Characterization of Fluids Confined in Porous Materials by NMR
Contents
1. M FYS KJM 4740 2015 Labkurs Praktisk NMR 2015 doc Preliminary experiments in FYS KJM4740 Obective Elucidation of some basic NMR concepts by practical NMR The present NMR tutorial room V170 in the Department of Chemistry is an offer to students who want to learn some of the NMR concepts by a practical approach The experimental results will be available on the home page of the course during January All students must write up a short report based on the experimental findings Exercise 1 a b c d Experiments on water confined between glass beads Practical Insert the sample in correct position Acquisition mode Sequence Load FID Parameters VT 30C DW 0 5 RD 3s NS 4 RG 10 SI 1K P90 1 95 The tg rf pulse duration is varied Start experiment GO Set tp 0 5 1 0 1 5 2 00 2 50 3 0 3 50 4 00 4 50 and 5 00 us and determine the initial signal intensity I of the FID vs tp What is the strength B gauss of the rf field Discuss your results Acquire an FID real imaginary for different rf frequency offsets O1 Plot the FID for different O1 and discuss your results with respect to the rotating frame of reference Set RD 3s VT 30C DW 0 5 SI 1K P90 1 95 NS 4 RG 10 O1 is varied Fit a single exponential function and a Gaussian function to the on resonance FID with tp 1 95 us Discuss your results Acquire an FID for different repetition delays trp 3s 2s 1s and 0 5s Plot t2. XE 3 Set RD to 5T1 i e RD 1 0s P90 2 15 us VT 30 C and RG 1 DW 0 1 SI 4K Optimizing relevant parameters 4 Command Auto O1 wait 5 Command Auto RG wait Use this value of RG throughout if not otherwise stated in the text 6 Command Auto P90 wait T measurement 7 Insert the sample in correct position 8 Acquisition mode Sequence Load INVREC 9 Set RD 1s RG 1 VT 30 and NS 4 DW 0 1s SI 4K 10 Write T1 T1 4740 open OK gt write a file name 11 A T1 plot will appear on the screen when the experiment is finished Make a screen dump Press Print Scrn and paste the image into Paint You will use the value of T in the report T2 measurement 12 Insert the sample in correct position 13 Acquisition mode Sequence Load CPMGF 14 Set RD 1s RG 1 VT 30 and P90 2 15 us tau 100 us NECH 4K 15 Write GO 16 Store File 17 Write T2 A plot will appear on the screen Make a screen dump Press Print Scrn and paste the image into Paint You will use the value of T2 in the report Miscellaneous Calculations using the NMR program WinFit 18 Open WinFit C ProgramFiles Resonance WinFit nmrfit double click 19 Retrieve a file File Open Select file data Select Fit Options number of exponents DC offset if possible Auto Initialize Fit Data Read out values or print i e File Prin
3. he initial signal intensity I 0 of the FID as a function of trp and discuss your results Set DW 2 SI 1K VT 30C P90 1 95 NS 4 RG 10 on resonance vary tgp Exercise 2 Inversion Recovery experiments on a series of CuSO4 solutions Concentrations 20mM 10mM 5mM 2 5mM 1 25mM and 0mM Practical Insert the sample in correct position Acquisition mode Sequence Load INVREC Set RD 1s RG 1 VT 30 NS 4 DW 0 1s SI 4K Write T1 T1 4740 open OK gt write a file name A T1 plot will appear on the screen when the experiment is finished Plot T1 vs CuSO4 concentration and discuss your results Exercise 3 CPMG experiments on a series of CuSO4 solutions Concentrations 20mM 10mM 5mM 2 5mM 1 25mM and 0mM Practical Acquisition mode Sequence Load CPMGF Set NS 4 RD 1s RG 1 5 VT 30 P90 2 0 us TAU 100 us NECH 4K Start GO When finished Write T2 A plot will appear on the screen Make a screen dump Press Print Scrn and paste the image into Paint You will use the value of Tz in the report Plot T2 vs CuSO4 concentration and discuss your results Write a report on your experimental work include relevant Figures Eddy W Hansen UiO January 2015 Practical NMR A Simplified User Manual for the Maran Ultra NMR Instrument Non expert User Initiate experiment 1 Insert a sample in correct position 2 Acquisition mode sequence load FID E
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