus will meet current specifications Testing Policy for Indirect Detection Probes used for Direct Observe Broadband Performance Probes designed for indirect detection applications are tested for indirect detection performance only Indirect detection acceptance tests are performed only if an indirect detection probe was purchased for use with the MERCURYplus 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 page 61 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 included in System Installation Checklist page 65 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 Software Obje
87. w The indanone sample does not have any significant NOE crosspeaks Figure 33 The main area of interest in this spectrum is to note that the diagonal will be negative and the NOESY crosspeaks will be positive Crosspeaks which appear to have both positive and negative components are actually not NOE correlations but coupling artifacts 01 999186 00 B0902 MERCURYplus Console Acceptance Tests amp Specifications 51 Chapter 4 Customer Training F2 P ppm a g 4 a a 2 aa 8 Impurities lt I a t 4 a 3 a 54 6e 7 3 a ean al e 84 TECTED LL 8 7 6 5 4 3 2 1 F1 ppm Figure 28 Gradient COSY of 2 Ethyl 1 Indanone In the gHSQC and HSQC experiment see Figure 34 the protons correlate with the carbons to which they are attached The detected nucleus is IH and this results in a higher signal to noise then the 13C detected hetcor experiment When compared to the HMQC experiment the HSQC experiment has the advantage that the IH H homonuclear coupling do not evolve As a result the resolution in the 2D plane is higher in the HSQC experiment The higher resolution has the added advantage of improving the signal to noise The version of the HSQC experiment supplied with the MERCURY has the added benefit that it will distinguish CH CH and CH3 groups In this case phase is indicated by whether the crosspeak is filled in with multiple contours above the plane o

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