GC/MS Determination of Acephate in Water

GC/MS Determination of Acephate in Water
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GC/MS 测定水中乙酰甲胺磷

DOI:
10.5985/jec.2.31
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发表时间:
1992
期刊:
影响因子:
--
通讯作者:
T. Okumura
T. Okumura
中科院分区:
--
文献类型:
--
作者:
T. Okumura

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介绍了水样中乙酰甲胺磷的测定方法。水样被蒸发干了。加入无水硫酸钠后,用二氯甲烷从残渣中提取乙酰甲胺磷。二氯甲烷提取液在库德纳-丹麦装置中浓缩至3-5ml,在氮气流下继续蒸发至0.5ml。采用毛细管气相色谱-选择离子监测法(GCSIM)测定,内标品为苊-d10 (0.5m1的1.0ppm二氯甲烷溶液)和乙酸(50μl)。由于乙酸的加入能有效地阻止乙酰甲胺磷在注射口的吸附,因此获得了高响应和低相对标准偏差。此外,由于甲胺磷对色谱柱条件非常敏感,在较差的色谱柱条件下,其峰极低。括号中蒸馏水和河水的回收率为91.8%(3.2%),相对标准偏差为96.4%(5.0%)。然而,由于被余氯分解,甲胺磷不能从自来水中回收。该方法对乙酰甲胺磷的检出限为0.5ng。
A method is described for the determination of acephate in water sample. The water sample was evaporated to dryness. After addition of unhydrous sodium sulfate, acephate was extracted with dichloromethane from the residue. The dichloromethane extract was concentrated in a Kuderna-Danish apparatus to 3-5ml and continue evaporation to 0.5ml under a nitrogen stream. Acenaphthene-d10 (0.5m1 of 1.0ppm dichloromethane solution) as internal standard and acetic acid (50μl) were added and determined by capillary gas chromatography-selected-ion monitoring (GCSIM) . As the addition of acetic acid was effective to prevent adsorption of acephate to injection port, high respons and low relative standard deviation were obtained. In addition, as acephate was very sensitive to column condition, the peak extremely tailed under inferior column condition. The recoveries and relative standard deviation in parenthesis for distilled water and river water were 91.8% (3.2%) and 96.4% (5.0%), respectively. However, acephate was not recovered from tap water, since it was decomposed by residual chlorine. In this method, the detection limit of acephate was 0.5ng.