Expanded utility of the Beilstein flame test for organically bound halogens as a sensitive and specific flame photometric detector in the gas chromatographic determination of R-X compounds as illustrated with organochlorine pesticides

1969 ◽  
Vol 4 (4) ◽  
pp. 202-213 ◽  
Author(s):  
F. A. Gunther ◽  
A. Lopez-Roman ◽  
R. I. Asai ◽  
W. E. Westlake
Keyword(s):  
Organochlorine Pesticides ◽  
Chromatographic Determination ◽  
Flame Photometric Detector ◽  
Photometric Detector

Gas Chromatographic Determination of Ametryn and Its Metabolites in Tropical Root Crops

1984 ◽  
Vol 67 (2) ◽  
pp. 280-284
Author(s):  
Promode C Bardalaye ◽  
Willis B Wheeler
Keyword(s):  
Anhydrous Sodium Sulfate ◽  
Residue Analysis ◽  
Gel Permeation Chromatography ◽  
Chromatographic Determination ◽  
Solvent System ◽  
Complete Separation ◽  
Flame Photometric Detector ◽  
Root Crops ◽  
Photometric Detector

Abstract Residue analysis of the herbicide ametryn (2-methyIthio-4-ethylamino-s-isopropylamino-s-triazine) is widely known but an analytical method for determining its metabolites has not yet been reported in the literature. A method has been developed for the extraction and determination of ametryn and 3 metabolites, 2-methylthio-4-amino-6-isopropylammo- s-triazine (GS-11354), 2-methylthio-4,6-diamino-.s-triazine(GS- 26831), and 2-methylthio-4-amino-6-ethylamino-s-triazine (GS-11355) in taniers, yams, cassava. Residues were extracted from crops with ethyl acetate-toluene (3 + 1 v/v), using a Polytron homogenizer and anhydrous sodium sulfate added for drying. The extracts were cleaned up by automated gel permeation chromatography on Bio-Beads SX-3 gel in the same solvent system. Quantitative determination was performed by gas chromatographic (GC) analysis on a column packed with 5% DEGS-PS on 100-120 mesh Supelcoport using either an N-P detector or a flame photometric detector (FPD) in the sulfur mode. Minimum detection by the flame photometric detector is 10 ng each for ametryn, GS-11354, and GS-11355 and 21 ng for GS-26831; by the N-P detector, 0.3 ng of each component gives easily quantitatable peaks. On a parts per million basis, starting with 25 g sample, the FPD detected a minimum level of 0.04 p.g/g each for ametryn, GS-11354, and GS-11355, and 0.08 p.g/g for GS-26831. The N-P detector could detect 0.0024 p.g/g for all 4 compounds. In addition to superior sensitivity, instrumental conditions allowed the complete separation of components in 10 min, for the N-P detector; more than 30 min was required for the FPD. Recoveries from fortified crops ranged from 67 to 111% at levels of 0.1-1.0 μg/g.

Gas Chromatographic Determination of Ethylene Thiourea Residues

1973 ◽  
Vol 56 (2) ◽  
pp. 333-337 ◽  
Author(s):  
Linwood D Haines ◽  
Irving L Adler
Keyword(s):  
Gas Chromatography ◽  
Sodium Borohydride ◽  
Chromatographic Determination ◽  
Food Crops ◽  
Alumina Column ◽  
Flame Photometric Detector ◽  
Photometric Detector ◽  
Ethylene Thiourea

Abstract Residues of ethylene thiourea on food crops are determined by extracting the sample with methanol, partially purifying the extract on an alumina column, and derivatizing the ethylene thiourea extracted with 1-bromobutane in the presence of dimethylformamide and sodium borohydride. The resulting derivative is measured by gas chromatography, using a flame photometric detector. The method is suitable for routine use and is sensitive to 0.01 ppm.

Gas-Liquid Chromatographic Determination of Sodium Bisulfite in Complex Matrices

1979 ◽  
Vol 62 (1) ◽  
pp. 15-18
Author(s):  
John J Czarnecki ◽  
Walter R Koehler ◽  
Aaron D Cooper
Keyword(s):  
Chromatographic Determination ◽  
Sodium Bisulfite ◽  
Experimental Conditions ◽  
Flame Photometric Detector ◽  
Photometric Detector ◽  
Specificity And Sensitivity ◽  
Combined Use ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic (GLC) headspace technique is described for determining sodium bisulfite in a dermatological cream. The sample is dispersed in an aqueous medium and acidified to convert sulfite to volatile sulfur dioxide which partitions into the headspace. An aliquot of the headspace vapor is analyzed by GLC using the sulfur-selective flame photometric detector. Advantages of the method include the facility of sample preparation, the specificity and sensitivity resulting from the combined use of the headspace technique and the flame photometric detector, and the applicability of the method to various types of sample matrices. Recoveries ranged from 95 to 102% for spiked samples containing 200—2000 ppm sodium bisulfite. For the sample size and experimental conditions used in this application, the detection limit is 0.02 mg sodium bisulfite.

