稻米中汞元素的样品前处理和检测关键因素研究  

Study on the Key Factors of Sample Pretreatment and Detection for Mercury in Rice

作　　者：陈曦 周明慧 伍燕湘 张洁琼 田巍 王松雪 CHEN Xi;ZHOU Minghui;WU Yanxiang;ZHANG Jieqiong;TIAN Wei;WANG Songxue(Academy of National Food and Strategic Reserves Administration,Beijing 100037)

机构地区：[1]国家粮食和物资储备局科学研究院,北京100037

出　　处：《分析科学学报》2022年第1期56-60,共5页Journal of Analytical Science

基　　金：国家重点研发计划(No.2017YFC1601300)。

摘　　要：为了减少因为样品前处理关键条件控制不当引起的汞元素损失,提高稻米样品中痕量汞检测的准确性,本文系统研究了消解温度、赶酸温度和时间、载流和还原剂浓度、负高压、标准溶液和样品液酸度的匹配程度对汞检测结果的影响,建立了微波消解-原子荧光光谱法精准测定稻米中的汞含量,同时进行方法学评价。结果显示,消解温度为180℃,温度110℃赶酸30 min,载流5%HNO_(3),还原剂0.5%KBH_(4),负高压270 V,标准溶液稀释剂的酸度与样品液的酸度保持一致,大米质控样品中汞的检测结果符合其标准值,加标回收率为96.0%~102.5%,方法准确性和灵敏度可满足日常检测要求。To reduce the loss of mercury in the sample caused by improper sample preparation and improve the accuracy of detection for trace mercury in rice,the effects of digestion temperature,acid removal temperature and time,concentration of carrier solution and reductants,negative high pressure,standard solution and sample solution matching the degree of acidity on mercury detection results were systematically studied.At the same time,the methodology was evaluated.The conclusion showed that the results of mercury in rice quality control sample met the standard value,when the digestion temperature,acid removal temperature,acid removal time,concentration of HNO_(3) and KBH_(4),and negative high pressure were 180℃,110℃,30 min,5%,0.5%and 270 V,respectively,meanwhile the acidity of diluent of standard solution was consistent with sample solution.The recoveries ranged from 96.0%to 102.5%,the accuracy and sensitivity of this method met the needs of daily detection.The optimized process for pretreating and detecting rice samples has significance for guiding practice.

关 键 词：汞 大米 微波消解 原子荧光光谱法 

分 类 号：O657.31[理学—分析化学]