Gas chromatography/mass spectrometry identification of cyclohexene artifacts formed during extraction of brine samples

Gas chromatography/mass spectroscopy identification of artifacts formed in methylene chloride extracts of saline water

“…Another reaction pathway may involve the oxidation of the halide ions such as bromide and iodide with the residual chlorine to other reactive species which react with the preservative to form halogenated organic compounds. This study has also shown that the replacement of cyclohexene with amylene as previously suggested (3) does not solve the problem.…”

“…They suggested that replacing the preservative or using solvent-free preservative would avoid this problem. Burdick and Jackson, one of the major producers of high-purity methylene chloride claimed that "amylene is now going to be used as the preservative in methylene chloride" (3).…”

Oxidation of phenolic acid surrogates and target analytes during acid extraction of natural water samples for analysis by GC/MS using EPA method 625

“…The samples that had zero or low recoveries usually contained iodocyclohexanol (peak 1 in Figure IB) and, to a lesser extent, chloroiodocyclohexane (peak 2 in Figure IB). Iodocyclohexanol (in some cases, bromocyclohexanol also) and halogenated cyclohexanes are artifacts formed in acidic media during extraction (4,5). Iodocyclohexanol is presumably a reaction product of iodine (generated in the sample under acidic conditions) with cyclohexene.…”

Flammable gas safety program. Analytical methods development: FY 1993 progress report

“…Typically, one would expect the acid fraction to contain little NPH; however, due to low extraction efficiency, NPH exists in both fractions, Stromatt also found NPH present in the samples from Tank 101-SY, window E (Jones et al 1992). The other peaks, particularly in the acid fraction, are compounds formed by addition reactions across the double bond in cyclohexene, used as an inhibitor in methylene chloride (Campbell et al 1987). The mass spectra of these components indicate a base peak at m/z 81.…”