May 2003 Meeting

CSSC Csaba Horvath Medal Lunch and Symposium

Date:

Friday, May 9, 2003

Location:

University of Connecticut
Nathan Hale Inn and Conference Center
Storrs, CT

Honoree:

Professor Harold McNair

Cost:

Lunch and Symposium $30 ($15 Students and Emeritus)
Symposium Only $10

Registration
Deadline:

Monday, May 5, 2003
NOTE: A $10 late fee will be assessed after this deadline!


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Agenda:

11:30 a.m.	Registration
12:00 - 1:30 p.m.	Lunch and Award Presentation
1:30 - 2:15 p.m.	Keynote Speaker: Professor Harold McNair Title: "Recent Advances in Gas Chromatography"
2:15 - 2:45 p.m.	Dr. Greg Slack, Wyeth Industries Title: " THE ROLE OF GAS CHROMATOGRAPHY IN A QUALITY ASSURANCE ENVIRONMENT"
2:45 - 3:00 p.m.	Refreshments
3:00 - 3:30 p.m.	Dr. Thomas Brettell, Chief Forensic Scientist, Forensic Science Laboratory Bureau, State of New Jersey. Title: "Detection of Gamma-Hydroxybutyrate (GHB) and Gamma-Butyrolactone (GBL) in Forensic Toxicological Investigations Using Headspace GC, SPME, and GC/MS"
3:30 - 4:00 p.m.	Capt. Richard Gaines, U.S. Coast Guard Academy Title: "New advances in multidimensional gas chromatography: Fast high-resolution separation of complex mixtures using comprehensive two-dimensional gas chromatography (GCxGC)"
4:00 - 4:30 p.m.	Gary Lavigne, UCONN Institute of Material Science Title: "A Syringeless Injection Device for the Introduction of Solids and Liquids into a Split/Splitless Capillary Injection Port"
4:30 - 5:30 p.m.	Concluding Remarks followed by Social Hour (Cash Bar)

Abstracts and Biographies:

Award Address: Professor Harold McNair

Talk title: "Recent Advances in Gas Chromatography".

Abstract: GC is a phenomenal analytical technique. Since its introduction in 1952 (1) it has rapidly grown to a major separation technique 1999 sales of $1 billion, and 28,000 units (2) it’s major application is trace organic analyses, with detection limits of ppm for most samples and ppb in selected cases. These trace levels are associated with good levels of precision, ± 1% for ppm and ± 10% for ppb concentration. Other major advantages include speed of analysis, high resolution (over 1000 peaks for cigarette smoke) and simplicity of operation. On the other hand, GC is limited to volatile compounds, and chromatographic data alone cannot confirm the identity of unknown peaks GC/MS is required in most cases.
This presentation seminar will focus on fast GC using commercially available hardware. Optimizing basic parameters (column length, film thickness, programming rate, column radius and flow rate will be discussed). It will be shown how many standard analyses can be performed 5 to 10 times faster with little loss in resolution. The Golay equation (3) for capillary columns will be used to illustrate the fundamental principles. Short columns are used for fast analyses, but these often demand small I.D., small film thickness and rapid injection techniques to preserve resolution.
For simple isothermal samples (less than 10 peaks) analysis times of 30 to 180 seconds is possible. For more complex samples, and particularly where high temperatures are required, longer times are required. For commercial instruments the major limitation to fast GC is the ability to heat and cool the column rapidly.
(1) James , A. T., and Martin, A. J. P., Biochem. J., 50, 679 (1952).
(2) McNair, H., “Current and Future Status of Separation Science”, Amer. Lab, 10-14, June 1997.
(3) McNair, H., and Miller J., “Basic Gas Chromatography”, John Wiley, New York, 1998.

Biography: Dr. McNair is professor of analytical chemistry at Virginia Tech, Blacksburg, Virginia. His research interests are the isolation, concentration and characterization of organic molecules by GC, GC/MS, HPLC and HPLC/MS. Current analyses of interest include: pesticides in soils and foods, biogenic amines in fish, trace bomb residues in air, water and soil samples, PNA’s PCB’s and toxic materials in water and soils. He has published over 150 original research paper and supervised over 50 graduate theses.
Professor McNair enjoys teaching both graduate and undergraduate classes; and a variety of short courses mostly for the American Chemical Society. He has received a variety of both teaching and research awards, including the Tswett Medal from the Russian Academy of Science, the Colacro Medal, the Keene Dimick Award, Dal Nogare Award and the J.C. Giddings Award.

Speaker 2: Dr. Greg Slack, Wyeth Pharmaceuticals, 64 Maple Street, Rouses Point, NY, 12979

Title: "THE ROLE OF GAS CHROMATOGRAPHY IN A QUALITY ASSURANCE ENVIRONMENT"

Abstract: This presentation will discuss the role of gas chromatography in the pharmaceutical industry, with a focus on its use in a quality assurance environment. The topics of discussion will be the importance of analyst training, method development considerations, and future trends in GC.

