Automated NMR

Bruker Avance-III 400 MHz NMR Instrument

Installed in November, 2009 with funding from the National Science Foundation (Award No. CHE-0840336, "A Cyber-Enabled 400 MHz NMR Spectrometer for Research, Education and Outreach", $467,000), the Bruker Avance-III NMR Spectrometer is fully automated and runs in a walk-up sample submission mode.

Here's how it works: The SampleJet has a carousel that holds 96 NMR tubes in the outer ring. These are 7" NMR tubes (5 mm OD) with a special purple cap sold by Bruker. A robot arm with a "gripper" picks up the sample BY THE CAP and takes it over to the NMR magnet. The spinner (or "shuttle") is held in place at the top of the magnet bore and the gripper arm inserts the NMR sample tube into the spinner. The spinner has a "clamp" that is held open while the tube is inserted, and then closes to grip the tube tightly. The spinner (with sample) is then lowered into the magnet for analysis. Analysis is fully automated: Spinning the Sample, Automatic Tuning and Matching of the Probe (ATM), Automatic Shimming ("topshim"), Receiver Gain Adjust, Data Acquisition and Data Processing. Then the sample is ejected and the gripper arm removes it from the shuttle (which releases the clamp) and puts it back in its slot.

There are also five racks in the carousel containing up to 96 samples each in 4" NMR tubes (also 5 mm OD). These are for undergraduate courses (Chem 243A, Chem 243B, Chem 244 and Chem 247). So the total capacity of the SampleJet is 96 + (5 X 96) = 576 samples!

To submit a sample, follow the simple steps below:

1. Put your sample (with special cap) in one of the 96 holders in the carousel outer ring. Remember the holder number.

2. Log on to the computer in room 124 Old Chemistry and select the holder number. Enter the following information:

     a. Sample Name (this is a folder name - no spaces, only A-Z, a-z, 0-9, underline and hyphen)
     b. Solvent

     c. Experiment Number (1,2,3,4, etc.)

     d. Experiment: Choose from the list, PROTON, C13, DEPT-90, DEPT-135, etc. You can add as many experiments as you want for the analysis of this sample.

Some longer experiments are "night" experiments, meaning that they will be deferred until 7:00 p.m. on weekdays to run in the "night queue".

3. Click on "Submit". Your request goes into the queue and will be run in the order of submission. LOG OUT: click on "Change User" and "Lock IconNMR".

4. Go back to your lab and get some work done! The SampleJet takes care of your NMR experiment.

5. You can check the progress of your sample in the queue by using the Icon-NMR Web Interface:

6. When your experiment is done, the data will be posted on the web as a zip file (, where expno is the experiment number (1,2,3, etc.) and filename is the Sample Name. You can pick up your NMR data at:

where "login" is your login ID on the AVIII-400.

7. Come back to the NMR room (124 Old Chemistry) and pick up your sample from the carousel.

8. Analyze your data using the MestReNova NMR software package. This software is available for free and can be installed on your desktop or laptop (Windows, Mac or Linux). With the NSF grant we purchased a permanent campus-wide site license for the software. Any time you are connected to the campus network (either here on campus or through VPN) you can download a license from our license site. This license lasts for 90 days and is renewed every time you start MestReNova while you are connected to the campus network. Instructions for downloading MestReNova and the license, activating the license and using MestReNova are available in PDF form below: