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Qualion NMR - User Manual

1. Figure 53 New Application Clicking the New button displays a new application window within the main window Clicking a second time adds another application window tiled within the main window Several such windows may be added You can select the tiling arrangement by means of the Windows button below ProcessNMR Running On Local Machine Data Tools Run Window Help ELIO i JM Modbus mcs Start Stop Sched Alarm Log Lag Client Calc Help E Eventk T Pred 5 Sched H Grid Results Figure 54 Windows Clicking the Window button displays a menu for selecting the tiling arrangement the application windows You can select either horizontal or vertical tiling EVENT TABLE N WARNING Actions desctibed in the following section should be performed only by properly trained personnel System Operation UM SW50407 05 5 Windows and Dialog Boxes Process NMR Application Click on the Event T button or select Event Table from the Data menu to display the screen shown in Figure 52 Event Table File Pulse Label Command Channel 0 Phase 11 004 AdcEn SO0 00u PreTx a nnu Tx TX 20 004 PreTx EX 0 AdcEn Offset 1 Mew Figure 55 ProcessNMR Menu Event Table Screen The Event Table is the primary means of controlling the timing and functioning of the main transmitter receiver
2. 4 Location 0 Reference Peak Figure 34 Peak Selection Dialog Box System Operation UM SW50407 05 55 System Operation Signal Processing Digital and Frequency Domain REFERENCE The dialog box shown in Figure 35 appears when you click on Peak in the Main Menu Top 1d Peak Referance Peak Identificatio Peak Thresh 1004 Stark Counting From Peak Index Width Peak Height 0 100 Peak Reterance Location Peak Figure 35 Peak Reference Dialog Box The top panel contains the parameters for identifying a peak In the top entry box enter a value for the threshold to be used for finding a peak usually set at a value of about 10 to 40 In the next box select a direction in which to search for a peak In the next box enter an index number such as 1 for the first peak identified 2 for the second peak and 3 for the third peak etc In the middle panel the Peak Width panel enter a value in decimal for measuring the width of the peak such as 10 or 50 0 1 or 0 5 Then click on Get Peak Width and the system displays the measured width in the panel The bottom panel permits you to set a reference for the peak To do so enter a location for the reference in units of PPM or Hz and then click on Reference Peak to execute your entry The system then measures shifts from the reference point you have set as shown
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4. Screen Displa Control Automated Analysis Screen Tools Vertical Grid Horizontal Grid oom oom oom X oom Reset tous eal Portion Imaginary Portion Both Portions Signal Analysis Menu Remove DC Zero Hil 2 zs Magnitude Phase Peaks Definition Symmetric Zero Order Zero Order Zero Order First Order Phase Phase Phase with Baseline 9 Table of Contents mW sonata 02 09 EEE LOS MUS sass ONERE E c mes e LOG MAINTENANCE AND DIAGNOSTICS 2 2 107 Preventive Maintenance RU Regular Maintenance Long Te
5. P ienal Processing Frequency 55525 Major Software EDITI M Maij Hardw C t 21 aJor ar are omponen AeeseseseceecsosceecceesssosecesseseceseecosescusoseeseeesecescesecosecsesceouceesseseeeecosesescosoceseescoesescedeeoseceeuDee ower OMMUMCATIONS CONNEC c HOS csc eo sve saa cnt tn Aes ata MM era eases aie nclosure Environmental Controls os cele cue cta c eh ee Arv c ES oa EE 1 d System Operation UM SW50407 05 System Overview Table of Contents s OO pe ADPU AO iiie gene een cda ES Measurement CAnalyticab Capables sarsii lise esa sevo ta orte edis ome Meri ae unde ed re User Calibragon Models sese A PpliCAliOMs MONT TG er Overall Systemi Descrip Hoher anen des tas Puth dude tau aero tub aha dotado Process NMR SOWA Ona aa e IN IVER Analysts
6. prora 175 T LE MEL LI MIL d ETE Figure 7 Heater Control Display As shown in Figure 7 the window has four displays The upper left panel shows a time varying trace of the measured magnet envelope temperature The lower left panel shows the trend record of the current supplied to the magnet envelope heaters the output of the envelope heater control loop Similarly the upper right panel shows the temperature record of the measured temperature of the magnet The lower right panel displays the trend record of the output signal of the magnet heater control loop the current supplied to the magnet heaters By observing these records you can evaluate performance of the heater control unit and adjust parameters for the loops The top panel of the display also shows the current values of MS Magnet Sense MH Magnet Heater ES Envelope Sense and EH Envelope Heater Just below these items the current temperature values of the Magnet and the Magnet Envelope are displayed along with the present offsets for each difference between desired value and actual value The procedure for entering or modifying parameter values is described in Chapter 5 Maintenance and Diagnostics System Operation UM SW50407 05 24 System Overview SHIM CONTROL UNIT A wanxING Actions described in the following section should be performed only by properly trained personnel Major Hardware Components The S
7. ea eee teet inae eim n YIN QR yn ER Ac vate an Existina Connections ressas nn a Ree e pite Ges Ies PRESE OLOR REIR OI REDE WINDOWS AND DIALOG 74 rocess pp 10n li i 5 a 78 albo cnet ocular AM uult M DL A hlc hti LG OR POUR T Lr Ey u oma e na 618 5 56 55555 26 55558 5 6 6 5 56659 86 6 5 6 5 6 66 6669 6 4 66 5 6569 6 6 66 9 6 669 6 MRA l 1 li 1 86 AA 1 1 8 E T M eee OF ys nee ee TU System Operation UM SW50407 05 System Overview Average BDC css Frequency Shim LOCK os
8. PULO APA pem TT Wen mii Data 77 99 Mac8011 Mim7586 58058 Daa 538 Mar533 Mi502 Mean 546 56019 B Figure 110 New Task System Operation UM SW50407 05 121 Maintenance and Diagnostics Diagnostics New Task Configuration Options To configure the new task right click in the window to display the menu of options as shown in Error Reference source not found The various options are described in Using NMR Diagnostics on page 109 amp x Task 31 f Zoom Plet Style Frequency Domain Unite Set Borders om ALL X Axis Rang UrnZoom Made Balistic History Zoom Borders Show Cursors Data File Figure 111 New Task Configuration Options Plot Style Options This option permits to select the style of the plot either a solid line or a dotted line Rename Define Zoom 2 k Plot Style d Solid Line Time Donain Units Sold Points Frequency Daman Umts e Set Borders x Axis Rang Satistic History Show Cursors Data File s Figure 112 New Task Configuration Plot File Options System Operation UM SW50407 05 122 Maintenance and Diagnostics Diagnostics Time Domain Units Options This option permits to select the units for the time domain x axis in either milliseconds or in points Rename Define oom Plot Style Time Dramain Units Mill5econd
9. Flle dsr pp Actual Max Result of Spectral Analysis Power Switch pp Default d i wmr canfig deFault pp 0 5556 lt 0 500 PROCESS Power Off d QUALION Ltd Copyright 2007 Figure 99 Max current Acquisition manager Debug Clicking on Debug displays the dialog box shown in Figure 99 These tools however are for use only by Qualion NMR technicians Shim Test Reset Exit Debug DAC no Loop duration 1n0 0 a Data Hes emove D Cim T ake Ech jc Stop Control ae 0 at ibe Power Data Jo Echa WT ibe Last error o Get Reset 65232 port Open Figure 100 Shim Test Debug Dialog Box DAC Map Clicking on this item displays the screen shown in Figure 100 This screen shows the status of all 40 shim coils and DACs in the magnet along with several buttons for selecting coils and starting stopping various types of tests The options System Operation UM SW50407 05 113 Maintenance and Diagnostics Diagnostics Select All Selects all coils Unselect All Deselects all coils Quick Test Performs a shortened test on all selected coils Find Zero Finds input values that give zero outputs for all selected coils Accurate Test Performs a complete test on all selected coils Address Test Displays address in selected units for each selected coil Read Reads the present value of
10. Event Table x fics B File Pulse shot CPMG Duration Channel Value Offset 1 48 Diagram Set 1 00u PreTx Set 299 000 AdcEn Set 21 00u Tx 120 Set TX Set 20 00 PreTx Set 2 0 AdcEn Phase 1 1 Figure 74 Event Table Screen with Pulldown Pulse Menu One Shot this selection permits you to load the event table with a set of default parameters as shown in Figure 72 This is a convenient way to start as many of the parameters are determined by the specific hardware configuration installed on your system OneShot delay 1 Hx Gain 20 Ts Gain 90 Cyclop Infinite Create Cancel Figure 75 OneShot Default Parameter Screen PW pulse width or duration of the main transmitter pulse Phase select phase of the pulse 0 90 180 or 270 from pulldown menu Rx main receiver on 1 or off 0 PreAcqDelay wait time before turning on the receiver Delay duration of the system recycle delay wait for relaxation times to complete System Operation UM SW50407 05 9 Windows and Dialog Boxes Automated Analysis Rx Gain Gain setting for the main receiver Tx Gain gain setting of the main transmitter Infinite When checked the system recycles continuously When not checked the System does not recycle Create Button Click to activate new data entries Cancel Button
11. N Phase Come ct On Baseline i 53 seline COMES LOM Peak aM um BR TCT ONC Coarse REPRE ATO WOOOVONVETTO aa pu Erebi sd Iti St 1 Stream sampin stem u 1 09060909000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000 unctiona escription o eaa STANDARD PROCEDURES orit Start the Anal y ive eeeeosceecovescesoveceeossvocoseecesscesecoeeseceesocesesosceesseccoseeseceseceeesovecevesvecoseces eseseceeesecessecesevoseecsoveeeseosecop sQues es 62 Initial S 62 testen apa eu Dues E EE Startup after Short Shutdown Magnet 62 Startup atter Lone Shutdown Magnet ColdY OZ Shutting Down the AnalyZGE o ormal Orderly Shutdown 606060606000600060000000600000000006000000000000000600000
12. Magnet Temperature out n eee lemperatures LI gt FinalMagi44 228 120 Offset 0 000080 FinslEgs23 201 190 Offset 0 000 000 Requested Envelope Temperature 13 temperatures CH Fna Mas 1238120 ORAT 28271197 EnvH Temperature Offset From Requested Envelop Temperature Figure 97 Typical Pop Up Labels SHIM TEST Shim Test Debug Coil Test Spacer Test Toggle Test File Exit 95232 part Open 2 Figure 98 Shim Test Screen Max Current Value Note Before starting the shimming process the max current should be defined A new mechanism is now limiting the current value to go above a pre defined value This value is defined in AcqMegr ini file The current overload event turn off power of magnet in order to prevent damage of magnet System Operation UM SW50407 05 112 Maintenance and Diagnostics Diagnostics After Shimming process stopped NMR applications stops work too In this case user have to reset gradients table in order to perform shimming process again Shim Gradients E Hotepad Set Method Gradients Log File Fie Edt Format Help 0 0 427 Gzyy 0 0 0 00 0005 Spectra Q 1 spectra Gxyz 0 0 Warning message Attention Shim current overload Shim process stopped 1 Spectra Wax currgnr 0 1 0 Post Processing Current
13. Integral Derivative 1 25 OK Cancel Set PID x Control Loop Envelope Proportional 05 Integral 0 000399 Derivative 1 28 OK Cancel Diagnostics Figure 95 Set PID Parameters Screen It is possible to control the parameters but not modifying them They are permanently set at factory To set the refresh screen data rate click Refresh Rate at the main menu The dialog box on Figure 95 then appears Enter the new refresh rate in seconds and then click OK to execute the change Set New Refresh Rate Enter new refresh rate seconds K Cancel il Figure 96 Set Refresh Rate Box To modify the time scale of the charts click on Time Scale Rang A dialog box then appears on which it is possible entering new ranges Click set to apply your changes and return to the main menu Save Click this item displays a dialog box that permits specifying a path and filename in which to save the displayed data Pop Up Labels The display screens are provided with pop up labels to help identify each item on the screen Position the cursor over the item on the screen and wait a few seconds The label for the item then pops up on the screen Typical examples are shown in Figure 96 System Operation UM SW50407 05 111 Maintenance and Diagnostics Diagnostics Temperatures C gt FinalMage 38 120 Offset 0 000 019 FinalEnv38 201 180 Offset 0 000 996 E
14. Width Peak Height 0 100 10 m Peak Referance Location 0 Peak Figure 89 Peak Reference Dialog Box Peak Identification Peak Thresh the value in this box determines what constitutes a peak Any point greater than this threshold 1s defined as a peak Start Counting From start looking for peaks from the Left or Right side of the display Peak Index select the peak first second third or other from the side specified Peak Width Specify the peak height at which you want to determine the width The choices are 50 10 and 0 5 percent After specifying the height click the Get Peak Width button Peak Reference System Operation UM SW50407 05 105 Windows and Dialog Boxes Automated Analysis Specify the reference location in ppm After specifying the location click on Reference Peak to execute the command Window Window Window Windowing Function A t H t LIT e Coefficients Filter Enable Filter Path to Filter File Humber of Points Figure 90 Window Function Dialog Box Theory this is a mathematical function that multiples the acquired data by an exponential equation It is normally used to smooth the data and minimize noise Coefficient a Use a negative value for a to make an exponentially decaying function that makes the FID close more quickly Note
15. 1 pee CALIBRATION MODEL 472 13 TERG ENAZ FEAT 29306 54 72 34448 020 314 Boe VALUES Figure 11 Typical Spectral Analysis of a Process Sample Constituents Identified by Chemical Shift Proves Binet im Lat al edis Sods OCG Gere 16 PEAK CHEMICAL SHIFT OF CH Pa CHEMICAL SHIFT OF CHa AROMATICS E n CALIBRATION MODEL OUTPUT 2 av 58 Yon 120 VALUES 477 13 Ge MAM 308 Se 23453548 314 3552 E Figure 12 NMR Spectrum Showing Chemical Shifts for Various Constituents Constituents Quantified by Integrating Peaks Integrated peak values are not displayed graphically in any of the standard screens If they are required System Operation UM SW50407 05 36 System Operation Overview as one more of the inputs to or outputs from a calibration model they may be displayed at the bottom of the screen along with other variables as shown in Figure 13 Fir CIT Pel coe Faj top eb I i 0 En 100 47719 RS 57742 906 5472 D3D 314 34 57 PNE d RESULTS OF CALIBRATION MODEL CALCULATIONS Figure 13 Results of calibration model calculations Use of Calibration Models Calibration or prediction models are mathematical models developed from empirical data that cotrelate
16. Not all nuclei have spin but almost all elements in the periodic table have at least one isotope with a non zero nuclear spin Also NMR spectroscopy can be performed only on isotopes that occur in 1 2 enough abundance to be readily detected Some of the nuclei that meet these qualifications P Na N si and Each type of nucleus has a specific identifying resonant frequency called the Larmor frequency System Operation UM SW50407 05 7 System Overview Measurement Principle NMR SPECTROSCOPY When a group of nuclei with spins is placed in a magnetic field each aligns with the field in either the low the high energy state At room temperature low energy spins slightly outnumber high energy spins As the temperature increases the ratio of low to high energy spins approaches unity As temperature decreases the ratio increases The signal detected by NMR spectroscopy is generated by the difference between the energy absorbed by spins that jump from low energy to high energy states and the energy emitted by the spins that move from high energy to low energy states The signal therefore is proportional to the difference in population between low energy and high energy spins The exchange of energy at a specific frequency identifies the type and concentration of a particular element If a signal of frequency F is turned on and then off again very rapidly the result is an output consisting of many fre
17. QUALIOH Ltd Copyright 2006 Figure 60 Outlier Menu DCS OverRide Menu This paragraph does not refer to the Lab Analyzer If the DCS Override is enabled the system looks into the address that writes in the DCS stream status address and looks for which streams the DCS operator wants to work on You can see the status by clicking on the read register button of this menu E E Conditions E X Check Outlier is OH DCS ouerRide is OH Send Stream DECS is OH Sample Grab is OH DCS OverRide Status Register Address Coi Address Read Coils E Reload Outlier Outlier Grabbing Streamout DCS Override Grabbing Streamout DCS OverRide OUALIOH Ltd Copyright 2006 Check Outlier is DCS OverRide iz OH Send Stream to DCS is OH Sample Grab is OH SE QUALIOH Ltd Copyright 2006 P Conditions DCS OverRide Status Register Address E Coil Address Read Register 400 4 2 4 s 8 LT NENNEN Figure 61 DCS OverRide Menu System Operation UM SW50407 05 1 Windows and Dialog Boxes Process NMR Application START Click the Start button to start the analyzer STOP Click the Stop button to stop the analyzer SCHEDULER Click the Sched button to start operation of the Multi Stream Scheduler HELP Click the Help button to determine the software
18. directory and then to start processing the data NMR Analysis Running On Local Machine File Archive Processing View Data Run Tools Hardware Help Source Directory p TH m bk Lo File Mame tart Stop E T Avg ADC Freg Shim Lock D b be be Remove DE zer Fill IFFT Magnitude Phe Figure 71 Main Menu Archive Processing Menu 4 Help Auto Predict Rl Start View The View button provides a path to the Screen Tools System Operation UM SW50407 05 88 Windows and Dialog Boxes Automated Analysis Data The Data button provides a path to the Event Table Average ADC Frequency Shim and Lock functions Run The Run button provides a path to the Start and Stop commands Tools The Tools button provides a path to the items in the Signal Analysis Menu These are Remove DC Zero Fill FFT IFFT Magnitude Phase Baseline Peaks and Window Hardware The Hardware button is only for use by Qualion NMR personnel Help Click on the Help button to determine the software version MAIN MENU COMMAND BUTTONS The Main Menu Command Buttons are shown in Figure 69 The function of each button is explained below NMRAnalysis Running Local Machine Fie Archive Processing View Data Run Tools Hardware Help EH 2 E Load Save Print Stark Stop Avg ADC Freg Shim Lock WE FSO Figure 72
19. start Scheduler operation click the Sched button on the main menu bar The Scheduler table details the sequence of operations and the filenames of all files used with each process stream These files define how the analyzer handles each sample The Scheduler is the top level controller for multi stream sampling To modify the functions or sequence make appropriate entries in the Scheduler table System Operation UM SW50407 05 85 Windows and Dialog Boxes Automated Analysis File Load fermon o 880225 AddRow road Select Event Table Prey ADC E Select Average Prev GED Select Automated Analysi Set 2 Shim Select Shim File Select Start Level Select Stop Level RMS Enter Stop Condition Goto Select Destination Enter Count Load Select Event Table Select ADC Select Average Select Gradients Select Automated Analysi i Select Shim File Select Start Level SelectStop Level RMS Enter Stop Condition Figure 67 Scheduler Table To define a schedule do the following 1 Select an Operation Click on Load and then the down arrow at the right side of the operation box on Row 1 to display a list of operation types Select one of the types 2 Enter Parameter Data The operation you select determines the number of data entry boxes that are displayed Enter appropriate data in each of the boxes for the selected operation 3 Click on Add Row to add the next row Then repeat Steps 1 and 2 for
20. Freq Dom ain Units Figure 121 New Task Configuration Frequency Domain Units Dialog Box Windows Menu The Windows menu allows you to arrange all windows in a tiled display Fe a DICES L E pe o one at ae ten eg INMEITI 1pm Tass p L rrer Ll y Ed Erg J PLPC A Figure 122 Windows Menu Options Clear Command This option clears the data from all windows Title Command This option displays a dialog box that permits you to enter a new title name for the window Figure 123 Title Command Dialog Box System Operation UM SW50407 05 127 Typical Configuration Examples Typical examples of configuring a window for plotting a variable are given below Example 1 Main Transmitter Frequency This example shows how a window is configured to plot main transmitter frequency WINDOW TITLE Frequency VARIABLE TO BE PLOTTED Use First Baseline Use First Phase Data 57405070 00 Max 57405240 00 Min 57404530 00 Mean 50405157 Std 39 934 _ PHF amp EFNT VAI TLF mI LIFE MINIMUM VAT TIE MEAN VAI TIE STANDARD DEVIATION VAI LIFE Figure 124 Plot of Main Transmitter Frequency Example 2 RMS Value of FID This example shows how a window 15 configured to plot the RMS value of the FID Free Induction Delay ine Use Fist Phase Figure 125 Plot of RMS Value of FID System Operation
21. I Lj Lj I I 1 1 1 1 1 1 1 1 4 20 40 100 120 140 160 180 200 220 240 250 280 300 320 340 360 380 400 420 440 460 mSeconds RMS 975202 Shit 31437 5 Figure 86 Display of Inverse FFT FID Magnitude The magnitude command computes and displays a power spectrum of all data in the frequency domain spectrum Essentially it squares all values thus eliminating all negative values and displays the relative power of the signal at each frequency regardless of polarity Phase Clicking this menu item displays the dialog box shown in Figure 84 Using this box you can define peaks and execute zero order and first order phase corrections gt Phase Correction Peaks Dsfinition syrnmetnic zero Order Phage i zero Order Phas Peak Thresh ils L th tal Angle eak Thresh 90 Tails Length 5 20 mm Total Angle Count i Step degrees 5 Direction Left Zero Order Phase With Manual First Order Phase First Order Phas Pre Delay se 0 Total Angle po foun Thresh 2 for Angle E Create PivotList 1855 Belta 2 Figure 87 Phase Correction Dialog Box Peaks Definition This panel contains parameters for selecting peaks for phase correction You can set maximum value for recognizing a peak Peak Thresh the direction in which to search for a peak Direction and the number Count of the
22. Qualion NMR Process Lab NMR Nuclei Magnetic Resonance Analyzer Model MASH Style D User Guide UM SW50407 05 Table of Contents Table of Contents Table oL Contents reface 0 090909000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000 tP 1 i 1 7 easuremen rincip e 06090909000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000000 i E 5 Transiti nersystates and INIVIR SPCC M T E SPP ACKO isis es A NAN Chemical Shif 10 ear te N tout AE A a Time D i d F yD in Data Pl 11 ime Domain and Frequency Domain Data 105 I ing F D in S 11 hiterpretimp Frequene y Domal as utum bed eat menace ale ena N ei a uiu 5 A al DZ ienal Proeessme Time Domain hcre ee veu ds ous den ep SE AAAS a N de deir e
23. Sample switching The processing of time sharing an NMR analyzer among several processes Samples are accepted from multiple processes by sequentially switching from one to the next Shim An adjustment of the gradients within the magnetic field to produce a more uniform field for a given type of process sample The hardware component that controls all shim coils in the magnet Shim gradient The difference in magnetic field strength between two points on any given axis Shim method The procedure for calculating required adjustments in currents to the shim coils 124 Signal averaging A technique for enhancing signal to noise ratio in data that performs a time average of multiple sequential signals that reduces errors due to random variations Software lock A debugging feature that permits the user to shut down the hardware automatic lock detection system and to simulate its function by manual means Spectroscopy The technique of analyzing the properties of a substance by generating a characteristic spectrum of frequencies peculiar to that substance Several different types of spectra may be used such as mass infrared or NMR A range of frequencies Ce exponential equation to that data applying a specific type of algorithm to the data A post processing function that enhanced digital resolution of a set of data by adding a group of zero data points thus increasing the resolution without degrading the spectral inform
24. 15 9 25 AUX LEDs on the front panel indicate the presence or absence of each voltage The AUX voltage 5 V provides power to auxiliary equipment The Power Supply of the Lab Analyzer does not have a I O Unit PLC since it is not required on this application COMPUTER The rack mounted computer provides supervisory control for all other units in the analyzer cabinet This unit is an Intel Pentium PC supplied with standard peripherals and I O functions such as an analog to digital converter for Channels I and Q a system control board control for the sample switching system and a direct digital synthesizer It also provides a communication link to a remote computer and the distributed control system Note that the computer is supplied with two removable hard drives both of which contain the system software The Hard Drives are connected to an internal Raid which keeps the data on both hard drive updated equally If one of the Hard drives fails in terms of Hardware it can be replaced with a new hard drive the in ternal Raid will re build the backup array automatically The direct digital synthesizer receives a buffered 36 MHz input signal from a crystal oscillator mounted in the Switching Control Unit The synthesizer uses this signal as a clocking reference and divides the 36 MHz signal by four to create 9 MHz signals which are used in creating the Main DDS and Lock DDS output signals The Main DDS frequency is set t
