微波消解ICP-AES法检测动物毛被中微量元素的方法研究  

Study of the Elements Determination Method in Animal Fur by Microwave Digestion ICP-AES

作　　者：侯天平[1] 王松君[2] 曹林[3] 常平[4] 侯悦[5] 

机构地区：[1]吉林工程技术师范学院,吉林长春130052 [2]苏州科技学院化学与生物工程学院,江苏苏州215009 [3]北京科技大学材料物理系,北京100083 [4]吉林大学地球勘探科学与技术学院,吉林长春130026 [5]浙江大学材料化工学院,浙江杭州310027

出　　处：《光谱学与光谱分析》2008年第8期1933-1937,共5页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(39970234)资助

摘　　要：针对动物毛被样品的复杂基质,对样品的预处理方法进行了专门研究,利用民用微波炉代替专业微波反应器,采用微波加热技术,利用试剂的不同特点,分别对试剂硝酸、过氧化氢、盐酸和水的配比及试液体积进行试验,对不同的反应功率和反应进行所需的时间都进行了条件试验的研究,优化实验条件,确定选择HNO3-H2O2-HCl-H2O酸溶体系,四种试剂配比为8∶1∶1∶5,输出功率360W条件下加热5min,进行试样密闭消解处理动物毛被样品,采用标准溶液基体匹配法消除动物毛被样品复杂的基体干扰,利用电感耦合等离子体原子发射光谱分析技术,同时检测18个动物毛被样品的常量和微量元素。该方法经国家人发标准物质GBW07601验证,测得方法相对误差在0.83%～9.59%之间,相对标准偏差在0.81%～5.20%之间,该方法的检出限、精密度和准确度各项检测指标在动物毛被实际样品分析中得到验证,均能满足生物样品检测要求。Considering the complex matrix of the sample, the animal fur is carried on to the sample pretreatment method studies specially. The microwave closed system has its unique merit： The microwave radiation has the very strong penetrability and the rapid in-depth heating function. After absorbing microwave the sample and the molecules of reactant may carry on the reaction in short time. But the microwave power is very weak, reaction consumes much time, the resolution is also incomplete. Besides the output excessively is high dispels in the pot the reagent differential pressure to increase the test solution to produce the storm rapidly to boil. As a result of those flaws, the minute step microwave heating digestion method is used to digest test specimen after treated by the acid pickling over night. In the experiment, the specialized microwave reactor is replaced by civil microwave; the microwave heating technology is adopted. According to the different characteristics of reagents, different allocated proportion and the test solution volume of nitric acid, hydrogen peroxide, hydrochloric acid and the water are tested separately. Meanwhile, in order to optimize the experimental condition, the different response power and respond time is also studied. At last, the experimental condition is determined： HNO3-H2O2-HCl-H2O acid system is chose（four reagent allocated proportions are 8 ： 1 ： 1 ： 5） ; test specimen is heated up 10 minutes when the output is 150 W and 5 minutes when the output is 360 W continuously; carries on the test specimen airtight resolution processing animal fur by the sample. To guarantee the standard solution system is consistent with the biological sample substrate, the artificial simulation biology Sample substrate is used to match law configuration standard solution; the ration the substrate element calcium is added. To eliminate disturbance of the sample complex substrate, the substrate match law, which reduces the substrate element disturbance is used. Inductive coupling plasma atom e

关 键 词：动物毛被 微波消解 电感耦合等离子体原子发射光谱法 元素 

分 类 号：O657.3[理学—分析化学]