Rapid Cleanup Procedure for Gas-Liquid Chromatographic Determination of Chlorpyrifos-Methyl Residues in Cat Food

1981 ◽  
Vol 64 (5) ◽  
pp. 1227-1231
Author(s):  
Richard A Simonaitis ◽  
R Spencer Cail ◽  
James M Zehner
Keyword(s):  
Chromatographic Determination ◽  
Flame Photometric Detector ◽  
Integration Limit ◽  
Photometric Detector ◽  
Limit Of Determination ◽  
Cleanup Procedure ◽  
Liquid Chromatographic Determination ◽  
Electronic Integration ◽  
Liquid Chromatographic

Abstract A simple and rapid gas-liquid chromatographic (GLC) method was developed for the determination of residues of chlorpyrifos-methyl in dry cat food. Cat food fortified with chlorpyrifos-methyl was extracted with acetone and cleaned up on a modified acetonitrile-on-Florisil partitioning column. The chlorpyrifos-methyl was determined by GLC with a flame photometric detector. Results were compared with those for known standards that had undergone the same cleanup procedure. The quantitative electronic integration limit of determination was 0.03 ppm. Average recoveries for 5 analyses at fortification levels from 0.052 to 51 ppm ranged from 90 to 102% and averaged 97%.

A Rapid Specific Method for the Gas Chromatographic Determination of Organophosphate Pesticides in Cold Pressed Citrus Oils

1967 ◽  
Vol 50 (6) ◽  
pp. 1236-1242
Author(s):  
Robert K Stevens
Keyword(s):  
Analytical Procedure ◽  
Chromatographic Determination ◽  
Specific Method ◽  
Organophosphate Pesticides ◽  
Gas Chromatograph ◽  
Flame Photometric Detector ◽  
Photometric Detector ◽  
Cold Pressed

Abstract Organophosphate pesticides in cold pressed citrus oils can be determined rapidly by a method using gas chromatographic procedures and the flame photometric detector developed by Brody and Chaney. This study revealed that cold pressed citrus oils obtained from the 1965— 1966 citrus crops from Florida and California contained from 1.5 to 20 ppm thiophosphate pesticides. The analytical procedure required approximately 40 min per analysis and eliminated the need for extensive preparation of the sample prior to introduction into the gas chromatograph. The procedure is more specific and less time consuming than methods previously described

Herbicidal Carbamates: Extraction, Cleanup, and Gas Chromatographic Determination by Thermionic, Electron Capture, and Flame Photometric Detectors

1971 ◽  
Vol 54 (6) ◽  
pp. 1366-1370 ◽  
Author(s):  
John H Onley ◽  
George Yip
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Chromatographic Determination ◽  
Food Crops ◽  
Water Mixture ◽  
Flame Photometric Detector ◽  
Photometric Detector ◽  
Electron Capture Detectors ◽  
Cellulose Column

Abstract Extraction, cleanup, and gas chromatographic procedures have been developed for the determination of carbamate herbicides in food crops. Each sample is extracted with ethanol or an ethanol-water mixture and then cleaned up on a MgO-cellulose column. Determinations are made by gas chromatography, using thermionic and electron capture detectors; a flame photometric detector may also be used to quantitate and confirm those carbamates containing sulfur. Recoveries from apples, potatoes, alfalfa, corn, and soybeans at fortification levels of 0.01 to 10 ppm exceeded 80%.

Improved Multiresidue Gas Chromatographic Determination of Organophosphorus, Organonitrogen, and Organohalogen Pesticides in Produce, Using Flame Photometric and Electrolytic Conductivity Detectors

1981 ◽  
Vol 64 (5) ◽  
pp. 1187-1195 ◽  
Author(s):  
Milton A Luke ◽  
Jerry E Froberg ◽  
Gregory M Doose ◽  
Herbert T Masumoto
Keyword(s):  
Petroleum Ether ◽  
Methylene Chloride ◽  
Organophosphorus Pesticides ◽  
Chromatographic Determination ◽  
Electrolytic Conductivity ◽  
Gas Chromatograph ◽  
Flame Photometric Detector ◽  
Initial Concentration ◽  
Photometric Detector

Abstract The multiresidue procedure of Luke et al., which uses extraction with acetone and partition with petroleum ether and methylene chloride, was simplified and shortened by eliminating the Florisil cleanup. Double concentration with petroleum ether in the Kuderna-Danish evaporator following the initial concentration removed the last traces of methylene chloride. The extract was then injected into a gas chromatograph, using a Hall electrolytic conductivity detector for organohalogen, organonitrogen, and organosulfur pesticides or a flame photometric detector for organophosphorus pesticides. Recoveries of 79 pesticides are presented.

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