269 Kb PDF file
Contents
1. DIASPEC Low field NMR system Diameter 42 18 mm DIALOG V2 4 User Manual ARTEC SYSTEM SARL au capital de 95 000 euros Si ge social 45 Avenue Rhin Danube 07100 Annonay France Tel 33 0 4 75 69 22 11 Fax 33 0 4 75 69 22 19 Mail info artec system com RCS Annonay 505 395 293 Banque Soci t G n rale Annonay 30003 02161 00020419085 20 ARTEC SYSTEM NMR Devices for Industrial Applications TABLE OF CONTENTS 1 DIASPEC CCONNECTIVIT loo 3 2 DIALOG SOFTWARE HUMAN MACHINE INTERFACE sise 4 ESA QUACK AA ne Mi ddr seed etes Madame ht sue este ler E net eee 4 22 Stand rd MODE 2d tn oa 6 2 3 EXpert Modes A cid 7 22 4 NeW sequence PrOBTOMMIAS adn pd 8 ARO UE Ei ta 10 a20 Exponential processing lt a Ra ee 11 1627 De CONVOLUTION PrOCeSS ME vrs Ent irene ardiente ant oie itin rante 12 220 S4ve0nd Exporcthe resuli ii tte 13 12219 Operator M Ode core EEA E tas 14 821 OPOPO SIV Mode ns es entend Res aug tae ae tse nn nn nn det St Retna ete aes 16 ERAN OLOS sent tas 18 3 OVERVIEW OF THE EQUIPMENT esse lens Pine tres ere teen E EEEE SESIO ES TEREE EEES OS 19 ARTEC SYSTEM NMR Devices for Industrial Applications 1 DIASPEC CONNECTIVITY Connect the 50 Ohm coaxial cable from the probe to the rear panel of the electronic rack Plug the USB cable from the rear panel of the rack to a USB port of the computer Turn on the power supply of the electronic rack with the rear panel switch and then turn on2. Dead time after a P90 impulse Avoids the recording of the LNA saturation phase Number of scan nScan Number of repetitions scan of the NMR sequence The recordings are accumulated and divided by the number of scans nScan enables to improve the signal to noise ratio Recommended values multiple of 4 with phase seg2 Be careful a high value of both nScan and nEch tends to heat the sample and degrade the signal Number of echoes nEch Number of stimulated echoes that defines the number of measured points of the signal For pure water measurement a small number of echoes is needed 50 In order to obtain the relaxation time constants of the samples increase nEch to obtain a curve that tends to zero Be careful a high value of both nScan and nEch tends to heat the sample and degrade the signal Repeat Delay RD ms Waiting time between two scans This time must be at least five time the dominant relaxation time of the sample For short RD times the residual magnetization is accumulated and degrades the signal Tau us Time between P90 and P180 impulses The CPMG echo appears Tau microseconds after the P180 Impulse Phase Phase type Recommended value SEQ2 ARTEC SYSTEM NMR Devices for Industrial Applications 2 5 Results This tab displays the results of the measurement The computed points correspond to the maximum of each echo within the same method Magnitude Rephased Noise The curve can be redraw
3. M values of the magnetization relaxation The magnitude is obtained with the following method M sqrt M M2 The CPMG curve s points correspond to the maximum of each stimulated echo Exponential The Exponential curve data can be exported the first column corresponds to the time t and the second one to the signal Mi Deconvolution the first column corresponds to the magnitude A and the second one to the associated Ti 13 ARTEC SYSTEM NMR Devices for Industrial Applications 2 9 Operator Mode In this mode the operator is able to use every sequences created by the expert and calibrate the device and test samples with them The mode compute the quantity of water contained in the samples File Processing Filtering Amplitude Options Operator mode Dperator mode Operator name Calibration Measure Options Sample weight mg D Sample 1 C Sample 2 Sample 3 _ r Calibration File name Reso N Water quantity Mass of Water mg Dried Material Save First of all the user should configure this mode by clicking the ou icon C Appareils DIASPEC 18 18001 Essai Mesure SGN Ghis 1 aa y Select measurement sequence sample type 1 CAppareisWDIASPEC 18 18001 Essai Mesure SGN Ghis 1f Select rm Select measurement sequence sample type 2 jc Appareils DIASPEC 1811800 1WEssai Mesure SGN Ghis 1 sxa r Select measurement sequence sample type 3 CMAppareilsDI
