Getting Results

by Dan Krauss 

If scientific capability could be measured in horsepower, the College's Analytical Facilities would put a Ferrari to shame. Under the hood is enough top-of-the-line instrumentation and expertise to uncover the molecular secrets of virtually any chemical sample.

 The muscle behind the Analytical Facilities is its five specialized service laboratories, which combined their administrative functions in March of last year to become a single College unit. At the same time, four of the facilities--Mass Spectrometry, Microanalysis, X-ray Crystallography, and Graphics and Computing--were moved from their various locations in the College and resettled into neighboring lab spaces in Lewis Hall. The NMR facility remains in its original location in nearby Latimer Hall.

 "It was clear to me that the Analytical Facilities needed to join together collectively because in these trying economic times, it was important to consolidate the group so we could all help each other," Director of Analytical Services Dr. Julie Leary said.

 According to Leary, an Adjunct Professor in the Department of Chemistry, the new proximity of the facilities permits improved communication and collaboration, which results in more comprehensive analyses.

 "There is much more talk among the supervisors of the Analytical Facilities and that helps us to better help clients in terms of interpreting their data," she said. "Before, many of the facility managers never even talked to each other. We were in completely different parts of the College."

 Leary said she would like to strengthen further the combined capability of the facilities by promoting cross-training among their members, thereby developing "a cross section of people who are well-versed in all of the analytical techniques."

Such improvements are giving academic and industry-based researchers additional incentive to turn to the College for their analytical needs. In particular, many outside clients are drawn by the fact that there is a very active research component in the Analytical Facilities, particularly in the areas of Mass Spectrometry and Microanalysis.

 "Since I have an active research program, the group keeps very current in the area of methods development and biomolecule analysis," said Leary. "We are attractive to various companies because we have the expertise to help them characterize particularly difficult and challenging samples."

 Leary's notion is evidenced by the fact that the Analytical Facilities regularly provide services to dozens of scientific companies and academic institutions around the country.

MASS SPECTROMETRY

More than 10,000 samples pass through the Mass Spectrometry facility each year, a fact that prompts facility director-in-training Dr. John O'Lear to remark wearily, "As academic labs go, we are very busy."

 According to Leary, who formerly headed the facility, the number of samples analyzed is "by far and away more than that of any other [mass spec] laboratory in the United States." Leary is credited by most with single-handedly building the now-renowned reputation of the lab over the last decade.

 To keep pace with the flood of incoming samples, the facility keeps two full-time spectroscopists who have at their disposal a $4-million arsenal of modern spectrometers. Among the techniques performed at the facility are electron impact, fast atom bombardment, electrospray, and laser desorption, in addition to conventional gas chromatography mass spectrometry.

 "For an academic institution, we have probably by far the largest and most completely diverse instrumentation," Leary said of the lab's six spectrometers .

 O'Lear was quick to agree, adding, "This is one of the best [facilities] you'll find anywhere."

 According to O'Lear, the primary clientele of the facility are synthetic chemists who need to verify the structure of newly synthesized compounds.

 "The information we provide, if it doesn't confirm what they hope is there, at least provides some indication of what they do have," O'Lear said.

 In addition, new techniques for generating ions, the key to mass spectral analysis, have opened the doors to experiments involving such molecules as peptides and nucleotides.

 "The technique has undergone an incredible revolution in recent years because we are able to do mass spectrometry on molecules of biological importance," O'Lear said, adding that this has resulted in a significant increase in the number of samples from biology-oriented scientists.

 "All these people are now using mass spectrometry. A few years ago they would have laughed at you if you had told them that mass spectrometry could give you sequence information of a protein."

 Embracing such cutting-edge technology has helped the facility establish good working relationships with several business organizations outside the university. In all, about 40 percent of incoming samples are sent by biotechnology firms, drug companies and other scientific corporations.

MICROANALYSIS

When two of the College's research groups needed to perform carbon, hydrogen, and nitrogen (CHN) combustion analyses on air-sensitive samples, the Microanalytical Laboratory devised an ingenious way to encapsulate the samples to shield them from air prior to analysis.

 In doing so, the facility emphasized its willingness to design specialized techniques based on its clients' needs--and became the pioneer of a new microanalytical method.

 "To my knowledge, we are clearly the best lab in the nation to do air-sensitive [analysis] on CHN," said facility director Dr. Steve Brimmer.

 Another instance of the facility's innovative approach is evident in its latest project: joining a mass spectrometer to one of its two combustion instruments. According to Brimmer, when the project is complete, the hybrid instrument will be able to analyze much smaller samples, permit simultaneous analysis of sulfur and halides, and give information regarding combustion efficiency.

 "Basically, we're trying to take combustion analysis and extend it into the 1990s," Brimmer said.

 On a daily basis, the facility performs quantitative determinations of elements in a variety of samples, using its two top-of-the-line Perkin-Elmer combustion instruments and atomic absorption spectrometer.

