Solution state NMR
The solution state NMR facilities are located in A74 (access via A73) Faraday Building, and are used for both research and teaching.
The instruments are run in open access mode 24-7, but users must have suitable training before being allowed access to the NMR suites, so contact Dr Geoffrey Akien beforehand. Trained undergraduates can access the space by themselves from 9 am - 5 pm, Monday to Friday, but must be supervised outside of these hours.
During peak hours (Monday to Friday, 8 am to 6 pm) the maximum time allowed per experiment is 15 minutes, although users may have more than one of these per sample. To maintain responsive access for others, the "Priority" ability is enabled for all users. At busy times of the year the peak/off-peak timings may change to maximise throughput of samples.
Liquid nitrogen fills are generally carried out every Monday morning, but one instrument will always be available for immediate use. Liquid helium fills take place approximately every 5-6 months, and users will be advised by e-mail when these take place, and if there are any other scheduled interruptions. A list of activity is also maintained on the Chemistry Booking System.
Users can contact Dr Geoffrey Akien at any time, or alternatively, concerns can be raised through the NMR Management Group via Dr Michael Coogan.
Research - Bruker AVANCE III 400
The Bruker AVANCE III 400 (NanoBay) is fitted with a 5 mm 1H-X broadband observe (BBO, 109Ag-19F) RT probe, and is currently equipped with a 16-position SampleXpress Lite autosampler. The instrument is currently controlled with TopSpin 3.5pl7 on Windows 7. It is primarily intended for research use, but from time to time it is also used for undergraduate teaching.
Owing to the higher sensitivity of the 400 compared to the 300, several of the longer experiments (e.g. carbon, HMBC) have versions appended with the ".fast" suffix so that they will run in less than 15 minutes each and so fit within daytime limits. Note that these will only give good-quality spectra if your sample is concentrated enough - 10-20 mg in 0.6 ml solvent is a reasonable concentration to use for this.
A wide variety of experiments are configured to run in automation, but if there's something missing just ask!
- 1H - qualitative and quantitative
- 1H with automated single and multiple solvent suppression
- 1H up to 75 °C in automation
- 1H with X-decoupling
- 13C (and up to 75 °C), DEPT135
- edited HSQC
- HMBC, H2BC
- NOESY, ROESY
- Support for a variety of X-nuclei including 2H, 7Li, 10B, 11B, 14/15N, 19F, 29Si, 31P, 89Y, 99Ru, 111/113Cd, 119Sn, 195Pt. For most nuclei experiments for 1D's and 1H,X-HMBC 2D spectra are available.
To access sub-ambient temperatures we need to replace the normal VT gas with a liquid nitrogen evaporator, so these must be run out of automation - book time here. We haven't needed to go this low yet, but the minimum temperature attainable is estimated to be substantially lower than -100 °C.
The maximum temperature possible for the BBO probe is 180 °C, but for safety and various experimental reasons anything above 75 °C will also be run outside of automation.
The instrument booking timetable is here so you can view busy times, or book time if you have been given permission to do so.
Teaching - Bruker Fourier 300
The Bruker Fourier 300 (MHz) instrument is fitted with a 5 mm 1H/13C-observe probe (DUL/ES) currently equipped with a 60-position SampleXpress autosampler. The instrument is controlled using TopSpin 3.2pl7 on Windows 7. The primary use of this is for teaching, but research samples can be run on this at any time.
Currently configured experiments in automation:
- 1H - qualitative and quantitative
- 1H with automated single solvent suppression (composite pulse with presaturation)
- 1H up to 65 °C
- 13C, DEPT135
- COSY (magnitude and phase-sensitive)
- Edited HSQC, HMBC
- NOESY, ROESY
The sensitivity of the 300 is about half of the 400, so that there are no pre-configured ".fast" versions of experiments. However, parameters can still be manually adjusted to fit into the 15 minute daytime limits if necessary.
Owing to differences between the 300 and the 400, the 300 is not recommended for use with deuterated solvents with more than one peak, with the exception of MeOH-d4 which has a workaround in place.
Note that during term-time sample holders 1-45 are sometimes in use for undergraduate samples, usually during the evening. The booking timetable is here, but if you wish to use the 300 for your own experiments you can always use the priority button to jump the queue and run your sample immediately.
Consumables and other equipment
Also available for communal use are:
- Limited amounts of inherited "vintage" NMR solvents for routine applications
- Coaxial inserts for external referencing
- Amberised tubes for light-sensitive samples
- Screw-cap and "Young's"-type tubes for air-sensitive samples
- 3 mm tubes and a 5 mm spinner adapter for DOSY measurements on convecting solvents (e.g. CDCl3)
- 5 mm Shigemi tubes for small samples, matched for either CDCl3 or D2O
- FEP tube liners for corrosive samples
- Aluminimum NMR tube heating block with thermocouple well for use with stirrer hotplates
- Butane torch for flame-sealing tubes
- Heat guns
- Ultrasonic bath
- Mini centrifuge
- Eppendorf mechanical pipettes and tips: 0.5-10 μl, 10-100 μl, 100-1000 μl
If there's something that we don't have that you think would be worthwhile for the department, let me know and we can look into buying it in for communal use.