4. exponentials is used in the Exponential routine The amplitude value allows the Expert to modify the signal computation methods Magnitude Rephased Noise It also allows change in the deconvolution parameters the computation windows and the smoothing Be careful when changing these parameters ARTEC SYSTEM NMR Devices for Industrial Applications 2 4 New sequence programming A new NMR sequence can be defined in the File gt New sequence menu A sequence can also be modified with the View button on the Calibration or Measurement panels The parameters can be modified according to the Expert or Standard modes limitations Advanced parameters Standard parameters ses Number of scan nScan 32 P180 Number of echoes nE ch Ie Repeat Delay RD i000 ms TACOSO si FID 480 en 100 a Gain Rg Freq Pulse DW Dead time DT Phase Sequence type Cancel The parameters used to create a NMR sequence are the following P90 Hs Duration of the impulse P90 P180 us Duration of the impulse P180 P180 duration is close to 2 P90 TACQ180 Hs Duration of the acquisition centred on the Echo CPMG A small value increases the USB communication stability TACQ90 Hs Duration of the acquisition of the magnetization relaxation after a P90 pulse FID Gain RG Not used Freq Pulse MHz Frequency of the pulse P90 and P180 ARTEC SYSTEM NMR Devices for Industrial Applications Dead time DT us
5. ASPEC 1811800 1WEssai Mesure SGN Ghis 1 Select Masse of calibration sample mg 1000 OK Cancel The user is allowed to choose 1 calibration sequence and 3 measurement sequences Do not forget to enter the mass of the aqueous calibration sample 14 ARTEC SYSTEM NMR Devices for Industrial Applications Insert a calibration sample in the probe and on the main panel click Calibrate After inserting the user name the sample weight and clicking Save a new calibration file is created in the Etalon folder date time eta Insert a sample in the probe and click Measure After inserting the user name the sample weight and clicking Save the results are saved in a CSV file in the Mesure Folder resultat date op This file contains all the measurement realised by the operators 15 ARTEC SYSTEM NMR Devices for Industrial Applications 2 10 Porosity Mode In this mode the operator is able to use every sequences created by the expert and calibrate the device and test samples with them The mode compute the quantity of water contained in the samples and the porosity File Processing Filtering Amplitude Options Porosity TELS Date Time Dperator name Calibration Measure Options CT Sample weight mg 0 r Calibration File name o Result Water percentage Mass of water Porosity 2 Grain density 24 Save Deconvolution First of all the u
6. ault parameters file View C Users artec Desktop LogicielClient_v2 2 E talon zeryhe Select r Information Measurement description Sample reference Date 17 08 2012 Measurement number 1 Cancel OK Choose ok Dialog software checks some information and shows the remaining time At the end of the measurement click OK ARTEC SYSTEM NMR Devices for Industrial Applications The result appears File Processing Filtering Amplitude Options Result Exponential Deconvolution r Information Sample reference N measure Description Calibration etalonnage_irta eta Sequence zeryhqsdpuifgogsdiuthploutch s Date Time 17 08 2012 15 49 34 Number of echoes to remove n 9 In the processing menu choose Exponential The software computes the water percentage referring to the calibration sample volume File Processing Filtering Amplitude Options Result Exponential Deconvolution r Exponential Number of exponential 1 Lio ai Legend 4322 129 a ES an Water percentage 6 23 Quantity of water mg The Exponential routine computes the water percentage through the evaluation of the main time constants Ti us and magnitudes Ai M 0 2 A exp t T LA is the magnitude of the signal used to compute the water content of the sample ARTEC SYSTEM NMR Devices for Industrial Applications 2 2 Standard mode In this mode the user can cr
7. cations 2 7 Deconvolution processing The deconvolution processing computes a Laplace inversion through the computation of the relaxation time distributions of the measured signal This method computes A parameters such as So NB gt gt AT ZE M t is the magnetization relaxation and A et Tj are respectively the magnitude and time constant computed for each T regularly spaced in the window defined in the advanced options panel Default is 0 1 1000 ms For a better computation be careful that the measured signal tends to zero The user should choose appropriate Tau and nEch The deconvolution method allows the expert to compute the relaxation times of the sample and then to choose the correct RD If T is the maximum relaxation time RD 5 Tog 12 ARTEC SYSTEM NMR Devices for Industrial Applications 2 8 Save and Export the results The files are defined with the following extensions e Sequence file seq e Measurement file mes e Calibration file eta A measurement can be stored using the Save as Menu Before each new measurement it is suggested to the user to save the current measurement A measurement can be imported with the Open menu It is also possible to save the measurement into an ASCII format Several data export modes may be used with data analysis softwares Raw data Export the values of the FPGA These values are the result of a quadrature detector module that returns real M et imag
