Sample Submission and Results
Sample Preparation
Essential for sample delivery are:
General Information
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Please ensure that the submission form is filled out completely (Full reaction scheme including sum formulae and mass information is advisable). It is not necessary to attach the sample directly to the form.
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The sample vial must be clearly and permanently labeled with the same name as provided on the form. (SpecQuest MS provides a label that can be attached to the vial using adhesive tape: First attach the label and after that fix independently on the form - if needed.)
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Make sure the sample can be removed easily by the operator personal without damaging or obscuring any information on the form or the vial label.
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Please note that measuring mass spectra of highly reactive samples (e.g., acid chlorides, sulfonyl chlorides, etc.) is generally not meaningful. These compounds tend to react with moisture, methanol, or other solvents, which makes accurate measurements difficult and limits the value of the results.
ESI / MALDI
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Please remove ionic components, especially buffer salts, from your sample, as they interfere with ionization.
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Submit clean samples in properly sealed, leak-proof vials. A small, clearly visible amount is sufficient. Since we will dissolve the sample, please indicate a suitable solvent. Information on alternative solvents is also helpful. If the sample is submitted in solution already (not preferred!), we need information about the solvent used and the concentration!
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If your compounds are sensitive to air or moisture, please contact us in advance.
GC-MS
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GC-MS samples must not contain strongly acidic or basic substances, nor non-volatile components. A rough purification using silica filtration is mandatory beforehand. Please confirm this step on the submission form under “Column Filtration for GC.”
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Ideally, samples should first be analyzed using GC-FID. Please submit the same vial along with the corresponding gas chromatogram. If an EI mass spectrum is already available, it must also be submitted with the request for accurate mass determination (mandatory for all groups with their own GC-MS systems). Please also indicate the temperature program, injection volume, and any solvents present in the sample.
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Important! Once a septum has been pierced, silicone may dissolve into the sample, which can easily dominate the chromatogram. The sample peaks may then become obscured by a "picket fence" of silicone peaks. To prevent this, always replace the septum with a new one immediately after your own measurements. (Also, do not tape the vial to the MS Request Form—place it upright in the rack of the delivery tray instead.)
TLC-Extraction Samples (primarily for ESI)
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Please schedule a measurement appointment in person to ensure that the sample can be analyzed in a timely manner and that the conditions for the measurement can be discussed. Substances on TLC plates degrade over time, so prompt measurement is always advisable. Therefore, submitting samples on Friday afternoon without a scheduled appointment is not recommended!
If you have questions feel free to ask us.
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MS Request Forms
SpecQuest MS (software for producing submission forms)SpecQuestMS is a software solution for producing MS and CHN submission forms. Those submission forms contain barcodes and are machine (and anyway better) readable.
Advantages:
- Operator: easy and error free entry of NameID, SampleID and Filenames
- Operator: no unnecessary further enquiries due to fragmentarily filled submission forms
- Customer: distinct and consistent file name generation (better searchable in case of further requests)
- Customer: fast generation of submission forms with less effort - sample labels are produced simultaneously.
Considerations for use:
- The software may be installed on any Windows computer (without admin rights).
- You can ether produce MS or CHN request forms selecting the appropriate register card.
- Each user is already in the institutes database when receiving his NameID. (Please supply missing information – MS-Department)
- You login by your surname/nameID. This combination already fills further information (phone, e-mail) from the database into the form.
- Printing the form is only possible after completing the requested information.
- Must-have information is marked in red. The read mark will disappear after completing the request. The form is ready for printout after completion of all red marked requests.
- For MS forms reaction schemes may be inserted by copy/paste from most chemical drawing programs. (Attention: Don't resize drawings within the drawing software before insertion!). Reaction schemes may also be drawn by hand after printout.
- As there will already be a (machine readable) filename for the sample, please use one form for each single sample. A label to be fixed on the sample vial may be cut from the form after printout.
- MS: For measurement an analytical question (like just molecular weight, accurate mass, fragmentation) has to be given. The choice of the appropriate mass spectrometry method or ionization technique is left to the operator. Information which method was used on similar previous samples and successfully gave the desired answer can and should be provided.
- The software can only be run within the university network. Otherwise a VPN connection has to be made to the university network.
- The software has a version control. In case of a too outdated version, the software will refuse to start.
- The use of previous forms (Word doc, pdf) is still allowed although machine readable forms will possibly be handled faster.
- Please use a Laser-Printer and take care for a good printing quality!
The software is still under development. All feedback and feature requests are welcome!
If you want to have samples from another institute measured in the Organic Chemistry Institute, please first contact the head of the mass spectrometry laboratory, Dr. Matthias Letzel.
Sample Delivery
© MLE Samples can be delivered and results collected in front of room 252a/b of the institut at any time.
Sample delivery is not structured whereas for the dispatch individual shelves are provided for most groups.
All samples are processed as quickly as possible, most of them within one day (depending on method).
Results
In order to accelerate spectra delivery (especially for groups residing outside this building) we are delivering spectra exclusively via e-mail attachments now.
For that reason please support this by using SpecQuest MS!
Please note that we will only provide results to Uni Münster (@uni-muenster.de) email addresses!
Attention: This University regulation (April, 18th 2016) prohibits e-mail forwording to external, private e-mail services! Existing forward settings will be deleted. Please take care that you are able to receive your university e-Mails!
Sample Return
© MLE Samples will be disposed after measurement in the MS department. They will only be returned on special request (please indicate on the request forms). Return samples have to be taken until fridays 9 am; otherwise they will be disposed.
The return shelves are accessable all day (24/7) in front of room 252a/b.