饮用水中五种有机磷农药的快速检测法

本文介绍了使用Ｗａｔｅｒｓ ＯＡＳＩＳ－ＨＬＢ固相萃取小柱从水中分离富集敌百虫、敌敌畏、乐果、甲基对硫磷，对硫磷五种有机磷农药的快速检测法。     

水相中三丁基锡预富集方法研究

首次用x－5树脂吸附三丁基锡（TBT）化合物。结果表明,X－5树脂吸附TBT化合物具有吸附容量大、吸附速度快等优点,符合Freundlich吸附等温式;用自制的吸附注（长度为11cm,内径为0.55cm的玻璃管,内装x－5大孔网状树脂,约0.7g）作TBT吸附剂,研究各种因素对吸附及脱附效率的影响。结果表明,吸附率主要取决于柱长及流速,而溶液的盐度及pH值影响不大;脱附率主要取决于洗脱剂的流速,而pH值影响不大;实际样品的回收率超过90％。     

NPD与FPD气相色谱法测定水中的黄磷

实验采用优化条件,对甲苯萃取水和废水中黄磷进行测定。萃取液经气相色谱仪毛细色谱柱分离后,氮磷检测器（NPD）或火焰光度检测器（FPD,带磷滤光片）检测,根据色谱峰的保留时间定性,外标法定量。使用NPD检测器分析时,本方法检出限为0.04μg/L;使用FPD检测器分析时,本方法检出限为0.1μg/L。     

静态顶空-气相色谱法测定水中二硫化碳

采用气相色谱法静态顶空进样,HP-1柱分离,FPD检测器检测,测定水中CS2,并对测定条件进行了探讨。实验表明,当取样量为10.0 mL,气液比为12.3,在40℃平衡25 min时,能获得满意的灵敏度,且稳定性很好。二硫化碳在0.63μg/L～502μg/L之间呈线性,相关系数为0.999 2,相对标准偏差为1.3%～5.7%、加标回收率为88%～105%,检出限可达0.3μg/L。干扰试验表明硫化氢、甲硫醇、甲硫醚不干扰二硫化碳的测定。本方法操作简便,测定快速,完全能够满足快速分析水中二硫化碳的要求。     

固相萃取法提取净化生物检材中三类农药的实验研究

本文以常见的六种有机磷类、四种氨基甲酸脂类和五种拟种虫菊酯类农药为对象，研究了用国产ＧＤＸ－４０３或Ｃ１８固相小柱同时提取净化环境样品和生物检材中三种类型的农药，分别采用ＧＣ／ＦＰＤ，ＧＣ／ＮＰＤ和ＧＣ／ＥＣＤ三种特征性气相色谱法进行分析鉴定，为系统分析有机农药提供了一套快速、简便的固相提取方法。     

气相色谱法测定水中七种有机磷农药研究

水中微量有机磷农药经二氯甲烷萃取、净化、凝胶净化色谱(GPC)浓缩,用带火焰光度检测器(FPD)的毛细管柱气相色谱仪测定.实验结果表明:七种有机磷农药曲线线性良好,相关系数可达0.999以上;检出限能够满足《地表水环境质量标准》限值要求;加标回收率范围为81.4%~92.4%,相对标准偏差范围为2.5%~7.3%,相对误差范围为1.9%~8.5%.可以同时测定《地表水环境质量标准》中规定的7种有机磷农药,提高工作效率.     

Comparative study of the linearity and sensitivity of electron capture and flame photometric detectors using a pesticide standard

Abstract

A study was undertaken to compare and evaluate the different types of ⁶³Ni and ³H electron capture (ECD) and flame photometric detectors (FPD) as part of the Canadian Check Sample Program on Pesticide Residue Analysis. Twenty‐seven laboratories were supplied with chlorpyrifos standard solutions for the determination of linear range and minimum detectable amounts (MDA). Each laboratory selected its own operating conditions except for the FPD study. Results for the FPD were compared with standardized flame conditions designed to optimize the exponential factor in the S‐mode. The MDA of the ECDs (pulsed and direct‐current) ranged from 0.09 to 0.17 pg/sec for ⁶³Ni and ³H sources respectively. The corresponding MDA for the linearized ECDs (pulse modulated or constant current) was 0.04 pg/sec and a linear range of 10⁴ or greater with nitrogen as the carried gas. Use of argon/methane and a pulse width of 0.1 usec extended this range to 10⁵ but the sensitivity was not as great as with nitrogen carrier gas. The practical limit of detector sensitivity was found to be instrument dependent depending primarily on the noise level. In the FPD study, operating in the P‐mode gave an average MDA of 5.97 pg/sec and a linear range of 2 x 10³. Similarly, the S‐mode parameters were 81.1 pg/sec and 8 x 10² respectively with an average exponential factor of n 1.8. Attempts to apply optimized detector gas‐flow conditions improved sensitivity and linearity in the S‐mode only.     

南极长城湾附近和台湾以南部分海域水样中丁基锡化合物分析

对南极长城站附近水域及中国台湾以南海域采集的水样进行了分析研究。应用顶空固相微萃取（SPME）技术富集丁基锡化合物，由气相色谱分离后，表面发射火焰光度检测器测定，在两个水域均未检出三丁基锡，但存在一定量的三丁基锡降解产物，即二丁基锡和一丁基锡。