25. 218 2b Gxyyz c 09 0 1 e Gpp 59 Gzpp 3 64 GHEHE 35 Gadd 0 0 0 5 Spectra ai 10 Spectra 450 Spectra Emergency Power Switch QUALIOH Ltd Copyright 2007 Figure 41 Shim Gradient Screen Result of Spectral Analysis Automatic Electrical Shim Electrical shimming can also be performed automatically using the Process NMR application To perform the automatic shimming do the following 1 2E LE Verify that on the Event Table the folloing parameters are set correctly accotding to the specific System a Ix Gain b Pulse Width in therms of time c Receiver Gain d DC offset 15 set to the right value Run the Process NMR from the menu click on the Sced button The Scheduler table will be displayed Click on and choose Load option Browse from the NMR Shim AutoShim folder and load the AutoShim schd file Click the Set Button on the scheduler table the table will be close automatically From the Process NMR run the Scheduler System Operation UM SW50407 05 65 Standard Procedures Perform Time Domain Signal Processing Perform Time Domain Signal Processing Several types of time domain signal processing are used with the Process NMR Analyzer such as setting parameters for the analog to digital converter signal averaging zero filling window smoothing function and removing zero offset T
26. 5 When the pulse widths are within spec you can proceed with normal operation Save the current shim set to file Be sure to include the date as part of the filename so that you can clearly determine when it was used in operation STARTUP AFTER LONG SHUTDOWN MAGNET COLD If the system has been down for several hours or more the magnet is cold Power and utilities may also have been shut off if the system has been off for an extended period of time Under such conditions use the following procedure 1 Turn on electric power and instrument air supply 2 Switch on purge system 3 Run for 12 hours to allow the magnet to warm up 4 Verify that sample is flowing properly to the analyzer If it is not contact the local plant personnel to remedy the problem 5 Run Heater Diagnostics System Operation UM SW50407 05 62 Standard Procedures Shutting Down the Analyzer 6 Check magnet temperature If the magnet temperature is approximately 41 C proceed If lower than 41 C let the system warm up longer until the temperature reaches the target 7 When the magnet is up to temperature and the system is running check the pulse width at 1 10 height and half height If widths are within spec proceed If not reload the most recent shim set file and re check the pulse widths If OK proceed If not you will have to re shim the magnet 8 When the pulse widths are within spec you can proceed with normal operation 9 Sav
27. Analysis on page 83 Help Click this button to display online Help SCREEN TOOLS Vertical Grid Click on this tool to add or delete a vertical grid System Operation UM SW50407 05 Automated Analysis 97 Windows and Dialog Boxes Automated Analysis Horizontal Grid Click on this tool to add or delete a horizontal grid Pan Click on this tool to move the screen in any direction by then clicking and dragging on any point in the screen Zoom X Click on a point and two cursors appear Click on the left cursor to set one end of the range to be zoomed Click hold on the other cursor and move it to the other end of the range you wish to zoom Release the mouse The screen then zooms the selected range in the X dimension Zoom Y Click on a point and two cursors appear Click on the left cursor to set one end of the range to be zoomed Click hold on the other cursor and move it to the other end of the range you wish to zoom Release the mouse The screen then zooms the selected range in the Y dimension Zoom X Y Click on a point and drag to define an area of the screen to be zoomed Release the mouse The screen then zooms the selected range in the X and Y dimensions Zoom All Reset Click on this tool to return the display to the original screen Clear Click on this tool to clear the screen display Real Portion Click on this tool to display the real signal Imaginary Portion Click on this t
28. Click to cancel and ignore new entries CPMG is an acronym for Carr Purcell Meiboom Gill a specialized method of performing an NMR experiment using echo pulses The CPMG method is not currently used in Qualion NMR applications Average This is the same function described in Signal Averaging on page 36 ADC This is the same screen described in Setting up the ADC on page 34 Frequency Clicking the Frequency button displays the screen shown in Figure 73 This tool is typically used for manually adjusting the main transmitter frequency during troubleshooting or initial startup Frequency Frequency 57742043 1000 Lock Status Freq Shift Software Lock Figure 76 Frequency Dialog Frequency this displays the current value of the main transmitter frequency which is normally controlled in a fixed ratio to the lock frequency Shift enter a value for the increment by which you want the main transmitter frequency manually increased ot decreased such as when you manually search for the proper main transmitter resonant frequency Set Button click to activate your data entries System Operation UM SW50407 05 92 Windows and Dialog Boxes Automated Analysis Software Lock click to operate with a software lock function instead of the normal hardware lock system If a value is displayed the system forces the frequency increment to equal the value displayed in this
29. To determine the values to enter for each parameter refer to the descriptions of each signal processing function which start on page 34 gt App 1 Automated An Select Functii Y 1 Select Function g Select Function Cancel Figure 63 Automated Operations Screen Automated Operations gt t Lert 1 001 200 0 3 Remove OC ero Fill Windaw JFET IFFT Magnitude Auto Phase Manual Phase Zero Order Phase First Order Phase Baseline Figure 64 Automated Operations Screen Function Select System Operation UM SW50407 05 53 Windows and Dialog Boxes Automated Analysis w Aul om ees 14111 Magnitude Auto Phase Manual Phase cero Order Phase Firat Order Frase Baseline Reference Remove DC From Channels 1 amp Fil Sad zeros bo signe Figure 65 Automated Operations Screen Tooltips PREDICTION Click on the Pred button to display a dialog box for setting up prediction calibration models for use with the DCS as shown in Figure 63 H Prediction x File D inmrtcallApi 5 18 cal 5 Valve Dime eal Valve 5 18 cal Valve D Anmrcal T50 5 1 a cal Value 18 61 1 Valve l Figure 66 Automated Operations Screen Prediction Function To set up a new calibration model click the
30. pcAnywhere Selection Screen 3 Click on the icon for the system you want to monitor or create a new Icon by editing a new Icon right click and following the Basic wizard The system then automatically attempts to establish the phone connection E pcAnywhere Connecting Connecting Dialing Connecting Waiting Far connection Figure 47 Dialog Box Indicating Call in Progress 4 Wait for system to dial and connect System Operation UM SW50407 05 71 Standard Procedures Activate an Existing Connection Symantec pcAnywhere Host Login Enter the Caller login credentials For connecting to the pcAnywhere Host User name Lu Password pO Cancel Figure 48 pcAnywhere Login Screen 5 Enter your name and password when requested If OK you will be connected to the remote system just as if it were a local system You can then perform all system functions as you would with a local system Some operations such as closing the session ot rebooting the remote system may require you to use standard pcAnywhere tools such as Exit Remote Control Session or Send Ctrl Alt Delete to Remote System To determine which icon you should use place the cursor on a pcAnywhere tool icon and wait for pop up help to appear For detailed information refer to the pcAnywhere manual supplied with your system e A typical example of remote monitoring is shown in Figure 46 Lm Irae cc ELE J
31. the screen Note that six windows are usually the maximum number of windows that can be viewed conveniently 5 When completing the configuration it is possible to save it to a file for later recall 6 To begin plotting data click on Start in the main menu If desired accept the default mode Ignore Errors which inhibits the display of any errors As an alternative it is possible to click on Ignore Errors and toggle the mode to Display Errors To stop gathering data at any time click on Stop 7 As data 1s plotted the x axis and y axis scales change automatically to accommodate the information gathered System Operation UM SW50407 05 120 Maintenance and Diagnostics Diagnostics File Menu This pull down menu shown in Figure 109 permits to recall a previously saved configuration setup or save a current configuration It is also possible to specify a backup directory and define the form in which the file is saved DIAGNOSTIC E New Task Stat Stop Windows Figure 109 File Menu Options New Task This menu item creates a new window for collecting and plotting data as shown in Figure 110 It first appears in the center of the screen Additional windows are cascaded in sequence as they are created Use the Windows tiling commands to arrange them on the screen NMR DIAGNOSTIC File New Task Start Siop Windows Ignore Errors Clear Title Heb du
32. ADC as described in Figure 17 The duration of the acquisition period is a function of the number of points acquired and the rate at which readings are taken The bandwidth 15 a value entered directly into the ADC parameter setup screen 90 Pulse The FID signal is controlled by changing the duration PW of the main transmitter pulse First you find the 180 point by adjusting the PW to generate a null RMS value You then set the PW to another phase by applying an appropriate percentage to the 180 PW value For a 90 pulse use 50 of the 180 value for 60 pulse use 33 3 for 45 use 25 SIGNAL RECEIVED The signal detected by the main receiver after the transmit pulse is removed is the Free Induction Decay or FID This is a time domain signal with an exponentially decaying shape as illustrated in Figure 16 Note that the RMS root mean square value for the FID is continuously displayed in the lower left corner of the screen The characteristics desired in an FID display see Figure 16 are A high RMS value which indicates a slowly decaying envelope This yields a narrower peak and better digital resolution in the frequency domain display A smoothly decaying envelope that reaches zero about halfway through the acquisition cycle This usually indicates a good signal to noise ratio If the signal does not approach zero further sional processing is needed to eliminate noise A total acquisition time that yields eno
33. Add Row button This adds a blank row to the screen The items you must enter are Register this is the modbus register address of the data point generated by the calibration model Time this is the modbus address of the time stamp that identifies the when the data point was stored Flag this is the modbus address of the flag which is set when a value is stored Confidence This is the address where the confidence level of a data point is stored System Operation UM SW50407 05 4 Windows and Dialog Boxes Automated Analysis Cal File this is the name location of the calibration file that you are using for this output The following six parameters relate to an Outlier condition Low Low limit for calculated values High High limit for calculated values Op AND OR logic used to test the M distance of a data point for acceptance If AND is selected the reading must be lower than the Low limit or higher than the High limit and higher than the M dist value for an Outlier condition to exist If OR is selected and the reading 1s lower than the Low limit ot higher than the High limit ot higher than the M dist value an Outlier condition exists M dist The Mahalanobis Distance for the calculated prediction data The M Distance 15 a statistical measure of the deviation of a data point from the statistical mean of a group of data points In ProcessNMR the M Distance is used in reference to
34. Enter a value for Mean Range This is the number of points starting at the leftmost point to be used for the range over which the baseline is to be corrected e Enter a value for Num Std Peak The 15 the number of standard deviations of noise to be used for peak detection In this case enter a 1 e Inthe Method window select a curve fitting method for computing the baseline cotrection The available choices are 1 Nearest ii Polynomial enter the degree of the polynomial in the next box Spline iv Cubic v Linear e When you have entered your parameters click on the Find Baseline button to make the computation and then click on the Correct button to execute the correction System Operation UM SW50407 05 54 System Operation Signal Processing Digital and Frequency Domain PEAK SELECTION The dialog box shown in Figure 34 appears when you click the Peak button in the Signal Analysis menu To define the desired peak enter the peak threshold value specify the direction of the search and enter the specific peak first second third or other To find width of that peak in Hz at a certain peak height select the peak height and click the Get Peak Width button To specify a reference location enter the location in ppm and click Reference Peak button 1 1 Peak Referance Peak Identificatia Peak Thresh 0 1004 90 Stark Counting From Peak Index Width Peak Height 0 100 Feak Referance
35. Main Menu Suto Predict Help NI Load This is a standard Windows Load command which displays a window that allows you to select a file to be loaded Save This is a standard Windows Save command which displays a window that allows you to select a directoty and filename in which to save your file Print System Operation UM SW50407 05 59 Windows and Dialog Boxes This is a standard Windows Print command which displays a Windows Print window with normal print options Start Click on the Start button to start the main transmitter and the data acquisition system Stop Click on the Stop button to stop the main transmitter and the data acquisition system Event Table The Event Table screen when called from the ET button has a menu with two pulldown submenus File and Pulse described below File Menu a Event Table File Pulse Offset E 42 Offset 1 45 Mew Set Table Channel 1 00u 299 nnu 21 00u Set 0 00u PreTx Set 2 0 oO oO Oo Figure 73 Event Table Screen Open this selection permits you to open a file with a stored set of parameters and use these parameters for the next analysis Save this selection permits you to save a set of parameters as a file for future recall Pulse Menu System Operation UM SW50407 05 Automated Analysis 90 Windows and Dialog Boxes Automated Analysis
36. Overview 2 System Operation A WARNING Actions described in this chapter should be performed only by properly trained personnel Improper modification of system parameters may void system warranties and performance guarantees Overview This chapter describes how you can operate the Process NMR Analyzer to achieve specific goals It is therefore primarily a description of the screens and software tools and how to use them to accomplish a task Operation of system hardware both mechanical and electronic is described in detail in Chapter k This chapter is organized into two main sections as follows Applications a list of typical process applications in which the analyzer is currently being installed showing the wide range of uses of the instrument Functional System Description a top level description of the complete system that shows how the system is structured to achieve the application goal and how each subsystem functions within it Chapter 3 Standard Procedures is designed to work with Chapter 2 as a quick how to reference that summarizes the procedures necessary to perform typical user functions Cross references to detailed functional descriptions or theory of operation are included where applicable Chapter 4 Windows and Dialog Boxes is a a quick reference chapter that includes all major windows and dialog boxes with short descriptions of each menu item Each screen description includes
37. TO ACTIVATE 3 VVAY PROCESS SAMPLE SELECTOR VALVES Figure 37 Multiplex Sampling System Functions performed by the multi input sampling system are described in more detail below FUNCTIONAL DESCRIPTION OF OPERATION Operation of the multi stream sampling system is controlled by three software items the Multi Stream Scheduler the Event Table and the Automated Analysis Table Scheduler The Multi Stream Scheduler is the top level controller of the sampling system It determines the order in which streams are analyzed loads all applicable files for each stream starts stops and repeats the sequence of operations performed on each stream Event Table The Event Table controls the sequencing and operation of various valves in the sampling system as directed by the Scheduler It also controls all functions related to data acquisition such as timing of transmitter pulses gain settings for transmitter and receiver turnaround time between transmit and receive etc Automated Analysis Table The Automated Analysis Table controls all post acquisition signal processing functions such as Remove DC Zero Fill perform FFT Auto Phase Baseline Correction Reference Averaging Prediction etc Typical Screens System Operation UM SW50407 05 58 System Operation Multi Stream Sampling System Typical screens for the Scheduler Event Table and Automated Analysis table are shown below These screens are accessed by right click
38. The pulse signal is sent to a diplexer circuit in the Main Receiver Module and then to the main coil in the probe The diplexer circuit switches the signal to the probe between the Main Transmitter and the Main Receiver After the pulse is transmitted to the probe the pulse is turned off for a specified wait time The receiver is then enabled and the signal generated by the coil during relaxation is sensed by the receiver This low level microvolt signal is amplified by a broadband low noise preamplifier to prepare it for mixing and further processing Before mixing the signal is nominally at the transmit frequency 57 60 MHz If the signal level is too high an 18 dB attenuator normally off may be switched in as needed An intermediate frequency IF is then created by adding 9 MHZ to the MTXLO signal and subtracting 9 MHZ from the received signal Gain control is applied in the IF section of the Main Receiver The IF NMR signal is mixed with the 0 9 MHz reference signal to create a non phase shifted audio signal centered at 0 Hz The audio signal is then split into audio signals phase separated by 90 The 0 signal is the Channel I audio output signal The other is the Channel Q audio signal This creation of two identical channels out of phase by 90 is called quadrature detection Its purpose is to differentiate between NMR signals from atoms spinning faster than the applied transmitter pulse and those spinning slower than the appli
39. a refernce WOODY AVERAGING Woody averaging is a digital signal processing technique for improving the signal to noise ratio of the data It is used with repetitive data sets in which the system generates a series of spectral traces that shift slightly from one another Woody averaging computes the center of gravity from a series of data sets and generates a single trace symmetrical about the center of gravity of all the data To use the Woody average function you must make appropriate entries in Automated Analysis on page 83 These entries require that you set up the sequence of operations so that you first save a series of data sets Then you can apply the Woody average function and save the result When you have Woody averaged the specified number of samples the result can be displayed or used as the input to the next operation in the sequence of automatic operations System Operation UM SW50407 05 57 System Operation Multi Stream Sampling System Multi Stream Sampling System The Process NMR Analyzer can be configured to accept samples from several different process units by using a separate automatically controlled sample switching system as shown in Figure 37 PHOCES S 1 PROCESS 2 PHOCESS 3 PROCESS 4 PHOCESS 5 SAMPLE SAMPLE DM ES SAMPLE SAMPLE SAMPLE SWITCHING UNIT SAMPLE RETURT EE V EE y STOP A FLOW VALVE MLILTIPLEX CONTROL SAMPLE MANIFOLD VALVES MMR ANALYZER ON OFF PNEUMATIC SIGNALS
40. and other associated items Each operation executes a selected command Set Reset or GoTo according to the parameters entered in the cells of the table When you add a new event you must also enter values in each cell duration channel and value associated with the function If no value applies enter a zero The two boxes at the top right of the screen are the values entered for correcting offsets from zero that may be found in the quadrature signals for Channels I and Q To determine these values display the two channels and observe the magnitude of the offsets for each channel Then enter values in the boxes fot each channel that reduce the offsets to zero To add a new function click the Add Row button new tow then appears at the end of the table Enter data as needed To add a tow at a point within the table click on a cell below which you want to add a row Then click the right mouse button window appears with several options such as Cut Paste Copy and Insert Row Select Insert Row and release the mouse button row 1s then added below the cell where the cursor is positioned Click the New button to create a new empty Event Table After you have entered parameter data click the Set Table button to make your data entries effective The Duration parameter as the name indicates is the time the function 1s to be applied Units may be minutes seconds milliseconds or microseconds The Channel parameter is selected from a
41. cross references to more detailed descriptions that appear in other sections of the document APPLICATIONS The table titled Refinery Applications on page 30 is a list of typical online process applications in which the Qualion NMR Analyzer is currently being installed Note that a single analyzer system through the use of multiple calibration models is capable of measuring many different process variables simultaneously from the NMR spectral analysis of a single sample stream Measurement Analytical Capabilities The primary output of the analyzer is a spectral analysis of a process sample as shown in Figure 11 Although the sample can theoretically be a liquid solid or gas the applications currently being installed are all liquids The trace of the sample spectrum is interpreted to indicate the presence of specific constituents of the sample and the quantity or concentration of each constituent in the sample The presence of a constituent is indicated by the chemical shift of a peak measured from a System Operation UM SW50407 05 J5 System Operation Overview reference see Figure 12 The quantity of the constituent present in the sample or concentration 15 determined by integrating the area under the peak for that constituent Presence and Quantity of all Constituents Spectral Analysis Acai DD L 0o E n CH PEAK CH PEAK AROMATICS
42. data points generated by a calibration model If a data point has an M Distance greater than a specified limit that point is not used in the data set and 1s instead flagged for evaluation by a qualified person A data point with an M Distance less than the limit 1s automatically included 1n the data set Count The number of consecutive counts required for the Outlier condition to activate a valve Valve The identification of the valve to be actuated This paragraph does not refer to the Lab Analyzer The index number is automatically incremented with each line you add This determines the order in which prediction results are displayed on the screen and or transmitted to the DCS To change the order of display change the position of the lines in the table As the model calculates values periodically during operation it outputs its results to the addresses you have entered above The system then transmits them to the DCS SCHEDULER N WARNING Actions described in the following section should be performed only by properly trained personnel Click on the Sched button to display the scheduler table shown in Figure 64 This dialog box 1s used with a multi input sampling system in which samples drawn sequentially from several different process units Up to five process sample streams and a grab sample may be connected to the switching unit The Scheduler table lets you define the sequence and content of the Scheduler
