标准加入-原子吸收光谱法测定钢渣中的铁
Determination of Iron in Steel Slag by Standard Addition- Atomic Absorption Spectrometry
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摘要: 样品经硝酸-氢氟酸混合酸溶解后,用标准加入-原子吸收光谱法测定钢渣中的铁。实验探讨了钢渣的均匀性等干扰因素对结果的影响,并提出基体高、浓度高的样品稀释倍数过高误差越大,建议采用如旋转燃烧头、选择次灵敏线等降低仪器灵敏度的方法或采用标准加入法。并将标准加入法与X射线荧光光谱、电感耦合等离子体发射光谱、原子吸收光谱直接测定法进行比较,铁的实验结果分别为51.6%、54.2%、46.2%、16.6%,相对标准偏差分别为2.8%、5.3%、2.0%、2.3%。标准加入-原子吸收光谱法在测定基体高、浓度高的样品时是准确可靠的。方法可用于环境类实验室用水剂标准溶液进行钢渣类样品中元素的分析。Abstract: Standard addition-atomic absorption spectrometry (AAS) was used to determine Fe content in steel slag samples after sample digestion with HNO3-HF mixed acid. The homogeneity of slag and other interfering factors on the determination results were studied. It was found that high dilution factors caused by high matrix and high Fe content of the samples lead to a large error. Standard addition-AAS method could avoid the large detection error. And use of AAS instrument with rotating burner and selection of secondary sensitive spectral lines were also recommended to reduce the detection error by reducing the detection sensitivity of Fe. The method has been applied to the determination of Fe in a steel slag sample and the result was compared with those from XRF, ICP-AES and AAS (without standard addition). The results show that standard addition-AAS can provide accurate and reliable results and is superior to the other methods for the samples with high matrix and high Fe content.