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Luong J.,University of Tasmania | Luong J.,Dow Chemical Company | Gras R.,Dow Chemical Company | Cortes H.J.,University of Tasmania | And 2 more authors.
Analytical Chemistry | Year: 2013

A portable, fast gas chromatographic method for the direct measurement of the parts per billion level of sulfur-free odorants in commercially available natural gas is introduced. The approach incorporates a resistively heated, temperature-programmable silicon micromachined gas chromatograph that employs a standard capillary column for the fast separation of methyl and ethyl acrylate from the natural gas matrix. The separation approach is coupled to a micromachined differential mobility detector to enhance analyte detectability, and the overall selectivity obtained against the matrix is described. A complete analysis can be conducted in less than 70 s. Furthermore, these two compounds can be measured accurately in the presence of other common volatile sulfur-based odorants such as alkyl mercaptans and alkyl sulfides. Repeatability of less than 3% RSD (n = 20) over a range from 0.5 to 5 ppm was obtained with a limit of detection for the target compounds at 50 ppb (v/v) and a linear range from 0.5 to 50 ppm with a correlation coefficient of at least 0.997. © 2013 American Chemical Society. Source


Luong J.,University of Tasmania | Luong J.,Dow Chemical Company | Shellie R.A.,University of Tasmania | Cortes H.,University of Tasmania | And 3 more authors.
Journal of Chromatography A | Year: 2012

Steam condensate water treatment is a vital and integral part of the overall cooling water treatment process. Steam condensate often contains varying levels of carbon dioxide and oxygen which acts as an oxidizer. Carbon dioxide forms corrosive carbonic acid when dissolved in condensed steam. To neutralize the harmful effect of the carbonic acid, volatile amine compounds such as morpholine, cyclohexylamine, and diethylaminoethanol are often employed as part of a strategy to control corrosion in the water treatment process. Due to the high stability of these compounds in a water matrix, the indirect addition of such chemicals into the process via steam condensate often results in their presence throughout the process and even into the final product. It is therefore important to understand the impact of these chemicals and their fate within a chemical plant. The ability to analyze such compounds by gas chromatography has historically been difficult due to the lack of chromatographic system inertness at the trace level concentrations especially in an aqueous matrix. Here a highly sensitive, practical, and reliable gas chromatographic approach is described for the determination of morpholine, cyclohexylamine, and diethylaminoethanol in steam condensate at the part-per-billion (ppb) levels. The approach does not require any sample enrichment or derivatization. The technique employs a multi-mode inlet operating in pulsed splitless mode with programmed inlet temperature for sample introduction, an inert base-deactivated capillary column for solute separation and flame ionization detection. Chromatographic performance was further enhanced by the incorporation of 2-propanol as a co-solvent. Detection limits for morpholine, cyclohexylamine, diethylaminoethanol were established to be 100. ppb (v/v), with relative standard deviations (RSD) of less than 6% at the 95% confidence level (n= 20) and a percent recovery of 96% or higher for the solutes of interest over a range of 0.1-100. ppm (v/v). A complete analysis can be conducted in less than 10. min. © 2012 Elsevier B.V. Source


Luong J.,University of Tasmania | Luong J.,Dow Chemical Company | Gras R.,Dow Chemical Company | Hawryluk M.,Dow Chemical Company | And 3 more authors.
Journal of Chromatography A | Year: 2013

Volatile organic compounds such as light hydrocarbons, dienes, and aromatic compounds are often encountered in the manufacturing and processing environments of chemical and petrochemical segments. These compounds need to be closely monitored for process optimization, plant maintenance and industrial hygiene purposes. A high throughput analytical approach has been successfully developed and implemented for the accurate measurement of fourteen commonly encountered analytes. The approach incorporates a recently introduced 5-port planar microfluidic device configured for use as a Deans switch for multidimensional gas chromatography. The use of multidimensional gas chromatography allows the elimination of potential chromatographic contaminants with a substantial enhancement of stationary phase selectivity via the use of columns with different separation mechanisms, and the back-flushing of heavier undesired hydrocarbons. A low thermal mass gas chromatographic module was employed in the second dimension of the two-dimensional gas chromatography system and was used to provide independent temperature control, and rapid heating and cooling to meet the high throughput requirements. By successfully combining these concepts, complete analysis of fourteen targeted components can be conducted in less than 120s. Repeatability of retention times for all compounds was found to be less than 0.05% (n=20). Repeatability of area counts at two levels, namely 10ppmv and 1000ppmv over a period of two days was found to be less than 3% (n=20). Apart from methane, which has a detection limit of 0.4ppmv, the rest of the compounds were found to have detection limits of less than 0.2ppmv. Compounds of interest were found to be linear over a range of 500ppbv-3000ppmv with correlation coefficients greater than 0.999. © 2013 Elsevier B.V. Source


