摘要:
采用智能样品消解仪并以硝酸、氢氟酸溶解样品,建立了电感耦合等离子体原子发射光谱仪(ICPOES)测定氟钽酸钾中钙、镁、铁、硅的分析方法。实验优化了仪器工作条件,选择Ca 396.847 nm、Mg 279.553nm、Fe 239.562 nm和Si 251.612 nm谱线作为分析线,采用基体匹配、扣除背景和标准加入法克服了基体效应和光谱干扰。结果表明,各元素的检出限为0.001 3-0.005 9μg/m L,加标回收率在94.4%-106.0%,相对标准偏差RSD ≤ 4.19%,钙、镁、铁测定结果与直流电弧原子发射光谱法测定结果吻合,硅测定结果与甲基绿-硅钼杂多酸分光光度法的一致,具有较好准确度和精密度。
Abstract:
The method for determining Ca,Mg,Fe and Si in potassium fluotantalate by inductively coupled plasma atomic emission spectrometry was established,with nitric acid and hydrofluoric acid to disolve the sample on ED16 digestion machine.The working parameters of instrument were optimized.Ca 396.847 nm,Mg 279.553 nm,Fe 239.562 nm and Si 251.612 nm were selected as analytical lines.Matrix matching method,background deduction and standard addition method were used to eliminate matrix effect and spectral interference.The results showed that the detection limit of each element was 0.001 3-0.005 9 μg/m L,that the standard addition recovery was 94.4% -106% and that the relative standard deviation was less than or equal to4.19%.The determination results of Ca,Mg and Fe agreed well with those obtained by direct current arc atomic enission spectrometry,and the determination results of Si were consistent with those from methyl green-molybdosiliscic acid spectrophotometry,indicating the method had good accuracy and precision.
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