43. determines the best placement of each segment in the final assembly to achieve a consistent uniform field for the assembled magnet The segments are then bonded together to form the final magnet assembly The assembly is placed inside a soft iron cylinder that constrains the magnetic flux and prevents the magnetic field outside the magnet housing from exceeding a value of as little as 1 gauss More importantly the iron cylinder raises field strength in the center of the magnet by pushing the flux toward the center a process called condensing the field Temperature of the shroud is maintained at a lower temperature than that of the magnet itself Since temperature of the magnet and sample must be so tightly controlled to achieve the desired accuracy of measurement four thermistors are mounted at various points on the magnet to sense magnet temperature A heater control unit receives temperature measurement information from the thermistors and regulates current to several resistance heating strips bonded to the outside of the magnet assembly Similarly four thermistors are bonded at various point to the magnet envelope The Heater Control Unit uses the thermistor signals as inputs to a control loop that in turn controls current to heaters bonded to the envelope The control functions for these two temperature PID loops are performed by the Heater Control Unit The software that executes the control algorithms which is supplies with the main syst
44. direction of the search Direction and enter the number Count of the specific peak first second third or other To perform a Symmetric Zero Order Phase correction go to the Symmetric Zero Order Phase panel Enter the Tails Length in percent and the Step in degrees and click on the GO button To perform an automatic Zero Order Phase adjustment go to the Zero Order Phase With Manual First Order Phase panel Enter the pre acquisition delay Pre Acq Delay in seconds the maximum angle or slope of the trace for defining a peak Thresh for Angle and the change in frequency ot ppm for recognizing a separate peak Delta Then click the GO button The Total Angle automatically appears in the Zero Order Phase panel To perform a First Order Phase correction go to the First Order Phase panel Click on the Create Pivot List button and then select the location of the First Order Phase pivot in the box at the right Click on the or buttons to make changes You can observe the effect of each incremental change by displaying the spectrum in another window When you have found a satisfactory value you can exit from the screen Lastly enter the Total Angle in Automated Analysis on page 83 If you choose to perform a manual Zero Order Phase correction go to the Zero Order Phase panel Click on the or buttons to make changes You can observe the effect of each incremental change by displaying the spectrum in another window When you hav
45. entire unit Refer to the Parts List in Reference Documents on page 1 for part number identification and ordering instructions Regular Maintenance Perform the following maintenance procedure at least once per month e Since the atmosphere in which the system is installed may be highly corrosive carefully check the air conditioning systems for corrosion and promptly replace any defective units before serious damage can occur Long Term Maintenance 1 Remove the top cover of the enclosure and clean the fins of the air conditioners Dust can be removed with compressed air 2 Since the atmosphere in which the system is installed may be corrosive carefully check the air conditioning systems for corrosion and promptly replace any defective units before serious damage can occur System Operation UM SW50407 05 107 Maintenance and Diagnostics Diagnostics Diagnostics N WARNING The diagnostic tools described in the following section should be used only by Qualion NMR technicians They are included here only for educational purposes HEATER DIAGNOSTICS The purpose of the Heater Diagnostics software is to permit you to monitor and evaluate performance of the heater control loops for magnet temperature and envelope temperature It is also possible to modify the control parameters for each PID loop A typical Heater Diagnostics screen is illustrated in Figure 88 Note that Figure 88 can display up to 4 windows The typical scr
46. file click on Plot File on the Chart Channels dialog box This opens a dialog box that allows you to select a file for display Chart Channels oon Menu Plot File ene s zoom r Zoom and zoom All Figure 93 Chart Channels Zoom Menu Options When the Add Window command on the Windows menu and the select Zoom are selected the dialog box shown in Figure 92 appears The options are Pan Permits to click and drag an object to any place on the screen Zoom X Permits to select a range using cursors in the X direction and expands its display Zoom Y Permits to select a range using cursors in the Y direction and expands its display Zoom X and Y Permits to select ranges using cursors in both X and Y directions and expands the display Zoom All reset Resets all ranges to the original screen display Magnet Menu I H eater d Magnet w 2 Lawers a l awers Figure 94 Magnet Menu This menu has only one option 2 Layers which refers to the type of magnet construction At present only the 2 Layers option 15 active Proportional Integral Differential PID To check control parameters for the PID loops click on PID in the main menu The following screen appears Select the loop to be displayed from the pull down list System Operation UM SW50407 05 110 Maintenance and Diagnostics Set PID Control Loop Envel pe PN Proportional
47. however that doing so broadens peaks in the frequency domain spectrum Coefficient b this coefficient affects the outer values of the function and is normally not used in NMR applications Quit Button Click this button to abort the operation Perform Button Click this button to execute the operation System Operation UM SW50407 05 106 Maintenance and Diagnostics Preventive Maintenance 5 Maintenance and Diagnostics This chapter defines recommended preventive maintenance procedures necessary to ensure optimum equipment performance and also describes the diagnostic software tools you can use to troubleshoot the system If replacement of parts is required please contact your distributor or Qualion Service Support Department Preventive Maintenance Purge System Regular Maintenance Drain and clean the air supply regulator s at least once per month Long Term Maintenance Perform the following maintenance procedure at least once every three months 6 Verify system operation by performing shut down and restart 7 Examine the entire Purge Protection System and the protected enclosures and replace any defective parts during the next routine shutdown of the system Refer to the Parts List in Reference Documents on page 1 for part number identification and ordering instructions AIR CONDITIONERS The air conditioning units are not designed for local servicing If a serious problem occurs replace the
48. in Figure 36 Typically you set the reference to the value at which the peak is presently located This effectively shifts the x axis zero to the center of the peak you have specified System Operation UM SW50407 05 56 System Operation Signal Processing Digital and Frequency Domain NMR Analysis Running On Local Machine File Archive Processing View Data Run Tools Hardware c c e M amp 2 Save Print Start Stop E T Avg ADC Freq Shim Lock Auto A Help Faaa Ree Remove DC Zero FFT IFFT Magnitude Real 800 700 600 500 400 300 200 100 100 200 400 500 500 700 800 900 1000 1100 RMS 9629 69 Shift 299 50 NMR Analysis Running On Local Machine File Archive Processing View Data Run Tools Hardware Help Sire m Load Save Print Start stop ET Avg ADC j Shim Lock Auto A HI lt O Ree Remove DC Zero Fil FFT IFFT Magnitude Phase Baseline Peaks Window 200000 14 Peak Referance 180000 Peak Identification Peak Theesh 0 10 n 160000 TE Stat Counting From Left 140000 h Peak Width 120000 With Peak Height 0 100 fio Tous Get Peak Width 80000 Peak Referance S a 60000 L LI s00 1000 1100 1200 1300 700 RMS 9559 89 Shit 271 89 After Figure 36 Setting
49. multi input sample switching system The physical and chemical characteristics of the sample affect the uniformity of the field and therefore the operation of the analyzer Because of this the system must be calibrated for each type of sample and a set of parameters developed for use with that particular type of sample These parameters which are largely associated with the shimming requirements for that sample are stored as a shim set Whenever you run that type of sample you can recall the stored shim set for that sample Similarly you also recall other sets of system setup parameters that apply to that sample type In current installations the analyzer operates on a stop flow cycle This means that the probe 15 first flushed or purged with the sample fluid or another purge fluid for a specified time The valve is then closed for a specified wait time which is related to the relaxation time of the sample nuclei A new sample is then admitted to the probe by opening the valve for a specified time The valve is then closed and a main transmitter pulse is applied for a specified time After a pause the valve is then opened for a specified time and the probe is purged The cycle is then repeated Use of a stop flow cycle means that the sample is stationary during the time the pulse 1s applied and the probe is flushed between readings Use of a stationary sample enhances overall accuracy and resolution of the analysis System Operation U
50. pcoinywhere aude a i T nantec pcAnywhere pcAnguihere Manager 8 Fermes Duck Connect Quck Deploy and Connect Syr Option Sete iD Sete Add to Favorites Properties 2 Refresh Start Host ay Explore Cures Direchon New Figure 45 Activate an Existing Connection Activate an Existing Connection To perform remote monitoring of an installed system via an existing dial up phone connection do the following 1 From the Start Menu select pcAnywhere As an alternative click on the pcAnywhere icon on your desktop NOTE Before you use pcAnywhete it may be useful to read the pcAnywhere instruction manual provided with the software for explanations of the standard tools and menus 2 In pcAnywhere click on Remote Control icon System Operation UM SW50407 05 70 Standard Procedures Activate an Existing Connection Symantec pcAnywhere File Edit View Help nantec 58 Quick Connect Quick Deploy and Connect Hosts CoM Remate Control Favorites File Transfer File Transfer Network Cable DSL Remote Control Command Queues ra Remote Management 1 Remare Management 88 pcAnywhere Tools EX Option Sets fra Serial ID Sets Device Connect to Stark Mode Fer Properties Refresh 51 Start Connection Explore Current Directory Mew Folder Figure 46
51. peak to look for such as first second or third System Operation UM SW50407 05 103 Windows and Dialog Boxes Automated Analysis Symmetric Zero Order Phase This panel contains parameters to perform a Symmetric Zero Order Phase Enter the Tails Length in percent and the Step in degrees and click the GO button Zero Order Phase with Manual First Order Phase This panel contains parameters to perform an automatic Zero Order Phase Enter Pre Acquisition Delay time Pre Acq Delay in seconds the maximum angle or slope of the trace for defining a peak Thresh for Angle and the change in frequency or ppm for recognizing a separate peak Delta Then click the GO button The Total Angle automatically appears in the Zero Order Phase panel Zero Order Phase This panel contains buttons to perform a manual Zero Order Phase correction Click on the or buttons in this panel to make changes You can observe the effect of each incremental change by displaying the spectrum in another window When you have found a satisfactory value you can either exit from the screen or continue with making a first order correction Lastly enter the Total Angle in Automated Analysis on page 83 First Order Phase This panel contains parameters to perform a First Order Phase correction Click on the Create Pivot List button and then select the location of the First Order Phase in the box at the right Click on the or buttons to make changes You ca
52. the Result box with the previous best result value in the Best Result box and decides whether to keep or discard the incremental change The process is then repeated with another change which is also tested for efficacy When a coarse optimum value is achieved the system applies increments to more than one gradient value and the process is repeated Multiple parameters are entered because of the interaction among the gradients changing one affects many others Typically up to 4 gradient values are changed at a time The Best Grad value is the gradient that corresponds to the Best Result value Level is the level of precision achieved 1 2 3 or 4 in shimming After finding an acceptable value for four gradients another set is modified in a similar manner Eventually all gradients are adjusted and readjusted in a trial and error hill climbing process that produces a set of optimum values for all gradients This group of values is then saved as a best gradients or any title including date The entire shimming process can take as little time as 1 2 hour for a previously shimmed magnet or as much as 4 or 5 hours for an unshimmed magnet System Operation UM SW50407 05 26 System Overview Major Hardware Components POWER SUPPLY AND I O UNIT The Power Supply and I O Unit which is mounted on a rack in the Electronics Compartment provides all DC operating voltages for the system The voltages 24V dc 15 volts
53. the signal and outputs a 49 MHz signal which is used as the main transmitter and receiver local oscillators MAIN LO and MAIN RX LO A 9 MHz signal from the DDS unit is added to the MAIN LO signal to produce the main transmitter frequency of 58 MHz which is transmitted to the diplexer and then switched to the main transmitter coil in the probe After the main transmitter pulse is removed the nuclei relax and generate a 58 MHz signal in the coil which flows to the diplexer where it is automatically switched to the receiver input The received signal is amplified and then mixed with the MAIN _RX_LO signal 49 MHz to produce an System Operation UM SW50407 05 18 System Overview Lock System Intermediate Frequency IP of 9 MHz This signal is then mixed with 9 MHz from the DDS card to produce an audio frequency of approximately 1 kHz The audio signal is then split into two equal channels I and phase separated by 90 The I and Q signals are then input to the ADC where they are converted to digital form for input to the PC The signal processing functions performed in the time domain are Quadrature detection Signal averaging Window function Remove dc offset ADC parameters bandwidth sampling rate Zero fill Brief descriptions of these functions are given below For detailed descriptions of each function refer to Chapter 3 Standard Procedures Quadrature Quadrature detection ena
54. to close the dialog box m Modbus Configuration Exit Port Settings Fort Number Parity Baud Rate Byte Size Stop Bits Flows Status closed Connect Sa Device ID 1 Denn Address 1 Read Silent Intr mx 2n Data h writ rite Timeout m BOO TEET egister Register Type Float POR M M RR 4 Double Double Reverse Figure 58 Config Modbus Dialog Box DCS This paragraph does not refer to the Lab Analyzer Click on the DCS button to display the menu shown in Figure 56 57 or 58 In the check boxes at the top of each screen you can enable or disable the Alarms Outlier or DCS Override menus These screens are used to configure your system for handling alarm information Click the button on the left of the display to access the menu you want to configure The choices are Alarms Outlier and DCS OverRide System Operation UM SW50407 05 79 Windows and Dialog Boxes Process NMR Application p Alarms Ignore Alarms Flag is OFF mE 1 TD FOXBORO HME Ltd Copyright 2005 Hormal State Current State User s Label Alarm Type Alarm Action DCS Address 0 Stream 1 Health Stream 1 Stream Skip R1199 Stream 2 Health Stream 22 Stream Skip R1199 Straem 3 Health Stream 3 Stream Skip R1199 Stream 4 Health Stream 4 Stream Skip R1199 High Inlet Temp Hone Sleep Sleep R1135 Bottle in place Hone Grab Hone R1199 Low Inlet Flow Hone St
55. to execute the task The recommended procedures for setting up a new connection and for activating or terminating an existing connection ate described below BEFORE SETTING NEW CONNECTION Make sure a Modem is installed and recognized by the Operation system and a telephone line is also connected it is recommended to dial from the PC via Hyper terminal or any other embedded SW to verify the Modem and the line are set correctly System Operation UM SW50407 05 67 Standard Procedures Set Up a New System Connection Set Up a New System Connection 1 Open the pcAnywhere application and choose the Host menu 2 Right click the Modem and choose properties See figure 42 San bec pA here Figure 42 Host System Setup Screen 3 Check from the device list the correct device Choose the modem name 4 Push the detail button verify all parameters are as in figure 2 Defaults parameters Host Properties Modem pe 2 4 Connection Info Settings Callers Security Options Encryption Conference Comments Choose up to bao devices for this commection tem by checking the bowes bo the left of the device mames To customize device click the dewice name and then chck Details Device list Intel V32 Data Fax Voice COM 1 COM COM Intel v97HaM Data Fax Voice Connection General Advanced preferences IBEIM CARE oa
56. 00000000000000000000000000000000000000000000000000000000000000000000000000000600009 63 SOU Up AM AMAL Rt Perform Perform SM E NER ENTON UII INI RH DIO RII I VR SERRE NEUE System Operation UM SW50407 05 System Overview Table of Contents erform Time Domain Signal Processing oes tette eere uaa Roa e eoe oe Qao SERVER ENS NE ee erform Frequency Domain Signal PEOCCSSIDS s 222225445846 eun e E onsoauteasaunceosssvesedenecebesecaneess et Up New Calibration Models deae exa neun UE AN unec DO DCS er D et Up Analog Digital Modem Inputs Outputs eee ee ee eee eee ee teet ee tette tete tete tette et Up Remote Control Connections via pcAnywhere 67 Betore setine NEW teda T et Up a New System 4
57. 83 Lock System 13 M Magnitude Command 92 Main Transmitter Pulse 33 Maintenance and Diagnostics 97 Maintenance Preventive 97 Measurement Analytical Capabilities 27 Measurement Principle 1 Chemical Shift 5 Energy States and Transitions 2 Interpreting Frequency Domain Spectra 6 NMR Spectroscopy 2 Pulse Sequences 6 Spin 2 Spin Packets 4 Time Domain and Frequency Domain Data Plots 5 Modbus 67 Multi Stream Sampling System 48 N New Application 62 NMR Analysis Application 75 NMR Analysis Main Menu Signal Analysis Menu 88 NMR Analysis Main Window 76 ADC 81 Archive Processing 77 Auto Analysis 87 Average 81 Axis Units 76 Baseline 94 Clear 88 Command Buttons 78 Data 77 Event Table 79 FFT 90 File 77 Frequency 81 Grids 87 Hardware 78 Help 78 87 IFFT 92 Imaginary Portion 88 Load Command 78 Lock 83 Magnitude 92 Main Menu 77 Pan 87 Peaks Command 94 Phase Command 92 Print Command 78 Real Portion 88 Remove DC 89 Run 78 Save Command 78 Screen Tools 87 Shim 81 Start Command 78 Stop Command 79 Tools 78 View 77 Window Command 96 Zero Fill 89 Zoom 87 MRD Diagnostics Clear Command 117 Configuration Examples 118 File Menu 111 Main Menu 109 New Task 111 New Task Configuration 111 Title Command 118 Windows Menu 117 P Pan 87 Peaks Command 94 Phase Command 92 Prediction Command 73 Preventive Maintenance 97 Print CommandPrint 78 ProcessNMR Scheduler 70 ProcessNMR Application 61 ProcessNMR Main Window 61 ADC 65 Auto Analysis 71 Average 64 DCS 68 Event Tab
58. 85 Modbus signals An Option 2 system shown in the middle diagram uses an Ethernet connection between the system PC server and a remote PC client The remote PC connects to a FieldPoint terminal which in turn communicates with a control system via 4 20 mA analog or discrete signals An Option 4 system shown in the bottom diagram uses an Ethernet link between the system PC server and a remote PLC which then communicates with the control system through an RS485 Modbus connection All systems accept internal inputs from the analyzer through a PLC terminal mounted in the analyzer cabinet power supply unit The Lab Analyzer does not include any interface to communicate with a Control room only a LAN Interface and a Telephone Modem However the Lab Analyzer contains an LCD Keyboard amp Mouse to control the Analyzer locally MAA ANALYZER RS 485 d Ero ES en OPTION 1 SOLID LINES Fa SAMPLE R5485 OE SWITCHING Ex eg SYSTEM 00 OPTIONAL n1 1 OPTION 3 0 7 DASHED LINES ero RS485 MODEBLIS e INTERFACE CONTROL SYSTEM SAMPLE PIPING PHEOCESZ TO RETUAN ARS48 N MODBUS MRA ANALYZER ETHERNET on ur OPTION 2 e NMA SERVER Zi REMOTE CLIENT pso32 ES ETHERNET COMMUNICATION E LL E amp amp nm PIPING ToO CONTROL T SYSTEMI PROCESS RETURN Figure 10 System Block Diagram with Communication Configuration Op
59. Actions described in the following section should be performed only by Qualion NMR personnel This operation is normally required only after the magnet or the system has been physically moved such as during initial installation Since this operation is performed only by Qualion NMR technicians it is not described in the manual Perform Electrical Shimming A WARNING Actions described in the following section should be performed only by properly trained personnel Manual Electrical shimming Manual Electrical shimming is a process that should be performed from the NMR Analysis To perform electrical shimming do the following 1 Run NMR Analysis 2 From the menu click on the Shim button This displays the Shim Gradient Display as shown in Figure 41 3 First click on Set Method A dialog box appears Select the shimming methods you want to use and then click OK 4 Ifyou want to keep a log file click on Log File and enter filename and path 5 To start shimming click on Start Shimming Observe the progress of the operation in the gradient window 6 To terminate the shimming process click the Stop Shimming button System Operation UM SW50407 05 64 Standard Procedures Perform Electrical Shimming Shim Gradients E E i x Set Method Gradients Log File Stark Shimming Stop Shimming Gz 0 4 Gzz 34 Gzzz 0 B3 Gzzzz 83 GH F 34 HH 0 20 Guxxx 1 0 61 Gzx H 6 46 GZHE 2 26 Gzxxx 1 82 Gy 4 34 Gyy
60. DAC output for each coil Stop Test Terminates current test Clear clears display for all coils The numbers on the right side of the display identify the coil numbers 1 to 40 To select a single coil Click on the box of the coil When a coil is selected the box changes from gray to white Quick Test Display Clicking Quick Test orders the system to perform a short test on all selected coils If all coils are selected the results of this test are displayed as shown in Figure 100 After test is completed a small dialog appeats asking if you want to save the test to file Click Yes to enter a name and path for the new file If saving is not needed click No Shim Test Display Set Reset File Exit al Coils Map Magnet MASH 40 e 3L 26 20 10 6 a Quick Test Accurate Test Read Clear MI Select All Unselect All Find era Stop Test BUT med Du ud 65232 port Open a Figure 101 Shim Test Coils Map Screen Find Zero System Operation UM SW50407 05 114 Maintenance and Diagnostics Diagnostics When on Find Zero is clicked the dialog box in Figure 102 appears This tool is for use only by Qualion NMR technicians I ShimBoxT est Figure 102 Shim Test Serial Number Dialog Box System Operation UM SW50407 05 115 Maintenance and Diagnostics Diagnostics Display Units This menu item permits to select either hexade
61. Digital and Frequency Domain NMR Analysis Running Local Machine File Archive Processing Mew Data Run Tools Hardware Help ao gt e load Save Print Start ato MS FERA Freq Shim Lock FA ppm Pts j 2000 1500 1000 500 500 1000 1500 2000 Jo RMS 955989 Shit 271 89 Figure 29 Frequency Domain Display with Phase Error Corrected Absorption PHASE CORRECTION Phase correction is performed by clicking on the Phase button in the NMR Analysis Main Window It may also be performed in ProcessNMR by making an appropriate entry in Automated Analysis on page 83 Clicking on the Phase button in the NMR Analysis Main Window displays the screen shown in Figure 30 Phase Correction Symmetric Order Phase ero Order Phase Tails Length 20 Step degrees 5 Feaks Definition Peak Thresh Count Total Angle 0 Direction Left Order Phase With Manual First Order Phase First Order Phase Pre Acq Delay sec 0 Total Angle p f Thresh 72 for Angle E Go Delta 200 E Create Pivot List Figure 30 Phase Correction Screen System Operation UM SW50407 05 51 System Operation Szgnal Processing Digital and Frequency Domain To define the desired peak go to Peaks Definition panel Enter the peak threshold value Peak Thresh specify the
62. E Pte D am Figure 49 Typical Example of Remote Monitoring System Operation UM SW50407 05 72 Standard Procedures Activate an Existing Connection 7 At the end of your session close the screen as you would with a local system then exit from pcAnywhere by closing the window clicking the X icon on the pcAnywhere menu This disconnects the phone line connection and shuts down the link Symantec pcAnywhere Figure 50 End Remote Control Session 8 To exit from pcAnywhere click the Exit icon the rightmost large icon and then click YES when the End Remote Session dialog box appears click the Exit icon the rightmost large icon and then click YES when the End Remote Session dialog box appeats PATEST Symantec pelmeheng Remote 1 Xi f iit Tek acters eh 2 Remote Cantal 13071 2 view Daa cun 005 Ferceae Feb 2 fm pars Xat 5x5 IT amp Feb E S F TR80 Oke 3 Zach T Hari Fha aste es wis Figure 51 Exit from pcAnywhere 9 At the end of your session close the screen as you would with a local system then exit from pcAnywhere by clicking the rightmost icon on the pcAnywhere menu as shown in Figure 50 This disconnects the phone line connection and shuts down the link System Operation UM S
