湿法消解-氢化物发生-原子荧光法测定海产品中的总锡

Determination of total tin in seafood by wet digestion- hydride generation- atomic fluorescence spectrometry

目的建立以硝酸-高氯酸-硫酸为消解体系的海产品中总锡的氢化物发生-原子荧光分析方法。方法优化消解条件,比较不同酸介质和还原剂效果,确定原子荧光法测定海产品中总锡含量的最佳分析条件。结果该法在线性范围为0.0 ng/ml^80.0 ng/ml时,荧光强度(If)与浓度值(C)存在良好的线性关系,回归方程为y=79.80x+3.18,相关系数(r)为0.999 8,检出限为0.029 ng/ml。在4.0 ng/ml、16.0 ng/ml和32.0 ng/ml 3种加标水平下,方法的加标回收率为96.9%~108.0%,相对标准偏差(RSD)为1.7%。结论该法取样量少、预处理简单、分析速度快、准确度高,可作为实验室开展海产品中痕量总锡检测的优选方法。

Objective To establish a method for determination of total tin in seafood by hydride generation- atomic fluorescence spectrometry（ HG- AFS） with nitric acid- sulfuric acid- sulfuric acid as the digestion system. Methods Through optimizing digestion conditions,comparing the effect of different acid medium and reducers,confirm the optimum analysis condition to determine the total tin in seafood by HG- AFS. Results When the linearity range was from 0. 0 ng / ml to 80. 0 ng / ml,there was a good linear relationship between the fluorescence intensity（ If） and the concentration value（ C）; the regression equation was y = 79. 80 x ＋ 3. 18,the correlation coefficient（ r） was 0. 999 8,the detection limit was 0. 029 ng / ml. Under 4 ng / ml,16 ng / ml and 32 ng / ml 3 kinds of standard addition level,the rates of recovery at three different concentrations were among96. 9%- 108. 0%,and RSD was 1. 7%. Conclusion The method needs less sample,simple pretreatment,quick analysis speed,high accuracy. It can be the preferred method in a laboratory to detect tin trace in seafood.