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建立了微波加湿法分段消解作为前处理,并通过氢化物发生原子荧光法测定贝藻产品中总砷含量的方法。研究了微波消解加酸体系和程序、湿法消解中高氯酸和硫酸用量对砷含量测定的影响,并通过添加质量控制标准样品计算回收率,检测了该方法的准确性。结果表明:用5 ml硝酸进行微波消解后再加1 ml高氯酸、2~3ml硫酸进行湿法分段消解使样品溶液成无色的样品前处理方法,具有消解效率高、操作过程可控、反应终点判断准确、试剂消耗少、环境污染少、检测数据准确稳定等优点。通过检测样品添加同类质量控制标准样品测得的砷回收率在90%以上,满足贝藻产品中总砷含量测定要求。
The microwave digestion method was established as a pretreatment method to determine the total arsenic in the products of Pui alga by hydride generation atomic fluorescence spectrometry. The effect of microwave digestion and acidification system and procedure on the determination of arsenic content in perchloric acid and sulfuric acid in wet digestion was studied. The accuracy of the method was tested by adding the standard sample of quality control. The results showed that the method of pretreatment with 5 ml of nitric acid for microwave digestion followed by 1 ml of perchloric acid and 2 to 3 ml of sulfuric acid to make the sample solution into a colorless sample digested by wet method has the advantages of high digestion efficiency and controllable operation process , Accurate judgment of the end of the reaction, less reagent consumption, less environmental pollution, accurate and stable detection data and the like. The recovery rate of arsenic measured by adding standard samples of similar quality control through testing samples is over 90%, meeting the requirement of determining the total arsenic content in the product.