Determination of trace boron in iron and steel by extraction separation-inductively coupled plasma atomic emission spectrometry
HU De-sheng1, ZHOU Xi-lin*2, LI Fen1, LIU Ai-fen3
1. Chongqing Technovocational College of Industry, Chongqing 401120, China; 2.Aluminum and Magnesium Center of Chongqing Academy of Metrology and Quality Inspection,Chongqing 401121,China;3. Zhongyuan Special Steel Co.,Ltd., Jiyuan 459008, China
Abstract：In order to reduce the lower limit of quantitation for determination of trace boron in iron and steel by inductively coupled plasma atomic emission spectrometry (ICP-AES) and meet the requirements for determination of boron in iron and steel with mass fraction less than 0.000 1%, a combined method by extraction separation and inductively coupled plasma atomic emission spectrometry was proposed for determination of trace boron in iron and steel. The sample was dissolved with hydrochloric acid-nitric acid mixed acid, sulfuric acid-phosphoric acid mixed acid and hydrofluoric acid in microwave digestion system. Then, the complex formed from boron and methylene blue was extracted with 1,2-dichloroethane at pH 0.4-0.8. The 1,2-dichloroethane organic phase was mixed with anhydrous ethanol for direct injection. The content of boron was determined under the selected instrumental parameters with B 249.678 nm as analytical line. The detection limit of method was 0.001 mg/L, which was 0.000 005% by converting it into the mass fraction of boron in iron and steel. The lower limit of quantitation was 0.000 05%. The proposed method was applied to the determination of trace boron in certified reference materials and synthetic samples of iron and steel. The results were consistent with the certified values or the theoretical values, and the relative standard deviation (RSD, n=10) was between 0.44% and 7.3%. The recoveries were 92%-100%.
胡德声,周西林,李芬,刘爱芬. 萃取分离-电感耦合等离子体原子发射光谱法测定钢铁中痕量硼[J]. 冶金分析, 2015, 35(6): 35-39.
HU De-sheng, ZHOU Xi-lin, LI Fen, LIU Ai-fen. Determination of trace boron in iron and steel by extraction separation-inductively coupled plasma atomic emission spectrometry. , 2015, 35(6): 35-39.
