Headspace Gas Chromatographic Method for Determination of Ethanol in Canned Salmon: Collaborative Study

1986 ◽  
Vol 69 (3) ◽  
pp. 524-526
Author(s):  
Thomas A Hollingworth ◽  
Harold R Throm ◽  
Marleen M Wekell ◽  
William F Trager ◽  
Michael W O’Donnell ◽  
...  

Abstract Six laboratories collaboratively studied a headspace gas chromatographic method for determination of ethanol in the aqueous phase of canned salmon. Ethanol is determined by a headspace sampling technique with tert-butanol as the internal standard, using a gas chromatograph equipped with a Super Q column and a flame ionization detector. With outliers excluded, the mean recoveries from samples spiked with 25.1 and 78.4 ppm ethanol were 112 and 110%, respectively. For the 4 sample pairs quantitated, repeatability coefficients of variation ranged from 1.42 to 4.25% and reproducibility coefficients of variation from 2.55 to 8.09%, with 3 of the 4 reported values less than 5%. The method has been adopted official first action.

1987 ◽  
Vol 70 (1) ◽  
pp. 55-57
Author(s):  
Daniel E Terry

Abstract A gas chromatographic method for the determination of isofenphos (OFTANOL®) in isofenphos technical and liquid formulations has been developed and collaboratively studied by 11 laboratories. Two technical samples and 2 liquid flowable samples were analyzed after shaking/extracting in methanol which contained diisobutyl phthalate as an internal standard. The extracts were analyzed by gas chromatography using an SP-2100 column and either flame ionization or thermal conductivity detection. Coefficients of variation were 0.57 and 1.27% for the technical and formulated products, respectively. The GC method has been adopted official first action as a AOACCTPAC method.


1987 ◽  
Vol 70 (1) ◽  
pp. 51-53
Author(s):  
J F C Tyler

Abstract A gas chromatographic method for determination of total cypermethrin in technical and formulated products has been developed and subjected to a collaborative study involving IS participating laboratories. Each sample was dissolved in methyl isobutyl ketone containing di(2-ethylhexyl) phthalate as internal standard and analyzed by gas chromatography on a glass column with 3% OV-101 on Chromosorb W-HP. Each collaborator was furnished with reference stdard and 4 samples of technical material, 3 emulsifiable concentrates, one wettable powder, and one ultralow volume formulation for analysis. The coefficients of variation of the results obtained ranged from 0.955 to 1.7462%. The method has been adopted as official first action by AOAC.


1987 ◽  
Vol 70 (1) ◽  
pp. 53-55
Author(s):  
J F C Tyler

Abstract A gas chromatographic method for determination of permethrin in technical and formulated products has been developed and subjected to a collaborative study involving 19 participating laboratories. Each sample was dissolved in methyl isobutyl ketone containing n-octacosane as internal standard and analyzed by gas chromatography on a glass column with 3% OV-210 on Chromosorb W-HP. Each collaborator was furnished with reference standard and 5 samples of technical material (90-95%), 8 emulsifiable concentrates (10-50%), 2 wettable powders (20-30%), one dustable powder (1-2%), and one mter-dispersible granules (1-2%) for analysis. The coefficients of variation of the results obtained ranged from 0.79 to 4.24%. The method has been adopted as official first action by AOAC.


1986 ◽  
Vol 69 (3) ◽  
pp. 488-490
Author(s):  
William R Betker ◽  
◽  
E W Balcer ◽  
O O Bennett ◽  
W R Coffman ◽  
...  

Abstract A collaborative study was conducted on a gas chromatographic method for determination of fensulfothion. Eleven laboratories analyzed 2 technical and two 6 lb/U.S. gal. spray concentrate samples. In the analysis, samples are dissolved in methylene chloride which contains 4-chlorophenyl sulfoxide as an internal standard, and solutions are injected into a gas chromatograph equipped with an OV-330 column. Withinlaboratory repeatability was 0.79% for technical product and 0.37% for the spray concentrate samples, with coefficients of variation of 0.88 and 0.58%, respectively. Among-laboratories reproducibility was 0.81% for technical product and 0.53% for the spray concentrate, with coefficients of variation of 0.91 and 0.84%, respectively. The method has been adopted official first action.