8. eate NMR sequences calibration samples and measurements with some limitations The main parameters are fixed save for the following at the creation of a new sequence or the modification of a selected one with the View icon Calibration Default calibration file C Users artec Desktop LogicielClient_v2 2 Etalon etalon Calibration sample weight 0 mg Measurement sequence parameters Default parameters file IC Users artec Desktop LogicielClient_v2 2 Etalon zeryhe roo Standard parameters P90 P180 i Number of echoes nEch i Information TACQ180 Repeat Delay RD Measurement description TACQ90 siFID 480 Tau Number of scan nScan Sample reference Gain Ag Date Freq Pulse DW Dead time DT Phase Measurement number Sequence type e tau is the time between a pulse and an echo measurement M t e RD is the waiting time between two sequences Repeat Delay e nEch is the number of echos stimulated or the number of measurement points M t e nScan is the number of scans used to improve the signal to noise ratio Some optional information can be associated to the measurement Measurement description Comments that describe the sample of the measurement For each measurement on the sample the reference is automatically set through the Sample reference and the Measurement number increased Number of echoes to remove main menu Allows to remove the very first p
9. n an average diameter of 18 mm and a height of 20 mm Bo induction 0 44 T dBo Bo homogeneity 10 The DIASPEC 42 measurement volume is considered as a cylinder with an axe parallel to BO static induction an average diameter of 40 mm and a height of 40 mm Bo induction 0 24 T dBo Bo homogeneity 10 19 ARTEC SYSTEM NMR Devices for Industrial Applications Structure geometry e Measurement tube external diameters 18 mm 40mm e Radial resolution diameters 18 mm 40mm e Vertical axial resolutions 20 mm 40mm The outer metallic enclosure of the probe is covered with an anti corrosion coating a Spectrometer and probe b Top view of the probe c Replaceable antenna 20 ARTEC SYSTEM NMR Devices for Industrial Applications System 21
10. n with another method choosing the Amplitude icon The following information are also reported e Measurement time and date e Description e Sample reference and number of measurements for this reference rr DIALOG File Processing Filtering Amplitude Options Result Exponential Deconvolution Information Sample reference N measure C CHE Description Calibration etalonnage_irta eta Sequence zeryhasdpuifgogsdiufhploutch s Date Time 17 08 2012 15 49 34 Number of echoes to remove n 9 10 ARTEC SYSTEM NMR Devices for Industrial Applications 2 6 Exponential processing After a measurement acquisition this processing can be used from the Processing menu After some computations the display of the results appears into the second tab Exponential It allows the visualisation of the computed curve with Levenberg Marquardt method Measured points are also displayed for comparison The measured signal M t is analysed with 1 2 or 3 exponentials within the default choice declared in the advanced options panel M t A exp t T A2 exp t T2 Az exp t T3 The magnitude of the signal S t 0 can be computed with S t 0 A Ao A3 The water percentage contained in the sample is defined as the ratio between the magnitude of the sample signal and the magnitude of the calibration sample signal water A1 A2 Az Acalibration ARTEC SYSTEM NMR Devices for Industrial Appli
11. oints of the curve Used to improve Exponential and Deconvolution methods Date Time BESS 17 08 2012 15 49 34 16 00 20 00 Number of echoes to remove n 9 X ARTEC SYSTEM NMR Devices for Industrial Applications 2 3 Expert mode In this mode the expert is able to access every sequences and options parameters To enable this mode choose Option icon and then Expert mode in the main window Enter the Password Expert mode allows the user to modify the default parameters the default calibration file the default sequence file every sequence s parameters Default configuration of the whole Software In the main window click Options icon and then Advanced Options Change default calibration file CAUserstarteciDesktopiLogicielClient_v2 2 Etalontetalonna Select Change default sequence file c Users artec Desktop LogicielClient_v2 2 Etalon zeryhgsd Select Set number of exponential for processing 1 Default filter No Filter y Amplitude value by default Magnitude Number of points to delete by default Dummy scans n 9 y Weight of calibration sample by default 0 mg Number of points for echo processing 1 NMR equipement C Diamat Diaspec 18 C Diaspec 42 Deconvolution option Time interval Tmin ms 0 1 Tmax ms 1000 Smoothing 0 3 Change password Cancel In this window the Expert user may change the default parameters for the non expert users The number of
