再造烟叶中碳酸钙质量分数的热分析检测法  

Determination of calcium carbonate content in reconstituted tobacco by thermal analysis

作　　者：郑泉兴 刘秀彩[1] 马鹏飞 蔡国华 钟洪祥 张建平 黄华发 鹿洪亮 黄朝章 蓝洪桥 许寒春 谢卫 李巧灵 ZHENG Quanxing;LIU Xiucai;MA Pengfei;CAI Guohua;ZHONG Hongxiang;ZHANG Jianping;HUANG Huafa;LU Hongliang;HUANG Chaozhang;LAN Hongqiao;XU Hanchun;XIE Wei;LI Qiaoling(Technology Center,China Tobacco Fujian Industrial Co.,Ltd.,Xiamen 361021,Fujian,China;Department of Chemistry,Xiamen University,Xiamen 361005,Fujian,China)

机构地区：[1]福建中烟工业有限责任公司技术中心,福建省361021 [2]厦门大学化学系,福建省361005

出　　处：《烟草科技》2020年第10期66-72,共7页Tobacco Science & Technology

基　　金：福建中烟工业有限责任公司科技项目“再造烟叶低温热解特性影响因素分析与应用研究”(FJZYKJJH2019002)。

摘　　要：为检测再造烟叶中碳酸钙的质量分数,采用热分析技术,以碳酸钙特征热解峰为定性手段、热解温度段CO2的质量损失为定量依据,建立了再造烟叶中碳酸钙质量分数的热分析检测方法。通过标准加入法验证了该方法的基体干扰,对比了氮气和空气气氛下的回收率;并将热分析检测结果与离子色谱法检测结果进行了对比。结果表明:①再造烟叶样品A中碳酸钙的热解峰位于870~980 K,此温度段对应CO2质量损失为3.62%,换算成碳酸钙的质量分数是8.23%;②通过标准加入法得到的标准曲线相关系数为0.999,通过标准曲线外推得到再造烟叶样品A中碳酸钙质量分数为7.59%,该结果与热分析直接检测结果8.23%的相对偏差为7.8%,说明再造烟叶基体对热分析结果基本无干扰;③在氮气和空气气氛下碳酸钙的加标回收率分别在97.50%~102.63%和60.71%~85.95%之间,说明氮气气氛的准确性更高,5次重复性实验检测再造烟叶样品A中碳酸钙质量分数结果的变异系数为0.76%,说明该法的稳定性好;④热分析法检测的再造烟叶样品A和B中碳酸钙质量分数略低于经典离子色谱法,偏差的绝对值均小于0.4百分点,但热分析法步骤少、快速、操作简便,且实验过程中无需使用任何有机或无机试剂,绿色环保。A method to determine the calcium carbonate content in reconstituted tobacco was established using thermal analysis technology.This method measured the characteristic peak of thermal decomposition of calcium carbonate and quantified the mass loss of carbon dioxide in the pyrolysis process.The matrix interference was verified by standard addition method.The recoveries of the thermal analysis in nitrogen and air atmosphere were measured,and the test results were compared with those obtained by a classical ion chromatography.The results showed that:1)The pyrolysis peak of calcium carbonate in reconstituted tobacco sample A was located at 870-980 K,and the mass loss of carbon dioxide corresponding to this temperature range was 3.62%,which converted into 8.23%calcium carbonate content.2)The correlation coefficient of the standard curve obtained by the standard addition method reached 0.999,and the calcium carbonate content in sample A was 7.59%by standard curve extrapolation method.The relative deviation between the results of the two method was 7.8%,which indicated that the reconstituted tobacco substrate had little interference on the thermal analysis result.3)The spiked recoveries of calcium carbonate in nitrogen and air atmosphere were 97.50%-102.63%and 60.71%-85.95%,respectively,which suggested that the accuracy of the results obtained in nitrogen atmosphere was higher.The method had a good stability with the variation coefficient of 0.76%by 5 repetitive tests of the same sample.4)The calcium carbonate contents in reconstituted tobacco samples A and B obtained by the thermal method were slightly lower than those by the ion chromatography with the absolute values of deviation less than 0.4 percentage points.However,the thermal analysis method was simple,fast,convenient,and environment-friendly with no reagent needed in experimental processes.

关 键 词：再造烟叶 碳酸钙 热分析 热解峰 质量损失 

分 类 号：TS411.1[农业科学—烟草工业]