Use of pressurized liquid extraction (PLE)/gas chromatography–electron capture detection (GC–ECD) for the determination of biodegradation intermediates of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) in soils

2005 ◽  
Vol 824 (1-2) ◽  
pp. 277-282 ◽  
Author(s):  
B ZHANG ◽  
X PAN ◽  
G COBB ◽  
T ANDERSON
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Liquid Extraction ◽  
Pressurized Liquid Extraction ◽  
Electron Capture Detection

Determination of Bromate Ions in Drinking Water by Derivatization with 2-Methyl-2-Butene, Dispersive Liquid-Liquid Extraction and Gas Chromatography-Electron Capture Detection

2020 ◽  
Vol 103 (5) ◽  
pp. 1243-1249
Author(s):  
Mehdi Nabi ◽  
Sayed Mehdi Ghoreishi ◽  
Mohsen Behpour
Keyword(s):  
Gas Chromatography ◽  
Detection Limit ◽  
Electron Capture ◽  
Liquid Extraction ◽  
International Standards ◽  
Electron Capture Detection ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Derivatizing Agent

Abstract Background A simple, rapid, selective and sensitive sample preparation and derivatization method was performed for determination of bromate ions in water by means of dispersive liquid-liquid extraction (DLLE) by gas chromatography-electron capture detection (GC-ECD). This method is based on 2-methyl-2-butene derivatization by bromine produced from bromate ions in acidic medium and extraction by n-hexane. Objective Derivatizing agent: It is cheap and available and it has high efficiency in reaction with Br2. Simplicity: Preparation and extraction process don't need to any specific equipment and procedure is completely simple and fast. Limit of detection: DL is as low as 0.43 µg/L. Methods Various effective factors on the derivatization and extraction efficiency, such as amount of derivatizing agent, volume of extraction solvent, bromide concentration, volume and concentration of sulfuric acid, type and volume of extracting and dispersing solvent, ionic strength, storage time before extraction and ECD makeup-gas flow rate were investigated. Results Under the optimum conditions, the method had a linear calibration curve ranging from 1.0 to 200.0 µg/L for bromate ions with a determination coefficient (R2) of 0.994 and the detection limit was 0.43 µg/L. The recovery percent and relative standard deviation for the determination of 1.0, 5.0 and 50.0 µg/L bromate ion was between 90 and 110%, and 3.0 and 8.0% (n = 3), respectively. Conclusions Finally, the method was successfully applied for the preconcentration and determination of bromate ions in water samples, and satisfactory results were obtained. Highlights (1) Fast, easy, accurate and economical innovative analysis of bromate ions in water and wastewater. (2) Determination of inorganic ion by GC-ECD after derivatization (3) Low detection limit (4) Optimization of different method parameters to obtain accurate results based on requirements of international standards, specifically ISO/IEC 17025.

Residue Analysis of Organophosphorus and Organochlorine Pesticides in Fatty Matrices by Gas Chromatography Coupled with Electron-Capture Detection

2006 ◽  
Vol 61 (5-6) ◽  
pp. 341-346 ◽  
Author(s):  
Jae-Woo Park ◽  
A. M. Abd El-Aty ◽  
Myoung-Heon Lee ◽  
Sung-Ok Song ◽  
Jae-Han Shim
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Simple Procedure ◽  
Linear Regression Analysis ◽  
Residue Analysis ◽  
Electron Capture Detection ◽  
Relative Standard ◽  
Wide Range ◽  
Repeatability And Reproducibility

A multiresidue method for the simultaneous determination of 22 organochlorine (OCs) and organophosphorus (Ops) pesticides (including isomers and metabolites), representing a wide range of physicochemical properties, was developed in fatty matrices extracted from meat. Pesticides were extracted from samples with acetonitrile/n-hexane (v :v, 1:1). The analytical screening was performed by gas chromatography coupled with electron-capture detection (ECD). The identification of compounds was based on their retention time and on comparison of the primary and secondary ions. The optimized method was validated by determining accuracy (recovery percentages), precision (repeatability and reproducibility), and sensitivity (detection and quantitation limits) from analyses of samples fortified at 38 to 300 ng/g levels. Correlation coefficients for the 22 extracted pesticide standard curves (linear regression analysis, n = 3) ranged from 0.998 to 1.000. Recovery studies from 2 g samples fortified at 3 levels demonstrated that the GC-ECD method provides 64.4-96.0% recovery for all pesticides except 2,4′-DDE (44.6-50.4%), 4,4′-DDE (51.1-57.5%) and 2,4′-DDT (50.0-51.2%). Both repeatability and reproducibility relative standard deviation values were < 20% for all residues. Detection limits ranged from 0.31 to 1.27 ng/g and quantification limits were between 1.04 and 4.25 ng/g. The proposed analytical method may be used as a simple procedure in routine determinations of OCs and Ops in meat. It can also be applied to the determination of pesticide multi-residues in other animal products such as butter and milk.

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