超声提取-连续流动分析法测定卷烟纸中钙的含量  

Determination of Calcium in Cigarette Paper by Continuous Flow Analysis Method with Ultrasonic Extraction

作　　者：潘力[1] 汤晓东[1] 赵攀攀[1] 黄华[1] 斯文[1] 蒋佳磊[1] 苏燕[1] 陆扬[1] 朱书秀[1] PAN Li;TANG Xiaodong;ZHAO Panpan;HUANG Hua;SI Wen;JIANG Jialei;SU Yan;LU Yang;ZHU Shuxiu(China Tobacco Zhejiang Industrial Co.,Ltd.,Hangzhou 310008,China)

机构地区：[1]浙江中烟工业有限责任公司,杭州310008

出　　处：《理化检验（化学分册）》2021年第12期1089-1093,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

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Ca^(2+)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。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 Ca^(2+) 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.

关 键 词：超声提取 连续流动分析法 DBC-偶氮胂 卷烟纸 钙 

分 类 号：O657.32[理学—分析化学]