原子吸收法测定烟灰中金属元素含量的前处理方法改进  

Improvement of pretreatment method for determination of metal elements in cigarette ash by atomic absorption spectrometry

作　　者：马胜楠 王建民 冯亚婕 赵怡凡 杨晗钰 MA Shengnan;WANG Jianmin;FENG Yajie;ZHAO Yifan;YANG Hanyu(College of Food and Biological Engineering,Zhengzhou University of Light Industry,Zhengzhou 450001,China)

机构地区：[1]郑州轻工业大学食品与生物工程学院

出　　处：《轻工学报》2019年第5期32-39,共8页Journal of Light Industry

摘　　要：针对原子吸收法测定卷烟烟灰中金属元素时,采用直接微波消解法处理样品所得消解液澄清度差、测定结果 RSD偏高的问题,提出了先进行灰化再微波消解的干湿结合前处理方法,并对微波消解酸体系和马弗炉灰化条件进行了优化研究.结果表明:酸体系主要影响测量结果的准确度,当HNO3,HF,H2O2的体积比为7∶0. 5∶1. 5时,微波消解效果最好;灰化效果主要影响测量结果的RSD,当样品质量取0. 10 g,灰化温度和时间分别取600℃和60 min时,RSD与预测值吻合较好;采用干湿结合法测量K,Ca,Mg,Fe,Mn,Zn,Cu 7种元素的含量,RSD较直接微波消解法均大幅下降,加标回收实验结果显示各元素测定结果的RSD为1. 33%~2. 41%,平均回收率为97. 77%~102. 05%,说明该方法可重复性和准确度均较好,可为非均质化样品前处理方式的选择所借鉴.In the process of measuring the content of metal elements in cigarette soot by atomic absorption method,if the pre-treatment method was used directly,the clarity of the digesting solution was poor and the RSD of the measurement results were high. In order to solve this problem,a pre-treatment method of combined ashing and microwave digestion was proposed. The digestion acid system of microwave digestion and ashing conditions of the muffle furnace were optimized. The results showed that the acid system mainly affected the accuracy of the measurement results. When the volume ratio of HNO3,HF and H2 O2 was 7∶0. 5∶1. 5,the microwave digestion effect was the best. The ashing mainly influenced the RSD of the results. When the sample quality was 0. 10 g,the ashing temperature and time were taken at 600 ℃ and 60 min,respectively,RSD values matched well with predicted values. Compared with direct microwave digestion,the RSD of potassium,calcium,magnesium,iron,manganese,zinc,and copper elements dropped dramatically,using the dry-wet combination method. The results of recovery experiments showed that the RSD of each element was 1. 33%~2. 41% and the average recovery was 97. 77%~ 102. 05%. Above all,this method had favorable repeatability and accuracy,and could be used for reference in the selection of pretreatment methods for homogenized samples.

关 键 词：卷烟烟灰 灰化 微波消解 原子吸收法 金属元素测量 

分 类 号：TS452[农业科学—烟草工业]