Gas Chromatographic Determination of Ethanol in Wine: Collaborative Study

1983 ◽  
Vol 66 (5) ◽  
pp. 1152-1157
Author(s):  
Arthur Caputi ◽  
Dennis P Mooney ◽  
◽  
J Cherolis ◽  
M Clements ◽  
...  

Abstract After a survey of laboratories using gas chromatographic procedures for wine alcohol analysis, 3 sets of columns and operating parameters were chosen on the basis of comparative reproducibility evaluations run in this laboratory. Fourteen collaborators participated in the study and were given their choice of any one of the 3 columns: (1) 1.8 m × 2 mm id glass, packed with 80-100 mesh Poropak QS; (2) 1.8 m × 2 mm id glass, packed with 0.2% Carbowax 1500 on 80-100 mesh Carbopack C; (3) 1.8 m × 6.35 mm copper, packed with 3% Carbowax 600 on 40-60 mesh Chromosorb T. Standards and samples were diluted 1:100 with 0.1% v/v n-butanol in water before analysis. Eight samples containing from 7.3 to 23.6% ethanol (v/v) were submitted as randomly coded duplicates along with a calibration standard and a practice sample. Two injections each of the diluted duplicates were made. On the basis of the reported results, 2 laboratories were rejected as outliers. The results of the remaining 12 collaborators showed an average reproducibility of 0.142 and a repeatability of 0.036. The method has been adopted official first action.

1972 ◽  
Vol 55 (4) ◽  
pp. 840-845 ◽  
Author(s):  
Charles R Midkiff ◽  
Willard D Washington

Techniques developed for use with gas-liquid chromatography for the examination of evidence collected at the scene of suspected arson fires and firebombings are discussed. Both solvent extraction and vapor phase examinations are employed. Internal standards are used for the identification of specific components in actual samples to allow confirmation of hydrocarbon type, e.g., gasoline and kerosene. Operating parameters and solvent selection criteria are included. Results obtained from known materials and residual hydrocarbons in actual samples are compared.


1991 ◽  
Vol 74 (2) ◽  
pp. 317-323 ◽  
Author(s):  
Mark E Oppenhuizen ◽  
John E Cowell

Abstract A new method for determination of glyphosate and amlnomethylphosphonlc acid (AMPA) residues In environmental water was collaboratively studied by 6 laboratories. The method Is simpler and shorter than previous methods. A filtered volume of water is evaporated to dryness and the residue Is dissolved In a buffered EDTA solution. Glyphosate and AMPA are determined by liquid chromatography with postcolumn reaction detection. The method was validated over the range 0.50-5000 ppb, although one of the collaborating laboratories could not reliably quantltate below 1.0 ppb. Statistical analysis of the results showed that typical reproducibility relative standard deviations (RSDR) ranged from 11 to 20% for both glyphosate and AMPA, which compares very well with predicted values for this concentration range. Total variability (as measured by sR) Increased with increasing fortification level. The method has been adopted official first action by AOAC.


1972 ◽  
Vol 55 (3) ◽  
pp. 549-556
Author(s):  
J H Kahn ◽  
E T Blessinger

Abstract Fifteen chemists participated in a collaborative study for the quantitative pas-liquid chromatographic determination of the individual fusel alcohols and ethyl acetate in whisky. Two levels of congeners represented by 4 coded samples of whisky were analyzed by using t h e proposed method, employing a glycerol-1,2,6-hexanetriol column, and the official AOAC method, 9.063-9.065. Since isobutyl and the atnyl alcohols comprise by far the greatest part of fusel oil, their determination is of major importance to the total fusel oil content . Statistical analyses show that the proposed method is superior to the AOAC method for the determination of these alcohols, whereas the official method is superior for the determination of ethyl acetate and n-propyl alcohol. In general, collaborators employing modern instrumentation preferred the proposed method over the AOAC method. The former method also separates and permits the quantitative measurement of active amyl and isoamyl alcohols. The proposed method has been adopted as official first action as an alternative to 9.063–9.065 for the determination of higher alcohols and ethyl acetate in whisky.


1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros

Abstract A stability indicating liquid chromatographic method for the determination of diazepam in tablets was collaboratively studied by 6 laboratories. The method uses a Cig reverse phase column, a methanolwater mobile phase, p-tolualdehyde as the internal standard, and photometric detection at 254 nm. The collaborators were supplied with a synthetic tablet powder and 3 commercial tablet samples. The mean recovery of diazepam from the synthetic tablet powder was 100.2%. For all samples analyzed, the coefficient of variation was < 1.5%. The method has been adopted official first action.


1984 ◽  
Vol 67 (3) ◽  
pp. 492-493
Author(s):  
Stephen C Slahck ◽  
◽  
A A Carlstrom ◽  
L T Chenery ◽  
N D Ellis ◽  
...  

Abstract An LC method for the determination of methiocarb in methiocarb technical and formulated products has been subjected to a collaborative study with 9 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with acetophenone as an internal standard. Collaborators were furnished samples of technical, 75% wettable powder, 75% seed treater, 75% concentrate, and 50% hopper box treater. Coefficient of variation values obtained on the 5 samples were 0.71, 0.83, 0.62, 1.57, and 0.82%, respectively. 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 (5) ◽  
pp. 915-918
Author(s):  
Edward J Kikta ◽  
◽  
E Bane ◽  
A Burns ◽  
A Christensen ◽  
...  

Abstract A liquid chromatographic (LC) method for the analysis of technical and formulated carbofuran samples was evaluated in a collaborative study. Carbofuran is determined by reverse phase LC, using a water-methanol mobile phase and acetophenone as internal standard, and detected at 280 nm. Twelve samples, 5 formulations and technical matched pairs, were analyzed by 17 collaborating laboratories. Accuracy and variability of results are typical of large LC data sets. 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.


1985 ◽  
Vol 68 (3) ◽  
pp. 586-589
Author(s):  
Stephen C Slahck

Abstract A liquid chromatographic method for the determination of triadimefon (Bayleton™) in triadimefon technical and formulated products has been developed and subjected to a collaborative study with 7 participating collaborators. Formulations were extracted with mobile solvent and analyzed by normal phase chromatography, with 4-chlorophenyl sulfoxide as an internal standard. Collaborators were furnished with standards and samples of technical products, 50% wettable powders, and 25% wettable powders for analysis. Coefficients of variation of the values obtained on these samples were 1.42, 0.82, and 1.05%, respectively. The method has been adopted official first action.


1968 ◽  
Vol 51 (4) ◽  
pp. 825-828
Author(s):  
Laura A Roberts

Abstract A method for the gas chromatographic determination of methylene chloride, ethylene dichloride, and trichloroethylene residues in spice oleoresins was studied collaboratively. The method employs a microcoulometric gas chromatograph fitted with a Porapak Q column and is based on the volatility of the solvent residues, their relative retention times on a polyaromatic bead chromatographic column, and their detectability by a halide-specific microcoulometric method. Recoveries were adequate when the method was closely followed; recoveries were erratic when collaborators deviated from the method. Further study is recommended.


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