1.Baotou Research Institute of Rare Earths,Baotou 014030,China; 2.National Engineering Research Centre of Rare Earth Metallurgy and Function Materials,Baotou 014030,China
Abstract: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 2 mL, the dosage of 1,10-phenanthroline ethanol solution was 2 mL, the coloring time was 2 min, the dosage of methyl isobutyl ketone was 5 mL, 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 1-9 μg. 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-manganese-cerium 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%.
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