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
-
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.Abstract: 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 H2O2 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.
-
-
[1]
胡清源,李力,石杰,等.微波消解-电感耦合等离子体质谱法同时测定烟草中27种元素[J].光谱学与光谱分析,2007(6):1210.
-
[2]
李力,戴亚,胡清源,等.卷烟中的锂、铬、镍、铜、砷、硒、钼、镉、铊和铅含量分析[J].烟草科技,2010(4):35.
-
[3]
何杰,旦有明,易建华,等.微波消解-电感耦合等离子体直角加速飞行时间质谱法测定17种进出口卷烟中的10种金属元素[J].安徽农业科学,2013,41(13):5954.
-
[4]
胡秋芬,张艳宏,王森,等.微波消化-原子吸收法测定卷烟中的钾、钠、钙、镁、铜、铁、锌、铅的研究[J].玉溪师范学院学报,2007(3):48.
-
[5]
谢玉龙,朱先约,何东香,等.微波消解-ICP-MS法测定卷烟纸中主要元素和重金属元素[J].分析仪器,2018(1):36.
-
[6]
中华人民共和国国家质量监督检验检疫总局.烟草及烟草制品调节和测试的大气环境:GB/T 16447-2004[S].北京:中国标准出版社,2004.
-
[7]
陈曦.高分辨连续光源原子吸收光谱法测定香烟及烟气中的重金属元素[D].北京:北京工业大学,2016.
-
[8]
钟宇,姜红,杨敏男,等.电感耦合等离子体质谱法分析烟灰中的微量元素[J].微量元素与健康研究,2017,34(6):58.
-
[9]
李力,黄馨,胡清源,等.电感耦合等离子体质谱法测定卷烟用纸中的铜、砷、钼、镉、铊和铅[J].理化检验(化学分册),2011,47(2):163.
-
[10]
国家烟草专卖局.烟草及烟草制品钙的测定原子吸收法:YC/T 174-2003[S].北京:中国标准出版社,2003.
-
[11]
国家烟草专卖局.烟草及烟草制品镁的测定原子吸收法:YC/T 175-2003[S].北京:中国标准出版社,2003.
-
[12]
余建英,何旭宏.数据统计分析与SPSS应用[M].北京:人民邮电出版社,2007.
-
[13]
孙红卫,吕春燕,祁爱琴,等.综合评价中数据标准化的原理研究[J].中国卫生统计,2015,32(2):342.
-
[14]
张林,张晶璇,范琼尹,等.均匀设计结合多元回归分析用于淫羊藿对大鼠肝毒性的影响[J].中国实验方剂学杂志,2018,24(6):189.
-
[15]
张朝晖,STAN O.利用国产TM-陶瓷纤维马弗炉进行样品预处理附生苔藓对大气中重金属元素的生物富集中子活化方法研究[J].现代科学仪器,2000(2):58.
-
[16]
王峰,乙小娟,张慧.微波灰化法测定进出口饲料中的灰分[J].分析测试技术与仪器,2006(2):125.
-
[17]
蒋次清,王岚,廖臻,等.微波马弗炉测定烟草中灰分的研究[J].安徽农业科学,2012,40(7):3980.
-
[18]
唐启义,唐睿.DPS数据数理系统(第2卷).现代统计及数据挖掘[M].北京:科学出版社,2017.
-
[19]
谷力.测定天然和栽培缬草根金属元素的微波和干灰化消解-FAAS法[J].分析测试学报,2002(6):56.
-
[1]
-
点击查看大图
计量
- PDF下载量: 9
- 文章访问数: 3346
- 引证文献数: 0
下载:
