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X-Ray Crystallography - How to Submit Samples, Scheduling and Lab Info

Single Crystal Sample Submission and Preparation

Samples for single crystal X-ray diffraction analysis from Purdue users should be submitted using the Purdue iLab web interface. Navigate to the X-ray Crystallography Laboratory page on the list of Core Facilities. Click the "Request Services" tab and select "Single Crystal X-ray Diffraction" ("Self Run" or "Service Request"). Sample submission includes an MS word single crystal submission form. Please fill out as many fields as possible. Missing important information may delay processing of samples.

Samples may be run by the crystallographer ("Service Request") or by approved trained users ("Self Run"). Samples to be run by facility staff should be brought to the XRD laboratory, WRTH 101, unless the samples are highly sensitive and likely to decompose rapidly. Samples can be given to the crystallographer, they can be left on the countertop to the right of the sink/faucet or in the refrigerator/freezer in the lab. Make sure your sample is properly labeled with the compound ID used on the submission form. Please use paper tags (no marker on glass vials).

A majority of samples grown from solution do crystallize with included solvent molecules, and many of these samples rapidly desolvate and loose crystallinity when taken out of solution or placed in a different solvent or oil. Crystal desolvation is the by far most common cause for failing data collections. To avoid these complications samples should be left in the mother liquor they were grown in. Exceptions are materials that are known to be completely solvent free, e.g. indicated by their NMR spectra, or for which thermal analysis data (TGA, DSC) show that they do not desolvate until well above room temperature. For samples that tend to rapidly redissolve split your sample and provide both crystals in mother liquor as well as without (dry or in protective oil).

Samples that are sensitive towards oxidation or humidity might need special care. Compounds known to be oxygen or water sensitive should be packaged under protective atmosphere (e.g. in a glove box). Place a part of the sample with some mother liquor into a small screw cap vial. Tightly seal the screw cap and seal it with electrical tape. Place the smaller vial into a secondary larger screw cap vial and seal it in a similar way. Place the sample into the fridge or freezer as any other sample and point out its sensitivity to the crystallographer.

 

Highly Sensitive Samples

Some extremely sensitive samples might need to be mounted in a capillary or embedded in a viscous oil such as polybutylene prior to be taken out of protective atmosphere. Please consult with the crystallographer in such cases.

 

Scheduling

Internal users will generally have preferred instrument access, with priority given to courses, and for teaching and training. Whenever possible, samples will be run in the order they are received. During times of high instrument demand, samples might be prioritized by urgency, e.g. for data needed for upcoming PhD defenses, revision requests for submitted publications, or for very sensitive or short-lived samples. Instrument booking is handled by the crystallographer.

Approved users are encouraged to collect and refine their own data. In general, the equipment cannot be reserved for use at a set time. The crystallographer or previous instrument user will call or e-mail the user when an instrument becomes available. If the user cannot be reached or is unavailable at that time the queue will proceed to the next sample in line and the skipped sample is rescheduled for the next available instrument slot. 

 

Independent Use of the Instruments

Both the single crystal as well as the multicrystalline ("powder") X-ray diffractometers are available for independent use, under the guidance of the crystallographer, for both Purdue researchers and visiting collaborators. Prior to being granted off-hour access and independent use of the instruments, users will be trained by the X-ray crystallographer in the safe and effective use of the diffractometers. For Purdue PhD and senior undergraduate students interested in independent use of the single crystal diffractometers the training is usually accomplished in connection with 12650 - CHM 69600-004, the hands-on single crystal X-ray class. Training can also be provided on an “as needed” or on an “one-on-one” basis.

Users will have to pass Purdue’s Office of Radiological and Environmental Management’s (REM) Analytical X-Ray Training quiz, following the guidelines set by the State of Indiana. Follow the link to the REM training module page, scroll down to X-ray Diffraction and Crystallography (alphabetical listing) and click the icon on the left to start presentation and quiz. Once you completed the online training you will receive an e-mail informing whether you passed. Forward this e-mail to Dr. Zeller. The form A4 is no longer required.

Users not fully approved for independent operation of X-ray producing equipment will be closely supervised by the crystallographer. Members of this group include but are not limited to: users in training, occasional users, short term visitors, or when the instrument is used for teaching purposes other than 12650 - CHM 69600-004 (the hands-on single crystal X-ray class).

 

X-ray Short Courses and Summer Schools

Coming Soon. Please contact the crystallographer for more information

Purdue University, West Lafayette, IN 47907 (765) 494-4600

Department of Chemistry, 560 Oval Drive, West Lafayette, Indiana 47907-2084 | Telephone: (765) 494-5200 | Fax: (765) 494-0239

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