顶空-气相色谱法测定土壤中乙酸正丁酯的残留量
|
摘要
本文建立了顶空气相色谱法测定土壤中乙酸正丁酯残留量的方法。方法:使用DB-1(30 m×0.25 mm×0.25μm),FID检测器,样品在80℃下平衡30分钟。结果:乙酸正丁酯在0.5～50μg/m L范围内线性回归方程为Y=89650.18*X+22035.84(r=0.9999);加标回收率(n=9)为90%～115%之间,重复性试验中浓度相对标准偏差为5.09%,检出限为0.0248 mg/kg。结论:该方法简便、准确度高、灵敏度高、重现性好,可满足多种土壤中乙酸正丁酯残留量的检测。
A headspace-gas chromatograph method was established for determination of residual n-butyl butyrate in soil. Method: Using a DB-1(30 m× 0.25 mm×0.25 μm)column with FID as detector, samples had been equilibrated at 80 ℃ for 30 minutes.Results: The calibration curves of n-butyl butyrate was Y=89650.18*X+22035.84 showed good linearity in the range of 0.5～50 μg/m L(r=0.9999).The standard recovery rate(n=9) was between 90 % and 115 %;The concentration relative standard deviation(RSD)in the repeated test was 5.09 %; T he detection limit was 0.0248 mg/kg. Conclusion: The method is simple, accurate, sensitive and reproducible, and can be used to detect the residual n-butyl acetate in various soils.
A headspace-gas chromatograph method was established for determination of residual n-butyl butyrate in soil. Method: Using a DB-1(30 m× 0.25 mm×0.25 μm)column with FID as detector, samples had been equilibrated at 80 ℃ for 30 minutes.Results: The calibration curves of n-butyl butyrate was Y=89650.18*X+22035.84 showed good linearity in the range of 0.5～50 μg/m L(r=0.9999).The standard recovery rate(n=9) was between 90 % and 115 %;The concentration relative standard deviation(RSD)in the repeated test was 5.09 %; T he detection limit was 0.0248 mg/kg. Conclusion: The method is simple, accurate, sensitive and reproducible, and can be used to detect the residual n-butyl acetate in various soils.
引文
[1]Li C S,Daisuke H,Suzuki K.N-Butyl acetate synthesis via reactive distillation:Thermodynamic,process design[J].Computers and Applied Chemistry,2007,24(12):1585-1589.
[2]陈烨,王红松,刘君峰,等.气相色谱内标法测定食品添加剂乙酸正丁酯中14种杂质[J].检验检疫学刊,2014(3):44-47.
[3]Iregren A,L?f A,Toomingas A,et al.Irritation effects from experimental exposure to n-butyl acetate[J].American Journal of Industrial Medicine,2010,24(6):727-742.
[4]李凤.乙酸正丁酯反应精馏生产工艺的模拟与研究[D].华东理工大学,2013.
[5]王晓明.热解析-气相色谱法测定室内空气中的总挥发性有机物(TVOC)[J].广州化工,2014(17):149-151.
[6]张晓淳,陈弘丽,李津津.溶剂解析-气相色谱法同时测定空气中12种挥发性有机物[J].东莞理工学院学报,2016(1):49-52.
[2]陈烨,王红松,刘君峰,等.气相色谱内标法测定食品添加剂乙酸正丁酯中14种杂质[J].检验检疫学刊,2014(3):44-47.
[3]Iregren A,L?f A,Toomingas A,et al.Irritation effects from experimental exposure to n-butyl acetate[J].American Journal of Industrial Medicine,2010,24(6):727-742.
[4]李凤.乙酸正丁酯反应精馏生产工艺的模拟与研究[D].华东理工大学,2013.
[5]王晓明.热解析-气相色谱法测定室内空气中的总挥发性有机物(TVOC)[J].广州化工,2014(17):149-151.
[6]张晓淳,陈弘丽,李津津.溶剂解析-气相色谱法同时测定空气中12种挥发性有机物[J].东莞理工学院学报,2016(1):49-52.