63. I 1 Figure 79 Lock Parameters Data Entry Screen This screen lists several parameters for running the lock system K1 this is the setting of the proportional coefficient of the PID loop for controlling main transmitter frequency Does not apply to most lock parameters defaults to zero if not applicable K2 this is the setting of the integral coefficient of the PID loop for controlling main transmitter frequency Does not apply to most lock parameters defaults to zero if not applicable Error High this is the setting of the high limit for the error signal of the PID loop for controlling main transmitter frequency Error Low this 15 the setting of the low limit for the error signal of the PID loop for controlling main transmitter frequency Observe Lock Frequency Ratio this is the setting of the ratio between the lock frequency and the main transmitter frequency Freq Shift this the value of the increment by which the main transmitter frequency 1s changed Hop Phase this function sets the phase of the lock signal when it jumps from an increasing sweep to a decreasing sweep and vice versa during the search for resonant frequency of the reference sample Low Freq Limit this is the low end of the sweep range for the lock transmitter frequency High Freq Limit this 1s the high end of the sweep range for the lock transmitter frequency Step this is the magnitude of the ste
64. M SW50407 05 39 System Operation Software Software MODBUS RS455 TO SYSTEM REMOTE FIELDPOINT RS485 peg COMPUTER TO REMOTE COMPUTER VIA PCANYWHERE ETHERNET SHIM TEST DIAGNOSTIC SOFTWARE CLIENT PROCESSNMR SOFTWARE SYSTEM SOFTWARE CLIENT SERVER NMRANALY SIS SOFTWARE GLIENT HEATER PROCESSNMR DIAGNOSTIC DIAGNOSTIC SOFTWARE SOFTWARE CLIENT Figure 15 General Software Structure The rack mounted system PC mounted inside the analyzer cabinet communicates with the remote computer through an Ethernet connection or dedicated telephone line The remote PC on the system communicates with a DCS through a Modbus connection as standard and through an RS485 National Instruments Fieldpoint module as an option Software running on the system computer in Windows 2000 is structured as a client server configuration The clients are ProcessNMR NMR Analysis Heater Diagnostics NMR Diagnostics and Shim Test PROCESS NMR SOFTWARE The ProcessNMR software is the analyzer software package designed for use with online applications in an industrial process plant environment The tools available with ProcessNMR are explained in detail later in this chapter NMR ANALYSIS SOFTWARE Another application package called NMR Analysis is also supplied with most installations NMR Analysis is used primarily for setting up and testing the system and for performing laboratory and or grab sample types of
65. Main Transmitter Frequency xample xampl xampl xampl xampl xampl t Fr Eri 5 00 000005 ON amp RMS Value of FID Frequency Shift Half Height Peak Width Ratio of Integrals Integral Count Table of Contents 113 113 114 114 116 116 117 118 118 119 119 121 121 122 122 123 123 123 125 125 126 126 126 127 127 127 128 128 128 129 129 129 130 MECEO lide pct s INDEX ER System Operation UM SW50407 05 Preface Preface N CAUTION The normal operating frequency of the NMR Analyzer 15 58 0 0 5 MHz for H This implies that the NMR Analyzer 1s susceptible to signals operating at that frequency Therefore the NMR Analyzer should not be installed in an area with an active transmitter at the operating frequency The magnet construction however is such that the core frequency can be shifted 100 kHz if required to avoid interference from the transmitter If a site 15 subject to broadband or multiple frequency interference that cannot be avoided by a frequency shift additional mitigation measures are required This may include the use o
66. NTED COMPUTER UNIT Sal SHS COR TROL SUPPLY AND I UNIT RE LITT PNEUMATIC LINES TO PROCESS SAMPLE SELECTOR VALVES IN SAMPLE SWITCHING SYSTEM Figure 4 System Block Diagram Accessory Systems One Purge Unit that supplies air purging to the enclosure For Process Analyzer only Three Air Conditioning For Process Analyzer Units Lab Analyzer has One A C two on the Hlectronics side and one on the Magnet side Functional Operation System Operation UM SW50407 05 15 System Overview Pulse Sequences A Lab Analyzer uses a tube for sampling and can not be attached to a sample system At the process analyzer a sample is drawn from the process line or sample switching system through the input manifold to the sample probe line within the magnet through the stop flow valve and then back to the process or the sample switching system Flow is stopped while an analysis is performed and resumed when the analysis is completed The sampling system operates on a repetitive cycle of flow purging the probe then flowing the sample to the probe stop flow sample analysis and flow purging the probe The sample probe mounted inside the magnet contains the sample flow tube and a sealed reference capsule filled with lithtum chloride A small radio frequency RF coil is wound around the outside of the sample flow tube and another RF coil is wound around the reference capsule Each coil i
67. OLS The environmental controls for the analyzer enclosure consist primarily of temperature controls as described in this section Purity of the atmosphere within the cabinet is a function of the air supply Temperature Controls As mentioned previously temperature control of the magnet and its environment are very important for good performance of the analyzer system Therefore separate controls and separate air conditioners are provided for the two cabinet enclosures as described below Magnet Cabinet There are 3 air conditioners for both compartments These solid state air conditioners provide cooling as well as heat The air conditioners run continuously temperature is controlled by an RTD mounted on the wall of the compartment which is used as the measurement input to a PID temperature indicating controller mounted in the electronics rack in the electronics side of the enclosure The Lab Analyzer is controlling the temperature inside the Magnet enclosure only with a PID loop based on the heater card It is not displayed at the Heater Diagnostic tool The temperature inside the Lab Analyzer is measured with an external PID thermocouple The Lab analyzer has only one A C unit mounted on the left side wall System Operation UM SW50407 05 31 System Overview Major Hardware Components Electronics Cabinet There is one air conditioner on the electronics side of the enclosure due the heat generated by the electronics The cont
68. Operation SW50407 02 1 Label Function 0 Remove DC Argument 1 Argument 2 Argument 3 Argument 4 Argument 5 A gument 6 TiZeroFill 2 Mi Aute Phase 4 Remove DC 5 Integral Ratio Integrals Remove DC Integrals count F Zero Fill FFT 5 Autc Phase 5 Integral Ratio 5 Integrals Integrals count 130 Glossary Diagnostics 6 Glossary Absorption Conversion of a time varying signal to a frequency domain signal by means of an FFT produces two spectra real and imaginary The real transform is called the absorption mode the imaginary transform is called the dispersion mode Since it is conventional to display NMR spectra in absorption mode the real transform 15 used for plotting results of the analysis In practice however both absorption and dispersion spectra are generated because the time at which the FFT is applied may not be in phase with the start of the time domain signal Phase correction therefore is used as a means of converting the spectra to pure dispersion and pure absorption Analog to digital converter Ait purge The accessory system that replaces the air within the NMR enclosure with clean instrument air and also maintains a safe positive air pressure within the enclosure at all times Baseline The post processing function that adjusts the d
69. Operator assisted manual dial Disconnect a call if idle for more than mins Cancel the call if not connected within 50 secs Data Connection Preferences speed 115200 Data Protocol Standard EC Compressor Enabled Flow contra Hardveare Figure 43 System Operation UM SW50407 05 68 Standard Procedures Set Up a New System Connection 5 Click the New item button marked red in figure3 a new caller session will be open 6 Fill the correct login name foxnmr and password yael apply and click O K a new item will be under the Name column Host Proportion Modem X symantec wr Comment Protect lien faxnmr yael Figure 44 7 Close all sessions and return to the main pcAnywhere application window see figure 4 8 Right click the modem again and choose the Stat Host option and check that there is a PC icon on the bottom of the screen 9 Point this icon with the mouse pointer indication should be Symantec pcAnywhere waiting if a PC icon was already displayed right click it and choose the cancel host option wait fro a few second till the icon will disappear then start this process from begging with a new Host name System Operation UM SW50407 05 69 Standard Procedures 2 Symantec
70. System Overview Major Hardware Components density in a small compact package Because the flux must be extremely uniform over the entire air gap construction of the magnet is complex The magnet is fabricated from several segments bonded together to form the basic assembly In addition to the bonded segments of magnetic material each magnet also contains 40 coils of wire arranged about a Shimming Unit mounted in the center of the magnet between the pole pieces These coils are used as small electromagnets the strength and polarity of which can be controlled by varying the current through them so as to improve uniformity of the overall field of the magnet assembly This adjustment process called shimming is analogous to the use of shims or spacers to make fine adjustments to the positions of physical objects A manual shimming procedure performed at initial installation mechanically aligns the faces of the magnet pole pieces to an optimum position This operation is performed by adjusting 8 pairs of adjusting screws at the outside ends of the magnet housing This operation is required only after shipping or relocating the magnet which might subject it to rough movement Prior to assembly in the manufacturing plant each magnet segment is cured at a high temperature to stabilize its field strength In the fabrication process the absolute field strength of each individual seoment of the magnet is measured A computer analysis of this data then
71. UM SW50407 02 128 Example 3 Frequency Shift This example shows how a window is configured to plot main transmitter frequency shift Program Of Frequency Shift Label Function D Remowe DE Tl Zero Fill 15384 FFT 3 Phase 0 9 Left 1 0 05 200 0 Freq Shift Use First Baseline Use First Phase Figure 126 Configuration of Plot of Frequency Shift Example 4 Half Height Peak Width This example shows how a window 15 configured to plot the peak width at half height Program Of 1 200 Height x kael O Remove iY Argument 6 1 Zero Fill 16384 2 FFT 3 Auto Phase 0 9 Left 1 0 05 200 0 m Remove DC 5 Peak Width Use First Baseline Use First Phase 90 right Figure 127 Configuration of Plot of Peak Width Half Height Example 5 Ratio of Integrals This example shows how a window is configured to plot a ratio of integrals DIAGNOSTIC File Program Of Task 1 PERE ee Set Remove DC Zero Fill 16384 Use First Baseline Use First Phase Auto Phase 0 9 Left 4 Remove DC 5 Integral Ratio 600 ntegral 2 To POINTS Figure 128 Configuration of Plot of Integrals Ratio System Operation UM SW50407 02 129 Example 6 Integral Count This example shows how a window is configured to plot an integral count value NMR DIAGNOSTIC Program Of Task DIAGNOSTIC System
72. W50407 05 73 Windows and Dialog Boxes Process NMR Application 4 Windows and Dialog Boxes This chapter is intended to be a quick reference to all major windows and dialog boxes Each screen 15 accompanied by a brief description of the window and its menu items Where needed cross references to more detailed descriptions of the tools and theory of operation are included ProcessNMR Application ProcessNMR MPSS Version n 0 is the software for running the process online continuously in a production environment The term MPSS means Multi Processing Single Schedule which refers to use of a single program sequence to control multiple functions and multiple samples Since most installations are also supplied with NNMRnalysis the software for off line setup and analysis descriptions of NNMRnalysis windows and dialog boxes are included after ProcessNMR descriptions PROCESSNMR MAIN WINDOW ProcessNMR Running On Local Machine Data Tools Run Window Help LN Be ERG H 2 New Event T Modbus DTS Start stop Sched Alarm Log Log Client Calc Help E x FR autc aid Pred 23 sched H Grid Gf Results 10 Exsemmate valve ses Figure 52 ProcessNMR MPSS Multi Processing Single Schedule Version 1 0 Main Window System Operation UM SW50407 05 74 Windows and Dialog Boxes ProcessNMR Application NEW APPLICATION E ProcesshMA Running On Local Machine
73. analyses The tools available with NMR Analysis are explained in detail later in this chapter DIAGNOSTIC SOFTWARE Three applications of diagnostic software are included with the system Heater Diagnostics System Operation UM SW50407 05 40 System Operation Main Transmitter Pulse Shim Test box NMR Diagnostics Each of these client applications is described in detail in Chapter 5 Maintenance and Diagnostics SHIMMING SOFTWARE Software for automatically determining optimum shim settings for the 40 pairs of shim coils is included with each system The functions performed by this software are described in detail later in this chapter Main Transmitter Pulse Characteristics The main transmit pulse is a broadband signal containing all frequencies within the spectral range of interest to the analyzer All such frequencies must be present in the pulse so that all nuclei in the sample will be excited by the pulse Frequency The main transmit frequency is 58 xx MHz 2000 Hz This is the resonant frequency of H in a magnetic field with a strength of 1 35 tesla Spectral Width The spectral width of the transmit pulse is typically 4000 Hz which 15 set by adjusting the ADC parameters The 4000 Hz range is selected because it encompasses the entire spectral range of resonant frequencies needed for analyzing samples Duration The duration and bandwidth of the FID are determined by the parameters entered for the
74. ary transform is called the dispersion mode Since it is conventional to display NMR spectra in absorption mode the real transform 15 used for plotting results of the analysis In practice however both absorption and dispersion spectra are generated because the time at which the FFT is applied may not be in phase with the start of the time domain signal Phase correction therefore is used as a means of converting the spectra to pure dispersion and pure absorption Electrical The process by which the currents supplied to each pair of shim coils are shimming automatically adjusted to achieve optimum uniformity of the magnetic field for a particular type of sample being analyzed EPCU An acronym for Electrical Power Control Unit used in the Bebco air purging system descriptions An acronym for Electrical Testing Laboratory a certifying agency for electrical safety Event table A sequence of operations stored in a table file performed by the NMR analyzer for control of the timing and functions performed by the main transmitter receiver and associated items Fast Fourier A standard mathematical technique for converting time domain data into a Transform frequency spectrum FID Acronym for Free Induction Decay the time domain representation of the relaxation of an NMR magnetization vector as it returns to its normal state after being deflected from its axis by a main transmitter pulse The manufacturer s tradename for hardware that
75. ata to fit a curve related to a correction selected section of a baseline Calibration model A mathematical model that correlates measured NMR spectral information with one or more physical or chemical properties of a process sample Sometimes called a prediction model CENELEC The Canadian safety testing and certification laboratory Chemical shift The difference in frequency between the NMR resonant peak of a known reference sample and the NMR resonant peak of a component in a sample being analyzed CPMG An acronym for the Carr Purcell Meiboom Gill experiment an advanced technique for measuring nuclear spin echoes that is shown on one of the NMR Analysis ProcessNMR menus but not currently used in operation of the analyzer Distributed control system such as an I A Series system that performs advanced process control functions DCS DDS Digital Data Synthesizer Delphian The manufacturer of the LEL Lower Explosive Limit monitoring system currently supplies with the NMR analyzer Dewar probe A sample probe consisting of an inner tube through which the process sample flows encased by an outer tube which is thermally insulated from the inner tube by vacuum as common vacuum bottle Conversion of a time varying signal to a frequency domain signal by means of an System Operation UM SW50407 05 131 FFT produces two spectra real and imaginary The real transform is called the absorption mode the imagin
76. ation Zero order phase correction A phase correction at the base or zero level Zoom A change in the scale of a display which may be in one or many dimensions Zoom in magnifies the display zoom out decreases magnification This command resets all zoom settings to a magnification ratio 1 System Operation UM SW50407 02 134 Index Diagnostics Index A ADC NMR Analysis 81 ProcessNMR 65 Analog Digital Modem Inputs Outputs Set Up 57 Auto Analysis NMR Analysis 87 ProcessNMR 71 Average NMR Analysis 81 Process NMR 64 Axis Units 76 B Baseline Command 94 Calibration Models Set Up New 56 Using 29 Clear 88 D DCS 68 Connecting to a 57 Diagnostics 98 Heater Diagnostics 98 NMR Diagnostics 109 E Event Table NMR Analysis 79 ProcessNMR 63 F FFT Fast Fournier Transform 90 Frequency 81 G Glossary 121 Grids NMR Analysis 87 ProcessNMR 75 H Hardware Components Major 15 Communication Links 20 Computer 20 Enclosure 23 Enclosure Environmental Controls 24 Heater Control Unit 16 Magnet 15 Power and Communications Connections 23 Power Supply and I O Unit 20 Probe Reference 16 Probe Sample 16 Shim Control Unit 18 Switching Control Unit 21 Heater Diagnostics Adding Windows 99 Magnet Menu 100 Main Menu 99 PID 101 Pop Up Labels 102 Start Save 101 Help 70 78 87 I IFFT Inverse Fast Fournier Transform 92 Imaginary Portion 88 System Operation UM SW50407 05 135 L Load Command 78 Lock
77. ation of the Lock transmitter and receiver Initialize loads a set of parameters Start activates the system and Stop interrupts operation of the pulse transmitter receiver Start Reading activates the data acquisition functions of the lock system and Stop Reading interrupts operation The Frequency display shows the current frequency being transmitted and received by the lock transmitter receiver The Status display shows the current operating state of the Lock system such as Searching Fine Lock 1 Fine Lock 2 Fine Lock 3 Fine Lock 4 and Fine Lock 5 The differences between Fine Lock 1 2 3 4 and 5 are the precision of the frequency lock Fine Lock 5 is the most precise and stable lock frequency Loop Parameters Clicking this item displays this screen shown in Figure 76 which is a dialog box for setting parameters for the PID loop that controls the Lock system 5 Lock Parameters Clicking on Lock Parameters displays the screen shown in Figure 76 System Operation UM SW50407 05 95 Windows and Dialog Boxes Automated Analysis 14 Lock Parameters B E xj E Error High Error Low ESO 2 5721 1 08 gaggi 100 Freq shift 00 Hop phase 0 2 2 246 07 High Freq 2 265 07 un Step 100 E 5000 Threshold 50 ASSI Threshold p Tx Gain 120 40 n Samples For Fine n Samples For Pre zz of ni Cancel QUALIOH Ltd Copyright 2007
78. automatically compensating for any minor variations in magnet field strength and temperature The lock system continuously detects the resonant frequency of the nuclei in a known sample fluid lithtum System Operation UM SW50407 05 19 System Overview Szgnal Processing Frequency Domain chloride and the sets the frequency of the main transmitter to be a fixed ratio to this reference Since the reference fluid capsule is located inside the main probe it is subjected to the same magnetic field and temperature as the main transmitter receiver Therefore a change in one affects the other The lock system functions generally in the same way as the main transmitter system see Figure 6 except that the basic transmitter frequency is approximately 22 MHz the resonant frequency of lithium in a magnetic field of 1 35 tesla PROGRAMMED SET POINT FROM LOCK DOS UNIT TR Sw TX RX 36 OSC MHz MULTADIVIDEY LOCK TX LO SPLITASHIFT 12 MHz MHz 22 MHz LPF jur CO 22 MHz lt a Figure 6 Block Diagram of Lock Signal Processing Functions The lock system functions as follows The frequency of the lock transmitter is swept over a range of about 1 MHz 22 23 MHz as it searches for the resonant frequency of lithium When it first detects a resonant response significant increase in signal level as it increases frequency during the search it stores this value and then jumps to a higher frequency and approaches resonance f
79. bles the system to discriminate between signals Detection Generated by nuclei that are precessing faster than or slower than the reference positive and negative frequencies effectively increasing the signal to noise ratio Signal Averaging Signal averaging computes the average either discrete or running of a series of signals for the purpose of minimizing random noise Window Function The window function multiplies a time domain signal by an exponentially decaying signal for the purpose of smoothing of the signal By varying the coefficients of the equation you can control the decay rate of the signal Applying this function has the undesirable effect of broadening a peak in the frequency domain Remove DC This function shifts the time domain signal by the amount of the DC Offset offset centering the signal around zero and reducing noise ADC Parameters The software as explained in Chapter 3 allows you to set parameters for the analog to digital converter ADC You can select the total number of samples the sampling rate and the bandwidth of the conversion Zero Fill The zero fill function permits you to increase the effective digital resolution of the system by increasing the total number of samples without increasing noise merely by adding samples with zero values to those produced by the ADC Lock System The purpose of the lock system is to provide control of the frequency of the main transmitter pulse
80. cade Display shows 0000 the far left digit is flashing Press the key Sequence on left side To enter Cade 0001 The preset M cade Confirm the code Input pressing Enter Button The main menu is now active The first sub menu Language appears an the display The default of ex works is German To alert the language press Enter euton Cin the left appears the ward Deutsch Press the un button to change the language The language English is now selected Press the Enter Euitan to confirm the change Category Structure appears Press the Erncer Burton to configure the EEX p system structure System Operation UM SW50407 05 Cant Flow E 4 c 4 H 2 c ce Bl gt r3 mm The present state is digital salenaid valve Change the state by pressing the UWo Key The new state is now Proportional Solenoid Valve Confirm by pressing the Enter Button This item iz the operational mode Continues flow or leakage compensation The ex works is already leakage compensation therefore skip this item by pressing Us Key The structure menu is now finished The main menu continues automatically vith the pre selected parameters Start the parameters category by pressing the Enter Key The first menu Item Purging volume appears Press the Enter Key to enter the desired volume Expecting a pre set purging volume of 500 L the input is as
81. cimal or decimal units for the display Shim Test Display Seb Reset File Exit Decimal Figure 103 Shim Test Display Units Selector Set Clicking on Set displays a menu of options Selecting an option displays an associated dialog box in which is possible enter data for that item The menu options ate Quick Test Error The associated dialog box permits entering a value for maximum error in the quick test Accurate Test Error The associated dialog box permits entering a value for maximum error in the accurate test either as an absolute value or as a percentage of full scale Address Test Error The associated dialog box permits entering a value for maximum error in the address test Slope The associated dialog box permits entering a value for maximum slope the tangent of the angle between two points Delay The associated dialog box permits entering a value for maximum time delay in milliseconds for performing the selected test Shim Test Display Set Reset File Exit ee Quick test error 1500 Accurate Test Error Minimum 16 ERROR ON THE LOWER BYTE 0 255 Address test error 3000 Percent 10 ERROR ON THE Slope 0 98 HIGHEH BYTE Delay 5 msec EIK Figure 104 Shim Test Accurate Test Error Display Selector System Operation UM SW50407 05 116 Maintenance and Diagnostics Diagnostics Accurate Test The accurate test consists of testing eac