Luong J.,University of Tasmania | Luong J.,Dow Chemical Company | Gras R.,Dow Chemical Company | Cortes H.J.,University of Tasmania | And 2 more authors.
Journal of Chromatography A | Year: 2013

An integrated gas chromatographic system has been successfully developed and implemented for the measurement of oxygen, nitrogen, carbon monoxide, carbon dioxide and light hydrocarbons in one single analysis. These analytes are frequently encountered in critical industrial petrochemical and chemical processes like catalytic cracking of naphtha or diesel fuel to lighter components used in gasoline. The system employs a practical, effective configuration consisting of two three-port planar microfluidic devices in series with each other, having built-in fluidic gates, and a mid-point pressure source. The use of planar microfluidic devices offers intangible advantages like in-oven switching with no mechanical moving parts, an inert sample flow path, and a leak-free operation even with multiple thermal cycles. In this way, necessary features such as selectivity enhancement, column isolation, column back-flushing, and improved system cleanliness were realized. Porous layer open tubular capillary columns were employed for the separation of hydrocarbons followed by flame ionization detection. After separation has occurred, carbon monoxide and carbon dioxide were converted to methane with the use of a nickel-based methanizer for detection with flame ionization. Flow modulated thermal conductivity detection was employed to measure oxygen and nitrogen. Separation of all the target analytes was achieved in one single analysis of less than 12min. Reproducibility of retention times for all compounds were found to be less than 0.1% (n=20). Reproducibility of area counts at two levels, namely 100ppmv and 1000ppmv over a period of two days were found to be less than 5.5% (n=20). Oxygen and nitrogen were found to be linear over a range from 20ppmv to 10,000ppmv with correlation coefficients of at least 0.998 and detection limits of less than 10ppmv. Hydrocarbons of interest were found to be linear over a range from 200ppbv to 1000ppmv with correlation coefficients of greater than 0.999 and detection limits of less than 100ppbv. © 2012 Elsevier B.V. Source


Luong J.,University of Tasmania | Luong J.,Dow Chemical Company | Gras R.,Dow Chemical Company | Cortes H.,University of Tasmania | And 2 more authors.
Journal of Chromatography A | Year: 2012

Oxygenated compounds like methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, acetaldehyde, crotonaldehyde, ethylene oxide, tetrahydrofuran, 1,4-dioxane, 1,3-dioxolane, and 2-chloromethyl-1,3-dioxolane are commonly encountered in industrial manufacturing processes. Despite the availability of a variety of column stationary phases for chromatographic separation, it is difficult to separate these solutes from their respective matrices using single dimension gas chromatography. Implemented with a planar microfluidic device, conventional two-dimensional gas chromatography and the employment of chromatographic columns using dissimilar separation mechanisms like that of a selective wall-coated open tubular column and an ionic sorbent column have been successfully applied to resolve twelve industrially significant volatile oxygenated compounds in both gas and aqueous matrices. A Large Volume Gas Injection System (LVGIS) was also employed for sample introduction to enhance system automation and precision. By successfully integrating these concepts, in addition to having the capability to separate all twelve components in one single analysis, features associated with multi-dimensional gas chromatography like dual retention time capability, and the ability to quarantine undesired chromatographic contaminants or matrix components in the first dimension column to enhance overall system cleanliness were realized. With this technique, a complete separation for all the compounds mentioned can be carried out in less than 15. min. The compounds cited can be analyzed over a range of 250. ppm (v/v) to 100. ppm (v/v) with a relative standard deviation of less than 5% (n= 20) with high degree of reliability. © 2012 Elsevier B.V. Source

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