1. Training: The importance of training analysts beyond the basics, in order to improve lab efficiencies, increase employee satisfaction and exceed the Code of Federal Regulations on personnel qualifications.
2. Method Development: Discuss why it is important to focus on the details of analytical instrumentation and techniques during method development. Consideration of the ultimate use of the method must also be taken into account early in the development process.
3. Future Trends in GC: Gas chromatography methods for the pharmaceutical industry in the near future will be discussed, such as, use of general methods, fast GC, and headspace analysis.

Biography: Gregory C. Slack Ph.D. is Manager-Analytical Applications, Technical Transfer and Training, Quality Operations Department at Wyeth Pharmaceuticals in Rouses Point, NY. He has over 10 years experience in the pharmaceutical industry in the areas of research, development, technology transfer and industrial training. Dr. Slack also directs the summer intern program and has been an instructor at numerous short courses in the separation sciences since 1987. He currently holds an adjunct appointment at the Plattsburgh State University of New York where he directs undergraduate research in separation science. He received a B.A. degree in 1985 from Potsdam State University of New York and his Ph.D. from Virginia Tech in 1992.

Speaker 3: Dr. Thomas A. Brettell, Chief Forensic Scientist, State of New Jersey Forensic Science Laboratory Bureau.

Title: "Detection of Gamma-Hydroxybutyrate (GHB) and Gamma-Butyrolactone (GBL) in Forensic Toxicological Investigations Using Headspace GC, SPME, and GC/MS".

Abstract: Gamma-hydroxybutyrate (GHB) has become a popular drug of abuse that has been commonly associated with sexual assault cases (Date rape) throughout the country. GHB is controlled in the United States, but is still abused by bodybuilders as an alternative to anabolic steroids to enhance muscle growth. Others also use GHB and other similar chemicals recreationally for its intoxicating effects as euphoria, reduced inhibitions, and sedation. Because of the use of GHB as a popular club (Rave) drug, an increase has been noted in suspected drunk driving cases in New Jersey. As a result, there has been an increase in requests for GHB analysis and the New Jersey State Police Forensic Laboratory have encountered a number of cases where GHB was detected in suspected drunk drivers. Examples of casework, methodology, and analysis challenges in the detection of GHB in biological fluids will be discussed and presented. Methodology used to detect GHB and related compounds consists of Headspace GC, Headspace SPME, and SPE and GC/MS.

Biography: Thomas A. Brettell is Chief Forensic Scientist of the New Jersey State Police Forensic Science Laboratory Bureau. He received his BA degree (1973) in Chemistry from Drew University, Madison, NJ; a MS degree (1975) in Chemistry from Lehigh University in Bethlehem, PA; and a Ph.D. degree (1987) in Analytical Chemistry from Villanova University, Villanova, PA. Dr. Brettell has worked for the New Jersey State Police Forensic Science Bureau for over 27 years and he presently teaches Forensic Science in the Law and Justice Departments at The College of New Jersey and Rider University. He is past President of the Chromatography Forum of the Delaware Valley and was presented the Chromatography Forum of the Delaware Valley Award in 1997. Dr. Brettell has also served on the Advisory Board of the Journal of Analytical Chemistry from 1996 - 1998. He is presently the Chairman of the Criminalistics Section of the American Academy of Forensic Sciences and a certified Diplomat of the American Board of Criminalistics.

Speakers 4: Richard B. Gaines and Glenn S. Frysinger, Department of Science, U.S. Coast Guard Academy, New London, CT 06320.

Title: "New advances in multidimensional gas chromatography: Fast high resolution separation of complex mixtures using comprehensive two-dimensional gas chromatography (GCxGC)"

Abstract: Under development since the late 1980s, comprehensive two-dimensional gas chromatography (GCxGC) has finally matured into a powerful analytical approach for the separation, identification and quantitation of compounds-of-interest from complex mixtures. GCxGC uses two chromatography columns coupled serially by a thermal modulator to spread mixture components over a two-dimensional retention time plane. The GCxGC two-dimensional separation produces many more resolved peaks than traditional GC methods, and the grouping of peaks in the GCxGC chromatogram facilitates the identification of unknown compounds. Spatial band compression during modulation produces very narrow peaks with increased signal-to-noise ratio, thus improving the detection and quantitation of minor components. GCxGC aids the effectiveness of mass spectrometric detectors by reducing or eliminating coeluents. GCxGC has produced separations approaching a resolved peak per second from complex mixtures containing thousands of components such as petroleum, environmental samples and kerogen pyrolysates. The design and operation of commercially available thermal modulators will be presented. Several applications that highlight the incredible resolving power of GCxGC will be discussed including petroleum analysis, environmental and criminal forensics, and analyses of bio- and geo-chemical importance.