82. connects the NMR analyzer to external systems Indication that lock has been achieved The number indicates the level of precision of the lock the higher the number the greater the precision Free induction The time domain representation of the received signal as the molecules relax and delay return to normal tip angles Frequency domain A display of data in which the x axis is a frequency spectrum rather than a time scale Frequency lock The action of determining the resonant frequency of a reference fluid achieved by sweeping a frequency across a spectrum and measuring the system response to a pulse of that frequency When resonance is detected the frequency is locked The system then sets the main transmitter frequency in a preset ratio to this reference lock frequency The post processing function of totalizing the measurement data over a selected range of frequencies The software program supplied with the analyzer for setting up the system and also for performing laboratory types of analyses An instrument for detecting whether an atmosphere contains explosive gases that exceed a specified Lower Explosive Limit LEL System Operation UM SW50407 02 132 The current state of the lock system searching or in Fine Lock 1 Fine Lock 2 ot Fine Lock 3 fluid lithium chloride vector magnetic field of a molecule command negative values excites the molecules in the sample maximum uniformity of the fi
83. consists of neutrons and protons the number of protons in the nucleus determines its atomic number Hydrogen for example which has one proton and an atomic number 4 ce 2 ec of 1 15 commonly referred to as or simply proton SPIN Some protons exhibit a property called spin Spin can be thought of as a magnetic moment vector that makes the proton behave like a tiny magnet When you place the proton in a strong static magnetic field the spin vector of the proton aligns itself with the magnetic field as a magnet would ENERGY STATES AND TRANSITIONS The poles of the proton can be aligned in either of two states a low energy state N S N S or a high energy state N N S S If a proton in the low energy state absorbs a photon it absorbs energy and jumps to the high energy state and vice versa The energy E of the photon which must equal the enetgy difference between the two states is related to a frequency called the resonance or spin frequency and Planck s constant h E hv Therefore when the energy of the photon matches the energy difference between the low energy and high energy states absorption of energy occur Planck s constant is a universal factor that defines the relation between the frequency of radiation of a process within a molecule and the quanta of energy emitted from the molecule The quanta of energy emitted are equal to the radiation frequency multiplied by Planck s constant
84. controlling the currents supplied to 50 pairs of shim coils within the magnet Electronics Compartment Temperature Control System controlling solid state air conditioners for both compartments consisting temperature controller and RTD as sensor Rack mounted Computer for controlling the various elements of the system and communicating information to other systems Switching Control Unit for applying and detecting RF signals on the RF coil in the sample line within the magnet and on the RF coil on the reference probe Main Power Supply tp rpovide power to all components in the system and I O Unit and handling signal inputs and outputs I O For Process Analyzer only System Operation UM SW50407 05 14 System Overview Pulse Sequences AIR f SOURCE AIR CONDITIONER AIR CONDITIONER COMPARTMENT PURGE UNIT TEMPERATURE CONTROL UNIT SAMPLE PROBE LINE MAGNET ENVELOPE TEMP VELOPE LITHIUM CHLORIDE REF PROBE MAIN PROBE MULTIPLE STRIP HEATERS BONDED ENVELOPE MULTIPLE STRIP HEATERS BONDED TO MAGNET HEATER CONTROL UNIT SUPPLY CONTROL BOARD MECHANICAL SHIM ADJUSTING SCREWS 8 EACH POWER DISTRIBUTION SIDE UNIT DIVIDED INTO SEVERAL SUBUNITS PROCESS SAMPLE LINE AIR SOURC nm d mih CONDITIONERS ELECTRONICS COMPARTMENT BOMM MOU
85. d Analysis table varies with each application is determined for specific installations by Qualion NMR application engineers System Operation UM SW50407 05 61 Standard Procedures Start the Analyzer 3 Standard Procedures This chapter is a quick reference of standardized procedures for executing common tasks Start the Analyzer The following section contains standard procedures for starting the analyzer under various conditions INITIAL STARTUP Initial startup is always performed by Qualion NMR technicians or only a trained person that was specialy qualified for that purpose therefore it is not included in this manual STARTUP AFTER SHORT SHUTDOWN MAGNET WARM The system should start automatically when power is restored after a power outage If the outage is 2 hours or less the magnet should still be warm Under these conditions the restart procedure is as follows 1 Verify that sample is flowing properly to the analyzer 2 Start Heater Diagnostics 3 Check magnet temperature If the magnet temperature is approximately 41 C proceed If lower than 41 C let the system warm up longer until the temperature reaches the target 4 When the magnet is up to temperature and the system is running check the pulse width at 1 10 height and half height If widths are within spec proceed If not reload the most recent shim set file and re check the pulse widths If OK proceed If not you will have to re shim the magnet
86. e Honzntaly Tile Vericaly Add windows In the Chart Channels box click on Chart Channels to display the Select Chart Channels dialog box shown on the right side Click the appropriate check box to select the variable s to be displayed Then click on Set to apply your selection and return to the main menu Note more than one variable can be displayed on each window Click on Windows on the main menu and then use Tile Horizontally and or Tile Vertically to select the type of display desired To start collecting data click on Start on the main menu To stop collecting data click on Stop To clear all windows of data click Clear To exit from the application click on the X at the top right corner of the screen display System Operation UM SW50407 05 109 Maintenance and Diagnostics Diagnostics As the system starts to collect data and plot the results on the windows the y axis scale automatically changes to accommodate the data always zooming the scale to the maximum extent possible and to still show all data points Use the zoom tools to expand the scale beyond this point Doing so however may cause some data points to lie outside the range of the display The x axis scale also changes automatically to ensure that all data points are always displayed Itis also possible to change the time scale range further by clicking the Time Scale Rang menu item and then entering a new value To plot data that was previously stored in a
87. e found a satisfactory value you can either exit from the screen or continue with making a first order correction Lastly enter the Total Angle in Automated Analysis on page 83 System Operation UM SW50407 05 22 System Operation Signal Processing Digital and Frequency Domain BASELINE CORRECTION Figure 31 shows a typical FFT spectral display that contains a baseline error Figure 32 shows the same display after applying a baseline correction Figure 31 Spectrum Display with Baseline Error Figure 32 Spectrum Display with Baseline Error Corrected System Operation UM SW50407 05 53 System Operation Signal Processing Digital and Frequency Domain The dialog box for performing a baseline correction function is illustrated in Figure 33 To display this dialog box click on the Baseline button in the NMR Analysis window You can perform the same function in ProcessNMR by making an appropriate entry in the Automated Analysis on page 83 i Baseline correction Baseline Parameter Mean Range 256 Mum Std Peak 2 5 Method Poly Degree Find Baseline Corect Figure 33 Baseline Correction Dialog Box The baseline correction is accomplished by applying one of a number of curve fitting methods to the spectral data such as linear or a polynomial of various degrees To perform this function enter parameters in the dialog box To determine the parameters to be entered do the following e
88. e the current shim set to a file and include the date as part of the filename Shutting Down the Analyzer Unless you plan to open the cabinet doors Qualion NMR recommends that you leave the air purge system ON during shutdown If you do plan to open the cabinet doors Switch off the purge system as you shut down following the procedures described below NORMAL ORDERLY SHUTDOWN N CAUTION When you shut down the analyzer be aware that no sample flow can occur while the system is out of service If non flowing sample fluids can cause problems in the probe be sure to purge the probe before shutting down the analyzer 1 Start pcAnywhere from the Start menu or by clicking on the pcANywhere icon 2 Click on Remote Control and then click on the icon for your analyzer 3 When the analyzer screen appears click on Start and then select Shutdown This terminates the application 4 In pcAnywhere click on Exit icon This closes pcAnywhere If you plan to leave the air purge running this terminates the procedure If you plan to open the cabinet howevet continue with the next step 5 Switch off the purge key and shut off system powet System Operation UM SW50407 05 63 Standard Procedures Set Up an Analysis Set Up an Analysis Since setting a new analysis or repeating a previous analysis requires input from Qualion NMR Application Engineering contact Qualion NMR for assistance Perform Mechanical Shimming WARNING
89. ed pulse The reason for using an intermediate frequency and an audio frequency is to drop the frequency to a range where the signal can be easily processed and manipulated System Operation UM SW50407 05 29 System Overview Major Hardware Components The two audio signals for Channels I and are then sent to the A D converter in the Rack Mounted Computer Unit In the A D process time domain signal processing methods such as signal averaging window smoothing spectral width bandwidth and zero fill are used to improve the quality of the incoming signals After conversion to digital form the computer software convetts the signals to the frequency domain and applies additional digital signal processing techniques to the data Note that in the system described above the transmitter frequency is present only during transmission of the main pulse Therefore no interference with the NMR signal generated by the main probe can occur ENCLOSURE The NMR Process analyzer is housed in a three door NEMA 4 IP 56 enclosure Floor stands approximately 200 mm high are welded to the body to make it a free standing enclosure The enclosure is fabricated from stainless steel with all seams continuously welded and ground smooth The three enclosure doors are hinged left or right for unobstructed access to the system components Continuous hinges and hinge pins are used A rolled lip formed around the four sides of the doors increases their st
90. een shows the measured magnet temperature the output current to the magnet strip heaters the magnet envelope temperature and the output current to the strip heaters on the magnet envelope The boxes in the center row contain the current values in arbitrary numerical units between 8192 and 8192 of magnet sense offset magnet heater current envelope sense offset and envelope heater current The present values 15 displayed in C in the bottom row of windows Note that both x and y axis scales change automatically as data points are added The vertical scale automatically expands or contracts to maximize the display of y axis data The x axis time scale automatically contracts so as always to display all data points from the beginning of the test Figure 91 Typical Heater Diagnostics Screen with Four Windows Main Menu System Operation UM SW50407 05 108 Maintenance and Diagnostics Diagnostics Figure 89 shows the main menu for heater diagnostics Each menu item is explained in detail in this section Heater Diagnostic File View Run Config Lis 45 NEMA Temp 5 Temp ES Temp LP35 Temp LP45 Figure 92 Heater Diagnostics Displayed Menu Adding Windows When the Heater Diagnostics screen first appears the main window is empty no sub windows Then it is possible to create up to 4 sub windows by clicking on Windows and selecting Add Windows as shown 1n Figure 90 MW Imdowis Til
91. eld LONE transmitting serial data Nuclear Magnetic Resonance a physical chemical property of a element that indicates the response of its nuclei to high frequency pulses when the molecule is placed in a strong magnetic field Optimization Supervisory application software designed to achieve optimum control of Mahalanobis distance The act of moving a display continuously from one point to another without changing any dimensions of the display telephone line or other data link accordance with a stored program The maximum value for accepting the calculated output of a prediction model Any value greater than this limit is considered an outlier Prediction model A mathematical model that predicts output values correlated to a set of input variables ProcessNMR The application software for performing NMR analyses on online process samples The series of functions performed in the process of generating a pulse Quadrature A data acquisition technique for determining the phase characteristics of a time domain detection NMR signal Without quadrature detection false frequencies appear in the FFT frequency display Also an aid in eliminating noise System Operation UM SW50407 02 133 Removing DC A post processing function that removes a zero offset from either a time domain or a offset frequency domain display An abbreviation for radio frequency SafeCAL A safety monitoring function of the Delphian LEL Monitoring system
92. em software is called Heater Diagnostics The shroud is mounted on a base plate equipped with rubber feet that reduce the transfer of any vibration from the external frame to the probe coil inside the magnet SAMPLE PROBE The sample probe is mounted inside the permanent magnet in the air gap between the magnet poles The probe itself is a Dewar vacuum insulated tube that is inserted in a hole through the shimming unit in the center of the gap between pole pieces of the magnet The inside diameter of the sample tube for D MASH Model probe is 7 mm For laboratory applications where a sample tube filled with a sample is manually inserted into the probe care must be exercised to ensure that the sample tube is completely filled with the sample fluid If an air gap is present in the sample tube results can become distorted because of sample interaction between liquid and vapor phases System Operation UM SW50407 05 22 System Overview Major Hardware Components The constant magnetic field of the permanent magnet 1s perpendicular to the axis of the transmitter coil in the sample probe Since the pulsed ac field introduced by the coil around the sample tube coincides with the vertical axis of the probe the pulsed magnetic field is therefore perpendicular to the constant magnet field of the permanent magnet REFERENCE PROBE A second sensor mounted on a sealed capsule beside the main sensor in the sample probe inside the permanent magnet
93. emperature Controls Electronics Cabinet 24 Magnet Cabinet 24 W Window Command 96 Windows and Dialog Boxes 61 NNMRnalysis Main Window 76 ProcessNMR Main Window 61 Z Zero 89 Zoom 87 System Operation UM SW50407 02 137 Qualion NMR and I A Series are registered trademarks of Qualion NMR Systems Inc 33 Commercial Street Qualion NMR is a trademark of Qualion NMR plc Qualion NMR MA 02035 2099 All other brand names may be trademarks of their respective companies United States of America www Qualion NMR com Inside U S 1 866 PHON IPS 1 866 746 6477 Copyright 2002 Qualion NMR Systems Inc Outside U S 1 508 549 2424 All rights reserved or contact your local Qualion NMR representative 0902 Printed in U S A Facsimile 1 508 549 4999 System Operation UM SW50407 02 138
94. er Pulse ADC Parameters E X TADC Parameters D File ES Humber of Samples gt 2048 Humber of Echoes gt Sampling Rate Sampling Rate gt Band Width varied i Band Width QUALIOH Ltd Copyright 2007 Figure 17 Setting ADC Parameters Enter the total number of data samples points desired in the box at the top of the screen A value 15 either 4000 or 8000 1s typically used Enter a 1 in the Number of Echoes box this function not used Then select a data sampling rate which 15 typically set at 4346 Hz combination of a sampling rate of 4346 Hz and a total number of samples of 4000 yields a total acquisition time of approximately 1000 milliseconds Similarly setting the number of samples to 8000 yields acquisition time of approximately 2000 milliseconds To prevent aliasing the sampling rate must be at least twice the highest data frequency to be captured the so called Nyquist frequency After you select a sampling rate of 4346 Hz the bandwidth you select in the lower box should not be greater than 2000 Hz Since 2000 Hz 15 greater than the spectral range of the data to be gathered 750 Hz 2000 1s an acceptable value Entering these values of parameters for the ADC means that the total acquisition time is approximately 1000 milliseconds the digital resolution is approximately 0 14 Hz and the pulse has a spectral bandwidth of 2000 Hz On initial startup of the system widen the ba
95. eration UM SW50407 05 17 System Overview Szgnal Processing Lime Domain Purge Control For the Process Analyzer Only The atmosphere within enclosure is maintained at a safe positive pressure relative to environment by a Purge Control Unit mounted externally to the unit The purge unit supplies instrument air to the cabinets Operation of the Purge Unit is described in more detail beginning on page 25 of this chapter Signal Processing Time Domain N WARNING Actions described in the following section should be performed only by propetly trained personnel Extensive signal processing in the time domain 1s required to produce a meaningful NMR pulse signal that can be detected converted to equivalent quadrature analog audio signals Channels I and Q and then converted to digital form for input to the digital signal processing system in the computet Figure 5 shows a block diagram of the functions performed in the analog portion of the system to prepare the data for input to the Rack Mounted PC SET POINT FOR MAIN TX FREQUENCY FROM LOCK STEM 1 MAIN OOS UNIT TX RX ES TR Sw MHz MULT DIVIDE MAIN TX LO SPLITASHIFT 40 MHz 58MHz 9 MHz FF 58MHz lt 58MHz Figure 5 Block Diagram of Main Signal Processing Functions The system operates as follows A crystal oscillator outputs a 36 MHz signal which is sent to the DDS card The DDS unit multiplies divides and or phase shifts
96. es over 80 C a high temperature cutout switch is mounted on the magnet to disconnect power to the system if the temperature exceeds the limit Similarly low temperatures can also damage the magnet N WARNING Care must be exercised to ensure that magnet temperature does not fall below 4 C at any time even during shipment and storage Low temperatures can permanently damage the magnet Magnet envelope shroud temperature also a critical control item in NMR analysis 1s maintained at 40 a value slightly lower than the magnet temperature Shroud temperature is measured by four thermistors and is also controlled by the Heater Control Unit and associated strip heaters in the same manner as magnet temperature On a Process Analyzer both Compartment temperatures are controlled at 24 the Lab Does Analyzer Does not contains a temperature controller for the internal enviroment This temperature is sensed by an RTD mounted on the wall of the compartment The temperature signal provides the measurement input to an indicating PID controller mounted on the interior wall of the Magnet Compartment Cabinet which provides a controlled output to five 4W electric heaters Air conditioning units mounted outside on top of the compartment runs continuously cooling the re circulated air inside the compartment Since the air conditioner continuously cools the air within the compartment to maintain a temperature of approximately 24 C System Op
97. es in as many windows that fit can fit on the screen Although each window can display multiple variables the practical limit is two variables per window the first plotted as a solid line and the second as a dotted line It is possible to save a configuration and recall it at a later time It is also possible to display a previously saved set of curves System Operation UM SW50407 05 118 Maintenance and Diagnostics Diagnostics NMR DIAGNOSTIC File Stat Stop Windows Ignore Errors Clear Tile Heb y Py MA Nu m um m d d dl Lal H mi TNT INT ada Ji P Yf LabNMR 1 0 Running On DIAGNOSTIC Figure 107 Typical Multi Window NMRDiagnostic Screen Main Menu The main menu for NMR Diagnostics is shown in Figure 108 Each menu option is described later in this section NMR DIAGNOSTIC Fie NewTask Stat Stop Windows Ignore Errors Clear Title Help Figure 108 NMRDiagnostics Main Menu Using NMR Diagnostics The general procedure for using NMR Diagnostics 1s as follows 1 From the File menu load a previously saved setup file configuration file If there is no previously saved configuration file define a new one by clicking on the New Task command 2 After displaying a new window by clicking on New Task right click on the new window to display the menu of setup options for that window Each option i
98. et Region Figure 40 TypicalAutomated Analysis Table In the table shown the first operation is to remove any dc offset in the FID measurement signal The next operation increases the digital resolution of the data by adding enough zero data points to total 8192 points The next step performs a Fast Fourier Transform on the data At this point you might also insert another Remove DC function to remove any offset in the frequency spectrum data computed by the FFT System Operation UM SW50407 05 60 System Operation Multi Stream Sampling System The next step is to correct possible phase errors by performing an Auto Phase operation Then a baseline correction is applied by fitting the baseline to a polynomial curve over a specified region of the spectrum Next a reference point is established Then integral values are computed over a specified range of frequencies These results may bee used in the prediction model calculations The next operation is to detect a peak looking for the first peak to the left of the reference This might be followed by measuring the width of the peak at 1 2 height or 1 10 height These values may also be used as inputs to the prediction model calculations In multi stream sampling applications the table in Figure 40 might be modified to add a Woody averaging function that computes the mean of several data acquisition readings The exact sequence of operations entered into an Automate
99. f isolation transformers line filters shielding or other means of attenuating interference A WARNING Many of the functions and operating tools described in this manual can seriously degrade analyzer performance if they are modified or adjusted by someone not skilled or properly trained in operating the analyzer Some of them must be performed only by Qualion NMR application or service personnel Since any such modification may void the system warranties or performance guarantees users should be particularly careful to heed this warning The specific items that should not be changed by untrained personnel are identified in this manual by warning notes preceding the item descriptions System Operation UM SW50407 05 System Overview Introduction I System Overview Introduction The D MASH Model Lab Process Analyzer is designed to analyze the composition of process fluids on an online continuous basis Using NMR spectroscopic techniques it can detect the presence composition and concentration of chemical constituents in a process stream and with appropriate software provide closed loop supervisory control of a process unit The range of applications is extensive and is limited only by the availability of reliable prediction models of the processes Typical user benefits are increased throughput better process control timely detection of off spec product and lower operating costs Measurement Principle The nucleus of an atom
100. fer to System Op Cf ation page 35 for a detailed description of these digital signal processing functions and the procedures for selecting parameters and executing the functions Major Software Components The major software applications supplied with the system are ProcessNMR Software for running the process online continuously in a production environment NMR Analyser Software for running the process online continuously in a production environment Diagnostic Software Heater Diagnostics Diagnostic package for analyzing performance of the magnet heater controls Shim Box Test Diagnostic package for analyzing performance of the magnet shimming functions NMR Diagnostics Diagnostic package for monitoring performance of a Process NMR Analyzer Communication Software pcAnywhere Communication package for performing remote monitoring and control of an NMR analyzer over a dialup telephone connection and LAN Connection anywhere in the world VNC Communication package for performing remote monitoring and control of an NMR analyzer ovet a LAN Connection anywhere in the world Each software item is described in detail later in this manual Major Hardware Components MAGNET The magnet in a Analyzer is a permanent magnet built from multiple segments of neodymium boron iron This material is used because its very high field strength to mass ratio achieves the desired flux System Operation UM SW50407 05 21
