ICP-OES法测定高镍合金铸铁中锰铬镍铜  

Determination of manganese chromium nickel copper in high nickel alloy cast iron by ICP-OES

作　　者：蹇福婷 王霜叶 刘鹏 刘小琴 谢成真 Jian Futing;Wang Shuangye;Liu Peng;Liu Xiaoqin;Xie Chengzhen(Chongqing Chongke Physical and Chemical Test&Metrology Center Co.,Ltd.,Chongqing 400020,China)

机构地区：[1]重庆市重科理化计量中心有限公司,重庆400020

出　　处：《分析仪器》2024年第4期54-58,共5页Analytical Instrumentation

摘　　要：高镍合金铸铁已广泛用于制造耐高温的反应器、换热器等设备和构件以及高强度、高韧性的机械零件,先行国家标准方法对铸铁中高含量元素的测定都有局限性。本实验建立了电感耦合等离子体原子发射光谱法(ICPOES)同时测定高镍铸铁中锰、铬、镍、铜元素的方法。试验探讨了不同溶解方法对分析结果的影响,优选出最佳溶样方法:先加(1+1)硝酸溶解样品至剧烈反应后滴加浓盐酸和氢氟酸,最后加入高氯酸加热至冒烟,定容后测定。将该法应用于实际样品测定,测定结果锰的质量分数在0.05%~4%,镍的质量分数在0.05%~40%,铬的质量分数在0.05%~5%,铜的质量分数在0.05%~10%范围内。在选定的仪器工作条件下,各元素的校准曲线线性相关系数均大于0.999,方法中各元素的回收率为98.0%~105.6%,实际样品分析相对标准偏差RSD≤2.00%(n=11),将本方法应用于高镍铸铁标准物质中锰、铬、镍、铜元素的测定,结果与证书标称值吻合。High nickel alloy cast iron has been widely used in the manufacture of high-temperature resistant reactors,heat exchangers and other equipment and components,as well as high-strength,high-toughness mechanical parts.There are limitations in national standards for determining the high content of elements in cast iron.The influence of different dissolution methods on the results was discussed,It is preferred to add(1+1) nitric acid to dissolve the sample and then add concentrated hydrochloric acid and hydrofluoric acid by drops after intense reaction,Finally,add perchloric acid for smoke generation,After constant volume,simultaneous determination of manganese,chromium,nickel and copper in high nickel cast iron by inductively coupled plasma atomic emission spectrometry(ICP-OES).The mass fraction of manganese is 0.05%-4%,the mass fraction of nickel is 0.05%-40%,the mass fraction of chromium is 0.05%-5%,and the mass fraction of copper is 0.05%-10%,under the selected instrument operating conditions,The linear correlation coefficients of calibration curves of all elements were greater than 0.999,The recovery ratio is between 98.0%-105.6%,relative standard deviation RSD≤2.00%,use the standard material of high nickel cast iron for verification,the result was in agreement with the confirmed value.

关 键 词：ICP-OES 高镍合金铸铁 回收率 

分 类 号：TG143.7[一般工业技术—材料科学与工程] O657.31[金属学及工艺—金属材料]