1971 ◽  
Vol 54 (3) ◽  
pp. 700-702
Author(s):  
R T Murphy ◽  
A H Hofberg ◽  
H R Buser

Abstract A gas chromatographic method for the determination of Diazinon in liquid formulations containing about 50% active ingredient was collaboratively studied, using a matched pair scheme. The sample was dissolved in acetone containing aldrin as an internal standard and chromatographed on silicone DC-200, using a flame ionization detector. Determinations on the 2 samples by 18 collaborators using peak height measurements show an overall coefficient of variation of 1.0%. The coefficient of variation of random error is 0.8%, and for the systematic error, 0.4%. Application of the F-test proved this systematic error not to be significant. The method has been adopted as official first action.


1971 ◽  
Vol 54 (3) ◽  
pp. 703-705
Author(s):  
R T Murphy ◽  
A H Hofberg ◽  
H R Buser

Abstract A gas chromatographic method for the determination of prometryne in wettable powder formulations containing about 80% active ingredient was collaboratively studied, using a matched pair scheme. The prometryne was extracted from the powder with chloroform containing dieldrin as an internal standard and chromatographed on Carbowax 20M, using a flame ionization detector. Determinations on the 2 samples by 12 collaborators using peak height measurements show an overall coefficient of variation of 1.4%, coefficient of variation of random error of 1.3%, and for systematic error, 0.4%. Application of the F-test shows the systematic error not to be significant. The method has been adopted as official first action.


1971 ◽  
Vol 54 (3) ◽  
pp. 697-699
Author(s):  
R T Murphy ◽  
A H Hofberg ◽  
H R Buser

Abstract A gas chromatographic method for the determination of atrazine in wettable powder formulations containing about 80% active ingredient was collaboratively studied, using the matched pair scheme. The atrazine was extracted from the powder with chloroform containing dieldrin as an internal standard and chromatographed on Carbowax 20M, using a flame ionization detector. Determinations on the 2 samples by 13 collaborators using peak height measurements show an overall coefficient of variation of 1.0% and a coefficient of variation of random error of 1.2%. Statistical evaluation of these factors reveals no evidence of systematic error contribution. The method has been adopted as official first action.


1984 ◽  
Vol 67 (2) ◽  
pp. 284-289 ◽  
Author(s):  
James A Ault ◽  
Tim E Spurgeon ◽  
◽  
M M Anderson ◽  
R Bowers ◽  
...  

Abstract A gas chromatographic electron capture detector method is described for the quantitative determination of organochlorine pesticide residues in poultry fat. The samples are rendered and cleaned up using automated gel permeation chromatography. The collaborative samples consisted of 10 fortified samples and one incurred residue sample, all in duplicate. Fortification levels ranged from 0.15 to 1.0 ppm for a-BHC, lindane, cis- and frans-chlordane, octachlor epoxide, o,p' and p,p'-DDT, p,p'-DDE, p,p'-TDE, hexachlorobenzene, heptachlor epoxide, dieldrin, endrin, methoxychlor, mirex, and toxaphene. The average recovery was 91.9% with a range of 81-102%. The ranges of coefficients of variation were: CVo = 3.39-14.79%; CVL = 0-16.6%; and CVx = 5.82-19.0%. The results indicate accuracy and precision comparable to other official methodology. The method has been adopted official first action.


1969 ◽  
Vol 52 (3) ◽  
pp. 435-438
Author(s):  
Albert J Gehrt

Abstract A GLC method (flame ionization detector) for ronnel in cattle feeds at levels of 0.038, 0.041, and 0.055% was studied by 11 collaborators. The method involves extraction of ronnel by shaking with acetone followed by direct chromatographic measurement. The method is simple and rapid (no cleanup required), measures true ronnel, and is free from interferences present in the UV methods previously studied. Agreement between laboratories was satisfactory; coefficients of variation were 11.0, 12.0, and 7.2%. Ronnel recoveries were 81.1, 93.5, and 98.0%. Low recovery from the first sample may be due to ronnel hydrolysis or binding during storage (sample was 8 months old). The Associate Keferee recommends that the method be adopted as official first action.


1981 ◽  
Vol 64 (4) ◽  
pp. 829-832
Author(s):  
Bram Van Rossum ◽  
Albertus Martijn ◽  
James E Launer ◽  
◽  
E C Calamita ◽  
...  

Abstract The gas-liquid chromatographic determination of tetradifon technical and formulations was collaboratively studied in duplicate with 12 laboratories. Six samples were dissolved in dichloroethane with n-hexacosane as the internal standard, chromatographed on a column of 3% SE-52, and detected by flame ionization. The average coefficients of variation were 1.2% for the 2 technical samples, 1.6% for the 2 wettable powders, and 1.5% for the 2 emulsifiable concentrates. The method has been adopted official first action.


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