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作 者:刘含笑 刘凯 王祥德 薛婷婷 郭飞 吕东芹 王巍 LIU Hanxiao;LIU Kai;WANG Xiangde;XUE Tingting;GUO Fei;LYU Dongqin;WANG Wei(China United Test&Evaluation(Qingdao)Co.,Ltd.,Qingdao 266000,China;China United Test&Certification Co.,Ltd.,Beijing 101400,China)
机构地区:[1]国合通用(青岛)测试评价有限公司,青岛266000 [2]国合通用测试评价认证股份公司,北京101400
出 处:《分析试验室》2024年第6期858-863,共6页Chinese Journal of Analysis Laboratory
基 金:中国有研科技集团有限公司青年基金(G12620213129047)资助。
摘 要:建立了铁中间合金中铁含量测定的自动电位滴定法,考察了溶样体系、还原剂类型及用量、滴定环境和共存离子干扰等因素的影响。结果表明,硝酸、过氧化氢和氢氟酸对测定结果有较大的影响,在滴定前应去除;磷酸会导致三氯化钛水解,影响测定结果,应避免引入;共存的Cr, Co和Cu等金属离子对测定结果没有影响。在1%~99%含量范围内,方法的相对标准偏差(RSD)为0.08%~0.26%。使用硅铁、锰铁和钕铁硼等有证标准样品验证了方法的准确度。该方法解决了可视滴定方法存在的滴定终点颜色干扰问题,减少了磷酸等试剂的用量,规避了分离干扰离子的复杂操作,简化了实验步骤,同时提高了铁含量测定的精密度。The automatic potentiometric titration method was established for the determination of iron content in intermediate ferroalloys.The factors affecting the determination results of iron content,including sample dissolving system,the type and amount of reducing agent,the titration environment and the interference of coexisting ions,were studied.The results showed that nitric acid,hydrofluoric acid,and hydrogen peroxide had great influence on the determination results,which should be removed before titration.Phosphoric acid promoted the hydrolysis of titanium trichloride and affected the determination results.Coexisting metal ions such as Cr,Co and Cu did not affect the determination results.Within the content range of 1%~99%,the relative standard deviations(RSDs)of the method were 0.08%-0.26%,and the accuracy of the method was verified with certified reference materials such as ferrosilicon,ferromanganese and neodymium iron boron.This method solves the problem of color interference of titration end point in visual titration method,reduces the amount of hazardous chemicals such as phosphoric acid,avoids complex operations that interfering ion separation and improves the precision of iron content determination.
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