Bill Winniford

Comprehensive two dimensional gas chromatography review

Advances, developments and applications in 2-D comprehensive GC (GC x GC) from 2007 through October 2008 are reviewed, with emphasis on modulation, and data handling, and applications of current relevance. Industrial perspectives as well as suggestions where further developments would be beneficial are summarized in the concluding remarks.

Dual-purpose gas chromatographic injection device for pressurized liquid and gas injection

A dual-purpose gas chromatographic injection device, capable of injecting pressurized liquid sample of up to 5000 psig and gas sample with a volume as high as 5000 microL, has been successfully developed and implemented. The injection device is synergized by the effectiveness of a classical flash vaporization of a syringe injection and the reliability of a proven rotary valve. Depending on the matrix involved, this injection device employs either a commercially available four-port internal valve for liquid sampling or a six-port external valve for gas sampling, a modified removable needle used in standard liquid syringe, and an auxiliary flow stream that can be either mechanical or electronic flow controlled for solute transfer. For pressurized liquid, the device was found suitable of up to nC(16) hydrocarbon with no observable carry-over despite the injection device was operating at ambient temperature. A relative standard deviation of less than 2% (n=20) was obtained for hydrocarbon compounds ranging from nC(8) to nC(16). For gas injection, the device performed well even under difficult chromatographic conditions such as with a low column inlet pressure of less than 1 psig. A relative standard deviation of less than 0.5% (n=10) was obtained for reactive sulfur compounds such as alkyl mercaptans. The device can be operated manually or automated with pneumatic or electrical actuator, is platform neutral, and can be moved amongst instruments without hardware modification as well as implemented for on-line or in situ applications. In this paper, the utility of the device was also demonstrated with selected GC applications of industrial significance.

Determination of short-chain branching content in polyethylene by pyrolysis comprehensive multidimensional gas chromatography using low thermal mass column technology

A research effort was undertaken to utilize the pyrolysis process to create fragments of polyethylene that could be indicative of branching, and allow quantitiation of said short-chain branches by pyrolysis comprehensive 2-D GC (Py-GC x GC). Several strategies for sample introduction and pyrolysis such as the in-column pyrolysis device and the programmed temperature vaporizer (PTV) were studied. The chromatographic separations were executed using low-thermal mass (LTM) comprehensive 2-D GC (GC x GC). A series of polyethylene-co-hexene samples were analyzed and a linear correlation of 1-hexene content with branching peak ratio was found. Correlation coefficients were determined as 0.97 for the measurements performed.