General rules for use of our equipment.
Never use any equipment without the proper introduction from the responsible person.
- Allways book the equipment via the webcalender (via the “equipment” link on the homepage of the MolMat department).
- Please be efficient in booking: don’t block a machine the whole day just to be sure that you can measure for half an hour; in general, you should start measuring not later than 15 minutes after the start of your booking period.
- On the other hand: if you find the machine unused (but booked by someone), please contact him/her BEFORE you conclude that you can start measuring yourself.
- Please treat the equipment and the area around it as you might expect in an analytical environment; keep everything clean and take your belongings/leftovers with you!
With a lab-population as big as ours, we should try to find the optimum between our own interests and those of our colleagues.
See a list with responsible persons on the website. Please contact that person to get instruction on how to use the machine.
In the case somebody from outside our cluster is interested to use our equipment, please direct them to one of the technicians. They will decide whether permission is granted, if necessary after consultation with staff members. If the decision is positive, this person will
- receive an introduction to the machine,
- follow the safety tour,
- be added to the users list of that machine
- be allowed to pick up a guest key at the secretary.
NMR
We have 2 NMR machines available, 300MHz (Cr4.315) and 600 MHz (Cr4.060). For the 600 MHz you have to fill in a request form, and after consultation with Bianca Ruel you can offer it together with your sample. The 300 MHz is equipped with a robot and is used as a ‘self service’ machine. You can use it after instruction given by Bianca Snellink,
- Fill in and sign the NMR USER LIST. This list can be found next to the computer where you enter your sample information.
- NMR-tubes should be of high quality. Check this carefully (507 pp or higher, 8 inch long, without damage).
- NMR-tubes should be coded (initials-sample code, like BS-05-01) labels are not allowed!
- NMR-tubes should be filled with at least 0.7 ml of deuterated solvent. Less solvent is one of the main reasons why a measurement fails.
- At daytime (8.30 a.m. -5.00 p.m.) not more than 5 quick NMR-experiments by the same user in a row.
- Quick NMR-experiments are: H1.
- From 5.00 p.m. – 08.30 a.m. advanced NMR-experiments can be performed on the 300 MHz NMR spectrometer.
- The advanced NMR-experiments are: H1S(1600 scans) , H1F(412 scans) C13(5000 scans), and C13L (20000 scans).
- It is only allowed to type the command ‘today’ in the computer.
- The text you type in the command line should contain at least your initials so we can find out who is the user.
- When your sample is not measured the first time, check if you put in the right solvent and try to measure it once again before asking help.
- Do not put your sample in the spinner while it is in the sample rack. Take the spinner out and put in the sample by hand. Check the right height carefully.
- Watch carefully where you put your sample in the robot sample rack. It is possible that the last sample is in the magnet. On the acquisition status, in the right corner of the computer screen, you can see which sample is in the magnet.
- When you are the first one in the morning please check if there is already a sample from position 1 in the magnet from the day before!
- Not-collected NMR-tubes will be stored for 5 working days.
- Your data is available on the hobby1 computer where you can process it.
- You can also transport your data to your own computer by using the little computer. Here you can copy your .FID file from Linux to Windows into your own directory. You should log in with your own username and password.
- Instructions of using the 300 MHz NMR by new users will be done exclusively by spectroscopy-coworkers. It is not allowed by for example PhD’s or postdocs, to teach their students.
- Don’t wear gloves in the NMR room. Leave them behind in the lab.
MS
There are 2 mass spectrometers in our lab. One for routine analysis (Advion ExpressionL) and one for accurate analysis and for molmasses >1500D (Micromass LCT -TOF).
The Advion is equipped with an ESI (Electrospray ionization) and APCI (atmospheric pressure chemical ionization) source. The Advion is coupled to a TLC plate express for quick analysis of organic compounds. Measuring solids is also an option.
The Micromass LCT-TOF is our back-up machine and only accessible for special requests such as high accuracy or higher masses (1500-2500D). Contact Regine van der Hee for more information.