Practical experience with a microwave plasma detector limits of measurement and examples of applications

Brenner, K.S.

doi:10.1016/s0021-9673(00)91170-1

Cited by 60 publications

(16 citation statements)

References 2 publications

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“…If the analyte did contain oxygen at measurable levels, the negative peak was preceded by a positive inflection in the chromatogram. This effect was documented in several publications (Brenner 1978;Slatkavitz, Uden, and Barnes 1986) and was observed in our laboratory. Thus, we were not able to obtain sufficient background reduction for oxygen or nitrogen to enable use of the GC-MIP for these elements.…”

Section: Identification Of Background Sourcessupporting

confidence: 81%

“…In its initial stages, most of the work with the GC-MIP used packed columns and dealt with standard compounds in single-element mode. Later studies incorporated the use of capillary columns (e.g., Quimby et al 1980;Wasik and Schwarz 1980;Hanie et al 1981;Estes, Uden, and Barnes !981) or polychromators (e.g., Bonnekessel and Klier 1978;Brenner 1978;Windsor and Denton 1979;Eckhoff, Ridgway, and Caruso 1983). The plasma portion of the GC-MIP technique has also evolved since its introduction.…”

Section: Introductionmentioning

confidence: 99%

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Multielement detector for gas chromatography

Sklarew¹,

Evans²,

Olsen³

1988

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This report describes the results of a study to improve the capabilities of a gas chromatography-microwave-induced plasma (GC-MIP) detector system, determine the feasibility of empirical formula determination for simple mixtures containing elements of interest to fossil fuel analysis and, subsequently, explore applications for analysis of the complex mixtures associated with fossil fuels. The results of this study indicate that the GC-MJP system is useful as a specific-element detector that provides excellent elemental specificity for a number of elements of interest to the analysis of fossil fuels. It has reasonably good sensitivity for carbon, hydrogen, sulfur, and nickel, and better sensitivity for chlorine and fluorine. Sensitivity is poor for nitrogen and oxygen, however, probably because of undetected leaks or erosion of the plasma tube. The GC-MIP can also provide stoichiometric information about components of simple mixtures. If this powerful technique is to be available for complex mixtures, it will be necessary to greatly simplify the chromatograms by chemical fractionation. i i ; A low-pressure version of a Beenakker source was designed and constructed that combined the most attractive features of the existing atmospheric-pressure Beenakker and the low-pressure Evenson sources. This new source proved to be excellent for the measurement of carbon, hydrogen, and sulfur, showing reasonably good sensitivity and good stability. Optimal operating parameters, including helium flow, scavenge gas flow, power level, and operating pressure, were determined for this source for C, H, N, S, and Cl. Parameters were chosen to minimize variation in elemental ratios resulting from instabilities in flow rates and power setting. v Vi Application of the GC-MIP technique to the complex mixtures found in fossil fuels was the final part of this study. Three different types of fossil fuels were used to explore these applications. Sulfur-, oxygen-, and nickel-containing species were considered. A series of alkylthiophenes and dimethyl disulfide were identified and quantitated in an oil shale retort gas condensate. The GC-MIP technique was successful in selectively detecting the sulfur components in this complex mixture, in concentrations ranging from 1.5 to 10.7 mol ppm. The detection limit was approximately 2 ng methylthiophene injected into the GC-MIP system. Attempts to determine stoichiometry of the sulfur components by comparison of carbon, hydrogen, and sulfur ratios with those of standards were unsuccessful because of the complexity of the carbon and hydrogen chromatograms. Aluminum-coated methyl-silicone capillary columns, which could withstand oven temperatures as high as 400•c, were successfully used to chromatograph several relatively nonvolatile porphyrin compounds. The GC-MIP system was able to detect a nickel(II)-etioporphyrin standard at a detection limit of approximately 200 ng porphyrin injected (or about 20 ng nickel injected). However, it was not able to detect nickel porphyrins in the appropriate fractions o...

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Section: Identification Of Background Sourcessupporting

confidence: 81%

Section: Introductionmentioning

confidence: 99%

Multielement detector for gas chromatography

Sklarew¹,

Evans²,

Olsen³

1988

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“…The actual coupling procedure is described in detail in the literature (4). A siliconized glass column (2 mm i.d., 2 m long) packed with 3 % SE 30 on Chromosorb Q 100-120 mesh was used.…”

Section: Gas Chromatography/microwave Plasma Detector (Gc/mpd)mentioning

confidence: 99%

The metabolic fate of2H-labelled propafenone in man

Hege

Hollmann

Kaumeier

et al. 1984

European Journal of Drug Metabolism and Pharmacokinetics

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The metabolism of propafenone was studied in three humans by using 300 mg of the deuterated compound given orally. The excretion of propafenone and its metabolites was assessed by measuring the deuterium content in the excretion products by means of a microwave plasma detector. At selected times the metabolic pattern in plasma, urine, bile and feces was determined. The metabolites were isolated and the structure of the main compounds was characterized. Propafenone is absorbed completely and quantitatively metabolized. Unchanged propafenone is excreted neither in the urine nor in the feces in amounts of more than 1% the dose. The percentage of free unconjugated propafenone of the total deuterium content in the plasma was about 10% 3 and 6 hours after application. Conjugates of hydroxylated derivatives of propafenone are present predominantly in the plasma. The excretion of the metabolites takes place mainly by way of the feces, 53% of the dose is excreted by this route within 48 hours. Urinary elimination accounted for 18.5 and 38% of the dose within 48 hours in two humans. It was possible to elucidate the structure of 11 metabolites, accounting for more than 90% of the dose administered. The major metabolites are conjugates of 5-hydroxypropafenone and hydroxy-methoxy-propafenone with glucuronic and sulphuric acid and propafenone glucuronide. Furthermore, metabolic products of oxydative deamination pathway were identified, i.e. a glycol and a lactic acid derivative. C-C splitting yields a relatively large amount of 3-phenyl-propionic acid, while cleavage of the ether group leads to a phenolic product and is only of minor importance.

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“…The performance of a commercial GC-MIP instrument using a multi-channel polychromator spectrometer was reported by Brenner [60]. For a helium plasma at 0.5-3 torr with oxygen or nitrogen scavenger gas, detection limits ranged from 0.02 ng/s for bromine to 4 ne/s for oxygen.…”

Section: Analytical Gc Applicationsmentioning

confidence: 95%

Determination of trace elements by chromatographic methods employing atomic plasma emission spectroscopic detection

Uden

1994

Determination of Trace Elements

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Practical experience with a microwave plasma detector limits of measurement and examples of applications

Cited by 60 publications

References 2 publications

Multielement detector for gas chromatography

Multielement detector for gas chromatography

The metabolic fate of2H-labelled propafenone in man

Determination of trace elements by chromatographic methods employing atomic plasma emission spectroscopic detection

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