硫氰酸钾—1,10-二氮杂菲分光光度法测定镁锰铈合金中铁  

Determination of iron in magnesium-manganese-cerium alloy by potassium thiocyanate—1,10-phenanthroline spectrophotometry

作　　者：于亚辉[1,2] 张术杰[1,2] 张秀艳[1,2] 张慧珍[1,2] 朱悦然 

机构地区：[1]包头稀土研究院,内蒙古包头014030 [2]稀土冶金及功能材料国家工程研究中心,内蒙古包头014030

出　　处：《冶金分析》2016年第2期53-56,共4页Metallurgical Analysis

摘　　要：使用盐酸溶解样品，在微酸性介质中，铁与硫氰酸钾、1，1O-二氮杂菲形成紫红色三元络合物，用甲基异丁基酮萃取该络合物，于分光光度计波长520nlil处测量其吸光度，从校准曲线上查得铁含量，从而建立了使用分光光度法测定镁锰铈合金中铁的方法。试验的最佳条件为：水相酸度在3％～7％（V／V），硫氰酸钾溶液加入量为2mL，1，1O-二氮杂菲乙醇溶液加入量为2mL，显色时间为2min，甲基异丁基酮加入量为5mL，振荡时间为60S。结果表明，试液中铁质量在1～9μg范围内与吸光度呈线性，校准曲线的线性回归方程为．y=14．743z-O．207，相关系数r=O．9993；方法中铁的检出限为0.000037％（质量分数）。按照实验方法测定两个镁锰铈合金样品中铁，结果的相对标准偏差（RSD，n=11）分别为0．23％和0．18％，结果与电感耦合等离子体质谱法（ICP-MS）测定结果相吻合；加标回收率为97％～107％。The sample was dissolved with hydrochloric acid.The iron could react with potassium thiocyanate and 1,10-phenanthroline to form purple red complex in weakly acid medium.The complex was extracted with methyl isobutyl ketone.The absorbance was measured on spectrophotometer at 520 nm.The content of iron was obtained from the calibration curve.Consequently,the determination method of iron in magnesium-manganese-cerium alloy by spectrophotometry was established.The optimal conditions were as follows:the acidity of water phase was 3%-7%(V/V),the dosage of potassium thiocyanate solution was 2mL,the dosage of 1,10-phenanthroline ethanol solution was 2mL,the coloring time was 2min,the dosage of methyl isobutyl ketone was 5mL,and the vibration time was 60 s.The results indicated that the absorbance was linear to the mass concentration of iron in sample solution in range of 1-9μg.The linear regression equation of calibration curve was y=14.743 x-0.207 with correlation coefficient of r=0.999 3.The detection limit of method was 0.000 037%(mass fraction).The content of iron in two magnesium-manganesecerium alloy samples was determined according to the experimental method.The relative standard deviation(RSD,n=11)was 0.23%and 0.18%,respectively.The found results were consistent with those obtained by inductively coupled plasma mass spectrometry(ICP-MS).The recoveries were between 97%and 107%.

关 键 词：硫氰酸钾 1 1O-二氮杂菲 分光光度法 镁锰铈合金 铁 

分 类 号：TG115.33[金属学及工艺—物理冶金]