电感耦合等离子体原子发射光谱法测定硼铁中多元素时分解方法的探究  

Discussion on decomposition method during the determination of multi-elements in ferroboron by inductively coupled plasma atomic emission spectrometry

作　　者：马书风 李雅华 张翠敏 MA Shufeng;LI Yahua;ZHANG Cuimin(NCS Testing Technology Co.,Ltd.,Beijing 100081,China)

机构地区：[1]钢研纳克检测技术股份有限公司,北京100081

出　　处：《冶金分析》2025年第3期57-63,共7页Metallurgical Analysis

摘　　要：随着新技术的发展,不同性能的新型硼铁合金应运而生,硼铁中不同元素的含量决定其不同的性能。目前对硼铁中各元素的检测通常采用碱熔法和酸溶回渣法进行前处理,虽可使样品溶解完全并实现其同时测定,但对某些元素,若要进行单独测定,使用该方法操作较繁琐,因此从经济性和时间成本考虑,针对不同元素选择合适的分解方法非常重要。本文采用不同分解方法对硼铁标准物质/标准样品进行消解,包括直接酸溶法(硝酸+氢氟酸+高氯酸)、微波消解法、酸溶回渣法和碱熔法,再使用电感耦合等离子体原子发射光谱法(ICP-AES)测定不同方式消解后的试液中铬、镍、钒、铜、钛、锰、铝和磷。结果表明:使用直接酸溶法和微波消解法处理后的试液中有少量黑色不溶物,但是不影响铬、镍、钒、铜、钛和锰的准确测定;而对于铝和磷元素,其测定结果与认定值/标准值相比偏低,尤其是磷元素显著偏低,即样品的溶解程度对铝和磷的准确测定有较大影响。因此对于铬、镍、钒、铜、钛和锰的测定,使用上述4种溶解方式均可;而对于铝和磷元素,则必须采用酸溶回渣法或碱熔法处理样品使其全部溶解才能准确测定。With the development of new technologies,some novel ferroboron alloys with different properties are developed.The contents of different elements in ferroboron determines the properties of alloys.At present,the alkali melting method or acid dissolution slag method is usually used for pretreatment of ferroboron sample before detection of elements.Although the sample can be dissolved completely and the simultaneous determination can be achieved,these methods are cumbersome if some elements are determined separately.Therefore,it is very important to choose the appropriate decomposition method for different elements in consideration of the perspective of economy and time cost.In this study,the certified reference materials(CRM)of ferroboron were digested using various decomposition methods including direct acid dissolution method(nitric acid+hydrofluoric acid+perchloric acid),microwave digestion method,acid dissolution slag method and alkali melting method.Then,the contents of chromium,nickel,vanadium,copper,titanium,manganese,aluminum and phosphorus in the digestion solution using different decomposition methods were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).The results showed that there were few black insoluble matters in the solution when the direct acid dissolution and microwave digestion were used,but the accurate determination of chromium,nickel,vanadium,copper,titanium and manganese was not affected.However,the determination results of aluminum and phosphorus were relatively lower than the certified values or standard values,especially for phosphorus.It indicated that the degree of dissolution of the sample had significant influence on the accurate determination of aluminum and phosphorus.Therefore,for the determination of chromium,nickel,vanadium,copper,titanium and manganese,the four dissolution methods above were all acceptable.However,for the determination of aluminum and phosphorus,the sample must be completely dissolved using acid dissolution slag method and alkali mel

关 键 词：硼铁 铬 镍 钒 铜 钛 锰 铝 磷 电感耦合等离子体原子发射光谱法(ICP-AES) 直接酸溶法 微波消解法 酸溶回渣法 碱熔法 

分 类 号：TF031[冶金工程—冶金物理化学] TF044[理学—分析化学] TF702.4[理学—化学] O657.31