101. follows cet the Purging Volume to 1500 Liter 9 System Overview The minimum flow while purging can be increased for special applications In this case set as defaults Min FI P P a 1 1L 5ec Confirm by pressing the Enter Button hin FLO Confirm it is set to 0 1 L Sec Confirm by pressing the Enter Button Rated FL Confirm itis set ta Sec Confirm by pressing the Enter Button The desired minimum pressure of is already adjusted ex works Continue skipping this menu tem pressing the up key or view by pressing the Pres Now enter the desired value of the maximum pressure Modify the present parameter to 12 0 mbar Confirm by pressing the Enter Button R Pre Pu The desir ed set point during the process of 10 0 mbar is already adjusted ex works Continue passing the menu pressing the up ke q System Operation UM SW50407 05 3r cL m By On 9r Major Hardware Components The parameters category is now finished The main menu continues automatically with the sub menu 0000 Madify M cade QOQ1 as shown before please nate that the M code can not be set to 0000 0001 Modify By code to 000Z 0002 aet the Code to switch the ignition Capable apparatuses on or off The main menu setting are now complete After pressing the Enter key the purging system is in operation state 34 System Operation
102. h bit out of 16 bits of the shim word aW Coils Map Magnet Type MASH 40 35 35 31 30 26 25 21 20 16 15 11 10 5d Quick Test Read Clear Find ero Address Test Stop Test Figure 105 Shim Test Accurate Test Results Screen E E pk Select All Unselect All i System Operation UM SW50407 05 117 Maintenance and Diagnostics Address Test Diagnostics The address test verifies the address in selected units of each coil and checks crossover between the addresses aW Coils Map Magnet Type MASH FOB FEED 14 DEFO 40 35 ADE FE BE F3F5 51 2 fi 247 35 31 4 i 106 381 fi 076 30 26 817 21 5 fi 617 25 2 FACD f fidDdA _ 0 15 11 Fe2E 2 F4 1065 pocs 78 Frar Bi 5 1 Select All Quick Test Accurate Test Read Clear Unselect All Find Zero Stop Test Figure 106 Shim Test Address Test Results Screen NMR DIAGNOSTICS This diagnostic tool permits monitoring trend data on many different variables in the NMR application A typical example of a six window configuration is shown in Figure 107 It is possible to define up to 18 different process variabl
103. he RF transmitter signal causes the protons in the sample to deflect from their aligned axes When the RF signal is removed the protons relax and eventually return to their original axes In doing so they generate an exponentially decaying RF signal which is sensed by the receiver This time domain analog signal is filtered processed and transformed into a frequency domain spectrum by the Rack Mounted Computer The frequency domain digital data is then further processed and manipulated to generate the displays and numerical information needed by the user to present the results of the NMR analysis showing the types and concentrations of various components present in the sample and the reference probe The methods used for analog and digital signal processing are described in more detail later in this chapter and in Chapter 2 System Operation Temperature Control Magnet temperature is an extremely critical element in the NMR analysis and at the center of the magnet where the RF coil is located must be controlled within 0 2 millidegrees of its typical operating temperature of 45 C Temperature within the magnet is sensed by 4 thermistors and 4 thermistors spare which provide the measurement input to the Heater Control Unit mounted in the magnet box The output of the Heater Control Unit varies the current supplied to strip heaters bonded to the outside of the magnet Since a magnet can be irreparably damaged by extremely high temperatur
104. he following table lists the page references in this manual where you can find a description of the technique and procedure for executing each signal processing function Setting ADC Parameters Removing DC Zero Offset Perform Frequency Domain Signal Processing Several types of frequency domain signal processing are used with the Qualion NMR system You can define and initiate these functions in ProcessNMR by making appropriate entries in the Automated Analysis Table The following table lists the page references in this manual for both ProcessNMR and NMR Analysis where you can find a description of the technique and procedure for executing each frequency domain signal processing function 2 System Operation UM SW50407 05 66 Standard Procedures Set Up New Calibration Models Set Up New Calibration Models Since setting a new calibration model requires input from Qualion NMR Application Engineering contact Qualion NMR for assistance Connect to DCS Since this is normally a part of system installation and commissioning Refer to the installation Guide for detailed information on this task The Lab Analyzer does not communicate to DCS Set Up Analog Digital Modem Inputs Outputs Refer to the installation Guide Set Up Remote Control Connections via pcAnywhere All system installations are designed to be controlled remotely for monitoring and troubleshooting The remote control function uses pcAnywhere software
105. he form in which the results of the NMR analysis are presented to the user INTERPRETING FREQUENCY DOMAIN SPECTRA When more than one bond is present in a molecule more than one frequency appears in the spectrum plot By counting the number of absorption lines we can count the number of bonds The atom to which hydrogen is bound determines the intensity of the signal the magnitude of the chemical shift and the time it takes for each species of atom to de phase randomize its orbit Bonds between atoms may create multiple lines in the spectrum plot singlets one line doublets two lines triplets three lines etc The height of the peak indicates the number of atoms present in the sample The relative heights and chemical shifts of multiple peaks identify particular molecules and compounds The breadth of a peak line shape is an indication of the de phasing time for a particular type of bond By analyzing the heights locations and shapes of the various peaks and comparing them with known characteristics of basic elements and compounds we can determine the presence and concentration of the components of a process sample System Operation UM SW50407 05 11 System Overview Pulse Sequences Pulse Sequences N WARNING Actions described below should be performed ONLY by properly trained personnel In pulse NMR the manner in which a pulse is applied and then detected is very critical The pulse is applied in a sequence of s
106. him Control Unit controls the currents to all shim coils The software displays the present values of parameters entered for each gradient as shown in Figure 8 Set Method Gradients Shim Gradients Gz 0 74 9 4 0 69 Gzzzz E 83 Gx r 34 GEX 0 28 GHEK 2 35 Log File Guxxx i0 61 G2 Hess GFK 71 Gezxxx 82 Gy 434 Gyy 218 5 5 Stark Shimming Stop Shimming Guy 23 Gxxyz n 25 Gxyyz E 09 0 1 Gpp 3 58 Gzpp Gadd 0 0 Result Best Result Best Grad Level 0 o0 0 50 Spectra Emergency Power Switch 0 5 Spectra 0 40 Spectra Current Actual Result of Spectral Anabsis PROCESS 4500 QUALIONH Ltd Copyright 2007 Figure 8 Shim Gradient Display The display does not show the actual currents applied to each coil but rather the gradients between coils in various directions x y or z axes and combinations thereof The system operates in the following manner 1 First you must bring up an FID display which shows the present RMS value for the FID in the lower left corner of the window Click the Shim Button in the side menu of the main application to call the Shim Gradient Window figure 8 Note that the shim window displays four boxes at the bottom of the window called Result Best Result Best Grad and Level The da
107. hit 31437 Figure 23 FID after Removing DC Offset Fast Fourier Transform The FID time domain signal is converted to a frequency domain display by applying a Fast Fourier Transform FFT to the data Since both of the quadrature channels are converted to the frequency domain two channels of frequency domain displays can be viewed Figure 24 shows a pure dispersion spectrum and Figure 25 shows a pure absorption spectrum In most cases applying the FFT function System Operation UM SW50407 05 47 System Operation Main Transmitter Pulse to an FID produces frequency spectra that show both absorption and dispersion Phase correction 15 used to convert them to pure absorption or dispersion NMRAnalysis Running On Local Machine Figure 24 Frequency Domain Display Showing Dispersion NMR Analysis Running On Local Machine ERSLICNEBARREA FRAG oe _ RemoveDC zem wm o Mee _ Pea Window Figure 25 Frequency Domain Display Showing Absorption No Phase Error System Operation UM SW50407 05 48 System Operation Signal Processing Digital and Frequency Domain Signal Processing Digital and Frequency Domain After the FID is converted to a frequency domain signal additional signal processing techniques may be used to modify the data so as to improve the quality or presentation of the process information The techniques available with the system are described below DC OFFSET A characteri
108. ing anywhere in the application window and then selecting the appropriate command from the menu displayed Scheduler peration AddRow 1 Select Event Table Prev ADC Select Average Prey GRD Select Automated Analysi Set Shim Select Shim File Select Start Level SelectStop Level RMS Enter Stop Condition 3 Fun 4 Goto Select Destination Enter Count Load Select Event Table Select ADC Select Average Select Gradients Select Automated Analysi Select Shim File Select Start Level Select Stop Level Enter Stop Condition Figure 38 Typical Scheduler Screens The top screen shows the menu pick Scheduler gt Define that calls the next screen The middle screen shows the sequence of operations initiated by the Scheduler Because the display is very wide only the left side of the display is shown in the middle screen The right side of the same display is shown in the bottom screen A typical sequence of operations similar to that shown in the middle screen and initiated by the Scheduler is as follows 1 LOAD the files for processing Stream 1 Event Table for stream 1 ADC parameters for stream 1 Averaging parameters for stream 1 post processing file automated analysis table for stream 1 gradient file shim set for stream 1 prediction file calibration models for stream 1 2 RUN the analyzer with this set of data This starts the data acquisition cycle calling the event table and automated analy
109. ing the signal to noise ratio It adds points with values of zero to the FID increasing the total number of points without adding noise This effectively improves resolution of the system without affecting the signal As shown in Figure 79 increasing the number of samples in the data entry box directly affects the system resolution the current value of which is displayed below the data entry box w eros Filling Numbers af Samples 4096 Sampling Aate 4346 Resolution Before 1 05Hz Resolution After 0 27Hz Fill Upto 1 5384 Figure 82 Zero Fill Dialog System Operation UM SW50407 05 99 Windows and Dialog Boxes Automated Analysis Theory zero fill increases the number of data points in an acquisition sample by adding points all with a value of zero Since the total number of points increases the digital resolution is enhanced Since the added points are all zeros no noise is added Therefore the signal to noise ratio of the entire sample is improved When Used this function 15 used to improve resolution without adding noise Howto No of Samples Points Enter a new value that increases the total number of data points In conjunction with the value entered for sampling rate this determines the total acquisition time for the analysis This should be set at a value consistent with the resonance characteristics of the sample being analyzed Sampling Rate this is the rate in Hz at
110. is provided as a reference standard for setting the frequency of the main transmitter This reference probe the lock coil also has an RF coil and associated tuned circuit around it and 1s filled with lithium chloride The fact that the reference probe 1s mounted in a location slightly displaced from the main probe introduces a small error in measurement data between the two probes MAGNET HEATER CONTROL UNIT The Magnet Heater Control Unit controls the temperature of the magnet and the magnet envelope The temperature of the magnet is set at 45 and the temperature of the envelope is maintained at 41 C The Heater Control Unit is mounted on the interior wall of the Magnet Cabinet and has two PID loops that accept measurement input signals from the thermistors mounted on the magnet itself and the magnet shroud or envelope The outputs of these two PID loops control the currents to electric heater strips that are bonded to the outside of the magnet and the magnet envelope N WARNING Actions described in the following section should be performed ONLY by properly trained personnel Operation of these loops can be monitored and displayed by running the Heater Control diagnostics software The window that appears when you run this software 1s shown in Figure 7 System Operation UM SW50407 05 25 System Overview Major Hardware Components c Hesur Desmesiki Pis fr oy Mhar nd HI ME ad LLL
111. ive to the noise They both build up gradually with time but the signal builds much more rapidly than the noise making it easier to discriminate between them Use the dialog box shown in Figure 53 to perform signal averaging in the time domain The screen allows you to enter the number of times the signal should be averaged for each channel You can setup a sequence of averaging operations for each channel by adding rows with the Add Row button and then selecting a channel and entering the number of times to average Then click the Set button to execute the entries Click the Overlap box if you want to compute moving averages average the last n values Click the Align Peaks box to synchronize the starting points when computing a nonmoving average System Operation UM SW50407 05 77 Windows and Dialog Boxes Process NMR Application Average Formula E Hew Set Overlap Alan Peaks Figure 56 Average Formula Dialog Box ADC A WARNING Actions described in the following section should be performed only by properly trained personnel Click on the ADC button to display the screen shown in Figure 54 Figure 54 shows the dialog box for setting parameters for the analog to digital conversion ADC Parameters Sampling Rate gt Band Width Figure 57 Setting ADC Parameters Enter the total number of data samples points desired in the Number of Samples box A value of either 4000
112. k Configuration Variable Definition Dialog Box 2 Continued System Operation UM SW50407 05 124 Maintenance and Diagnostics Diagnostics X Axis Range Setting This item permits to enter a maximum value for the x axis of a plot e Figure 118 New Task Configuration X Axis Range Options Statistical History Setting This menu item lets entering the number of points of historical data used for computing the statistics to be displayed in a given plot Resize Satistic History System Operation UM SW50407 05 125 Maintenance and Diagnostics Diagnostics Data File Options This item displays information about the data file currently in use Rename Define zoom Plot Time Domain Units Comm F Frequency Womar Urte Set Borders Axis Aang Gatske History Hide Cursors Data File Figure 119 New Task Configuration Data File Dialog Box Save Chart Data Command This command permits you to save plotted data to a file Save Chart Data Save in a Servers 5 him Save type Chart Data dat File dat Cancel Open as read only Figure 120 Save Chart Data Dialog Box Frequency Domain Units Options This menu option permits selecting units for a frequency display The choices are Hertz PPM or Points System Operation UM SW50407 05 126 Maintenance and Diagnostics Diagnostics ine Warren me 2 uency Domal
113. ld along the X axis Using a frame of reference that rotates about the Z axis at a frequency equal to that of the alternating current in the coil the magnetic field along the X axis 1s held constant This 1s the same as moving the coil about the coordinate system at the Larmor frequency In NMR the magnetic field created by the coil passing an alternating current at the Larmor frequency is called the B field When the current is turned on and off it creates a pulsed D magnetic field along the X axis The spins respond to this pulse so as to cause the net magnetization vector to rotate about the direction of the B field A 90 pulse rotates the magnetization vector clockwise by 90 about the X axis the rotating X axis and rotates the equilibrium magnetization down to the Y axis the rotating Y axis The net magnetization at any orientation behaves according to a rotation equation For example a net magnetization vector along the Y axis shifts to the Y axis when acted upon by a 180 pulse of B along the X axis CHEMICAL SHIFT When an atom is placed in a magnetic field its electrons circulate about the direction of the applied magnetic field This generates a weak magnetic field that opposes the applied field The effective field is therefore usually less than the applied field The electron density around each nucleus in a molecule varies according to the types of nuclei and bonds in the molecule The opposing field and therefore
114. le 63 Grids 75 Modbus 67 New Application 62 Prediction 73 Scheduler 74 Screen Tools 70 Start 70 Stop 70 Purge Control System 25 R Real Portion 88 Reference Documents 1 Remote Control Connections via pcAnywhere Set Up 57 Remove DC 89 System Operation UM SW50407 02 136 Sampling System Multi Stream 48 Save Command 78 Scheduler 70 74 Screen Tools NMR Analysis 87 Process NMR 70 Set Up an Analysis 54 Shim 81 Shim Test Accurate Test 107 Address Test 108 Config 103 DAC Map 104 Debug 103 Display Units 105 Find Zero 105 Quick Test Display 104 Shimming Electrical 55 Mechanical 55 Shut Down the Analyzer 54 Signal Analysis Menu 88 Signal Processing Frequency Domain 14 39 56 Baseline Correction 43 DC Offset 40 Peak Selection 45 Phase Correction 42 Phase Errors 41 Reference 46 Woody Averaging 48 Signal Processing Time Domain 11 34 56 Fast Fourier Transform 38 Quadrature Detection 35 Removing DC Offset 37 Setting up the ADC 34 Signal Averaging 36 Window Function 37 Zero Filling 36 Software 32 Diagnostic 33 NMR Analysis 32 ProcessNMR 32 Shimming 33 Software Components Major 14 Standard Procedures 53 Start Command 70 78 Starting the Analyzer 53 Stop Command 70 79 System Components Major 7 System Description 7 Analysis of the Sample 10 Block Diagram 7 Functional Description 7 Functional Operation 9 Major System Components 7 Purge Control 11 Temperature Control 10 System Operation 27 System Overview 1 T T
115. lect the units in which the data is displayed PPM Hertz Points or Milliseconds click on the units displayed below the axis The menu shown in Figure 66 then appears Select the desired units and then click outside the menu The screen then displays the desired units The preferred unit for displaying NMR frequency domain data is PPM the unit preferred for a time domain FID 15 milliseconds m Hz 1000 1500 2000 Figure 69 Axis Units Selection Menu System Operation UM SW50407 05 87 Windows and Dialog Boxes Automated Analysis MAIN MENU File Clicking the File option displays the menu shown in Figure 67 las NR DIAGNOSTIC File Acquisition Task Start Stop Load Configuration Save Configuration Input Source d w Server Backup Directory Save Spc Save Ascii UnSave Figure 70 Main Menu File Menu Load This is a standard Windows Load command which displays a window that allows you to select a file to be loaded Save This is a standard Windows Save command which displays a window that allows you to select a directoty and filename in which to save your file Print This is a standard Windows Print command which displays a Windows Print window with normal print options Archive Processing This command permits you to retrieve a previously generated data file and then apply signal processing techniques to that data The menu shown in Figure 68 lets you retrieve a file from a source
116. luding one A C mounted on the left side wall The samples are inserted only with a Tube to the probe that can be also be heated to a defined temp erature POWER AND COMMUNICATIONS CONNECTIONS Power is required as 380 415 VAC 25 A three phase uninterruptible power connection Installations require 5 conductor power cables with L1 L2 L3 N and G ground or earth conductors The analyzer generally draws less than 16 A during operation Power and communication cables enter through two cable glads into the terminal box JB 1 mounted on the left side of the cabinet The Lab Analyzer can be connected to a 220 240 VAC or 110 VAC one phase only via a connector placed n the back panel of the Analyzer System Operation UM SW50407 05 30 System Overview Major Hardware Components Power Distribution Panel A Power Distribution Panel is mounted inside the Process analyzer enclosure on the left side of enclusore magnet side This unit contains all the circuit breakers for the system except the purge system and interlocks transformet The Lab Analyzer Distribution pane is placed on the front panel and includes also the main power switch of the analyzer Interlocks The purpose of the Interlocks is to completely isolate the any non explosion proof certified equipment contained NMR system when the system is shut down either by the purge system or power outage Lab Analyzer does not contain an Interlock mechanism ENCLOSURE ENVIRONMENTAL CONTR
117. lution of the system without affecting the signal As shown in Figure 20 Zero Fill Dialog Box increasing the number of samples in the data entry box directly affects the system resolution the current value of which is displayed below the data entry box Feros Filling Numbers of Samples 2048 Sampling Rate 4346 Resolution Before 2 12Hz Resolution After 0 53Hz Figure 20 Zero Fill Dialog Box To open the Zero Filling dialog box push the ZeroFill button from the Tools menu it can be enabled only after starting scanning System Operation UM SW50407 05 45 System Operation Main Transmitter Pulse Window Function The Window Function tool multiplies the acquired signal by an exponential equation as shown in Figure 21 The first order coefficient affects the shape of the FID curve at the low end of the time scale the second order coefficient influences the high end of the time scale In most cases only the first order coefficient is used If a negative first order coefficient is entered and the second order coefficient is set to zero the function is a decaying exponential which serves to smooth and shorten the decay time of the FID In the frequency domain it tends to broaden the width of a peak This function is often used with a truncated FID to eliminate a discontinuity and smooth the envelope Window Windowing Function A t B t tt Coefficients Filter Enable Filter Path to Filter File Humber of P
118. n Chapter 2 System Operation BLOCK DIAGRAM Figure 4 is a schematic block diagram of the major system components that shows the relation of each unit to the others and how they interact It is of necessity a simplified representation of the system designed to show general concepts rather than specific detail More detailed information about the operation of each unit can be found in Chapter 2 System Operation UM SW50407 05 13 System Overview Pulse Sequences FUNCTIONAL DESCRIPTION As shown in Figure 4 the system consists of a main cabinet divided into two compartments a Magnet compartment and an Electronics compartment which contain the components listed below and accessory systems for controlling the environment within the enclosure The enclosure is rated as IP56 NEMA 4X For Process Analyzer only Major System Components Magnet Compartment Magnet and Magnet Envelope containing a sample Lab probe for passing the sample through the field of the magnet and a reference or lock capsule filled with a known reference fluid Heater Control Unit for controlling temperatures of the magnet and the magnet envelope Bypass Flow Valve to interrupt sample flow during the measurement process For Process Analyzer only Power Distribution Unit for the system Pneumatic Manifold for controlling the stop flow sample switching and grab sample valves For Process Analyzer only Shim Control Unit for
119. n bypass mode you can access the enclosure without automatically de energizing power or triggering an alarm Before using the bypass function observe the following DANGER note DANGER To prevent personal injury or death do not place the system in bypass mode unless you certain the area is non hazardous When the system is in bypass mode do not leave the system unattended To use the bypass mode you first turn the system on in the normal manner and when safe pressure is established turn the key switch to the bypass position Bypass mode temporarily latches the enclosure power relays on Before returning to normal operation after you have accessed the enclosure you must re seal the enclosure and wait for safe pressure to be re established When the pressure is safe you can move the System Operation UM SW50407 05 32 System Overview Major Hardware Components key switch to the normal ON position without interrupting power If you move the switch to the ON position before safe pressure is detected however the system automatically shuts down and activates an alarm The operating procedure for using bypass mode is as follows 8 CI EX T Be D Sprache Deutsch English 8 Structure 3r Press the Enter Button to start main Menu The Control Unit calls for the M code to be entered The Ex Vvorks M Cade is 0001 Press the Enter Button to insert the M
