Determination of Calcium in Cigarette Paper by Continuous Flow Analysis Method with Ultrasonic Extraction
摘 要
建立了超声提取-连续流动分析法测定卷烟纸中钙含量的方法。取已处理为2 mm×2 mm的卷烟纸样品0.1 g,用0.050 mol·L-1硝酸溶液100 mL超声30 min,过滤。利用Ca2+与3-(2-胂酸基苯偶氮)-6-(2,6-二溴-4-氯苯偶氮)-4,5-二羟基-2,7-萘二磺酸(DBC-偶氮胂)在一定碱性介质中发生显色反应,生成的蓝色络合物可用于钙的测定的原理,在pH 11的缓冲溶液条件下,以1.0 g·L-1 DBC-偶氮胂溶液为显色剂,滤液用连续流动分析仪测定,检测波长630 nm。结果表明:钙的标准曲线的线性范围为40~200 mg·L-1,检出限(3s)为1.02 mg·L-1;方法用于样品分析,所得测定值的相对标准偏差(n=6)均小于2.0%;按标准加入法进行回收试验,回收率为96.1%~102%;将该方法与YC/T 274-2008进行比对,t检验所得P值大于0.05,两种方法无显著性差异。
Abstract
A method for determination of calcium in cigarette paper by continuous flow analysis method with ultrasonic extraction was established. The cigarette paper sample (treated to 2 mm×2 mm) of 0.1 g was extracted with ultrasonic in 100 mL of 0.050 mol·L-1 nitric acid solution for 30 min, and the resulting solution was filtered. Based on the principle that Ca2+ reacted with DBC-arsenazo in a certain alkaline medium and the blue complex obtained could be used for determination of calcium, the filtrate was determined by continuous flow analyzer with 1.0 g·L-1 DBC-arsenazo solution as the chromogenic reagent under the condition of buffer solution at pH 11, and the detection wavelength was 630 nm. As shown by the results, the linear range of the standard curve of calcium was 40-200 mg·L-1, with detection limit (3s) of 1.02 mg·L-1. The method was used for sample analysis, giving the results of RSDs (n=6) of the determined values less than 2.0%. Test for recovery was made by standard addition method, giving values of recovery in the range of 96.1%-102%. The proposed method was compared with YC/T 274-2008, and P value obtained by t-test was above 0.05. There was no significant difference between the two methods.
中图分类号 O657.32 DOI 10.11973/lhjy-hx202112005
所属栏目 工作简报
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收稿日期 2020/10/23
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备注潘力,工程师,主要从事烟草化学分析研究
引用该论文: PAN Li,TANG Xiaodong,ZHAO Panpan,HUANG Hua,SI Wen,JIANG Jialei,SU Yan,LU Yang,ZHU Shuxiu. Determination of Calcium in Cigarette Paper by Continuous Flow Analysis Method with Ultrasonic Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(12): 1089~1093
潘力,汤晓东,赵攀攀,黄华,斯文,蒋佳磊,苏燕,陆扬,朱书秀. 超声提取-连续流动分析法测定卷烟纸中钙的含量[J]. 理化检验-化学分册, 2021, 57(12): 1089~1093
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参考文献
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【7】冯然军,何恩鹏,粟智,等.微波消解-火焰原子吸收法测定谷物食品中的钙元素[J].应用化工, 2014,43(12):2289-2291.
【8】王颖,张威,李雪,等.干法灰化-离子色谱法测定烟草中的钾、钙和镁[J].烟草科技, 2012,45(1):43-46.
【9】冯广林,李力,朱立军,等.微波消解样品-离子色谱法测定卷烟纸中钠、钾、镁、钙的含量[J].理化检验-化学分册, 2012,48(4):449-451.
【10】张国强,黄朝章,谢卫,等.超声提取-电感耦合等离子体质谱法快速测定卷烟纸中钾、钠、钙、镁的含量[J].中国烟草科学, 2014,35(3):79-84.
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【13】王巍,杨秀云,张晓霞,等.DBC-偶氮胂分光光度法测定水样中钙[J].光谱实验室, 2004,21(3):511-513.
【14】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):36-42.
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