Research Facilities

X-Ray Crystallography Facility

McMaster University boasts an X-ray facility which offers crystal and molecular structure analyses on single crystal samples. The lab houses diffractometers and cameras, adjacent to a powder diffraction laboratory run by McMaster's Brockhouse Institute for Materials Research. The state-of-the-art instruments, computers and software offer the most powerful small molecule X-ray structure determination facility in any University. It includes a Mo rotating anode X-ray source with a CCD area detector, the first of only two in the country. This has reduced the data collection time from days per sample to just hours, and allowed the analyses of very tiny crystals. An average of 200 structures per year are determined.

The facility is run by Dr. James F. Britten, a professional crystallographer who assists students in obtaining analysis of organic, organometallic, and inorganic materials. Routine analysis of samples is carried out for both the research labs within McMaster University, and for other universities within Canada and the United States. In addition, every year, Dr. Britten offers a graduate course in small molecule crystallography which comprises lectures, tutorial sessions, and solving actual structures as part of the laboratory component.

Optical Spectroscopy and EPR Facility

The facility is home to several cutting edge research instruments, all purchased by various members of the department. Mr. George Timmins makes sure the facility operates smoothly, trains many graduate and undergraduate students to run their own spectra, and runs samples submitted from outside the department.

The most recent purchase was an upgrade to the Bio-Rad FTS-40 FT-IR to Win-IR software. This user-friendly PC-based operating system has considerable spectral manipulation capabilities and can be used to import and process spectra from many other instruments. Normally, the machine is configured for the spectral range of 5000 to 400 cm^-1, but near-IR (500 to 50 cm^-1) is available, as is GC-IR capability with a HP 5890 gas chromatograph.

Two UV instruments are available. The HP8451 machine is a diode-array spectrometer mainly used for routine spectra, while the Perkin-Elmer (PE) Lambda 9 dual beam instrument is used for quantitative work. The latter machine has greater sensitivity, resolution, a much better linearity at high absorbance and can provide useful data as low as 185-nm.

Electron paramagnetic resonance (EPR) users rejoiced recently with the purchase of a Bruker EMX 8/2.7 EPR instrument, a significant improvement over the old machine. The temperature controller can be set as low as 100 K.

Raman spectroscopists also have the benefit of using a very good machine, a Jobin Yvon/ISA with a 1 meter monochromater and double monochromater/pre-filter. There is considerable versatility in that both large and small samples may be run (the latter via a microscope), low temperatures may be accessed, and either argon or krypton lasers may be used.

Rounding out the list is a fluorimeter (a PE LS-5) for fluorescence/phosphorescence work and a polarimeter (PE 241MC) for measuring the optical rotations of chiral compounds.

Nuclear Magnetic Resonance Facility

The Nuclear Magnetic Resonance Facility was established in 1986 with funding provided by NSERC and McMaster University. The NMR facility contains four spectrometers, including a recently-upgraded 500 MHz spectrometer with state-of-the-art console and probes. The facility is highly regarded in the Canadian chemical community for its versatility in the types of samples (organic, inorganic, biochemical, geological, industrial, forestry, agricultural, and biomedical materials) and nuclei (40 different nuclei are observed routinely) that can be studied by solution and solid-state NMR.

The Bruker DRX-500 instrument represents the newest generation of NMR spectrometers which incorporate digital signal processing technology. State-of-the-art accessories include two Silicon Graphics Indy workstations and pulsed field gradient capability. In addition, a microprobe allows for aquisition of ¹H and ¹³C NMR spectra of microgram-sized samples, and the newest probes have ¹⁹F decoupling capability which has a number of applications in both organic and inorganic chemistry. A Bruker 300 MHz instrument is also available for rapid access to nuclei such as ¹⁹F and ³¹P, and two Bruker 200 MHz instrument are available for routine ¹H and ¹³C analyses.

Gradient COSY-45 spectrum of the aliphatic region of the
Lythraceae alkaloid decodine acquired in six minutes
on the Bruker Avance DRX-500 spectrometer.

The facility is run by a support staff that consists of Brian G. Sayer who is manager of the facility, Dr. Donald W. Hughes, an application specialist who also teaches graduate courses every year in 1-D and 2-D NMR theory and applications, and George Timmins who is the facility's instrument specialist.

Mass Spectrometry Facility

The McMaster Regional Centre for Mass Spectrometry was opened in 1986 with funding provided by NSERC and McMaster University grants. The facility houses four mass spectrometers and is operated by a professional manager and a support staff consisting of Tadek Olech and Leah Allan, who analyse approximately 4000 samples a year. The state-of-the-art Micromass Quattro-LC Triple Quadrupole Mass Spectrometer is dedicated to liquid chromatography (LC) /mass spectrometry (MS) and LC/MS/MS, employing electrospray ionisation which offers unique possibilities for the analysis of high molecular weight polar or charged species such as peptides, proteins, nucleic acids, and nucleotides. The instrument also utilizes atmospheric pressure chemical ionisation for analysis of low molecular weight polar and non-polar compounds. In addition, two Finnigan 4500 Quadrupole Mass Spectrometers are dedicated to the analysis of both pure compounds and mixtures through gas chromatography/mass spectrometry. Research projects involving the development of Neutralization-Reionization Mass Spectrometry and other sophisticated MS/MS techniques are carried out on a VG Analytical ZAB-R instrument.

Posing by the Electrospray are top (L to R):
Lorne Fell, Lisa Heydorn, and Dave Lavorato.
Adrienne Boden is at the controls.

Last year long-time facility manager Richard Smith left McMaster for NovoPharm Inc.. His many duties were carried out in the interim by graduate student Dave Lavorato. This fall, Dr. Kirk Green joins the department as the new manager of the Mass Spectrometer facility. He graduated with an M.Sc. from U. of Alberta in Edmonton, and completed his Ph.D. work at the Univ. of California at Davis. He joins us from a joint position at U. of Delaware and Dupont Central Research.