120. n observe the effect of each incremental change by displaying the spectrum in another window When you have found a satisfactory value you can exit from the screen Lastly enter the Total Angle in Automated Analysis on page 83 Baseline Clicking this menu item displays the dialog box shown in Figure 85 Using this box you can enter parameters that define a baseline region and a method of correcting the data to conform to the selected baseline Baseline conection Baseline Parameter Mean Range Mum Std Peak 25 Method m Poly Degree 2 Find Baseline Correct Figure 88 Baseline Correction Dialog Box System Operation UM SW50407 05 104 Windows and Dialog Boxes Automated Analysis Baseline Parameters enter values for defining the baseline region 1 the mean value for setting the center of the region usually at the peak 2 the number of standard deviations on either side of the mean for setting the total width of the region and 3 the curve fitting method to be used for correcting the data to the baseline Find Baseline Button click this button to find the baseline defined by the parameter values you entered Correct Button click this button to execute the operation Peaks Clicking on Peaks displays the dialog box shown in Figure 86 14 Peak Referance Peak Identificatio 02 10021 Start Counting From Let Peak Index
121. ndwidth to the maximum to obtain lock and measurement quickly Then narrow the bandwidth to achieve an optimum signal for continuous Operation Quadrature Detection Quadrature detection is employed as a means of determining the phase characteristics of a time domain NMR signal Phase information is needed to distinguish between magnetization components that are precessing in one direction or the opposite Without quad detection false frequencies appear in the FFT frequency display Quad detection also helps increase the signal noise ratio by positioning the reference frequency so that the system can discriminate between signal and noise and thus eliminate the noise As shown in Figure 18 quadrature detection splits the incoming signal into two channels that are out of phase by 90 The channel in phase with the reference frequency is called Channel I the real System Operation UM SW50407 05 43 System Operation Main Transmitter Pulse component the channel 90 out of phase with the reference is called Channel Q the imaginary component The system can selectively display either channel or both channels together CHANNEL DIGITIZER REAL PHASE SENSITIVE DETECTOR O REFERENCE MMR REFERENCE FREQUENCY 90 REFERENCE PHASE SENSITIVE DIGITIZER CHANNEL Q DETECTOR MAGINARY Figure 18 Quadrature Detection Signal Averaging The system signal to noise ratio can be improved by averaging the signal ove
122. nits are composed of an inductor coil and a capacitive element The resonant frequency is determined by the inductance L and capacitance C of the circuit As mentioned previously the capacitor is manually tuned during installation of the probe Before performing an analysis of a process sample the system repeatedly applies an RF signal to the reference probe The frequency of the excitation signal applied to the lithium chloride capsule coil is varied over a narrow range until a satisfactory response is detected The purpose of this exercise is to establish the reference point or lock frequency for the system When the desired signal is detected the system is locked to use this frequency as the reference for setting the main transmitter frequency in a fixed ratio to the lock frequency Analysis of the Sample When the sample flow tube is filled an RF signal is applied to the RF coil The signal is applied at a frequency of approximately 58 MHz for approximately 15 usec at a power level of approximately 4 watts The signal is then removed After a delay of about 30 usec the Switching Control Unit listens for a response from the coil as the nuclei relax and return to random orbits The time required to receive a characteristic signal from a sample varies with the composition of the sample Typically the time ranges from 100 milliseconds to a minute System Operation UM SW50407 05 16 System Overview Pulse Sequences T
123. o Main frequency minus 9 MHz plus Lock Offset frequency times the Lock to Main frequency ratio 16 Lock to Observe ratio is the natural relation between the resonant frequency of lithium and the resonant frequency of hydrogen at a specific magnetic field streneth The main transmitter frequency is the actual resonant frequency of hydrogen at the magnet temperature at which the Lock system achieved lock The offset frequency is a user entered value that temporarily modifies the main transmitter frequency It is used as a convenience in a manual search for resonance when lock is turned off System Operation UM SW50407 05 27 System Overview Major Hardware Components COMMUNICATION LINKS Communications between the NMR analyzer and the remote computer is handled via Ethernet or a dedicated phone line and between the remote PC and a DCS by RS485 Modbus or 4 to 20 mA analog and discrete signals as illustrated in Figure 10 As shown in Figure 10 an Option 1 configuration communicates with the control system by means of a National Instruments FieldPoint terminal which can supply 4 20 mA analog and discrete signals to the control system The FieldPoint terminal and the analyzer communicate over an RS485 connection Also shown in the top diagram an Option 3 system communicates with the control system through an internally mounted PLC which recetves Modbus signals from the system PC and which also transmits data to the control system via RS4
124. oints Figure 21 Window Function Dialog Box Removing DC Zero Offset An FID signal may contain a steady state offset from zero as shown in Figure 22 Use the Remove DC tool as shown in Figure 23 to eliminate this error This is accomplished by making an appropriate entry in the Automated Operations table as described in Automated Analysis on page 83 where it is described in detail System Operation UM SW50407 05 46 System Operation Main Transmitter Pulse NMR Analysis Running On Local Machine 181 xj File Archive Processing View Data Run Tool Hardware Help 283 2 Load Save Print Stop E T Avg IME Faaa D kk tk Remove DC Zero FFT IFFT Magnitude Phase Baseline Peaks Window Real DC OFFSET Jo NMR Analysis Running On Local Machine A Save Prit n Sta Avg ADC Freq Shim Lock Auto A raaaa eee Zero FFT IFFT Magnitude Phase Baseline Peaks Window DC OFFSET EQUAL ZERO MILA A ILL SAANAANANAAANAAADAANA AAS iii ij UTE UT PAA AROS A PARAS AAD AAA AA DD AANA ASAD DADRA AA AAA AD EA LARA AAA AAA AAA mSec Pts 1 L I 1 1 1 1 1 1 1 1 40 100 120 140 160 180 200 220 240 260 280 20 340 360 380 400 420 440 450 mSeconds S
125. ool to display the imaginary signal Both Portions Click on this tool to display both the real and imaginary signals System Operation UM SW50407 05 98 Windows and Dialog Boxes Automated Analysis SIGNAL ANALYSIS MENU This menu provides access to all signal processing functions both analog and digital that you may need in setting up the analyzer for a specific application Use of the commands in the signal analysis menu normally requires that you STOP the data acquisition process while you manipulate the data If you want to use these functions while data acquisition is running use the Automated Analysis table instead refer to Automated Analysis on page 83 Enter desired functions in the Automated Analysis table and continue to run the acquisition process The available functions are shown in Figure 78 AMBnalysis Running On Local Machine P 5 m x File Archive Processing View Data Run Tools Hardware Help os us emu mm x e iM Predick A Auto 9 Help Load Save Print Start Stop E T Av ADC Freq Shim Lock WE FRAR D Remove DC ero Fill FFT IFFT Magnitude Phase Baseline Peaks Real Figure 81 Signal Analysis Menu Remove DC An FID signal may contain a steady state offset from zero Use the Remove DC button to eliminate this error Zero Fill filling is a means of increasing digital resolution of the system without degrad
126. or 8000 15 typically used Enter a the Number of Echoes box This function not used Then select a data Sampling Rate which is typically set at 4346 Hz The combination of a sampling rate of 4346 Hz and a total number of samples of 4000 yields a total acquisition time of approximately 1000 milliseconds Similarly setting the number of samples to 8000 yields acquisition time of approximately 2000 milliseconds To prevent aliasing the sampling rate must be at least twice the highest data frequency to be captured the so called Nyquist frequency After you select a sampling rate of 4346 Hz the bandwidth you select System Operation UM SW50407 05 78 Windows and Dialog Boxes Process NMR Application in the lower box should not be greater than 2000 Hz Since 2000 Hz is greater than the spectral range of the data to be gathered 750 Hz 2000 is an acceptable value Entering these values of parameters for the ADC means that the total acquisition time is approximately 1000 milliseconds the analog resolution is approximately 0 14 Hz and the pulse has a spectral bandwidth of 2000 Hz MODBUS This paragraph does not refer to the Lab Analyzer Click on the Modbus button to display the dialog box shown in Figure 55 Enter appropriate parameter values in the Port Settings boxes at the top section of the display Then enter other parameter values in the rest of the screen as needed When complete click on Exit at the top left of the display
127. p size used in sweeping the lock frequency Jump this is the magnitude of the change in lock frequency as the transmitter jumps from an increasing sweep to a decreasing sweep as the lock system searches for a resonant response Threshold this is the minimum value used to define a resonant response as the lock system searches for resonance of lithium chloride RSSI threshold this function is not used in the system at present Tx Gain this is the setting of the lock transmitter gain System Operation UM SW50407 05 96 Windows and Dialog Boxes Set Button click this button to accept the parameter values entered in the table Cancel Button click this button to reject changes in the parameter values in the table Lock Pulse Parameters Figure 77 1s the dialog box for displaying and entering parameters for the lock pulse Pulse 0x4 Anes MARS gt 0 0003 aaaeaii QUALIOH Ltd Copyright 2007 Figure 80 Lock Pulse Dialog Box The parameters are Pre2Tx pretransmission delay time OFF Tx transmitter ON time Rx receiver ON time Tx2Rx transmitter to receiver OFF time Rest recycle delay time Set Button click to accept changes in parameters Cancel Button click to reject changes in parameters Exit click to exit from the dialog box Automated Analysis Click this button to perform and automated analysis For details see Automated
128. presence of a phase error which should be corrected NMR Analysis Running On Local Machine Figure 84 Frequency Display before Auto Phase Correction System Operation UM SW50407 05 101 Windows and Dialog Boxes Automated Analysis Display after Auto Phase Correction Figure 82 shows the spectrum after applying autophase correction to the data NMR Analysis Running On Local Machine je f x File Archive Processing View Data Run Tools Hardware oes gt wo ADC Freq Shim Lock Auto A Load Save Pr Stat Stop Avg Faaa k k ke Remove DC Zero Fil FFT IFFT Phase Baseline Peaks Window 1 2000 1500 1000 500 RMS 9559 89 Skt 27189 I qo Figure 85 Frequency Display after Phase Correction IFFT The IFFT function is included as a convenience to view the inverse of the FFT operation It is not used in normal operation of the analyzer System Operation UM SW50407 05 102 Windows and Dialog Boxes Automated Analysis NMR Analysis Running On Local Machine 2 File Archive Processing View Data Run Tool Hardware Help c 3 11 Save Prnt Start Sto Avg 9 Shim Lock s 400 200 Lia 200 I ai 400 600 800 EN _ ay I 1
129. pulldown list select a parameter highlight the parameter and release the mouse button The available choices are PreTx time delay before transmission of main pulse Tx main transmitter Rx main receiver AdcEn ADC enable 1 or disable 0 Phase phase set at 90 180 or 270 System Operation UM SW50407 05 76 Windows and Dialog Boxes Process NMR Application Valve 1 Sample valve 1 determined by hardware configuration Valve 2 Sample valve 2 determined by hardware configuration Valve 3 Sample valve 3 determined by hardware configuration Valve 4 Sample valve 4 determined by hardware configuration Valve 5 Sample valve 5 determined by hardware configuration Lock this parameter permits you to start or stop the lock function To start lock enter a 1 in the value box To stop lock enter a 0 in the Value box The Value parameter 15 for entering data such as On 1 Off 0 transmitter or receiver gain value ot Label No for GoTo functions The Lab Analyzer does not use Valves AVERAGE N WARNING Actions described in the following section should be performed only by properly trained personnel Click on Avg button to display the screen shown in Figure 53 The system signal to noise ratio can be improved by averaging the signal over a period of time Since white noise is random and signal is not time averaging tends to reinforce the signal relat
130. quencies centered about F with a bandwidth of 1 t where t is the duration of the pulse Radiation is produced of all frequencies in the range F 1 t If t is very small a large number of frequencies is produced simultaneously and all target nuclei in the sample are excited To understand the effect of the RF pulse consider the following Bo 7 Figure 1 Precession of Nuclei Since more nuclei are aligned with the applied field than against it a net magnetization vector is aligned with the field Imagine now that the room itself is spinning at the Larmor frequency To an observer in the room the nuclei appear to be stationary not processing and the net magnetization vector is aligned with the field The concept of spinning the room 15 called the rotating frame of reference Using the rotating frame of reference the magnetic behavior of the system be shown as Bo System Operation UM SW50407 05 System Overview Measurement Principle Mo STATIONARY BULK MAGNETIZATION VECTOR Figure 2 Magnetization Vector A pulse of radio frequency energy is applied along the x axis The magnetic field of this radiation 1s given the symbol B In the rotating frame of reference B and M ate stationary and positioned at right angles to the plane The pulse causes the bulk magnetization vector Mo to rotate clockwise about the x axis The extent of this rotation is determined by the duration of the pulse In many Fo
131. r The lock transmitter frequency is first swept in an increasing direction until near resonance is detected The frequency then hops to a higher frequency and starts to approach resonance in a decreasing direction As the sweep nears resonance the transmitter jumps to a frequency that is midway between the high and low near resonance values Lock is established at this frequency When resonance is detected and lock is achieved the main transmitter frequency is set at a specific ratio to the lock frequency observe to lock ratio because the resonant frequency of proton at a given magnetic field strength has a fixed relation to the resonant frequency of lithium at that same field strength The lock frequency is the means of determining what the main transmitter frequency should be and therefore plays an extremely important role in operation of the analyzer Screen Display As shown in Figure 75 the Lock Menu displays time varying curves of Channels I and Q of the Lock Receiver signal which give a live indication of the status of the Lock system When the system 15 approaching lock the displays show a slowly oscillating characteristic that smooths out as lock is achieved Control The Control menu controls operation of the frequency sweeping and other control functions of the Lock system Initialize loads a set of parameters Start activates the system and Stop interrupts operation of the system Pulse The Pulse menu controls oper
132. r a period of time Since white noise is random and signal is not time averaging tends to reinforce the signal relative to the noise They both build up gradually with time but the signal builds much more rapidly than the noise making it easier to discriminate between them Use the dialog box shown in Figure 19 to perform signal averaging in the time domain To display this dialog box click the Average button in the Main Menu Side of NMR Analysis The screen allows you to enter the number of times the signal should be averaged for each channel You can setup a sequence of averaging operations for each channel by adding rows with the Add Row button and then selecting a channel and entering the number of times to average Then click the Set button to execute the entries Click the Overlap box of you want to compute moving averages average the last n values Click the Align Peaks box to synchronize the starting points when computing a non moving average Average Formula Label a _Add Row 2 0 1 Mew Set Overlap Align Peaks Figure 19 Signal Averaging Dialog Box System Operation UM SW50407 05 44 System Operation Main Transmitter Pulse Zero Filling filling is a means of increasing digital resolution of the system without degrading the signal to noise ratio It adds points with values of zero to the FID increasing the total number of points without adding noise This effectively improves reso
133. ream Hone R1199 Logger OH Figure 59 Alarms Menu Alarm Menu This paragraph does not refer to the Lab Analyzer This menu shows the byte addresses of the three types of alarms Cabinet Health NMR Health and Outlier A 1 indicates the first byte a 2 the second byte a 3 the third byte and so forth Digital inputs are configured at system manufacturing and should not be changed Enter the applicable data for your system configuration Outlier Menu This menu is used with multi stream sampling systems to assist in evaluating an outlier alarm If the Enable Sample Grab box is checked the sampling system automatically performs a grab sample operation and checks the result against the outlier value You can then determine whether the outlier is acceptable If the Stay On Current Stream box is checked the sampling system continues to analyze samples from the current stream This generates additional analyzer outputs against the outlier can be evaluated Select the option for your system System Operation UM SW50407 05 80 Windows and Dialog Boxes Conditions Check Outlier is OH Send Stream DCS is OH Outlier Continue gt Flag Message lt Continue gt Flag Address T m 5 E g 5 m ProcessNMR Application a DCS OuerHRide is EN xj Sample Grab iz OH Enable Sample Grab Stay On Current Stream 123 J943
134. rength and channels liquids away Stainless steel screws and clamps on three sides ensure a watertight and airtight seal The ambient temperature in the enclosure is maintained within 1 C This is accomplished by means of solid state air conditioners on top of the enclosure The air conditioners run continuously The temperature is controlled at 22 1 C by a temperature controllers with an RTD To minimize ambient temperature effects all external walls of the enclosure are insulated The system is designed for Zone 1 and 2 Gas Group IIB amp area classifications Power and communication cables enter through two cable glads into the terminal box JB 1 mounted on the left side of the cabinet Attached to the terminal box JB 1 1s the interlock box that contains the main circuit breakers for the purge system and interlock transformer the main contactor interlock transformer and interlocks All other circuit breakers are located on the power distribution panel in side the enclosure of the left side Process sample flow into and out of the process analyzer passes through the sample valve The purpose of this valve in to block the sample in the NMR during the analysis and the valve is mounted on the left side of the enclosure There are drain and flush valves also mounted on the left side of the enclosure and are used for periodic cleaning of the flow line tubing and the magnet probe The Lab Analyzer has a temperature controlled enclosure inc
135. results of NMR spectral analysis constituent concentrations with results of laboratory tests of other variables such as Research Octane Number Motor Octane Number Cloud Point Pour Point etc These models can then be used for online prediction of characteristics of the sample from the results of the NMR analysis Users of the NMR analyzer can develop their own mathematical prediction calibration model using software tools like the GRAMS software package from Galactic Software of Salem N H or they can participate with other Qualion NMR users in developing general calibration models for typical processes The general models which are available from Qualion offer the advantages of using shared data from a large number of users and processes The following is a list of typical processes and the sample variables that can be continuously measured online through the use of the Qualion NMR online NMR analyzer and Qualion NMR developed calibration models System Operation UM SW50407 05 37 System Operation Overview Refinery Applications D86 T10 50 T90 End Point Cloud Point Pour Diesel Point Cetane No API Gravity Viscosity Sulfur RON MON D86 n T50 790 Benzene Total Gasoline Blending Gasoline Blending 0 2 Aromatics VP D86 T5 795 Flash Point Freeze Point D86 T5 785 T90 T95 Cloud Pour Flash API Crude Distillation Light Gas Oil Fm 195 Cloud Pour Flash API Sulfur Crude Distilla
136. rm Maintenance Air Conditioners Regular Maintenance Long Term Maintenance eraut E07 NR 07 LO MOY a Heater Diagnostics Main Menu Adding Windows Magnet Menu Proportional Integral DAVE Pop Up Labels Shim Testis Max Current Value System Operation UM SW50407 05 ti l L 09 LAO 0 Lb e ENT M A D CUM System Overview Debs ier DAC Map uick Test Display ind Zero isplay Units ccurate Test ddress Test NMR Diagnostics ain Menu sing NMR Diagnostics oerte ew ew Task Configuration Options Plot Style Options Time Domain Units Options Rename Options Variable Definition Options X Axis Range Setting Statistical History Setting Data File Options save Chart Data Command Frequency Domain Units Options dows Men eaten aeos reet lear Command itle Command oett oreet pical Configuration Examples
137. rol is via a PID controller which sends a smoothly modulated average current signal to the air conditioners The Lab Analyzer has no ANC on the Electronic compartment Purge Control System The Lab Analyzer has no Purge control System The Process analyzer is currently provided with a Rapid Exchange Purging System which uses compressed instrument air to remove and prevent flammable vapor accumulation within the sealed analyzer enclosure On startup the purge system causes rapid air exchanges to occur and then maintains a safe positive pressure of 10 mbar Each system includes a control valve to control the pressure and flow with in the enclosure An electrical power control unit EPCU that monitors operation of the purge system and controls power to the system All startup requirements must be satisfied before the EPCU applies power to the enclosure To start up the purge system do the following 1 Verify that power is available that the Rapid Exchange Timer is set for 1 minute per 2 5 cubic feet and that the air supply 15 on 2 When the rapid exchange cycle is completed enclosure power is turned on 3 If safe pressure or power lost an alarm is activated and power is automatically disconnected 4 When power and safe pressure are restored the system attempts an automatic restart 5 shut the system down remove power to the system or switch the purge system circuit breaker off Bypass Mode Conditional Bypass I
138. rom the other direction When it detects a resonant response as it approaches from the other direction it stores this frequency and then jumps to a frequency at the mid point between the two stored values and then locks on this frequency as the resonant frequency of lithium The output of the lock system is used as the set point of the main transmitter circuit which maintains the main transmitter frequency in a fixed ratio to this lock frequency If the resonant frequency changes slightly during operation because of a deviation in field strength or temperature the control loop acts to maintain lock at whatever the resonant frequency is and changes the main transmitter frequency accordingly Signal Processing Frequency Domain N WARNING Actions described in the following section should be performed only by properly trained personnel After the time domain signals are converted to frequency domain by the Fast Fourier Transform process they are further processed by numerical methods and software techniques to produce frequency domain data that accurately represents the composition of the process sample The types of signal processing available to you System Operation UM SW50407 05 20 System Overview Major Software Components Woody Averaging Remove DC Offset Baseline Correction Finding Peaks Setting Peak References Performing Integrals Zeto Order Phase Correction First Order Phase Correction Please re
