Analytical Spectroscopy Laboratory

Staff 

Gordon Renkes | Laboratory Manager | B 084 CBEC | 614-292-3977 | renkes.1@osu.edu

Phuong Tran | GTA for XRD | tran.445@osu.edu


Services Provided 

The Analytical Spectroscopy Laboratory provides centralized care of, and training on, a variety of instruments for use by the graduate research program. Researchers may have access to instruments which are not available in their own labs because they are expensive or used infrequently. New ideas can be tested. Results and publications generated from ASL instruments can be used to justify proposals for instruments for a Principal Investigator's own laboratory.

The Lab Manager trains the users how to operate the instruments, and is available for advice on how to get the best results out of the measurements. Users who are certified have around the clock access. Descriptions of the instruments and their capabilities, and procedures and policies for using them are listed below.

(Note: The Circular Dichroism spectrometer, the Polarimeter, and UV-Visible spectrometer are now housed in the Biophysical Interaction and Characterization Facility)


Available Equipment

Bruker EPR | B 081 CBEC

Bruker D8 Advance X-Ray Powder Diffractometer | B 073 CBEC | 614-292-1116

Renishaw inVia Raman & Smiths IlluminatIR IR Combined Microprobe | B 075 CBEC

Perkin Elmer Spotlight 300 IR Imager | B 075 CBEC

Rigaku Geigerflex X-Ray Powder Diffractometer
0069 Evans Laboratory
Routine powder diffraction patterns of polycrystalline samples in air are easily recorded. Examples of typical uses include the verification of syntheses, determination of the presence/absence of crystalline phases, identity of phases in mixtures, crystallite sizes, the observation of phase changes after heating samples, and the determination of unit cell parameters. MDI Jade software controls data collection and allows data analysis. The ICDD Powder Diffraction Files are installed for search-match identification of unknowns.  For specialized experiments, consider the Bruker D8, listed just below.

Bruker D8 Advance X-Ray Powder Diffractometer
073 CBEC
A high resolution versatile instrument which has several different sample holders. These include a standard flat sample reflection holder, a transmission/reflection holder (useful for films), a 9-sample changer which permits both reflection and transmission geometries, a capillary holder, a low temperature camera (80 K - 450 C) and a high temperature oven (100 C - 1200 C). Those needing only routine flat sample reflection measurements should consider the Rigaku diffractometer described above.

Bruker EMXPlus Electron Paramagnetic Resonance Spectrometer
081 CBEC
This is a standard Continuous Wave Electron Paramagnetic Resonance spectrometer, for the detection of unpaired electron spins. The standard temperature controller regulates the temperature from 100K to 100C. A helium refrigerator may be available for work down to 4K. Samples may be illuminated while in the cavity. (This instrument is an update from the previous ESP300 spectrometer.)

Perkin Elmer Spectrum Spotlight 300 IR Microscope
075 CBEC
This permits recording of mid IR spectra of areas as small as 10 micrometers diameter, and the fast mapping of IR spectra over much larger areas.  Both transmission and reflection modes are available. 
 
075 CBEC
This permits recording of mid-IR and Raman spectra on exactly the same spot using the same instrument system.  IR and Raman spectral maps can also be recorded on exactly the same area.  Temperature controlled sample cells will permit temperatures to range from 100K to 1500C.
 

General Laboratory Policies

Who may use the facilities
Training policies and procedures
Materials which the research groups must provide
How to reserve time on the instruments
How to pay for instrument use
Laboratory Course use of instruments


Who May Use the Facilities

The Analytical Spectroscopy Laboratory is open for use by any of the research groups in The Ohio State University or other academic institutions for legitimate academic research.

Because it is a part of the Chemistry Department, department personnel will often receive priority in scheduling and assistance.

Training Policies and Procedures

Students and Post Doctoral researchers should contact the manager of the laboratory to schedule training. Because these instruments are expensive, and because several research groups share their use, they must be used carefully. Also, researchers should want to obtain the best and most useful data possible to enhance the quality of their theses and publications. Therefore the training is intended to help the researchers understand what the instrument is measuring, and how to make decisions which provide the best possible data.

Some new users may want to observe other members of their research groups operate the instruments as a part of their training. This is allowed and encouraged, because it acquaints the new user with the particulars of how that group typically uses the instrument. But before new users actually operate the instrument alone, they need to have the appropriate training sessions with the lab manager to make sure the various necessary operational details have been explained.

