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13.10 Acquiring Stop-Flow LC-NMR Data Using Enter the autoaa macro. (The autoaa macro is equivalent to autosa aa and is currently required to completely abort an automation run.) Note that autoaa generates an (inconsequential) error in the Status window for the last experiment. Stop-flow data files can be transferred to the NMR after the LC run is completed. 13. Transfer the stop-flow data can be to the Sun after the LC-NMR 2000 run is finished. a. Go to the communications window. b. Click on the radio button to Upload .lcdfiles from disk. c. Click on Browse to find the .lcd file. Click on Upload. The display window will monitor the progress of the file transfer, see Figure 119. Experiments started using either lcgo or by pushing the Start LC RUN Button start the lclisten routine. The lclisten routine will look for a .lcd file to be written in /vnmr/tmp and then start a UNIX process that converts this file to a UNIX text file. This UNIX text file is placed in the current experiment as LC data. The NMR data and LC data are then automatically processed and displayed. 14. To review the data, enter the status command in VNMR. The files, which are stored in the ScoutDirectory , can be read back into the current experiment and reprocessed automatically by clicking the Retrieve Data button in the Status window. At that point, processing parameters can be altered and the data set reprocessed by clicking he Process LC-NMR button (wftlc), or the data set can be reprocessed without altering the processing parameters by clicking the Process button (wft). Note that two files are created for each slice. The first files (0#01.fid) arise from the Scout Scan run (nt=1) while the second files (0#02.fid) are the proper signal-averaged data. 13.10 Acquiring Stop-Flow LC-NMR Data Using Enter Stop-flow experiments can be used with the ENTER program to allow the user to perform different NMR experiments on each sample stopped in a flow probe. Also the selection for each sample in the queue may be different. Stop-flow experiments with ENTER are especially useful for setting up NMR experiments on samples stored in the Analyte Collector. How Custom Stop-flow Works with ENTER This mode uses the enter program that is modified for LC-NMR to input information about each experiment to be performed. One difference is that the Sample# does not refer to a sample in a sample changer, but rather to the peak number in the stop-flow run, or to the loop number in the loop-flushing mode. In this case, you currently need to use sequential (and continuous) numbers, although the defined experiment can be made quite short (nt=1; however, the program acquires data on each Sample #). The Save And Exit button in enter is used to write the experiment queue out to a file (e.g., lcqueue). The queue of sample peaks (or loops) just represents another sample changer, with special macros to ensure that the parameters involved in running the Scout Scan and then setting up solvent suppression are properly handled. Global parameters autodir and autoname as well as the local parameter savefile, are used to keep track of the run; all these parameters are created automatically. In addition to the normal automation parameters, in LC runs, the parameters ntrig and dtrig are also created to specify the 01-999161-00 B0801 VNMR 6.1C User Guide: Liquids NMR 429
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