气相色谱法测定工业冰乙酸中甲醇的含量

  1范围
  
  本标准规定了测定工业冰乙酸中甲酸含量的气相色谱法。
  
  本标准适用于工业冰乙酸产品中甲酸含量的测定。
  
  2方法提要
  
  工业冰乙酸中各组分在癸二酸/GDX103柱上分离,热导检测器检测,乙酸乙酯为内标物,内标法定量。
  
  3试剂和材料
  
  3.1氢气:纯度99.9%V/V。
  
  3.2试剂
  
  3.2.1甲酸:色谱纯。
  
  3.2.2乙酸乙酯:色谱纯。
  
  3.2.3冰乙酸:优级纯。
  
  3.2.4高锰酸钾:分析纯。
  
  3.2.5无水乙醇:分析纯。
  
  3.2.6固定液:癸二酸。
  
  3.2.7载体:GDX103,孔径0.18~0.25mm。
  
  4仪器
  
  4.1气相色谱仪。
  
  4.2检测器:热导检测器。
  
  4.3记录仪:满量程为1mV,或色谱数据处理机。
  
  4.4色谱柱
  
  4.4.1柱管:1.5~2.0m,内径2~3mm的不锈钢管或硼硅玻璃管。
  
  4.4.2填充物
  
  固定液:载体=7:100。
  
  涂渍固定液的方法:称取0.28g癸二酸,置于200mL烧杯中,加约23mL无水乙醇溶解,然后加4.0g载体,使载体完全浸没,稍加搅拌,在水浴上缓慢挥发溶液至干,然后移至100℃电热恒温干燥箱中干燥2h。
  
  4.4.3填充方法
  
  将色谱柱的出口端(接检测器端)塞上玻璃棉,接真空泵,另一端接漏斗,开启真空泵,在轻轻地振动下装入固定相,填充均匀,紧密。填充量约2g。再用玻璃棉塞好。
  
  4.4.4色谱柱老化
  
  将填充好的色谱柱安装在色谱仪柱箱中,出口与检测器断开,于120℃老化8h以上,直至基线稳定。
  
  4.5进样器
  
  微量玻璃注射器:容量10

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  86. Знаете ли вы?
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  88. Знаете ли вы?
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