Gas Chromatographic Determination of 1,4-Dioxane in Polysorbate 60 and Polysorbate 80

1979 ◽  
Vol 62 (4) ◽  
pp. 931-936
Author(s):  
Thomas J Birkel ◽  
Charles R Warner ◽  
Thomas Fazio

Abstract A gas chromatographic method is presented for the quantitative determination of 1,4- dioxane in polysorbate 60 and polysorbate 80. Dioxane is isolated from the matrix by closedsystem vacuum distillation with water as the carrier solvent. The distillate is chromatographed on Chromosorb 104 and detected by flame ionization. Recoveries of dioxane from polysorbate 60 samples fortified at 0.5, 1, 2, and 20 ppm averaged 90, 91, 85, and 75%, respectively. Recoveries from polysorbate 80 fortified at the same levels averaged 100, 88, 95, and 95%, respectively. Samples of polysorbate 60 and polysorbate 80 were found to contain from 5.5 to 378 ppm dioxane.

1970 ◽  
Vol 53 (3) ◽  
pp. 566-568
Author(s):  
J E Paterson

Abstract A gas chromatographic method is described for the quantitative determination of dioxathion and chlorfenvinphos in emulsifiable concentrates and livestock dips. A convenient quantity of the emulsifiable formulation is dissolved in xylene and the aqueous dip is extracted with xylene for gas chromatographic analysis, using a mixed silicone oil stationary phase and a flame ionization detector. The coefficients of variation for the dioxathion and chlorfenvinphos determinations in the emulsifiable concentrate are 2.4 and 1.0%, respectively. Recoveries of the former from a fouled dip ranged from 97 to 103% and recoveries of the latter ranged from 92 to 97%.


1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi

Abstract A gas chromatographic method is described for the quantitative determination of N-butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-tolindine and α,α,α-trifluoro-2,6-dinitro-N,N-dipropyI-p-toluidine herbicides in formulations. The sample is extracted with benzene, and equal amounts of sample and reference solution in the same concentration range are analyzed by gas chromatography, using an electron capture detector and an SE-30/Diatoport S column. The method has been applied successfully to laboratory-prepared and commercial samples.


1974 ◽  
Vol 57 (1) ◽  
pp. 189-191
Author(s):  
James B Leary

Abstract A gas chromatographic method is described for determining acephate (O,S-dimethyl acetylphosphoramidothioate) and a metabolite, Ortho 9006 (O,S-dimethyl phosphoramidothioate), in a variety of crops. After extraction of the sample with ethyl acetate, the solvent is evaporated, and an ether solution of the residue is passed through a silica gel column to remove interferences. Acephate and Ortho 9006 are eluted from the column with 10% methanol in ether and measured simultaneously by programmed temperature gas chromatography, using an alkali flame ionization detector.


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.


2000 ◽  
Vol 83 (4) ◽  
pp. 1020-1026 ◽  
Author(s):  
Dirk Joye ◽  
Hubert Hoebregs

Abstract A high-temperature capillary gas chromatographic method was developed for the quantitative determination of oligofructose in foods and food products. Sample preparation involves oxymation and silylation of the extracted sugars. The oximetrimethylsilyl derivatives are analyzed on an apolar capillary column, with detection by flame ionization. The method is accurate, with recovery of spiked samples at >96%. Repeatability was excellent; RSD values of 1.1% were obtained. Other common oligosaccharides, such as malto-, isomalto-, and galactooligosaccharides, and levan do not interfere, making the method specific and reliable.


1972 ◽  
Vol 55 (5) ◽  
pp. 907-912
Author(s):  
Vernon J Meinen

Abstract A gas chromatographic method is described for the quantitative determination of d-trans-allethrin in the technical product and in various formulations. The samples are diluted with acetone and analyzed by gas chromatography, using a flame ionization detector and a column packed with OV-1 on Chromosorb W (HP). Preliminary work indicates that satisfactory results can be obtained with the technical material and several different formulations. Since this method is more rapid and specific than the present AOAC titrimetric method, it is expected that it will be a valuable supplement to or alternative for the AOAC method for the analysis of allethrin.


Author(s):  
N. Carugno ◽  
S. Rossi ◽  
G. Lionetti

AbstractA qualitative and quantitative procedure has been developed for the determination of humectants in manufactured tobacco by gas-chromatographic method with a flame ionization detector. It consists of extraction with methanol, concentration of the extract and treatment with Tri-Sil reagents. The operating gas-chromatographic conditions are set forth. Samples of tobacco containing glycerine, propylene glycol, diethylene glycol, triethylene glycol, 1-3 butylene glycol and sorbitol have been analysed with recoveries, for the first five ones, in the range of 95-104 %. In order to verify that each chromatographic peak corresponded to the relative glycol, with no interference by other silylated compounds, the mass spectra were obtained through the combination of gas-chromatography with mass spectrometry. The results achieved confirm, as far as tobacco is concerned, that the procedure is accurate and precise. The same method for the determination of humectants was extended to cigarette smoke. Even though this involves morecomplicated problems, as compared to tobacco, because of the presence of silylated compounds, it was found that, for certain glycols, the gas-chromatography of the trimethyl derivatives can be also used as a method of analysis. The mass spectra of some polyhydric alcohols are shown


1996 ◽  
Vol 79 (2) ◽  
pp. 587-588 ◽  
Author(s):  
Lan Zhao ◽  
De-Fang Fan

Abstract A gas chromatographic method is described for determination of chlorothalonil residues in leaves and roots of Scrophularia and in soil. Samples were extracted with acetone and cleaned up on a Florisil column. Chlorothalonil residues are chromatographed directly on a glass column of 1.5% OV-17 and 2% QF-1 coated on 80-100 mesh Chromosorb W (HP) support and measured with a 63Ni electron capture detector. Detection limits are 0.001 ppm for leaf, 0.005 ppm for root, and 0.001 ppm for soil.


1987 ◽  
Vol 70 (4) ◽  
pp. 745-748
Author(s):  
Uaz Ahmad

Abstract A capillary column gas chromatographic method is described for determining parts-per-trillion (ppt) levels of chlorsulfuron in agricultural runoff water. The water sample is acidified with acetic acid and extracted with methylene chloride. The chlorsulfuron in the extract is derivatized to its monomethyl derivative. After Florisil column cleanup, the methylated chlorsulfuron is determined by electron-capture gas chromatography. Recovery of chlorsulfuron from fortified water samples is greater than 80%. Detection limit of the method is 25 ng chlorsulfuron/L water (25 ppt). There are 2 reaction sites on the chlorsulfuron molecule, both of which are susceptible to methylation leading to monomethyl chlorsulfuron and dimethyl chlorsulfuron. A procedure is described to methylate selectively the sulfonamide nitrogen of chlorsulfuron.


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