scarx400.doc –
Using the
ARX400 Sample Changer
I. Sample
Preparation:
A. You must use a deuterated solvent.
B. Label your sample with a Sharpie pen using a unique name (not "A" or "1"). Do not use tape or tags.
C. Make sure the NMR tube is ³ 16 cm. (below the cap) and that the column of liquid in the tube is ³ 4 cm.
D. Make sure the NMR tube is clean on the outside.
II. In
the NMR lab (Room 1421
A. If you have a heart pacemaker, do not enter the NMR lab! (See NMR lab personnel.) Do not take metal items (e.g. spatulas) into the area near the magnets. If you do not wish to demagnetize your credit cards or to magnetize your mechanical watch, also do not take them near the magnets.
B. Insert your sample into a spinner and make sure that it is a snug fit. Set the depth with the aluminum depth gauge labeled "Maximum Depth". (If the column of liquid is less than 4 cm long, be sure to center it around the center of the receiver coil using the depth gauge with the graduated scale.) Wipe the outside of the sample with a Kimwipe. Place the used Kimwipe in the trash!!
C. Place your sample in the sample changer rack in the position where the dummy sample sits. Move the dummy sample to the next rack position after your sample(s). Note the number(s) of the rack position(s) of your sample(s). This is probably the holder number that you will use. The smaller numbers correspond to the inner row.
D. Select the button on the lower right labeled "Change User"
E. Type in schanger (or your NMR User name) as the User ID. (Be sure to hit "Enter" on the keyboard. If you use the mouse to select OK, it will ignore what you have typed and select the highlighted user.)
F. Double-click the number that corresponds to your sample. (Check that the user name at the right edge is correct. If not, move your sample to the next higher holder number that has no user name already and continue with this new number.) You will need to select a solvent and an experiment, and input a title.
1) To input the title, select the icon that looks like a pencil. At the top of the title area, you must input your Account no. or the sample will not run. In the box below the Account no. box, you may input a title that will appear on the plot.
2) All parameter files contain 8 scans. If you would like to change the number of scans, select Parameters on the menu bar. Move the mouse down and select User Specific Parameters/ Commands. You will find ns, i.e. number of scans. Use multiples of 8. (Notice that there are other parameters in the list that you can change.)
3) If you would like to add another experiment to this sample setup, select Add. (The "wheel" to the right of the Add button indicates how many experiments will be added. Make sure it is set properly before you select Add.) You will then only need to select an experiment. You can change the title of the additional experiments if you want.
G. Once all the required information for the sample has been input, select the line with the sample holder number. Then select the “button” on the lower left labeled Submit. The sample will not run if it has not been submitted!
1) If the sample has not started running, you can make changes in the setup. Select the experiment to be changed. If only parameters are to be changed, do so as described above for changing ns.
2) To change to a different solvent or experiment, select Cancel, then Edit. After making all the required changes, again select Submit.
H. After you have finished the setup and submission for your sample(s), select the button on the lower right labeled "Change User". (This will assure that the next user does not accidentally set up spectra in your directory.)
I. A plot of your spectra will come out on the printer next to the spectrometer workstation.
1) If a proton spectrum has peaks downfield from 9.4 ppm, these peaks will be plotted on a 2nd page. Be sure to check the printer for possible 2nd pages for proton spectra.
2) If your spectrum contains only the solvent peaks, you will obtain a blank spectrum. Consider making your sample more concentrated. If this is not a possibility, run the spectrum on a different spectrometer.
III. To Reprocess Data Remotely (for users who have
completed the Processing check-out):
A. If you set up the data using your User name, then the data will be in your directory as usual.
B. If you set up the data using the schanger user name, you can use the guest account for data transfer or data processing. DO NOT PROCESS DATA USING THE SCHANGER ACCOUNT!!!
1) Processing with Topspin:
a) In WS-FTP, log on as guest. Then transfer to the appropriate directory.
2) Processing with Xwinnmr:
a) Telnet to nmr400a and log on using guest.
b) Type search. Select the schanger user name. Select the data set that you want to put into the guest directory. Select append, then apply. You will then be displaying your data set but you will not be able to do any processing because you don't own it.
c) To copy it to the guest directory where you will own it, type wrd. You must enter guest as USER. To switch to the copy that you just made, type new and input all the same information as used with wrd. You will then be able to process the data as usual.
IV. Stopping
and Starting a Sample Changer Run for users authorized for manual Acquisition
on the ARX400 – All others should not stop the run unless troubleshooting is required.:
A. Stopping:
1) When the last sample is finished or when the time allocated for the sample changer is up, type in schanger as the user name, then press “Enter” on the keyboard.
2) Select the red STOP button, then select YES.
File STOP
ß ß
GO Þ
3) On the green background menu bar, select:
File ® Exit ® Yes
4) On the remaining green background menu bar, select:
File ® Logout ® Yes ® Yes
5) The system will be left with no sample in the magnet. Please put the dummy sample in, turn on the spinner, and turn off the Autoshim.
6) Select “Log-off someone else” in LinRL to log off the current user.
B. Starting a Sample Changer run:
1) Either from the unix window that comes up when you log onto the computer or from xwinnmr, type iconnmr. From iconnmr, select Automation.
2) Proceed as above to input sample information.
3) Select the green GO button.