4 一氧化碳的直接進(jìn)樣—?dú)庀嗌V法
4.1 原理
空氣中的一氧化碳用注射器采集,直接進(jìn)樣。一氧化碳在氫氣中經(jīng)分子篩與碳多孔小球串聯(lián)柱分
離,通過(guò)鎳催化劑轉(zhuǎn)化為甲烷,用氫焰離子化檢測(cè)器檢測(cè);以保留時(shí)間定性,峰高或峰面積定量。
4.2 儀器
4.2.1 注射器,100ml,2ml。
4.2.2 氣相色譜儀,氫焰離子化檢測(cè)器,帶一氧化碳鎳催化劑轉(zhuǎn)化爐。
儀器操作參考條件
色譜柱:1.2m×3mm5A 或13X分子篩,放在前;0.8m×3mm 柱內(nèi)裝碳多孔小球;兩柱串聯(lián)。
柱溫:60℃;
汽化室溫度:130℃;
檢測(cè)室溫度:130℃;
轉(zhuǎn)化爐溫度:380℃;
2
GBZ/T160.28—2004載氣(氫氣)流量:55ml/min;
氮?dú)饬髁?130ml/min。
4.3 試劑
4.3.1 5A 或13X分子篩,60~80目。在550℃活化2h,于干燥器中冷卻后立即裝柱。
4.3.2 碳多孔小球(TDX-01),60~80目。
4.3.3 一氧化碳標(biāo)準(zhǔn)氣:用國(guó)家認(rèn)可的標(biāo)準(zhǔn)氣配制。
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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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