摘要
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。
A digestion method which consists of microwave digestion and wet digestion for subsection by using hy-dride generation atomic fluorescence spectrometry was established to determine the total arsenic content in the shellfish and algae products. The effects of different acid systems and digestion processs in microwave digestion and different con-tents of perchloric acid and sulfuric acid in wet digestion were studied. The sample prepared by microwave digestion with 5 ml nitric acid and wet digestion with 1 ml perchloric acid and 2-3 ml sulfuric acid were digest to colorless solution. The pretreatment showed such advantages as high digestion efficiency, controllable operation process, well-judged reaction end point, less reagent consumption, environment friendly, and accurate and stable test data. The spiked recovery rate of arsenic was over 90%, which satisfied the requirement of total arsenic determination in shellfish and algae products.
出处
《江苏农业学报》
CSCD
北大核心
2017年第3期695-700,共6页
Jiangsu Journal of Agricultural Sciences
基金
江苏省农业自主创新基金项目[CX(13)3039]
江苏省大型仪器平台新方法开发项目(BZ201304)
国家海洋公益性行业科研专项(201105023
2013418007-1)
关键词
微波消解
湿法消解
砷
贝藻产品
原子荧光光谱法
microwave digestion
wet digestion
arsenic
shellfish and algae
atomic fluorescence spec-trometry
