摘要:
利用纯化合物CaCO_3的热分解,建立了热重质谱(TG-MS)联用法定量分析逸出组分CO_2的标准工作曲线.采用Freeman-Carroll方法,从单次反应计算得到了CaCO_3分解反应的表观活化能.利用TG-MS结合有机质谱EI法,分析了卷烟纸热裂解气相产物的逸出行为,确定了惰性气氛下卷烟纸中CaCO_3的分解温度区间,建立了测定卷烟纸CaCO_3含量的简便方法.结果表明:在25℃·min~(-1)升温速率、200 mL·min~(-1)载气流速、氦气氛围下,CO_2定量的标准曲线方程为Y=10~(-8) X+O.162 9,R~2=O.998 2.利用TG-MS法可快速确定卷烟纸中CaCO_3含量.
Abstract:
The calibration curve for quantitative analysis of evolved CO_2 during thermal decomposition in a thermogravimetric analyzer coupled with mass spectrometer (TG-MS) was made by the decomposition of pure CaCO_3. The activation energy of the decomposition reaction was calculated from a single experiment using Freeman-Carroll method. Using electron ionization, TG-MS in inert atmosphere was firstly performed to analyze the evolved behavior of gaseous mixture released by thermal decomposition of cigarette paper, to obtain the temperature range of the decomposition reaction of CaCO_3 in cigarette paper, and to build the quantitative method of CaCO_3 of cigarette paper. The results show that the calibration curve for the quantitative analysis of evolved CO_2 by TG-MS is Y =10~(-8)X+0. 162 9,R~2=0. 998 2 under He atmosphere at heating rate of 25 ℃ · min~(-1) and gas flow rate of 200 mL ·min~(-1). Using the calibration curve, the amount of CaCO_3 in cigarette paper can be determined easily by TG-MS.
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