浩瀚HJ/T 33-1999 固定污染源排气中甲醇的测定填充柱5%Carbowax 20M Carbopack B

HJ/T 33-1999 固定污染源排气中甲醇的测定 气相色谱法
1 适用范围

1.1 本标准适用于固定污染源有组织排放和无组织排放的甲醇测定。

1.2 以3倍噪音色谱峰高值计算，当色谱进样量为1.0 ml时，方法的检出限为2 mg/m3；定量测定的浓度范围为5.0-104 mg/m3。

2 方法原理
      载气携带含有甲醇(CH3OH）的试样通过装有固定相的色谱柱，流出色谱柱的甲醇由氢火焰离子化检测器(FID)测定。以标准样品色谱峰的保留时间进行定性，以峰高（或峰面积）定量。

3 引用标准

      下列标准所包含的条文，通过在本标准中引用而构成为本标准的条文。

      GB 16297-1996 大气污染物综合排放标准

      GB 16157-1996 固定污染源排气中颗粒物测定和气态污染物采样方法

4 试剂和材料

4.1 色谱固定液：5%聚乙二醇(Carbowax 20M)。

4.2 载体：石墨碳黑(Carbopack B) 80~120目。

4.3 载气：体积分数为高纯氮99.99％。

4.4 燃烧气：体积分数为纯氢99.9%。

4.5 助燃气：空气。

4.6 无碱玻璃棉。

4.7 甲醇标准气。

      甲醇标准气的稀释方法：根据需要用100 ml全玻璃注射器进行稀释配气（参考《空气和废气监测分析方法》(1990) P42)。 

5 仪器

5.1 气相色谱仪

5.1.1 检测器：氢火焰离子化检测器。

5.1.2 色谱柱

5.1.2.1 色谱柱类型：2m×2~3mm的玻璃（或不锈钢）填充柱

5.1.2.2 色谱柱填充物：5%Carbowax 20M Carbopack B 80-120目。

      色谱柱的填充方法见附录B。
  HJ/T 33-1999 Determination of methanol in exhaust gas from stationary pollution sources-Gas chromatography
1 Scope of application

1.1 This standard is applicable to the determination of methanol in organized and unorganized emissions from stationary pollution sources.

1.2 Calculated by 3 times the noise chromatographic peak height, when the chromatographic injection volume is 1.0 ml, the detection limit of the method is 2 mg/m3; the concentration range of quantitative determination is 5.0-104 mg/m3.

2 Principles of the method
      The carrier gas carries a sample containing methanol (CH3OH) through a chromatographic column equipped with a stationary phase, and the methanol flowing out of the chromatographic column is measured by a hydrogen flame ionization detector (FID). Qualitative by the retention time of the standard sample chromatographic peak, quantitative by peak height (or peak area).

3 Reference Standards

      The following standards contain provisions which, through reference in this standard, constitute provisions of this standard.

      GB 16297-1996 Comprehensive emission standard of air pollutants

      GB 16157-1996 Determination of particulate matter in exhaust gas from stationary pollution sources and sampling methods for gaseous pollutants

4 Reagents and Materials

4.1 Chromatographic fixative: 5% polyethylene glycol (Carbowax 20M).

4.2 Carrier: Graphite carbon black (Carbopack B) 80~120 mesh.

4.3 Carrier gas: the volume fraction is high-purity nitrogen 99.99%.

4.4 Combustion gas: the volume fraction is 99.9% pure hydrogen.

4.5 Supporting gas: air.

4.6 E-glass wool.

4.7 Methanol standard gas.

      Dilution method of methanol standard gas: use a 100 ml all-glass syringe for dilution and gas distribution as needed (refer to "Analysis Methods for Monitoring and Analysis of Air and Waste Gas" (1990) P42).

5 Instruments

5.1 Gas Chromatograph

5.1.1 Detector: hydrogen flame ionization detector.

5.1.2 Chromatographic column

5.1.2.1 Chromatographic column type: 2m×2~3mm glass (or stainless steel) packed column

5.1.2.2 Column packing: 5% Carbowax 20M Carbopack B 80-120 mesh.

      See Appendix B for the packing method of the chromatographic column.