Biography: During his 25 years as a Coast Guard officer, Captain Rick Gaines has interdicted drugs, cleaned up oil and hazardous materials spills, instructed cadets at the Coast Guard Academy, and developed new technology for the Coast Guard’s marine environmental protection mission. Since 1990, he has been a member of the Permanent Commissioned Teaching Staff at the Coast Guard Academy as a Chemistry Professor. He received his BS in Physical Sciences from the Coast Guard Academy in 1978, an MS in Chemistry from UConn in 1981 and a PhD in Chemistry from UConn in 1998 – developing comprehensive two-dimensional gas chromatography technology and applications with Professor Stuart as his major advisor. In addition to his teaching and research, Captain Gaines is also the Assistant Women’s Basketball coach, and administers the cadet sail training program during the summer months.

Speaker 5: Mr. Gary Lavigne, UCONN Institute of Material Science

Title: "A syringeless injection device for the introduction of solids and liquids into a Split / Splitless Capillary Injection Port".

Abstract: A syringeless injection device has been developed to expand the capabilities of Split/Splitless Capillary Injection Ports to include solid sampling. The syringeless injector allows a glass sample vial to be moved into and out of the inject port, by controlled venting of carrier gas. During the injection process the sample vial surrounds the inlet of the capillary column allowing the volatile gases to be swept into the capillary column for collection and separation. This unique arrangement allows for dynamic thermal desorption of solids and liquids directly within the injection port at temperatures from ambient to 400C without the need for external heaters, pressure / flow controllers or transfer lines. The result is greatly enhanced detectability of volatile and semivolatile compounds for both qualitative and quantitative analysis.

Biography: Gary Lavigne is a graduate of Hartford State Technical College with 25 years of experience in Gas Chromatography. The past 22 years he has been managing the Gas Chromatography and Spectroscopy laboratory at the University of Connecticut, Institute of Materials Science. He is the inventor of the Syringeless Injection Device and President of Lavigne Laboratories. He and co-author Myer Ezrin were awarded the Frank Giblin Memorial Award by Society of Plastics Engineers, Polymer Analysis Division, for the best paper presented at the 2002 Annual Technical Conference.

Directions:

General Directions to the UCONN's Nathan Hale Inn & Conference Center

For directions and parking, please assess their web site: http://www.nathanhaleinn.com/

Telephone (860)427-7888 Fax (860)427-7850

Rhode Island:
Take Route 6 West into North Windham. Once in North Windham (past Wal-Mart) take a right onto Route 6 West, take the 1st exit. At the end of the ramp take a right. At the next light take a left onto Route 195 North. Proceed straight for approximately 10 minutes. Take a left onto Mansfield Road (near Fine Arts Complex). Proceed straight to the first stop sign; take a left onto Gilbert Road. Take the 2nd left and the Hotel will be straight ahead.

Stamford:
Take 95 North to 91 North to 84 East. From 84 East, get off at exit 68. Once off exit make a right onto 195 South. Proceed straight for approximately 10 minutes. Once on UConn campus take a right onto Mansfield Road. Proceed straight to 1st stop sign; take a left onto Gilbert Road. Take the 2nd left and the Hotel will be straight ahead.

Boston:
Take 90 West to 84 West. From 84 West, get off at exit 68. Once off exit make a left onto 195 South. Proceed straight ahead for approximately 10 minutes. Once on UConn campus take a right onto Mansfield Road. Proceed straight to 1st stop sign; take a left onto Gilbert Road. Take the 2nd left and the Hotel will be straight ahead.

Springfield/Holyoke:
Take 91 South to 84 East. From 84 East, get off at exit 68. Once off exit make a right onto 195 South. Proceed straight ahead for approximately 10 minutes. Once on UConn campus take a right onto Mansfield Road. Proceed straight to 1st stop sign; take a left onto Gilbert Road. Take the 2nd left and the Hotel will be straight ahead.

Bradley International Airport:
From the airport, take 91 South to 84 East. From 84 East, get off exit 68. Once off exit make a right onto 195 South. Proceed straight for approximately 10 minutes. Once on UConn campus take a right onto Mansfield Road. Proceed straight to 1st stop sign; take a left onto Gilbert Road. Take the 2nd left and the Hotel will be straight ahead.

84 West:
Take exit 68 off of 84 West, from 84 West get off exit 68. Once off exit make a left onto 195 South. Proceed straight for approximately 10 minutes. Once on UConn campus take a right onto Mansfield Road. Proceed straight to 1st stop sign; take a left onto Gilbert Road. Take the 2nd left and the Hotel will be straight ahead.

84 East (Hartford):
From 84 East get off exit 68. Once off exit make a right onto 195 South. Proceed straight for approximately 10 minutes. Once on UConn campus take a right onto Mansfield Road. Proceed straight to 1st stop sign; take a left onto Gilbert Road. Take the 2nd left and the Hotel will be straight ahead.


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