This year alone the facility will analyze about 6,000 samples--many sent from other academic institutions and scientific companies. Brimmer said that when he first came on board three years ago, there was virtually no interaction between the facility and outside organizations. Today, the phone rings incessantly with calls from potential clients.

 "That's the routine," he said smiling.

X-RAY CRYSTALLOGRAPHY

Students and scientists are literally lining up to use the X-ray Crystallographic Facility's (CHEXRAY's) new diffractometer. The reason, according to facility director Dr. Fred Hollander, is that the new diffractometer allows analyses that would have previously taken days to be performed in hours. More important, Hollander said, is that the instrument can analyze samples that not long ago would have been impossible to use.

 "It's a brand-new instrument, not only to us, but to the crystallographic community as a whole," Hollander said of the $300,000 apparatus, brought on-line in March. Because the facility is now at the front of its field, Hollander said he expects to see many more outside labs soon taking a place in line, too.

 "The new instrument has given us an order of magnitude decrease in the volume of the crystal that will give us a usable diffraction pattern," he said. "We can now take much smaller samples. There were a lot of samples out there that were in that range where they were a little bit too small to use with our old diffractometers."

 In the past, said Hollander, his facility catered to mostly traditional synthetic chemists. Because the new instrument yields much more complete evaluations of samples, it is useful to materials scientists and polymer chemists who often need to see entire diffraction patterns.

 The diffractometer will also enable new ways of displaying molecular structures derived from the instrument, according to Hollander.

 "I see the possibility of using the Graphics Facility in combination with the diffractometer to develop methods for visualizing scattering intensity in ways other than what we're doing now," he said, referring to the already extensive interaction between CHEXRAY and the Graphics Facility.

GRAPHICS AND COMPUTING

Computer graphics are pervasive throughout the modern scientific community. However, few chemical science departments in the world have established their own computer graphics facility, which is exactly what the College did in 1990.

 Fresh from Berkeley's graduate chemistry program where he made extensive use of computers, Dr. Tim Robinson was the ideal candidate to head the facility.

 "It's very essential to have someone who is able to both deal with the computers and also understand science," Robinson said.

 The facility's high-performance computers are often used for visualizing the structures of molecules and making presentable images of scientists' findings. Some of the images produced in the lab have been published on the cover of Science and in the pages of Time magazine.

 "It was very time-consuming in the past to build a three-dimensional model of a structure," he said. "Now, it has become well-accepted to visually communicate chemical concepts."

 In addition to computer time, the facility offers color scanning and printing as well as videotape recording at relatively low cost.

 Robinson emphasized, though, that the facility is as much a computing center as it is a graphics lab. Many clients use the computers' high-speed processors to carry out complex mathematical computations.

 "Our computers are set up so that they can be taken advantage of by faculty, and also for that matter, by outside businesses who are using all the analytical facilities," said Robinson.

 When used in conjunction with other analytical services, the computers play the role of "idea machines," according to Robinson, helping scientists to process and understand their data.

"We have pieces of software which, to varying extents, can model the properties and structures of molecules. That's where some ideas are generated," said Robinson. "And you can visualize the results of those calculations."

 Robinson often collaborates with scientists on research projects, sometimes developing specialized software to suit the scientists' needs.

 "We do research as well as service work because one of the things we have to do is create ways of visualizing assemblies of molecules in chemical systems," he said.

NMR

While support for sophisticated experiments is
an important part of the NMR facility's operation, facility director Rudi Nunlist prides himself on providing an environment where non-specialists can run routine as well as more complex analyses in a straightforward fashion.

 To this end, Nunlist has reconfigured many systems in his lab such as poorly-designed hardware components and needlessly intricate computer software.

 "It's sometimes difficult to program your VCR, but it doesn't have to be," he analogized. "We're trying to un-VCR [our equipment]."

 As another means of increasing the usability of his facility, Nunlist has established an information repository on the World Wide Web containing facts about the lab's spectrometers, operating procedures, and recommended techniques. Clients can even reserve time on the instruments or check up on an experiment via the internet.

"If we don't have to reinvent the wheel, we'll do it," Nunlist said of his innovations.

According to Nunlist, more than 250 people used the lab's spectrometers in the last 10 months--a figure which demonstrates that use of the facility is steadily increasing. Nunlist also noted a recent increase in the number of scientific companies that wish to collaborate with the facility on projects in which NMR is an integral technique.

 "[The companies] find it more expedient to use our equipment and talent to draw upon. There's a lot of experience in chemistry available at the College," said Nunlist. Companies typically use the facility for structure elucidation or analysis of large biological compounds in solution, he added.

At the heart of the facility are its five modern spectrometers which operate at a range of frequencies, from 300 MHz to 500 MHz. Nunlist routinely oversees the use of the instruments--even from home, where his personal computer is set up to monitor their operation.


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