电感耦合等离子体原子发射光谱(ICP-AES)法测定钢中硼时样品溶解损失及空白控制研究  

Study on Loss in Sample Digestion and Blank Control during the Determination of Boron in Steel by ICP-AES

作　　者：徐建平[1] 程德翔[2] 

机构地区：[1]武汉科技大学省部共建耐火材料与冶金国家重点实验室,武汉430081 [2]江汉大学,武汉430049

出　　处：《中国无机分析化学》2016年第2期31-34,共4页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家自然科学基金项目(51274156)资助

摘　　要：用电感耦合等离子体原子发射光谱(ICP-AES)法研究了钢中硼的测定。实验发现,分析线在硼182.64nm处无硼铁基体空白值低于纯试剂(无铁)空白值。样品分析时,应进行无硼铁基空白实验,结果计算只能用此空白值。对普通玻璃烧杯和聚四氟乙烯烧杯的酸溶样品测定结果进行了比较,结果表明,测定结果和空白值相近且都很低,无硼普通玻璃烧杯也能满足钢中低含量硼的测定需要。通过对实验与报道结果比较分析表明,硝酸或王水加热溶解样品得到的溶液中硼没有损失,此溶液可测定钢中酸溶硼;用高氯酸发烟处理后,样品中酸不溶硼可能会溶解,但硼会挥发损失。因此,高氯酸发烟处理不能测定硼。A method for the determination of boron in steel samples by ICP-AES was established. The results indicated that the blank values obtained by no ferro matrix without boron were lower than those obtained by pure reagents （iron-free） with boron 182.64 nm as the analysis line. Thus, it is necessary to prepare blank tests using no ferro matrix without boron, and the analytical results should be calculated by these blank values. The determination values of acid-soluble samples were similar between glass beakers and teflon beakers, therefore, glass beakers can meet the requirements of the determination of low content boron in steel samples. The results compared with the literature show that nitric acid or aqua regia can be suit for sample digestion due to its no loss of boron. However, perchloric acid is not a suitable option for its volatilization loss of boron during the sample pretreatment.

关 键 词：硼 空白 损失 ICP-AES 

分 类 号：O657.31[理学—分析化学] TH744.11[理学—化学]