139. s w Point MALAM T peguero Umts Set Borders X ue Hang b Satistic History Show Cursors Data File Figure 113 New Task Configuration Time Domain Units Options Rename Options This item permits to enter a name for the plot Hew Task Enter New Task Name Cancel Figure 114 New Task Configuration Rename Dialog Box Variable Definition Options Figure 115 shows the dialog box for defining the plot of a variable after post processing The first function selected is automatically assigned a label of 0 the second is assigned a label of 1 and so on FEM Program Of Label Function Use First Baseline Use First Phase Figure 115 New Task Configuration Variable Definition Dialog Box 1 Figure 116 shows the first 12 variable types that may be selected for a plot System Operation UM SW50407 05 123 Maintenance and Diagnostics Diagnostics im Program Function Rermowe Use First Baseline Zero Fill Use First Phase Windows FFT IFFT Magnitude Manual Phase Zero Order Phase First Order Phase Auto Phase Baseline Reference ET Figure 116 New Task Configuration Variable Definition Dialog Box 2 NMA DIAGNOSTIC File me ig Manual Phase Use First Baseline Sawa DEdBFHESCE Use First Phase First Order Phase Peak width IriLeur als Integral Fatia Frequency Freq Shift m Figure 117 New Tas
140. s connected to a capacitor to form a tuned circuit which is manually tuned at installation Since accurate analysis of a sample requires an extremely uniform magnetic field the linearity of the field of the permanent magnet is shimmed by adjusting the currents supplied to each of forty pairs of small electromagnets located on a shimming unit mounted between the pole pieces in the center of the magnet The Shim Control Unit mounted in the Electronics Compartment determines and controls the current to each set of shim coils The fields generated by the shim coils modify portions of the field of the permanent magnet to increase uniformity of the resultant field A computer program is used to sense uniformity of the field by detecting good bad changes in the FID and to determine automatically the correct value of current for each set of shim coils An RF Unit mounted in the Electronics Compartment supplies a radio frequency excitation signal to the sample and reference RF coils during analysis The same coils are used to sense the RF signal generated by the sample and the reference fluid during the relaxation phase after the excitation signals are removed The RF coils create the field which rotates the net magnetization vector in a pulse sequence They also detect the transverse magnetization as it precesses in the XY plane Each of the rf coils must resonate at the Larmor frequency of the nucleus being examined by the analyzer Therefore the coil u
141. s described in detail within this section The options are Rename Permits entering a name for the window Define Gives you the option to define the automatic analyses and the variable s that will be plotted in the window Zoom Permits selecting any of a number of zoom functions for displaying the data Plot Style Permits choosing either a solid or dotted line for plotting a particular System Operation UM SW50407 05 119 Maintenance and Diagnostics Diagnostics variable Time Domain Units Permits selecting either milliseconds or points from the x axis of the plot Frequency Domain Units when a frequency domain variable is selected it is possible to select either MHz or PPM for the x axis of the plot Set Borders Permits setting the width of the borders for the window X Axis Rang Permits setting the maximum range of the x axis of the plot Statistic History Permits setting the maximum size in x axis units of the data to be plotted Show Hide Cursors Permits either showing or hiding cursors in the display Data File Displays the filename and path of the file you are using for this plot 3 To add another window repeat the procedure described above The new window is overlaid on the previous window in cascade mode 4 After defining the content of each window that was added click on Windows in the main menu and select a tiling option vertical or horizontal to arrange the windows on
142. s gradients in the magnetic field These are not the values of the currents supplied to each shim coil but rather the net results of the various currents For example Gz is a first order gradient of the magnetic field in the Z direction along the main axis of the field Gzz is a second order gradient Gzzz a third order and Gzzzz a fourth order Using these in combination you can describe almost any shaped profile of field strength in the z direction Similarly Gx Gxx Gxxx Gxxxx describe gradient profiles in the x direction and so forth System Operation UM SW50407 05 93 Windows and Dialog Boxes Automated Analysis It is difficult to set these gradients because they are all interactive setting one upsets all the others Therefore it requires the use of repetitive trial and error hill climbing techniques to arrive at the optimal values for each gradient and shim coil current Fortunately the NMR system includes a program that automatically determines the best values for each gradient To execute the automatic shimming program from the NMR Analysis Main Window click on the SHIM button in the side menu The screen shown above then appears Click on Set Method to select the shimming methods click OK and then click on Start Shimming to begin the process Click on Stop Shimming to terminate the process Display Result Best Result Best Grad Level These windows display the current operating results of the shimming program Res
143. sis functions as needed 3 GOTO 1 two times and then exit to the next step This causes the analyzer to make two sets of measurements and then move to the next sample Stream 2 LOAD the files for processing Stream 2 RUN the analyzer with the Stream 2 data files GOTO 4 Repeat the measurement cycle 3 times and then proceed LOAD the files for Stream 3 RUN the analyzer with the Stream 3 data files pe ie X dow GU oum GOTO 8 three times and then exit to the next step 10 GOTO 1 1 Repeat the whole sequence continuously until interrupted by the operator System Operation UM SW50407 05 59 System Operation Multi Stream Sampling System Event Table The following screen shows a typical event table for an NMR analysis Event Table File Pulse Commandi Duration Channel value _ Osea 127 Phase 11 00u AdcEn 300 0054 PreTx a nuu Figure 39 Typical Event Table Screen An Event Table for use with a multi stream sampling system would be modified to add controls for sequencing valves in the sampling system and the analyzer Automated Analysis Table gt Automated Analysis i Ox Function d edm BER FFT 1 Woody Average B 5 0 5 2 Remove DC bd Auto Phase an Left 1 1 200 Auto Phase Symmetric Auto Phase Manual Phase Order Phase First Order Phase Baseline Reference Integrals Normalize Res
144. stic of the FFT function is that frequency domain data may exhibit a DC offset in the same manner as that of a time domain signal as shown in Figure 26 To reduce this error to zero as shown in Figure 27 you apply a Remove DC function as you did in the time domain This is accomplished by making an appropriate entry in the Automated Analysis table refer to Automated Analysis on page 83 where it is described in detail FE PracessMMR I Flu r wales OCS Stat ZERO DC OFFSET 0 nn 2000 3100 I I rlon 7500 ai 8510 S000 9500 Figure 26 Frequency Domain Display with DC Offset Removed System Operation UM SW50407 05 49 System Operation Signal Processing Digital and Frequency Domain Procesa NHR Fi nning Lacal Machine EINE eu ur s Spates Stay ZERO DC OFFSET we Figure 27 Frequency Domain Display with DC Zero Offset PHASE ERRORS The trace shown in Figure 28 indicates the presence of phase errors because it shows dispersion instead of absorption The trace can be modified by performing a phase correction function which can be either automatic or manual NMR Analysis Running On Local Machine gt 7 B lt m 2 z E IL Star stop 2 Avg i i Ami Figure 28 Frequency Domain Display with Phase Error Dispersion System Operation UM SW50407 05 50 System Operation Signal Processing
145. ta that appears in these boxes determines how the shimming software functions Also the current value is displayed as actual current and max current according to the definition in the AcqMgr ini file Click on the Set Method command The dialog box shown in Figure 9 appears Select the shimming methods and defining the stop condition criteria of the electrical shim process according to the lower table as shown in figure 9 and click OK Auto Shim can also be preformed by running the Autoshim file from Scheduler System Operation UM SW50407 05 25 System Overview Major Hardware Components x Method File Lualion HMR Ltd Copyright 2005 Figure 9 Set Method Dialog Box 4 Ifyou want to keep a log file click on the Log File command Assign a filename and path and then click on Start Shimming This starts the shimming process When you want to terminate the shimming process click on Stop Shimming 5 general concept by which this system finds the optimum values for each gradient 15 to make a small incremental change in one value and observe the resulting RMS value of the FID the next time it is generated The system compares the current RMS value of the FID with the previous value If the new value is greater than the previous value the trial increment was beneficial and should be saved If it is lower the increment was not beneficial and should be discarded The system thus compares the latest RMS result value in
146. teps that first enable the transmitter then transmit the pulse for a predetermined time turn off the transmitter and wait for the receiver circuit to settle and then turn on the receiver to listen for the generated signal from the probe In the Process NMR Analyzer this sequence is controlled by the Event Table Refer to Event Table on page 75 for more detailed information The length of time the pulse should be applied is determined by the sample being analyzed If you want to apply a pulse that deflects the nuclei by 90 you must determine the desired pulse time for a specific sample by varying the pulse duration time and sensing the received signal until you detect a null The null output indicates that the pulse is a 180 pulse To generate a 90 pulse divide the duration of the 180 pulse by 2 Then enter this value in the Event Table The length of the wait time between pulses must be long enough for the nuclei to relax completely Applying pulses with too short a wait time between pulses can cause saturation and consequent loss of measurement information System Operation UM SW50407 05 12 System Overview Pulse Sequences System Description This section is a top level functional description of the overall system hardware and its major equipment components Detailed descriptions of the individual units are included at the end of this chapter and detailed descriptions of the system software and operating procedures are included i
147. the effective field at each nucleus vary This is called the chemical shift phenomenon The chemical shift of a nucleus is the difference between the resonant frequency of a nucleus and a reference standard and 1s a very precise indicator of the chemical environment around a nucleus System Operation UM SW50407 05 10 System Overview Measurement Principle TIME DOMAIN AND FREQUENCY DOMAIN DATA PLOTS An NMR spectrum may contain many different absorption lines at different frequencies In pulsed NMR spectroscopy the signal is detected after the magnetization vectors are rotated into the XY plane by applying and then removing an ac field Once a magnetization vector is in the XY plane it rotates about the Z axis and induces an ac current in a coil of wire oriented along the X axis Plotting current as a function of time yields a sine wave which decays with the dephasing of the spin packets after the applied field is removed This decaying signal is called a free induction decay FID The time domain signal is then converted to a frequency domain diagram by applying Fast Fourier Transforms to the data To avoid masking of one component by another and to minimize the effects of noise and interference several standard data processing techniques are applied to the raw frequency data These methods reduce the effects of noise and or increase the level of definition and separation of the various frequency peaks in the spectrum display This is t
148. the next operation in the sequence Refer to Figure 64 for a typical Scheduler sequence 4 When finished click on Set to save your entries GRIDS Click on the Grid button to add or delete a horizontal grid Click on the V Grid button to add or delete a vertical grid NMRANALYSIS APPLICATION NMR Analysis software 1s supplied with most systems in addition to ProcessNMR The NMR Analysis software package is intended primarily for use in laboratory environments where samples are manually inserted into the probe and experiments are run on a batch basis However it is also very useful in online process applications for setting up the analyzer and in modifying parameters to meet specific operating needs N WARNING Actions described in the following section should be performed only by properly trained personnel and or Qualion NMR technicians System Operation UM SW50407 05 86 Windows and Dialog Boxes Automated Analysis NMRANALYSIS MAIN MENU COMMAND Wem Dun Tat Hb BUTTONS SCREEN IE HEunaumxnDxkk TOOLS pee Heer zn FT IFFT Wap dale Phas rds 10m SIGNAL ANALYSIS MENU TYPICAL FID DISPLAY AMS VALUE 4 OF FID DR SON a a ae eas ues FREQUENCY SHIFT OFFSET AXIS UNITS Figure 68 NMR Analysis Main Window AXIS UNITS To se
149. tion Using a conventional 3 axis NMR coordinate system the net magnetization vector M and the vector of the applied magnetic field B lie in the same Z direction The magnitude of M can be altered by applying energy to the nuclei equal to the energy difference between the spin states If enough energy is applied M can be made to equal zeto When the energy is removed M returns to its equilibrium value The time constant for this return is called the spin lattice relaxation time which is defined as the time required reducing the difference between M and equilibrium by a factor of e If the net magnetization vector is placed in the XY plane it will precess rotate about the Z axis at a frequency equal to the frequency of the photon that would cause a transition between the two energy levels of the spin This frequency is the Larmor or resonance frequency In addition to the rotation the net magnetization vector starts to de phase return to random orbit because each of the component spin packets rotates at its own Larmor frequency The longer time is elapsed the greater the phase difference The time constant that describes the return to equilibrium of the transverse magnetization M is called spin spin relaxation time T2 XY Xv Passing a dc current through a coil of wire placed around the X axis provides a magnetic field along the X axis Similarly an alternating current produces an alternating magnetic fie
150. tion Heavy Gas Oil TBP Water API Gravity Crude Analysis Limited OVERALL SYSTEM DESCRIPTION Figure 14 1s a block diagram that illustrates the signal processing functions performed by the analyzer Refer to Chapter 1 for a functional description of the major hardware elements SAMPLE SWITCHIMG PHOCESS SYSTEM PROCESS SAMPLE SAMPLE SWITCHING AND CYCLE CONTROL PULSE CON TAOL EVENT TABLE LOCK PULSE CONTRO LOCK PARAMETER TAB TIME DOMAIN SIGNAL DIGITAL PROCESSING SIGNAL PREDICTION AND A D DOMAIN PROCESSING MODELS CONVERSION CLUIADRATURE DETECTION ZERO ORDER PHASE CORRECT ICM SIGNAL AVE AAG ING FIRST ORDER PHASE CORRECTION TO WINDOW FUNCTION EXPONENTIAL SMOOTHING WOODY AVERAGING DES REMOVE DC OFFSET REMOVE DG OFFSET ADC PARAMETERS BASELINE CORRECT ION ADC ZERO FILL SETTING A PEAK REFERENCE PERFORM INTEGRALS PEAK REFERENCE WIOTH AUTOMATED ANALYSIS SCHEDULE Figure 14 Functional Block Diagram of NMR Signal Processing System Operation UM SW50407 05 38 System Operation Overview A sample stream is fed directly from the process into the analyzer through the probe through an on off control valve stop flow valve and then to drain or back to the process When the sample is not being analyzed it is returned to the process in a recycle loop Note that in some installations the sample is sequentially selected from up to 6 process units by the use of an automatically controlled
151. tions System Operation UM SW50407 05 28 System Overview Major Hardware Components SWITCHING CONTROL UNIT The Switching Control Unit contains the following major components 36 MHz crystal oscillator RF Sources Module Lock Transmitter Module Lock Receiver Module Main Transmitter Module Main Iransmitter Receiver Module 36 MHz RF Filter The crystal oscillator generates a 36 MHz signal which 15 used as the basic frequency and phase reference for the whole system This frequency was chosen because it lies midway between the Main Transmitter frequency approx 58 MHz and the Lock Transmitter frequency 22 MHz The 36 MHz sional is buffered in the Switching Control Unit and sent to the Direct Digital Synthesizer DDS board in the Rack Mounted Computer Unit The DDS board divides the 36 MHz by 4 to generate a 9 MHz signal The RF Source Module within the Switching Control Unit receives the 36 MHz output from the DDS board divides it by 4 to produce a 9 MHz signal and phase encodes it to one of four phases 0 90 180 270 The 9 MHZ at 0 Main Phase0 is sent to the Main Transmitter and is also buffered and sent to the Main Receiver the Lock Transmitter and the Lock Receiver The Main Transmitter Module divides and adds mixes the 9 MHz and Local Oscillator signals to produce the Main Transmitter frequency This signal is then enabled disabled by the MN_TX_PRE_EN signal to produce the Main Transmitter pulse
152. ugh data points to ensure a good value of digital resolution Increasing the total acquisition time beyond that required for the FID to reach System Operation UM SW50407 05 41 System Operation Main Transmitter Pulse zeto does not add to the spectral data but does improve digital resolution This is explained further in the descriptions of ADC parameter setting and the Zero function T Purine g Om Local Machine Fie Andhe Processing View Data Rum Tools Hardware Help gt mM 5 x 9 Load Save me Start 24 E T ADC Freg Shin Lock Auto Help keke Remove Zeno Fil FFT IFFT Magnitude Phase Baseline Peaks nidos ana TOU 5D 11111111 soo LU LLL E zoo soo se m peii ka parl 1 FREQUENCY a RMS OF FID 9HIFT 1000 mSec Pts W 40 so 120 140 160 180 220 200 300 320 340 360 3900 400 420 440 460 eee opaca 3 2 Figure 16 Typical Free Induction Decay FID Display SIGNAL PROCESSING ANALOG AND TIME DOMAIN Setting up the ADC Figure 17 shows the dialog box for setting parameters for the analog to digital conversion This box 15 displayed by clicking on the ADC button in the Main Menu System Operation UM SW50407 05 42 System Operation Main Transmitt
153. ult is the current value of the gradient Best Result is the best RMS achieved up to the present time Best Grad is the best gradient value achieved up to the present time and Level is the criterion used in the shimming operation Lock Click on the Lock button on NMR Analysis Main Menu to display the screen shown in Figure 75 amp Lock Hex File Version 0 Observe 57370334 3 i i rel QUALIOMH Ltd Copyright 2007 Figure 78 Lock Menu Screen Before describing this screen it is useful to review operation of the hardware lock system The purpose of the Lock system is to control main transmitter frequency The probe contains a separate sealed capsule of lithium chloride which is mounted within the magnetic field next to the main sensor coil but not exposed to the sample fluid The capsule has a sensor coil wound around it similar to that of the main sensor This coil is part of a tuned circuit that is excited by a pulse from the lock transmitter After the lock transmitter is turned off the lock receiver senses the NMR signal produced by the coil The lock transmitter frequency is automatically swept through a range to find the resonant frequency of the lithium chloride sample When resonance is detected the servo system locks on that frequency System Operation UM SW50407 05 94 Windows and Dialog Boxes Automated Analysis Resonance is detected in a complex manne
154. urier Transform NMR experiments such as in the Qualion NMR Process Analyzer the duration of the pulse is selected so that the magnetization vector rotates by 90 as shown in Figure 3 Bo Bo Mp PULSE Figure 3 Rotation of Magnetization Vector with 90 Pulse Applied The detector is aligned along the axis If we return to a static frame of reference rather than the rotating reference the net magnetic moment spins around the y axis at the Larmor frequency This motion generates an RF signal that can be detected When the pulse is removed the nuclei relax and return to their equilibrium positions and the signal decays The decaying signal contains the sum of the frequencies of all the target nuclei Since the frequency of the signal is too high to be recorded directly it is mixed with a lower frequency signal to produce a low frequency interferogram The interferogram called the Free Induction Decay FID is then Fast Fourier transformed into a frequency domain spectrum for analysis System Operation UM SW50407 05 9 System Overview Measurement Principle SPIN PACKETS A spin packet is defined as a group of spins with the same magnetic field strength At any instant the magnetic field of the spin packet can be represented by a magnetization vector M the magnitude of which is proportional to the population difference between low energy and high energy spins The vector sum of all spin packets is called net magnetiza
155. version SCREEN TOOLS Right clicking anywhere within the window displays a menu as shown in Figure 59 This menu lets you select the pan and zoom functions for the display Set App Mame Pan ZOOM A w nnm Y zoom Zoom All Figure 62 Right Click Menu The display commands Pan Select this option to change the location of the display using the mouse Zoom X Select this option to zoom the display in the X direction only Use the mouse to select the range to be zoomed Zoom Y Select this option to zoom the display in the Y direction only Use the mouse to select the range to be zoomed Zoom XY Select this option to zoom the display in both X and Y directions Use the mouse to select the ranges to be zoomed Zoom All Select this option to reset the zoom to the original settings System Operation UM SW50407 05 82 Windows and Dialog Boxes Automated Analysis Automated Analysis Click on the Auto A button to display the screen in Figure 60 Note that when you select a function you also have to enter parameters in some of the table cells The entries you make are stored in a pp file post processing To determine what types of data you should enter in each cell place the cursor over each cell in the row in sequence and wait for a pop up caption to appear This tells you what parameter you should enter in that cell Typical examples of pop up captions are shown in Figure 61 and Figure 62
156. which data samples are to be acquired This total number of points divided by this value points millisecond gives the total acquisition time in milliseconds Total acquisition time is a function of the NMR characteristic of the material being analyzed Resolution resolution is the fineness of the data the greater the number of points the finer the resolution The dialog box displays the current value of resolution before zero filling Samples Increasing to this is the new total number of points in the acquisition after adding the zero values data points New Resolution this is the new resolution after zero filling is performed Apply Button click this button to execute zero filling with the parameters you entered FFT This function applies a Fast Fourier Transform to the FID data converting it to a frequency domain spectrum FID Display with RMS and Frequency Shift the figure below shows the time domain data display FID before it is converted to a frequency spectrum by means of an System Operation UM SW50407 05 100 Windows and Dialog Boxes Automated Analysis NMR Analysis Running On Local Machine TEIL Figure 83 FID Display with RMS and Frequency Shift Values Absorption Display with RMS and Frequency Shift After FFT Conversion Figure 81 shows the result of an FFT conversion Note that the shape of the spectrum indicates the
157. window Add Button active only when software lock is on clicking this button increases the main transmitter frequency by the amount displayed Sub Button active only when software lock is on clicking this button decreases the main transmitter frequency by the amount displayed Shim Shimming is the process of adjusting the currents to 40 pairs of shim coils so as to modify the strength of the magnet field at precise points within the field Its purpose is to compensate for any irregularities in field uniformity caused by characteristics of the magnet hardware or the chemical physical properties of the sample being analyzed When the shimming process is completed the resultant values can be saved to a file as a shimset This file can be recalled later whenever a new sample of a similar type is to be analyzed Shim Gradients E E x Set Method Gradients Log File Start Shimming Stop Shimming Gz TA Gxexxfi0 61 29 Gzz 4 GzXx gag Gxxyz n 26 Gzzz 069 Gzxx 225 Gxyyz 5 09 Gzzzz 5 23 Gezxxx 82 D EE 1 2 Gx 34 1 Gpp 3 58 GEX Gyy 2 18 Gzpp 0 64 GXXX 2 35 Gyyy Gadd 0 0 Best Result Best Grad 0 5 Spectra 10 Spectra 40 Spectra Em Emergency Result of Spectral Analysis Power Switch QUALIOH Ltd Copyright 2007 Figure 77 Shim Gradient Screen Shim Gradient Display Figure 74 shows the current values of the variou

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