NMR Facility Laboratory

        Chemistry C237

        Phone:  (812)-855-6492

        Fax:  (812)-855-8300

        Address:        Chemistry Building

                                Indiana University

                                Bloomington, IN 47405-7102

        Email:  chemnmr@indiana.edu

        URL:  http://nmr.chem.indiana.edu

NMR Facility Staff

NMR Facility Manager                      Dr. Ulrike Werner-Zwanziger

                                                                Phone:  (812)-855-4629

                                                                Location:  Chemistry C237C

                                                                Email:  uwerner@indiana.edu

                                                                URL:  http://nmr.chem.indiana.edu/~ulli

NMR Facility Coordinator                  John Tomaszewski

                                                                Phone:  (812)-855-4478

                                                                Location:  Chemistry C237E

                                                                Email:  jtomasze@indiana.edu

NMR Facility Associate (part time)                                                       Frank Gao

                                                                Phone: (812) 855-6492 (general facility phone)

                                                                Location:  Chemistry C237D

                                                                Email: xgao@indiana.edu

Introduction

The NMR facility is a service and research laboratory operated by and for the Department of Chemistry at Indiana University.  The laboratory performs and assists in magnetic resonance spectroscopy activities that further the research goals of departmental faculty, post-doctoral fellows, students, and staff.  The following report summarizes the service and research activities of the NMR Facility during 2001.

Staff

The NMR facility is operated by three staff members: John Tomaszewski works full time as our NMR facility coordinator.  Dr. Ulrike Werner-Zwanziger, the NMR facility manager, works half time with a short period in June 2001 of full time work. Then she asked to be put on half time leave again to be with her little daughter.  Frank Gao also serves in the NMR facility on half-time base.  Jeff Frey left the NMR facility to fulfill his dreams of volunteer work in South America. Angela Hanson went back to work for the Mass Spec facility full time.

Summary of Facilities

The NMR Facility includes the following NMR spectrometers dedicated for liquid samples:

• Varian Unity^INOVA spectrometer operating at a 500 MHz ¹H Larmor frequency (I500)

• Varian Unity^INOVA spectrometer operating at a 400 MHz ¹H Larmor frequency (I400)

• Varian VXR-Unity spectrometer operating at a 400 MHz ¹H Larmor frequency (VXR400)

• Varian Gemini-2000 spectrometer operating at a 300 MHz ¹H Larmor frequency (Gem300)

In addition the NMR Facility operates a spectrometer dedicated for solid samples:

• Bruker Avance spectrometer operating at a 400 MHz ¹H Larmor frequency (NMRSS1)

• and oversees and services a

• Varian Gemini spectrometer operating at a 200 MHz ¹H Larmor frequency in the undergraduate teaching laboratories (Gem200).

In conjunction, four Sun workstations, two SGI workstations, and seven Windows-NT and Linux workstations provide processing, simulation, and administrative capabilities in the NMR Facility laboratory.  A variety of probes are available for the observation of all possible nuclei and for conducting a wide variety of multinuclear experiments.

Summary of Research Activities

Research collaborations

Non-routine research collaborations are development of new NMR techniques or interpretation of spectra beyond daily interactions between Staff and Users. Research collaborations in 2001 include

• two-dimensional experiments for analyses of organic molecules (Evans, Johnston, and Williams groups)

• experiments observing ¹¹B (Todd group), ⁵¹V (Christou group), ²H (Christou, Caulton groups), ²⁹Si (Zwanziger group), and ¹⁵N (Linn group, IUPU Fort Wayne)

• pulse sequence development (homo-decoupled ³¹P experiments, ³¹P{³¹P,¹H}, Caulton group) and creation of macros (several plotting and processing macros)

• interpretation of higher order coupling patterns (Montgomery group)

• multinuclear solid state NMR experiments for polymer and glass ceramics characterizations (Zwanziger group)

• alignment studies in the solid and liquid crystalline state of Nickel and Zinc porphyrines (Chisholm and Zaleski groups)

•  measure ¹³C NMR spectra of kerogen samples (Schimmelmann group, geology)

Publications

• Structure and Magnetic Alignment of Metalloporphyrazine Columnar Aggregates in Their Mesophases and Crystalline Phases.  Brian D. Pate, Sung-Min Choi, Ulrike Werner-Zwanziger,_­ David V. Baxter, Jeffrey M. Zaleski, Malcolm H. Chisholm, Chemistry of Materials, in print

Poster Presentations

Invited Seminars

Summary of Facility Services

Profile of Spectrometer Utilization

The NMR Facility is available 24 hours per day, each day of the year, for collaborative or independent use by trained researchers.  The Graph Gallery shows the utilization of each spectrometer from Jan. 1 to Dec. 31, 2001, in several formats.  The following observations (shown in bold) and interpretations are derived from the Graph Gallery:

•  Inorganic chemists dominate utilization of the Gem300 and I400.  Organic chemists dominate utilization of the VXR400.  Biochemists dominate utilization of the I500.  Data stations were used by a variety of research interests. Utilization of the I400 by organic chemists or of the VXR400 by inorganic chemists has not shifted the major user groups from their traditional use.

