Features Diagram Attentions Experimental Types
Experimental Steps Exchange Probes Turn off and on Spectrometer
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Ultra-stabilized magnet of 14.1-Tesla magnetic field strength. The proton frequency is 600 MHz. The temperature of liquid helium in the magnet is 4.2 K. |
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Three radio frequency channels with 2H decoupling of 20 Watts. The powers of 1H and two broadband channels are 50, 300 and 300 Watts, respectively. |
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35 Gauss/cm xyz-axis pulsed field gradient (PFG). |
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Two probes: |
TXI: three-channel inverse probe (1H/13C/15N)
QXI: four-channel inverse probe (1H/13C/15N/31P)
1. NMR spectrometer is very expensive, please run experiments as efficiently as possible.
2. Once you hear the sound (the sound of air flow) from magnet after you press the LIFT ON/OFF button on BSMS keyboard, you can insert spinner with your sample into magnet, otherwise you may break probe.
3. 120dB of power level corresponds to zero output of radio frequency power. -6dB of power level corresponds to maximum output. In order to protect probe, please don’t set the power level to a value less than specified values. You should be very careful when you change pulse widths and power levels.
4. When you manually tune and match probe, you should be very careful and don’t turn screw fast, otherwise you may break probe.
5. Please fill in log book.
6. You can always get help from the manager.
TXI Probe (1H/13C/15N with 2H-decoupling):
All multi-dimensional 1H or 13C-detected multiple-resonance NMR Experiments
QXI Probe (1H/13C/15N/31P with 2H-decoupling):
Besides the experiments being performed with TXI probe, NMR experiments related to 31P can be performed.
1.Type in login and enter your password to login the computer.
2.To enter the NMR software, click XWIN-NMR 3.0 icon on desktop.
3.To get a data set similar to your experiment, click File button, click search button, select a data set, and finally click Append button and Apply button.
4.To change the name, expno and user of the current data set, type in edc command. In dialog, change the name, expno and user. Finally click the save button.
5.Insert your sample tube into spinner and adjust the position of the sample tube in the spinner with gauge.
6.Press LIFT ON/OFF button on BSMS keyboard, once you hear the sound (the sound of air flow) from magnet, you can insert the spinner with your sample into magnet. Then press LIFT ON/OFF button again. If your experiment takes long time, please place the cap on the upmouth of magnet.
7.Type in edte command to change the temperature of your sample. After the temperature is stable, you can perform the following steps.
8.Type in A command to switch to acquisition window. Type in atma command to automatically tune and match the probe.
9.Do manually shimming to get lock signal as high as possible. Then type in gradshim command to shim automatically.
10. Type in edprosol to set proper probe. Type in gpro command to get standard values of power levels and pulse widths.
11. To calibrate parameters, such as p1, type in paropt command and input proper initial value, increment and number of steps.
12. Type in zg command to start acquisition.
13. Type in efp command to process your data and get your spectrum.
14. To plot your spectrum, type in edg command, and modify related parameters. Type in view command to preview your plot, then type in plot command to print out your spectrum.
I. Taking out a probe (TXIxyz)
1. In XWIN-NMR, type in edte command, click turn off button in edte dialog.
2. Disconnect the cold gas tube from probe.
3. Disconnect all cables from probe.
4. Alternatively loosen two screws under probe. Slowly lower down probe and finally place it into a hard paper box.
II. Installing a probe (TBI-BB)
1. Slowly insert TBI-BB probe and alternatively fasten two screws under probe.
2. Connect all cables. If nucleus P-31 is detected, take away the filter for 13C between pre-amplifier and probe.
3. Connect cold gas tube to probe. Exchange heater lines before console and close the console door.
4. In WIN-NMR, type in edte command and click turn on button in the edte dialog.
5. Type in edhead command. In edhead dialog, choose TBI probe, click defines as current probe button, and finally click Exit button.
6. Type in edprosol command, confirm the pulse widths and power levels were all changed to fit the TBI probe.
7. Type ii (initialize interface) a few times.
8. Type in rsh command and choose appropriate shimming file.
I. Turn off spectrometer
1. Type in edte command, click off button in edte dialog.
2. Turn off BCU05.
3. Kill all jobs in XWIN-NMR.
4. Exit XWIN-NMR and close all windows.
5. Turn off two power amplifiers. Finally press the red button on front of console.
6. Click start button on computer, select shut down computer.
II. Turn on spectrometer
1. Turn on computer and login.
2. Press the green button on front of console. Fingers touch console frame a few times to discharge, then turn on the two power amplifiers.
3. Click XWIN-NMR 3.0 icon on computer to start NMR software. Type in ii command a few times to initialize interface.
4. Turn on BCU05.
5. Type in edte command to change temperature.