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电感耦合等离子体原子发射光谱法测定萤石中硫 被引量:10

Determination of sulphur in fluorite by inductively coupled plasma atomic emission spectrometry
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摘要 试样经硝酸和氢氟酸低温溶解,加入高氯酸冒烟,盐酸溶解盐类,用电感耦合等离子体原子发射光谱法测定了萤石中硫的含量。研究了基体效应、共存元素间干扰及校正。结果表明,基体氟化钙和共存元素A1、Fe、Ba、Mn、P对测定无影响。在选定条件下,硫的含量在0.003%~6.5%范围内与发射强度线性关系良好,相关系数大于0.9990。方法应用于萤石标准样品YSBl479-02和实际样品分析,结果与认定值或燃烧碘量法吻合,11次平行测定的相对标准偏差(RSD)不大于1.5%,回收率在96%~104%之间。 The sample was dissolved with nitric acid and hydrofluoric acid at low temperature. After perchloric acid was added for fuming, the salts were dissolved with hydrochloric acid. Then, the con- tent of sulfur in fluorite was determined by inductively coupled plasma atomic emission spectrometry. The matrix effect, interference and correction among coexisting elements were investigated. The re- sults showed that, the matrix calcium fluoride and coexisting elements (such as A1, Fe, Ba, Mn and P) had no influence on the determination. Under the selected conditions, the content of sulfur in the range of 0. 001%-6. 5% showed good linearity to the emission intensity with correlation coefficient higher than 0. 999 0. The proposed method was applied to the determination of certified reference ma- terials YSB14794-02 and actual sample of fluorite. The results were consistent with the certified val- ues or those obtained by combustion iodometry. The relative standard deviation (RSD, n= 11) was not more than 1.5%, and the recoveries were between 96% and 104%.
作者 高亮
出处 《冶金分析》 CAS CSCD 北大核心 2013年第9期49-52,共4页 Metallurgical Analysis
关键词 电感耦合等离子体原子发射光谱法 萤石 inductively coupled plasma atomic emission spectrometry fluorite sulfur
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