论文部分内容阅读
目的建立湿法消解-原子荧光光谱法同时测定海产品中总砷、总汞含量的分析方法。方法采取硝酸、高氯酸和硫酸混合体系的冷消解及热消解结合的方法,并采用电炉高温短时间加热的优化条件进行消解样品,利用氢化物原子荧光光谱法同时进行总砷、总汞的测定。结果砷在0～40μg/L浓度范围内呈良好线性关系,汞在0～12μg/L浓度范围内呈良好线性关系,相关系数均大于0.999。砷的检出限为0.037μg/L,回收率为94.36%～96.62%,精密度为0.86%～1.36%,汞的检出限为0.048μg/L,回收率为93.33%～95.28%,精密度为0.88%～2.62%。通过对能力验证HMRL1601海鱼粉中总汞、总砷的检测,检测结果总汞为0.30 mg/kg,总砷为2.06 mg/kg,均为满意结果,黄鱼、紫菜质控样的检测值均在参考值允许范围内。结论该方法操作简便、准确灵敏,适用于每一个实验室开展海产品中总砷总汞的同时测定。
Objective To establish a method for simultaneous determination of total arsenic and total mercury in seafood using wet digestion - atomic fluorescence spectrometry. Methods The combination of cold digestion and thermal digestion in a mixed system of nitric acid, perchloric acid and sulfuric acid was adopted. The samples were digested with the optimized conditions of high temperature and short time heating in an electric furnace. Hydridex atomic fluorescence spectrometry was used for the simultaneous determination of total arsenic and total mercury Determination. Results Arsenic showed a good linearity in the range of 0 ~ 40μg / L. The linearity of mercury was in the range of 0 ~ 12μg / L with the correlation coefficients greater than 0.999. The detection limit of arsenic was 0.037μg / L, the recovery was 94.36% ~ 96.62%, the precision was 0.86% ~ 1.36%, the detection limit of mercury was 0.048μg / L, the recovery was 93.33% ~ 95.28% The degree is 0.88% ~ 2.62%. Through the test of total mercury and total arsenic in the proficiency testing HMRL1601, the total mercury and the total arsenic in the test results were 0.30 mg / kg and 2.06 mg / kg, respectively. Reference range allowed. Conclusion The method is simple, accurate and sensitive. It is suitable for the simultaneous determination of total arsenic and total mercury in seafood in every laboratory.