X射线衍射K值法测定氧化铁皮中游离α-SiO2的含量
防城港出入境检验检疫局, 广西 防城港 538001 |
Determination of Free α-SiO2 Content in Mill Scale by X-ray Diffraction K Value Method
Fangchenggang Entry-Exit Inspection and Quarantine Bureau, Fangchenggang 538001, China |
摘要：目前通常采用焦磷酸法和X射线衍射法测定游离α-SiO2的含量, 其中焦磷酸法不能消除氧化铁皮中FeO、Fe3O4和Fe2O3等焦磷酸难溶物质的影响, 不适合用于测定氧化铁皮中的游离α-SiO2。本文建立了采用X射线衍射K值法测定氧化铁皮中游离α-SiO2含量的方法。以α-Al2O3作为参考物质, 以α-SiO2(101) 衍射峰和α-Al2O3(012) 衍射峰作为测量谱峰, 将α-SiO2和α-Al2O3(质量比1:1) 混合均匀制备成测量K值的试样, 获得K值为7.86, 应用此值分析已知游离α-SiO2含量的氧化铁皮样品, 游离α-SiO2含量的测定值与实际值相符。该方法的测定范围为游离α-SiO2含量≥0.50%, 测量范围宽, 且方便快速, 能够满足进口氧化铁皮检验监管的工作需求。
Determination of Free α-SiO2 Content in Mill Scale by X-ray Diffraction K Value Method
ABSTRACT At present, free α-SiO2 content is often determined by the pyrophosphate method and X-ray Diffraction (XRD) method. However, insoluble materials including FeO, Fe3O4 and Fe2O3 in mill scale cannot be decomposed by pyrophosphate, and thus the pyrophosphate method is not suitable for the determination of free α-SiO2 content in mill scale. A method for detecting free α-SiO2 content in mill scale through X-ray diffraction K value method has been developed. α-Al2O3 was used as the reference material. Diffraction peaks of crystal face (101) for α-SiO2 and crystal face (012) for α-Al2O3 were used for measured diffraction peaks. Samples for detecting K value were prepared by mixing α-SiO2 with α-Al2O3 at a mass ratio of 1:1. The acquired K value is 7.86. The measured K value has been applied to the determination of mill scale samples with known free α-SiO2 content, and the analytical results of free α-SiO2 content are in good agreement with practical values. Detection range of this method is that free α-SiO2 are equal or greater than 0.5%. This method is convenient and rapid, and has a wide detection range and can meet the need of imported mill scale inspection and supervision work.
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