高碘酸钠氧化分光光度法测定硼铁中锰  

Determination of manganese in ferroboron by sodium periodate oxidation spectrophotometry

作　　者：孟伟 李雅华 周胜强[2] MENG Wei;LI Yahua;ZHOU Shengqiang(NCS Testing Technology Co.,Ltd.,Beijng 100081,China;Tangshan lron and Steel Group Co.,Ltd.,Tangshan 063000,China)

机构地区：[1]钢研纳克检测技术股份有限公司,北京100081 [2]唐山钢铁集团有限责任公司,河北唐山063000

出　　处：《冶金分析》2024年第12期72-77,共6页Metallurgical Analysis

摘　　要：锰元素可提高硼铁韧性,对锰的准确测定有助于生产更高质量的硼铁基合金材料。采用王水低温溶解后冒高氯酸烟消解样品,在硫磷酸介质中高碘酸钠将锰氧化至七价,于530 nm处采用分光光度法进行测定,建立了一种高碘酸钠氧化分光光度法测定硼铁中锰的方法。分别采用在硫磷酸存在下冒高氯酸烟、冒高氯酸烟后补加硫磷酸、酸溶回渣3种方式处理样品进行试验,结果表明,采用这3种方式溶样,硼铁样品中锰测定结果基本一致,硼铁标准物质/样品中锰测定结果与认定值/标准值相符,其中,冒高氯酸烟后补加硫磷酸法操作最为简单。方法的测定范围为0.050%~1.00%(质量分数,下同),校准曲线的线性相关系数为0.99999,表观摩尔吸光系数为2.3×10^(3) L·mol^(-1)·cm^(-1);方法中锰的检出限和定量限分别为0.004%和0.012%。方法用于测定硼铁标准物质和硼铁样品中锰的含量,测得结果的相对标准偏差(n=11)为0.25%~0.46%。按照实验方法测定3个硼铁标准物质/样品和2个硼铁样品中锰含量,标准物质/样品的测定值与认定值/标准值相符,实际样品测定值与酸溶回渣-电感耦合等离子体原子发射光谱法(ICP-AES)测定结果相吻合。Manganese could enhance the toughness of ferroboron.The accurate determination of manganese is helpful for the production of high-quality ferroboron alloy materials.The sample was dissolved in aqua regia at low temperature and digested by perchloric acid fuming.Manganese was oxidized to septivalent with sodium periodate in sulfuric acid-phosphoric acid medium and then determined at 530nm by spectrophotometry.Thus,a method for determination of manganese in ferroboron was established by periodate sodium oxidization spectrophotometry.The samples were treated by three methods,i.e.,perchloric acid fuming in presence of sulfuric acid and phosphoric acid,perchloric acid fuming followed by adding sulfuric acid-phosphoric acid,and slag dissolution with acid.The results showed that the determination results of manganese in ferroboron samples were basically consistent by the three methods above.The determination results of manganese in certified reference materials/reference material of ferroboron were consistent with the certified values/standard value.Wherein,the operation of perchloric acid fuming followed by adding sulfuric acid-phosphoric acid was the most simple.The determination range of method was 0.050%-1.00%(mass fraction,the same below).The correlation coefficient of calibration curve was 0.99999.The apparent molar absorptivity was 2.3×10^(3) L·mol^(-1)·cm^(-1).The limits of detection and limits of quantification for this method were 0.004%and 0.012%,respectively.The contents of manganese in certified reference material and actual samples of ferroboron were determined according to the proposed methods.The relative standard deviations(RSD,n=11)of determination results were between 0.25%and 0.46%.The contents of manganese in three certified reference materials/reference material and two actual samples of ferroboron were determined according to the proposed methods.The determination results of certified reference materials/reference material were consistent with the certified values/standard value,and the determi

关 键 词：酸溶回渣 硼铁 锰 高碘酸钠 分光光度法 

分 类 号：O657.32[理学—分析化学] TG115.3[理学—化学]