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CASE
Simultaneous determination of tetraethyl lead and benzidine in surface water with gas chromatography–mass spectrometry by using solid phase extraction
Keywords tetraethyl lead; benzidine; solid phase extraction; gas chromatography–mass spectrometry; Come on ion
monitoring mode; surface water
monitoring mode; surface water
Details
Abstracts: A gas chromatography mass spectrometry(GC–MS) method with solid phase extraction(SPE) was
developed for the determination of tetraethyl lead and benzidine simultaneously in surface water. The factors affecting solid phase extraction were investigated, including solid phase extraction column, pH of water sample and the elution solution. pH of the water sample was adjusted to 12, then the water sample was concentrated by HLB extraction cartridge, and elutedwith dichloromethane. The analytes were separated on a DB–5MS capillary column and detected by Come on ion monitoring mode. The mass concentration of tetraethyl lead and benzidine was linear with the chromatographic peak area in the range of 20–200 μg/L and 40–400 μg/L, respectively, with the correlation coefficients of 0.995 8 and 0.993 9. The concentration was enriched 1 000 times under the optimum conditions, and the detection limit of tetraethyl lead and benzidine was 0.003μg/L and 0.008 μg/L, respectively. Mean recoveries of tetraethyl lead and benzidine from surface water samples ranged from 47.5%–89.4% for two different fortification levels, and the relative standard deviations of the determination results were 5.4%–8.9%(n=6). The method is simple, sensitive and efficient, which is suitable for routine analysis in surface water.
Influence of pH value of water sample on the determination results
The mass concentrations of tetraethyl lead and benzidine in the prepared water samples were both 0
1 μ g / L, adjust the pH value of water sample, and determine the water sample in different pH values The recovery rate of tetraethyl lead and benzidine at pH value is shown in Figure 2.
The mixed standard solution was prepared for selective separation
The ion flow chromatogram was obtained by sub scanning
developed for the determination of tetraethyl lead and benzidine simultaneously in surface water. The factors affecting solid phase extraction were investigated, including solid phase extraction column, pH of water sample and the elution solution. pH of the water sample was adjusted to 12, then the water sample was concentrated by HLB extraction cartridge, and elutedwith dichloromethane. The analytes were separated on a DB–5MS capillary column and detected by Come on ion monitoring mode. The mass concentration of tetraethyl lead and benzidine was linear with the chromatographic peak area in the range of 20–200 μg/L and 40–400 μg/L, respectively, with the correlation coefficients of 0.995 8 and 0.993 9. The concentration was enriched 1 000 times under the optimum conditions, and the detection limit of tetraethyl lead and benzidine was 0.003μg/L and 0.008 μg/L, respectively. Mean recoveries of tetraethyl lead and benzidine from surface water samples ranged from 47.5%–89.4% for two different fortification levels, and the relative standard deviations of the determination results were 5.4%–8.9%(n=6). The method is simple, sensitive and efficient, which is suitable for routine analysis in surface water.
Influence of pH value of water sample on the determination results
The mass concentrations of tetraethyl lead and benzidine in the prepared water samples were both 0
1 μ g / L, adjust the pH value of water sample, and determine the water sample in different pH values The recovery rate of tetraethyl lead and benzidine at pH value is shown in Figure 2.
The mixed standard solution was prepared for selective separation
The ion flow chromatogram was obtained by sub scanning