Gas Chromatographic Determination of Metolachlor in Pesticide Formulations: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 570-572
Author(s):  
Thomas G Gale ◽  
Arthur H Hofberg

Abstract A gas chromatographic (GC) procedure for the determination of metolachlor in emulsifiable concentrate formulations containing about 76% active ingredient was collaboratively studied using the matched pair scheme. Metolachlor was extracted from the formulation with acetone containing dipentyl phthalate as the internal standard, chromatographed on OV-101, and detected by flame ionization. Determinations on the 4 samples by 21 government, university, and industrial collaborators using peak area measurements showed within-laboratory repeatability of better than 0.5%. Reproducibility was better than 1% for the formulation. The method has been adopted official first action.

1985 ◽  
Vol 68 (3) ◽  
pp. 589-592
Author(s):  
Thomas G Gale ◽  
Arthur H Hofberg

Abstract Agaschromatographic (GC) procedure for the determination of chlordimeform in emulsiflable concentrate formulations containing about 46% active ingredient was collaboratively studied using the matched pair scheme. Chlordimeform was extracted from the formulation with methylene chloride containing diethyl terephthalate as the internal standard, chromatographed on CBWX-20M, and detected by flame ionization. Determinations on the 4 samples by 20 government, university, and industrial collaborators using peak area measurements showed within-laboratory repeatability of better than 1%. Reproducibility was 1.2% for the formulation. The method has been adopted official first action.


1985 ◽  
Vol 68 (3) ◽  
pp. 592-595
Author(s):  
Peter D Bland

Abstract A method is described for the determination of cypermethrin, 3-(2,2- dichloroethenyl)-2,2-dimethyl-cyclopropanecarboxylate cyano-(3- phenoxyphenyl)methyl ester, in technical and formulated material by capillary gas chromatography (CGC). Samples of technical or formulated material are dissolved in CH2Cl2 containing dicyclohexyl phthalate as internal standard. The solution is injected into a gas chromatograph fitted with a flame ionization detector and capillary column of 25 m x 0.32 mm fused silica with a thick film OV-1 phase at 240°C. Injection is made into a heated injection port fitted with an antidiscrimination device in a split mode. Peak areas obtained at retention times of the internal standard and active ingredient are measured with an integrator. The quantity of cypermethrin is determined by comparing the internal standard and active ingredient peak areas with those obtained from a calibration solution containing known amounts of internal standard and pure active ingredient. Five samples were chosen for collaborative study: technical cypermethrin, 70% liquid concentrate, 3 lb/US gal. emulsifiable, 3 ib/US gal. oil concentrate, and 40% wettable powder. Twelve collaborators carried out replicate determinations on each sample on separate days. Coefficients of variation between laboratories (CVX) were 2.13 for the technical, 2.94 for the emulsifiable concentrate, 3.51 for the liquid concentrate, 2.66 for the wettable powder, and 2.29 for the oil concentrate. The method was adopted official first action.


1986 ◽  
Vol 69 (4) ◽  
pp. 723-725
Author(s):  
David F Tomkins ◽  
◽  
W C Caparoon ◽  
I M Galoux ◽  
G M Gentry ◽  
...  

Abstract An isothermal gas chromatographic (GC) method for measuring propachlor in formulations was tested by 12 collaborators. Samples are prepared in acetone and determined using a GC column of 10% SP-2250 on 100-200 mesh Supelcoport, and diisobutyl phthalate as internal standard. Collaborators made single determinations on each of 2 similar materials (matched pairs) on 2 days for 3 pairs of samples. The study generated 62 matched pairs which were used in Youden’s matched pair calculations. The coefficients of variation (CV,) for flowable formulations were 0.84 and 1.48%; the CV, for the granular formulation was 1.28%. The method was simple to use and did not reveal any interferences in the samples tested. The method has been adopted official first action as an AOAC-CIPAC method.


1984 ◽  
Vol 67 (3) ◽  
pp. 499-502
Author(s):  
Peter D Bland ◽  
◽  
L Chenery ◽  
N Ellis ◽  
L Firestone ◽  
...  

