光谱学与光谱分析, 2011, 31 (1): 244, 网络出版: 2011-03-24  

悬浮液进样自吸扣背景石墨炉原子吸收光谱法测定高纯氧化铝中铜、 铁和钠含量

Direct Determination of Copper, Iron and Sodium in High-Purity Alumina by Slurry Introduction Furnace Atomic Absorption Spectrometry with Smith-Hieftje Background Correction
作者单位
1 中国科学院上海硅酸盐研究所, 上海200050
2 长春工业大学, 吉林 长春130012
3 复旦大学化学系, 上海200433
摘要
采用悬浮液-自吸扣背景石墨炉原子吸收法测定了高纯氧化铝中痕量元素铜、 铁、 钠含量。 实验对灰化温度、 原子化温度和自吸扣背景灯电流等石墨炉原子吸收工作条件等进行了优化, 确定了最佳测定条件。 样品测试采用标准水溶液进行校正, 方法准确性采用氧化铝AKP-30在高温高压和浓硫酸密闭条件下溶解样品进样分析测定结果与文献报道的其他测定方法结果进行了对比。 研究表明本方法简单, 结果可靠, 适用于氧化铝中痕量元素的快速测定。 校正曲线的线性相关性大于0.999 0, 方法对铜、 铁、 钠的检出限分别为0.66, 2.5, 0.13 ng·g-1 , 相对标准偏差小于5.2%。
Abstract
Direct determination of copper, iron and sodium in high-purity alumina was performed by slurry-furnace atomic absorption spectrometry with Smith-Hieftje background correction (S-H-GFAAS). Instrument conditions of GFAAS such as pyrolysis, atomization and hollow cathode lamp current by S-H background correction were optimized, and the optimal experimental conditions were selected. Calibration was performed using aqueous standards method for sample analysis. The accuracy of the proposed method was shown for the case of Al2O3 (AKP-30), and compared with those obtained by furnace atomic absorption spectrometry subsequent to decomposition by sulfuric acid in PTFE pressure vessels. The results were in agreement well with values found in the literature by different methods. It is a simple, convenient and accurate method and it is suitable for the rapid analysis of trace element in alumina. The linear regression coefficients of the calibration curves were better than 0.999 0. The detection limits were 0.66, 2.5 and 0.13 ng·g-1, respectively, with a relative standard deviation being not more than 5.2%.

卢桂萍, 汪正, 邱德仁, 邹慧君, 贺岩峰. 悬浮液进样自吸扣背景石墨炉原子吸收光谱法测定高纯氧化铝中铜、 铁和钠含量[J]. 光谱学与光谱分析, 2011, 31(1): 244. LU Gui-ping, WANG Zheng, QIU De-ren, ZOU Hui-jun, HE Yan-feng. Direct Determination of Copper, Iron and Sodium in High-Purity Alumina by Slurry Introduction Furnace Atomic Absorption Spectrometry with Smith-Hieftje Background Correction[J]. Spectroscopy and Spectral Analysis, 2011, 31(1): 244.

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