4 一氧化碳的直接进样—气相色谱法
4.1 原理
空气中的一氧化碳用注射器采集,直接进样。一氧化碳在氢气中经分子筛与碳多孔小球串联柱分
离,通过镍催化剂转化为甲烷,用氢焰离子化检测器检测;以保留时间定性,峰高或峰面积定量。
4.2 仪器
4.2.1 注射器,100ml,2ml。
4.2.2 气相色谱仪,氢焰离子化检测器,带一氧化碳镍催化剂转化炉。
仪器操作参考条件
色谱柱:1.2m×3mm5A 或13X分子筛,放在前;0.8m×3mm 柱内装碳多孔小球;两柱串联。
柱温:60℃;
汽化室温度:130℃;
检测室温度:130℃;
转化炉温度:380℃;
2
GBZ/T160.28—2004载气(氢气)流量:55ml/min;
氮气流量:130ml/min。
4.3 试剂
4.3.1 5A 或13X分子筛,60~80目。在550℃活化2h,于干燥器中冷却后立即装柱。
4.3.2 碳多孔小球(TDX-01),60~80目。
4.3.3 一氧化碳标准气:用国家认可的标准气配制。
Direct injection of carbon monoxide - gas chromatography method
4.1 Principle
Carbon monoxide in the air is collected using a syringe and injected directly. Carbon monoxide in hydrogen gas is separated by a series column of molecular sieves and carbon porous spheres
Separation, converted into methane through nickel catalyst, detected by a hydrogen flame ionization detector; Qualitative retention time, quantitative peak height or peak area.
4.2 Instruments
4.2.1 Syringe, 100ml, 2ml.
4.2.2 Gas chromatograph, hydrogen flame ionization detector, with carbon monoxide nickel catalyst converter.
Reference conditions for instrument operation
Chromatography column: 1.2m × 3mm5A or 13X molecular sieve, placed in front; 0.8m × 3mm column with carbon porous spheres inside; Two columns connected in series.
Column temperature: 60 ℃;
Vaporization chamber temperature: 130 ℃;
Testing room temperature: 130 ℃;
Converter temperature: 380 ℃;
two
GBZ/T160.28-2004 Carrier gas (hydrogen) flow rate: 55ml/min;
Nitrogen flow rate: 130ml/min.
4.3 Reagents
4.3.1 5A or 13X molecular sieve, 60-80 mesh. Activated at 550 ℃ for 2 hours, cooled in a dryer and immediately packed into columns.
4.3.2 Carbon porous spheres (TDX-01), 60-80 mesh.
4.3.3 Carbon monoxide standard gas: prepared using nationally recognized standard gas.
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