If you want to be trained and approved for access to one of these instruments, be sure to contact the lab manager long enough ahead of your planned experiments, so that we can plan agreeable schedules, and avoid delay.

Materials Which the Research Groups Must Provide

Research groups are expected to purchase and maintain their own sample cells, and other pieces of equipment which come in contact with the samples. This is intended to reduce cross contamination, and to minimize disruption when cells are lost or broken. The group members are responsible for storing these cells in a secure place which is known and accessible to all group members who wish to use them.

Also, other materials and supplies which are specific to a research group's experiment may also need to be supplied by that group. Common examples of this include cylinder gases, and cryogens for sample cooling if the cryogens are not routinely used for most uses on the instrument.

If a group wishes to purchase, or devise and construct, a specialized sample holder or accessory, be sure to discuss this thouroughly with the manager starting early in the planning phase. The manager must approve this design and construction before it is used with the instrument.  The chemistry department Machine Shop and Chemical Instrumentation Support Group are experts at designing and building special devices for experiments not possible in the OEM equipment.

How to Reserve Time on the Instruments

First, read the FOM calendar user manual [pdf], and follow its instructions.  Sometime after you fill that in, I should receive notification, and I can then contact you to continue the process.

Note that this FOM calendar system is now used to both reserve time and to calculate the monthly billing report.  You will want to start your measurements as soon as possible after your reservation starts.   If you finish before the end of your reserved time, log on to the calendar and log out of your reservation.  This will save your advisor some money in his/her research account.  Also, if you need to work beyond your reserved time, set up a new reservation which starts when your current reservation ends.  (Unfortunately it is not possible to simply extend a reservation.)  

Heavily Used Instruments

Some of the instruments are heavily used. All users need to cooperate with each other to share these resources equitably.

Please show up for your scheduled time on-time. If you arrive greater than 20 minutes late, you’re scheduled time is no longer guaranteed and any user that sees the instrument is available may use it. There are certain situations in which a late arrival may be necessary due to sample preparation, but please leave a note on the instrument computer as to when you will return for instrument use and adjust the calendar.

Do not go over your scheduled time, especially if there is a user scheduled directly after you. Several users have time-sensitive samples for which they must run measurements immediately. If you think you will be running over your time, notify the following user and ASK THEM if it is okay. If it is not, then you must relinquish your time.

If doing long measurements, please try to do night and weekend scans.

The Following Pertains specifically to the X-Ray Diffractometers

Any requests for different XRD modes can be directed to the TA for the semester as indicated on the ASL website. Do not begin scheduling time on the calendar unless a mode is listed. Any times scheduled without a specific mode listed will be deleted at the TA’s discretion.

When finished with measurements, turn the current and voltage down (20 kV, 5 mA for the Bruker and 20 kV and 2 mA for the Rigaku). Unless the following user is in the room or they have asked you to leave it up, turn these down every time.\

How to Pay for Instrument Use

Use of instruments will be billed monthly. Read the FOM calendar user manual [pdf], and follow its instructions.  Sometime after you fill that in, I should receive notification, and I can then contact you to continue the process.

Note that this FOM calendar system is now used to both reserve time and to calculate the monthly billing report.  You will want to start your measurements as soon as possible after your reservation starts.   If you finish before the end of your reserved time, log on to the calendar and log out of your reservation.  This will save your advisor some money in his/her research account.  Also, if you need to work beyond your reserved time, set up a new reservation which starts when your current reservation ends.  (Unfortunately it is not possible to simply extend a reservation.)  

Laboratory Course Use of Instruments

From time to time, chemistry lab courses will want to use one of the ASL instruments.  This is expected, and is a useful augmentation to the learning experience of OSU students.

The Teaching Assistants for the lab must be familiar with the operation of the instrument.  If the TA already uses the instrument for thesis research, there probably won't be much more to do than to make sure that the particular experiment will work as expected.  If the TA('s) has no experience on this instrument, (or has not used it for a long time), then the TA('s) should be trained by the ASL manager before the instrument is used for the lab course.  A trained TA must be present with the registered lab students as they perform the measurements.

Contact the ASL manager well before the start of the quarter so that arrangements and needed training happen before the scheduled experiment.

 

[pdf]- Some links on this page are to .pdf files.  If you need these files in a more accessible format, please email support@chemistry.ohio-state.edu. PDF files require the use of Adobe Acrobat Reader software to open them. If you do not have Reader, you may use the following link to Adobe to download it for free at: Adobe Acrobat Reader.

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