12. ser should configure this mode by clicking the Options icon Select calibration sequence 1 C Documents and Settings Mathieu Rousseau Mes documer Select r Select measurement sequence C Documents and Settings Mathieu Rousseau Mes docume Select Default grain density 24 Default saturing liquid density fi Mass of calibration sample mg 2000 Number of points for calculating the amount of water 20 Cancel The user is allowed to choose 1 calibration sequence and 1 measurement sequences Do not forget to enter the mass of the aqueous calibration sample the default grain density of the sample the density of the saturing liquid The number of points for calculating the amount of water is used to improve the Exponential method 16 ARTEC SYSTEM NMR Devices for Industrial Applications Insert a calibration sample in the probe and on the main panel click Calibrate After inserting the user name the sample weight and clicking Save a new calibration file is created in the Etalon folder date time eta Insert a sample in the probe and click Measure After inserting the user name the sample weight and clicking Save the results are saved in a CSV file in the Mesure Folder resultat date por This file contains all the measurement realised by the operators 17 ARTEC SYSTEM NMR Devices for Industrial Applications 2 11 Notes The Signal to Noise ratio quality of signal can be impro
13. the power supplies of the electronic cards with the front panel switch Turn on the computer If Windows detects a new device the USB port used is different from the one used during the manufacturing tests Follow the Windows standard instructions to install DIASPEC During this procedure you may indicate the driver path C Program Files Dialog Driver The USB port is now configured WARNING WHEN THE FRONT PANEL SWITCH IS OFF THE POWER AMPLIFIER IS STILL POWERED ON THE REMOVING OF POWER SUPPLIES CAUSES CAPACITANCES DICHARGING THAT LASTS FEW HOURS DO NOT OPEN THE ELECTRONICAL RACK ARTEC SYSTEM NMR Devices for Industrial Applications 2 DIALOG SOFTWARE HUMAN MACHINE INTERFACE 2 1 Quick start Insert a sample into the probe Start DIALOG software by double clicking the Dialog Icon on the Desktop linked to C Program Files Dialog Dialog exe The following window should appear File Processing Filtering Amplitude Options Result Exponential Deconvolution r Information Sample reference N measure 0 Description Calibration Sequence Date Number of echoes to remove n 9 In the File Menu click new Upon delivery the system is already configured A default folder contains default calibration and sequence files Calibration Default calibration file C Users artec Desktop LogicielClient_v2 2 Etalon etalon Calibration sample weight 0 mg Measurement sequence parameters Def
14. ved by accumulating several sequences nScans However the increase of the sequence number makes the measurement time increase The following calculus approximates the simulation time Measurement time nScan nEch 2 tau RD The relaxation time of free water is 2700 ms and requires a RD value of 15s lt is recommended to perform a calibration with a 2 g L CuSO4 aqueous solution This will shorten the relaxation time to about 100 ms and thus the measurement time RD 1s is sufficient This way the conditions are as close as possible to common conditions Glass containers are recommended If none is available the container chosen should be made out of insulating and non magnetic material Plastics are usually suitable but they may generate parasitic signal mostly with short relaxation times under 1 ms Be careful to test the empty container before inserting the sample 18 ARTEC SYSTEM NMR Devices for Industrial Applications 3 OVERVIEW OF THE EQUIPMENT The general structure of the NMR Sequencer is pictured in the figure below Power Amplifier Mother board AE Decoupling LNA and quadrature detector gt High power signals Low power signals gt Digital signals Probe static induction The probe magnets are made of NdFeB which shows good thermal stability up to 80 C The DIASPEC 18 measurement volume is considered as a cylinder with an axe parallel to BO static inductio
Download Pdf Manuals
Related Search