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磷钼蓝光度法测定冶金硅中痕量磷含量

Determination of Phosphorus in Metallurgical Grade Silicon by Phosphorus & Molybdenum Absorption Spectra

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【作者】 李京伟郭占成唐惠庆孙士瞳林银河余锦涛

【Author】 Li Jingwei,Guo Zhancheng~*,Tang Huiqing,Sun Shitong,Lin Yinhe,Yu Jintao(State Key Laboratory of Advanced Metallurgy,University of Science and Technology Beijing,Beijing 100083,China)

【机构】 北京科技大学钢铁冶金新技术国家重点实验室

【摘要】 本文选用盐酸羟胺和抗坏血酸作为还原剂,使磷酸根与钼酸铵生成磷钼蓝杂多酸,利用磷钼蓝光度法测定冶金硅中磷的含量。结果表明810 nm波长时所得吸光度最大,生成的络合物10 h内显色稳定,即为工作波长。磷标准曲线是:Y=0.00252+0.01645X(X单位为μg),R=0.99995。磷含量在0~50.00μg范围内,服从朗伯-比耳定律,摩尔吸光系数为2.12×104L·moL-1·cm-1,检出限是0.005μg/ml。由标准加入实验可知,当待测样品加入量为5 ml时,相对误差为0.09%,表明硅中其它杂质元素对磷检测的干扰可以忽略。由准确度结果证明该方法可行,准确度高。

【Abstract】 Phosphorus & molybdenum absorption spectra which selected hydroxylamine hydrochloride and ascorbic acid as reducing agents,was proposed to determine the content of phosphorus in metallurgical grade silicon.At determination wavelength of 810 nm,linear relationship between absorbance and mass of phosphorus was obtained in the range of 0~50.00μg as shown by the linear regression equation Y=0.00252+0.01645X (X represents phosphorus mass,μg),R=0.99995.Molar absorp- tion coefficient was 2.12×104 L·moL-1·cm-1.Detection limit was 0.015μg/ml.Using Standard Addition Method in phosphorus & molybdenum absorption spectra,△R between experimental result and horizontal intercept value of phosphorus in MG-Si was 0.09%when the tested sample volume was 5 ml.The result indicated that the interference of other impurity elements could be ignored for phosphorus detection.Accuracy result verified that this method was feasible.

【基金】 国家自然科学基金(51174187)
  • 【会议录名称】 2012年全国冶金物理化学学术会议专辑(下册)
  • 【会议名称】2012年全国冶金物理化学学术会议
  • 【会议时间】2012-08-01
  • 【会议地点】中国云南昆明
  • 【分类号】O657.3;TF03
  • 【主办单位】国家自然科学基金委员会工程与材料科学部、中国有色金属学会冶金物理化学学术委员会、中国金属学会冶金过程物理化学学术委员会、中国稀土学会
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