Abstract A method is described for the determination of butyl 2-(4-(5-trifluoromethyl- 2-pyridinyloxy)phenoxy) propanoate in technical and formulated material by gas chromatography (GC). Samples of technical or formulated material are dissolved in methylene chloride containing dibenzyl succinate as internal standard. The solution is injected into a gas chromatograph fitted with a flame ionization detector and a 6 ft × 2 mm glass column. The column is packed with 3% OV-17 on 100–120 mesh Chromosorb WHP and is maintained at 230°C. Peak areas obtained at the retention times of the internal standard and the active ingredient are measured with an integrator. The quantity of fluazifop-butyl is determined by comparing the internal standard and active ingredient peak areas with the peak areas obtained from a calibration solution containing known amounts of internal standard and pure active ingredient. Four samples were chosen for collaboration: technical fluazifop-butyl, a 4 lb/US gal. emulsifiable concentrate, a 560 g/L oil concentrate, and a 5% granular. Fourteen collaborators carried out replicate determinations on each sample. Coefficients of variation between laboratories were 0.80 for the technical, 0.88 for the emulsifiable concentrate, 1.03 for the oil concentrate, and 2.04 for the granular. Parallel peak height determinations showed substantially higher coefficients of variation for all except the granular sample. The method has been adopted 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.


1992 ◽  
Vol 75 (6) ◽  
pp. 1103-1106
Author(s):  
Benjamin A Belkind

Abstract An isocratic normal-phase liquid chromatographic (LC) method for measuring methazole in technical and formulated products was collaboratively studied by 12 laboratories. Samples of technical or formulated products are dissolved in 1,4-dioxane-hexane containing 2-chloro-5-nitrobenzophenone as internal standard. Following centrifugation and further dilution, the sample is analyzed by LC on a 25 cm x 4.6 mm stainless steel column packed with 5 μm silica, with ultraviolet detection at 254 nm. Premixed 1% 2-propanol in hexane is used as the mobile phase. Peak areas are obtained at the retention times corresponding to the internal standard and methazole. The quantity of active ingredient is determined by comparing the area ratio of active ingredient to internal standard in the sample with the same ratio in a single calibration solution. Collaborators were provided with 1 Youden matched pair for each of the technical, 75% wettable granular, and 4 lb/gal flowable products studied. The reproducibility relative standard deviations (RSDR) for the product types studied were 1.05% for technical, 1.80% for granular, and 4.76% for flowable. The method has been adopted first action by AOAC International.


1975 ◽  
Vol 58 (3) ◽  
pp. 516-519
Author(s):  
Arthur H Hofberg ◽  
Lee C Heinrichs ◽  
Gene A Gentry

Abstract A gas-liquid chromatographic method for the determination of chlorobenzilate and chloropropylate in liquid formulations containing about 46 and 26% active ingredient, respectively, was collaboratively studied, using a matched pair scheme. The samples were dissolved in acetone containing dibenzyl succinate as an internal standard and chromatographed on Carbowax 20M, using a flame ionization detector. Analyses of 4 samples by 13 collaborators using peak height measurements showed the following results: chlorobenzilate—2.5% overall coefficient of variation, 1.0% coefficient of variation for the random error; and 0.7% systematic error; chloropropylate—2.0, 1.4, and 0.4%, respectively. The method has been adopted as official first action.


1985 ◽  
Vol 68 (3) ◽  
pp. 573-575
Author(s):  
David F Tomkins

Abstract An isothermal gas chromatographic method for measuring alachlor in formulations was tested by 26 collaborators. The samples were prepared in acetone and determined with a gas chromatographic column of 10% SP 2250 on 100-120 mesh Supelcoport and with di-n-pentyl phthalate as internal standard. Collaborators made single determinations on each of 2 similar materials (matched pairs) on 2 days for 3 pairs of samples. The study generated 44 matched pairs which were used in Youden's matched-pair calculations. The coefficients of variation (CV,) for liquid formulations were 1.23% and 0.94%, while the CV, for the granular formulation was 1.60 %. The method was simple to use and did not reveal any interferences in the samples tested. 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.


1973 ◽  
Vol 56 (3) ◽  
pp. 586-590
Author(s):  
Arthur H Hofberg ◽  
Robert T Murphy

Abstract A gas chromatographic method for the determination of ametryne and terbutryn in wettable powder formulations containing about 80% active ingredient and prometone in liquid formulations containing about 25% active ingredient was collaboratively studied, using a matched pair scheme. The ametryne was extracted from the powder with chloroform containing dieldrin as an internal standard and chromatographed on Carbowax 20M, using a flame ionization detector; the same method was used for terbutryn. The sample containing prometone was dissolved in chloroform containing dieldrin and chromatographed in the same manner. Two samples of each pesticide were analyzed, using peak height measurements, with the following results: ametryne (14 collaborators)—1.63% overall coefficient of variation, 0.68% coefficient of variation for the random error, and 1.05% systematic error; prometone (15 collaborators)—2.27, 1.47, and 1.21%; and terbutryn (15 collaborators)—0.95, 0.51, and 0.56%, respectively. The method has been adopted as official first action.


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