Varian UnityInova 300 NMR User GuideVarian UnityInova 300 NMR User Guide

A UserGuide for the INOVA 300

Temple Chemistry Department

NMR Facility

July 2009

Rev 2.2 10 July 2009

Some Computer Information

Finding the Inova 300 over the Network….. Network Name of the computernmr300.chem.temple.edu login IDtemple Password for templechem300 data pathway/home/temple/vnmrsys/data/…

This password is also to be used if the screen saver has locked you out at the console.

In this manual, the LMB instruction means click the leftmost of the three mouse buttons. RMB means click the rightmost mouse button.

“<rtn>” means press the return or enter key. Don’t type the letters or the brackets or the quotes.

Getting Started

  

• There will be a chloroform standard in the magnet when you start

• Put the mouse in the command window, type “e <rtn>” .”<rtn>” means carriage return or enter. Don’t type the quotation marks)

• Remove the existing CDCl3

sample, and exchange your sample for the chloroform in the spinner collar.

• Position your tube using the depth gauge marked “300”, wipe with kimwipe

• Put your sample into the top of the magnet bore

• With the mouse in the command window, type “i <rtn>” Your sample will lower into the magnet

If the blue prompter in the command line is not solid, click into the command line with the LMB (left mouse button)

Next, on the command line, type:

shimnow<rtn>

shimnow

Now you select the automated protocol to be used…

Mouse to the side bar buttons and left Click (LMB) on the button labeled “CustomQ”

Next Make the Choices for your experiment

First select the deuterated solvent for locking. This button lets you drag down to the solvent choice.

Next, mouse to the center block of buttons. These are labeled e.g. “H1only”LMB click the proper choice

Some of the other buttons give choices for linked, successive experiments, such as proton followed by COSY. Experiments are done in the order selected. Be sure to note the time requirements, before starting.

Now the File-naming Dialog Box Appears

Now many actions flash across the screen. When it stops, you will see a dialog box.

Typically you will leave the default choices about locking, plotting and shimming engaged, as shown here.

LMB click in the “Save As” field, and at the insertion point, type your user name (which you will be given, use this consistently) then type “/” and then an appropriate filename. Make this systematic, so it will make sense later. Your notebook code is a useful convention. In this field, do not use spaces, asterisks, tildes, or other slashes (these are reserved for directory pointing) Type <rtn> when you are finished.

You may enter some descriptive text into the lower box.

Then LMB “OK”, then “Exit”

Now Another Dialog box Appears

In this Example We Had Selected the H-1 Only Button from CustomQ We can choose some parameter options here, by LMB clicking on the indicated values. Here we have chosen Spectral Width from -0.5 to 9.5 ppm, and 32 scans, along with a 2-second delay between repetitions.

Your choice will become shaded as you select it. LMB “OK”, “Exit”

An Option--Change the Set Up Parameters

You may change some of the conditions before starting the experiment. In the sidebar, click (LMB) the Acq&Obs tab.

In the boxes on this screen you might alter the delay time or the number of pulses.

Then, LMB CustomQ

You are Almost Ready to Start! Reclick into the CustomQ Menu

You need to do this action again, to get to the Start ACQ button

LMB click on the “Start ACQ” button.

Now the Automatic Locking and Shimming Takes over

You will see the banner that tells you what is happening.

Your role is to watch! The message window will display some “RMS err” output, during this process. This is not an error, but normal.

The gradient shimming will finish when the agreement is >1%

After the Shimming finishes, the Scanning starts

The Acquisition Status window tells you what is happening, and how far has experiment proceeded (CT, completed transients)

This is also the window that tells you if e.g. the autolock has failed.

Information about the spinner status etc. also is reported

If you need to Halt an experiment

Should you need tostop a process(shimming,acquisition, etc., LMBclick the Abort AcqbutttonFor example, if the lock or spinning Fails. 

 

After the Acquisition Status window shows that the job is idle, you can eject, change CustomQ choices, put a new sample in etc.

When the experiment is Finished

When the job is finished, it will be automatically processed (FT, phased etc.), then plotted on the laser printer.  You can pick up the hard copy, and reverse the steps on page 1, to retrieve your sample and replace the CDCl3 standard.

 Your Spectrum can be FTP transferred over the network for NUTs processing. You should navigate to: nmr300.chem.temple.edu: /home/temple/vnmrsys/data/(your name) /(todays experiment)

Last Step

Remove your sample by reversing the steps on page 2. Replace with the standard sample, and insert. Sign the logbook to record your use, files created, and any comment on instrument problems.