• Utilization of the I500 and NMRSS1 is extremely high.  The I500 is efficiently used by the biochemists for large blocks of time. NMRSS1 is specialized on long duration solid state NMR experiments.

• The monthly use of the VXR400 is fairly even throughout the year. Increased use in May probably results from the end of the semester and a shift towards research activities. The departure of Professor Chisholm's group in summer 2000 impacted the use of the I400 and Gem300 NMR spectrometer. Their utilization dropped in the second half of the year after an increase just prior to the shrinking of his laboratory.

Notable services

• In the summer the Staff offered a "NMR mini course" discussing practical aspects and background of NMR experiments. This class is held as a block class with several morning sessions in two parts covering simple and advanced techniques.

• The staff submitted a proposal to the NSF CRIF program for the upgrade of the VXR400 NMR spectrometer with a new console, refurbishment of the magnet and acquisition of a gradient unit. Also, the staff contributed to a NIH proposal for the acquisition of new 600 MHz NMR spectrometer. Unfortunately, neither of the proposals was successful.

•  The staff beta-tested the computerized Aldrich Spectral Database, a program that offers the previous printed database in a searchable, extended computer version. This program also offers nice spectral interpretation features. This service to Aldrich allows us to purchase the final software package at a greatly reduced price.

• The staff installed a new freeware program "Spin Works" that allows the simulation and fitting of experimental spectra to determine J-coupling and chemical shift information.

• The staff prepared a summary statement for the physical possibilities of placing higher field NMR magnets into our current NMR facility with the view of replacing some spectrometers with higher field NMR systems.

• The staff presented a guest lecture in the C443 class about the NMR facility services and capabilities.

Summary of Facility Developments

NMR Hardware Installation and Upgrades

• The computers of the I400 and VXR400 Spectrometers were upgraded with Sun Blade Systems. Simultaneously the spectrometer software was upgraded to VNMR 6.1c and Solaris 8. These upgrades sped up the login process considerably.  Likewise, the nmrsun3 and nmrsun4 workstations have been upgraded to Solaris 8, with the other workstations to follow.

• The VXR400 Spectrometer Monitor was upgraded with a flat screen monitor. These are insensitive to magnetic fields and therefore give a nice display close to the magnets.

• The I400 spectrometer was equipped with a uninterruptible power supply to protect against damage from power losses.

• The magnets of both Gemini spectrometers quenched. Our staff member, Frank Gao, was trained in his prior job as Bruker Applications Specialist of China to charge this type of magnet. By purchasing a used power supply, and being able to revitalize both magnets, he saved around $15,000  for the NMR facility in the current instance, and possibly more in the future, if either magnet were to quench again

• The NMR facility staff in collaboration with personnel from Bruker Instruments Inc. finished the installation of the Bruker 400 MHz DSX NMR spectrometer. This instrument is optimized for the study of solids.

• The 400 MHz Inverse probe head had to be repaired, since the X-band components could not withstand the necessary power input. The probe had not been used in years, so it probably was broken in years past.

• The quad probe of the I400 NMR spectrometer had to be repaired when a detection coil surrendered to the permanent friction from the spinning of the samples.

Laboratory Improvement

• Computer security has been improved by upgrading several services and disabling others and keeping up with patches for the operating system software.

• The Web pages were updated with various help and “how to” items in the “User’s Guide”.

• The Web signup software MAG RES was improved by color coding the use of non-standard probes, repair times and the spectrometer use of the Stone Group.

• Perl scripts for the backing up of data were improved.

• A new printer facilitating 17"x11" paper and standard paper output was purchased. The old one suffered too many paper jams.

• A CD writer was added to a PC in the laboratory. This allows the general user to write their data onto their own CD's.

• Handouts for personal use are now provided and displayed on stacked, easily accessible stands.

• New handouts and a poster describing the use of the Gem200 in the undergraduate teaching lab were written.

• A hardware monitoring system was implemented on our Linux PC that sends a page and/or e-mail notice to the staff signaling when any of the computers, spectrometers, or printers have lost power, crashed, or otherwise been disabled.  This allows us to “keep an eye” on the facility at all times.

Organizational Changes

•  In order to facilitate the use of the I500, a regular monthly schedule was implemented.

1. The week beginning with the first Monday of each month is designated for general use on a sign-up basis.

2. Weeks two and three are generally reserved for the Stone group.

3. Week four is also available for general use upon prior request with the NMR staff at least three days in advance. In the absence of such reservation, the Stone group can opt to use some, or all of the machine time during this week.

       The reservations are posted and color coded on the MagRes website and on a wall calendar.

Continuing Projects

• Proposals for funds for the upgrade of the VXR400 to the NSF will be written (completed in 1/2002).

• The electronic and paper forms of our User Guides will be updated.

2001 Graph Gallery

Data for the Graph Gallery was derived from NMR Facility accounting records from January, 1^st to December, 31^st 2001. These records were automatically generated from the spectrometer & datastation login/logout processes.