Comprehensive supercritical fluid extraction/gas chromatographic analysis for organic compounds in soil matrices with an element-selective radiofrequency plasma detector

Wu, Mingin; Liu, Zaiyou; Farnsworth, Paul B.; Lee, Milton L.

doi:10.1021/ac00065a004

Cited by 19 publications

(6 citation statements)

References 9 publications

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“…A description of the modulator and its use as an interface between SFE and GC have been recently published [8,10,12]. For these experiments the TDM was constructed from 8 cm of the front portion of the analytical column by repetitively coating that segment with automotive window defroster paint and drying with a heat gun until the resistance reached approximately 2.0 ohms.…”

Section: Methodsmentioning

confidence: 99%

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Supercritical fluid extraction/gas chromatography with thermal desorption modulator interface and nitro‐specific detection for the analysis of explosives

Francis

Farnsworth

et al. 1995

J Microcolumn Separations

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Abstract. Supercritical fluid extraction (SFE) can greatly reduce the sample preparation time of analytes in solid matrices. The on-line coupling of SFE with high-speed gas chromatography (GC) can further reduce the total analysis time. SFE has been coupled to GC with a thermal desorption modulator (TDM) interface. A thermal energy analyzer (TEA), a chemiluminescence detector which is specific for nitro and nitroso compounds, has been coupled to the system to analyze explosives in soil samples.The use of organic modifiers to increase the solvation power of carbon dioxide was necessary for the extraction of various explosives, and did not adversely affect the performance of the system. Thermally labile compounds, however, such as the nitrate esters, were shown to decompose in the modulator before the chromatographic separation.This method allows for the rapid analysis of relatively volatile and thermally stable nitro compounds from solid matrices. The system can be used for screening small samples in short periods of time. Total analysis can be completed in less than 10 minutes and requires only 200 mg of soil. The minimum detectable quantity for the analysis of 2,4-DNT was found to be 2.6 ppb in an actual soil sample.

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Section: Methodsmentioning

confidence: 99%

“…The benefit of eliminating interferences from co-eluting compounds is obtained by the use of selective detection for the analytes of interest. Wu et al used a radiofrequency plasma detector with an SFE/GC system for the selective detection of chlorine and sulfur in pesticide contaminated soil [12].…”

Section: Introductionmentioning

confidence: 99%

Supercritical fluid extraction/gas chromatography with thermal desorption modulator interface and nitro‐specific detection for the analysis of explosives

Francis

Farnsworth

et al. 1995

J Microcolumn Separations

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“…Supercritical fluid extraction, supercritical fluid chromatography, high-temperature capillary gas chromatography, and high-performance liquid chromatography address the issue of quantifying semivolatile and heavier hydrocarbons in petroleum products (Akhlaq, 1993;ASTM, 1984;DeAngelis, 1987;Di Sanzo and Yoder, 1991;George, 1994;King, 1989;Leazar, 1986;Lee, 1994;Levy etal, 1989;Lopez-Avila etal, 1992. McCormick et al, 1991Maynard and Michalik, 1988;Rhodes et al, 1991;Tong et al, 1993;Trestlano et al, 1985;Wu et al, 1993). Every method or protocol has its limitations, and these limitations must be defined so that its usefulness in a particular application can be ascertained.…”

Section: Introduction /mentioning

confidence: 99%

Determination of gasoline range, diesel range, and mineral oil range organics in soils and water by flame lonization gas chromatography

Sawyer

1996

Journal of Soil Contamination

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To cite this article: G. M. Sawyer (1996) Determination of gasoline range, diesel range, and mineral oil range organics in soils and water by flame lonization gas chromatography, Journal of Soil Contamination, 5:3, 261-300, This article describes a method for the determination of gasoline range, diesel range, and mineral oil range organics in soils and water. It represents the culmination of a series of efforts to go beyond typical GRO and DRO methodology currently available in the literature to include a quantitative determination of mineral oil organics having a boiling range up to C 44 . It also is the result of an attempt to develop a cost-effective method that enables the analyst to quantify three different types of hydrocarbon components in one GC run under conditions without a concentration step. Method performance is comparable to that of current protocols for GRO and DRO determinations and validated further by comparisons to certified standards and in-house standards. Accuracy as percentage recovery for GRO in water is 82 to 84 and 91 to 92% for soils. Accuracy as percentage recovery for MRO in water is 84 to 102 and 75 to 80% for soils. Accuracy as percentage recovery for DRO in water is 78 to 100 and 71 to 90% for soils.Results from the analysis of in-house standards and certified standards for DRO and MRO gave higher recoveries than was demonstrated in the MDL studies. The MDL for DRO in water is 31 mg/l and 14 mg/kg for soils. The MDL for GRO in water is 8 mg/l and 4 mg/kg for soils. For MRO in water, the MDL is 7 mg/l and for soils 10 mg/kg. Future proposed improvements to this method will involve updated software that will allow automatic blank subtraction, automatic calculation of surrogate recoveries and the automatic incorporation of dry weight factors in the final calculations for soils. In addition, a GRO method with a run time of only 24 min will be used routinely when only GRO analyses have to be performed.

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“…Therefore, in the present work, a 350 kHz helium plasma was utilized due to the straightforward energy coupling and because of the excellent analytical properties, as demonstrated for gas chromatographic detection. [24][25][26][27][28][29][30][31][32][33][34][35][36][37] To enhance the sensitivity of the method, the extraction solvent was evaporated prior to analysis. The solid sample was subsequently introduced at the plasma inlet by a sample probe.…”

mentioning

confidence: 99%

“…Microwaves have frequently been applied to sustain small helium plasmas, but the energy coupling is relatively complicated and requires the use of special cavities. Therefore, in the present work, a 350 kHz helium plasma was utilized due to the straightforward energy coupling and because of the excellent analytical properties, as demonstrated for gas chromatographic detection. − To enhance the sensitivity of the method, the extraction solvent was evaporated prior to analysis. The solid sample was subsequently introduced at the plasma inlet by a sample probe.…”

mentioning

confidence: 99%

Determination of Extractable Organic Chlorine and Bromine by Probe Injection Dual-Microplasma Atomic Emission Spectrometry

1997

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A probe injection dual-microplasma spectrometer is evaluated as a low-cost alternative for the determination of extractable organic chlorine and bromine (EOCl and EOBr). The system consists of two 350 kHz plasmas sustained in the same stream of helium and a probe for sample application in the interplasma region. The sample was applied with a microsyringe into a small cup on the sample probe. Subsequently, the extraction solvent was gently evaporated, and the sample cup was pushed into the interplasma region. The first plasma was in direct contact with the sample probe and served to rapidly vaporize the sample material. The vaporized sample was then transferred to the second plasma, where atomic emission was measured for the determination of EOCl and EOBr. For both Cl and Br, 120 pg detection limits and 1000:1 halogen-to-carbon selectivities were obtained, and responses were linear over 3 orders of magnitude.

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Comprehensive supercritical fluid extraction/gas chromatographic analysis for organic compounds in soil matrices with an element-selective radiofrequency plasma detector

Cited by 19 publications

References 9 publications

Supercritical fluid extraction/gas chromatography with thermal desorption modulator interface and nitro‐specific detection for the analysis of explosives

Supercritical fluid extraction/gas chromatography with thermal desorption modulator interface and nitro‐specific detection for the analysis of explosives

Determination of gasoline range, diesel range, and mineral oil range organics in soils and water by flame lonization gas chromatography

Determination of Extractable Organic Chlorine and Bromine by Probe Injection Dual-Microplasma Atomic Emission Spectrometry

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