微波消解—电感耦合等离子体质谱法测定钢铁及合金中总铝和总硼  

Determination of total aluminium and total boron in iron,steel and alloys by microwave digestion-inductively coupled plasma mass spectrometry

作　　者：刘正[1] 张翠敏[1] 王明海[1] 张华[2] 

机构地区：[1]钢铁研究总院,北京100081 [2]首都师范大学,北京100037

出　　处：《冶金分析》2007年第5期1-7,共7页Metallurgical Analysis

基　　金：科技部新技术;新方法基金项目(2003-34)

摘　　要：建立了微波消解分解样品,电感耦合等离子体质谱法测定钢铁及合金中总铝和总硼的方法。采用自制的提纯装置提纯氢氟酸。借助微波消解炉,用3mL盐酸、1 mL硝酸和1 mL氢氟酸(1+1),在适宜的压力和温度下消解可将样品消解完全。铍、钪随仪器参数波动引起的信号变化规律与硼、铝的相同。以被测样品主量元素和样品分解的酸进行基体匹配,采用Be和Sc内标补偿仪器漂移和校正基体效应。用本法测定样品中总铝和总硼,快速、简便、精密度好,测定结果与认定值符合较好,适于测定钢铁及合金中质量分数为0.0001%～0.1%总铝和总硼。方法的检出限:Al为0.1 ng/mL,B为0.2 ng/mL。A method for the determination of total boron and total aluminium in iron, steel and alloys by inductively coupled plasma mass spectrometry（ICP-MS）after microwave digestion has been developed. Hydroflouric acid was purified using self-reading purifying equipment. In microwave oven, sample was completely digested with 3 mL of hydrochloric acid, 1 mL of nitric acid and 1 mL of hydrofluoric acid（1＋1） under optimal pressure and temperature. The Influence of ICP-MS parameters on signal of beryllium,scandium was similar with that of aluminium and boron. Be and Sc were selected as internal standard to correct the matrix effect and instrument drift. Determination range of total aluminium and total boron was between 0. 000 1% and 0.1%. The detection limits（3σ）were 0.1 ng/mL for aluminium,0.2 ng/mL for boron. The method has been succesfully used for determination of total aluminium and total boron in iron, steel and high temperature alloy standard samples. The results compare favourably with the certified values, indicating the accuracy of method.

关 键 词：微波消解 电感耦合等离子体质谱法 钢铁 合金 铝 硼 

分 类 号：TG115.3[金属学及工艺—物理冶金]