HH-5 水质 硝基酚类化合物的测定毛细管柱

 警告：实验中使用的标准物质和有机溶剂为有毒有害物质，试剂配制和样品前处理过程  应在通风橱内进行；操作时应按要求佩戴防护器具，避免接触皮肤和衣物。

1 适用范围

      本标准规定了测定水中硝基酚类化合物的气相色谱-质谱法。

      本标准适用于地表水、地下水、生活污水、工业废水和海水中 2-硝基酚、3-甲基-2-硝基酚、4-甲基-2-硝基酚、5-甲基-2-硝基酚、2,5-二硝基酚、3-硝基酚、2,4-二硝基酚、4-硝基酚、2,6-二硝基酚、3-甲基-4-硝基酚、6-甲基-2,4-二硝基酚和 2,6-二甲基-4-硝基酚等 12 种硝基酚类化合物的测定。

      当取样体积为 1000 ml，试样定容体积为 1.0 ml 时，12 种硝基酚类化合物的方法检出限为 0.2 μg/L～2 μg/L，测定下限为 0.8 μg/L～8 μg/L。详见附录 A。

2 规范性引用文件

      本标准引用了下列文件或其中的条款。凡是不注日期的引用文件，其有效版本适用于本标准。

      GB 17378.3 海洋监测规范 第 3 部分：样品采集、贮存与运输

      GB/T 14581 水质 湖泊和水库采样技术指导

      HJ/T 91 地表水和污水监测技术规范

      HJ 91.1 污水监测技术规范

      HJ/T 164 地下水环境监测技术规范

3 方法原理

      样品经酸碱分配净化后，在酸性条件下（pH 值为 1～2），采用液液萃取法或者固相萃取法提取硝基酚类化合物，萃取液经脱水、浓缩、定容后用气相色谱分离，质谱检测。根据   保留时间、碎片离子质荷比及丰度比定性，内标法定量。

 水质 硝基酚类化合物的测定毛细管柱  测试谱图：



Water quality - Capillary column for the determination of nitrophenols
 Water quality Capillary column for the determination of nitrophenols Details:


Name: capillary column
Stationary Phase: 5% Phenyl-95% Methylpolysiloxane
Specifications: 30m*0.25mm*0.25um
Model: HH-5
Application: HJ 1150-2020 Water Quality Determination of Nitrophenol Compounds Gas Chromatography-Mass Spectrometry

 Warning: The standard substances and organic solvents used in the experiment are toxic and harmful substances, and the preparation of reagents and sample pretreatment should be carried out in a fume hood; during operation, protective equipment should be worn as required to avoid contact with skin and clothing.

1 Scope of application

      This standard specifies the gas chromatography-mass spectrometry method for the determination of nitrophenolic compounds in water.

      This standard applies to 2-nitrophenol, 3-methyl-2-nitrophenol, 4-methyl-2-nitrophenol, 5-methyl- 2-nitrophenol, 2,5-dinitrophenol, 3-nitrophenol, 2,4-dinitrophenol, 4-nitrophenol, 2,6-dinitrophenol, 3-methyl- Determination of 12 kinds of nitrophenols such as 4-nitrophenol, 6-methyl-2,4-dinitrophenol and 2,6-dimethyl-4-nitrophenol.

      When the sampling volume is 1000 ml and the constant volume of the sample is 1.0 ml, the detection limits of the 12 nitrophenolic compounds are 0.2 μg/L～2 μg/L, and the lower determination limits are 0.8 μg/L～8 μg /L. See Appendix A for details.

2 Normative references

      This standard refers to the following documents or clauses thereof. For undated references, the valid edition applies to this standard.

      GB 17378.3 Marine Monitoring Specification Part 3: Sample Collection, Storage and Transportation

      GB/T 14581 Water Quality - Technical Guidance for Sampling in Lakes and Reservoirs

      HJ/T 91 Technical Specification for Surface Water and Sewage Monitoring

      HJ 91.1 Technical Specification for Wastewater Monitoring

      HJ/T 164 Technical Specification for Groundwater Environmental Monitoring

3 Principles of the method

      After the sample is purified by acid-base distribution, nitrophenolic compounds are extracted by liquid-liquid extraction or solid-phase extraction under acidic conditions (pH value is 1 to 2). Chromatographic separation, mass spectrometry detection. According to retention time, mass-to-charge ratio of fragment ions and abundance ratio, quantification was carried out with internal standard method.

 Water quality Capillary column for the determination of nitrophenolic compounds Test chromatogram: