Fumigant residues of carbon tetrachloride, ethylene dichloride, and ethylene dibromide in wheat, flour, bran, middlings, and bread

1974 ◽  
Vol 22 (6) ◽  
pp. 977-984 ◽  
Author(s):  
Ben. Berck
1985 ◽  
Vol 68 (4) ◽  
pp. 759-762
Author(s):  
Jonathan W Devries ◽  
Paul A Larson ◽  
Raymond H Bowers ◽  
Joyce A Keating ◽  
James M Broge ◽  
...  

Abstract A method is described for the determination of the common fumigants carbon tetrachloride (CC14), ethylene dichloride (EDC), and ethylene dibromide (EDB) in grain and grain-based products. A properly prepared sample is mixed with water and hexane, an internal standard mixture of 1,2-dichloropropane (DCP) and 1,2-dibromopropane (DBP) is added, and the fumigants are codistilled with the hexane into an appropriate receiver. After the hexane solution is dried over sodium sulfate, the quantities of fumigants present are quantitated on a gas chromatograph (GC) equipped with an electron capture detector (ECD). For the matrices investigated, the relative standard deviation of the method was 6.0,9.7, and 23.1% for CC14, EDC, and EDB, respectively. Recoveries of added fumigants were 107, 95, and 101%, respectively. Comparison with an acetone-water soak extraction method gave a correlation of 0.967 between methods for EDB with odds of a difference between methods of 35%.


1980 ◽  
Vol 63 (3) ◽  
pp. 539-545
Author(s):  
Marion Clower Jr

Abstract The official first action AOAC method for determination of residues of fumigants in grains has been modified for use by 6 laboratories in an FDA pesticide surveillance program. A 15% OV-I7 gas-liquid chromatographic column, installed in a chromatograph equipped with a constant current 63Ni electron capture detector, provides for improved resolution, multiresidue capability, and lower limits of detection. A study was made of the behavior of chloroform, carbon tetrachloride, ethylene dichloride, trichloroethylene, tetrachloroethylene, and ethylene dibromide through the method. Recoveries from fortified wheat samples averaged 105-115%. Experimental evidence is presented which suggests that part of the consistent trend toward high recovery can be attributed to selective sorption of acetone by the CaCI2 used in the final drying step.


1986 ◽  
Vol 69 (4) ◽  
pp. 575-580
Author(s):  
Thomas G Alleman ◽  
Robert A Sanders ◽  
Bryan L Madison

Abstract A method is described for the simultaneous measurement of parts per billion levels of the fumigants ethylene dibromide, carbon tetrachloride, and ethylene dichloride in grain and grain-based products. The fumigants are isolated by hexane co-distillation, separated by capillary gas chromatography, and detected with a mass spectrometer in the selected ion monitoring mode. Recoveries are greater than 90% and standard deviations are approximately 10% of the quantity measured. The method is free of interferences and its precision and accuracy are enhanced by the use of tetradeuterated ethylene dibromide and ethylene dichloride as internal standards.


1969 ◽  
Vol 52 (4) ◽  
pp. 800-805
Author(s):  
Bernadette Malone

Abstract A sweep co-distillation procedure, a published steam distillation procedure, and an adaptation of an established acid reflux procedure for isolating fumigant residues were compared. Residues were detectable by electron capture gas chromatography at levels approaching or surpassing 0.1 ppm. Fumigants used were carbon tetrachloride, carbon disulfide, ethylene dichloride, ethylene dibromide, methyl bromide, and chloroform. Comparison of the three methods, using the same detection for all, showed that acid reflux was the most promising procedure for recovering added fumigants from grain and extracting fumigation residues. This procedure should be further refined.


1970 ◽  
Vol 53 (4) ◽  
pp. 742-746
Author(s):  
Bernadette Malone

Abstract A method is described for determination of residues of the fumigants methyl bromide, carbon disulfide, chloroform, ethylene dichloride, carbon tetrachloride, and ethylene dibromide in cereal grains. Whole or ground grain is boiled in an acid medium, and the volatile fumigants are dried and collected in cold solvent. Residues are determined by analyzing aliquots of the collected solution by electron capture GLC. Recoveries range from 59 to 105%. Extraction appears to be complete in the 2 hr boiling period specified. An unexplained conversion of carbon tetrachloride to chloroform is described.


1965 ◽  
Vol 48 (3) ◽  
pp. 576-579
Author(s):  
M F Loucks

Abstract Preliminary studies were made of the composition of grain fumigants. The most common constituents are carbon disulfide, carbon tetrachloride, ethylene dichloride, and ethylene dibromide. Gas chromatography seems to be a suitable technique for analysis.


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