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研究了土壤中钒的3种测定方法,ICP-AES、石墨炉原子吸收光谱法和X射线荧光光谱法。其中ICP-AES选用谱线V 311.1nm,用干扰系数法,干扰系数用多个土壤标样的标准值和测定值的最小二乘法来确定;石墨炉原子吸收光谱法用新、旧石墨管(热解涂层),加与不加基体改进剂(硝酸镁)分别进行测试;X射线荧光光谱法样品无需前处理、无需做校准曲线,测定前仪器用自带校正钢片单点法进行校正。通过测试结果的比较得出:ICP-AES测定土壤标样中的钒,精密度高,准确度好,适合土壤中钒的实验室分析;石墨炉原子吸收光谱法灵敏度过高(高一个数量级),信号稳定性较差,对高温元素钒的测定最好加硝酸镁机体改进剂消除基体干扰且每只石墨管分析次数不超过100次;X荧光光谱法较适合于野外监测或土壤样品无损检测,操作方便快速。
Three methods of determination of vanadium in soils, ICP-AES, graphite furnace atomic absorption spectrometry and X-ray fluorescence spectrometry were studied. The ICP-AES selected line V 311.1nm, with the interference coefficient method, the interference coefficient with multiple soil standard values and determination of the least squares method to determine; Graphite Furnace Atomic Absorption Spectrometry with new and old graphite tube Pyrolytic coating), respectively, with or without matrix modifier (magnesium nitrate) were tested; X-ray fluorescence spectrometry samples without pretreatment, without the need to do the calibration curve, before the measurement instrument with a single point of correction with steel correction . Through the comparison of test results: ICP-AES determination of vanadium in soil samples, high precision, good accuracy, suitable for laboratory analysis of vanadium in soil; Graphite Furnace Atomic Absorption Spectrometry sensitivity is too high (an order of magnitude higher) , The signal stability is poor, the determination of high temperature element vanadium is best to add magnesium nitrate body improver to eliminate matrix interference and analysis of each graphite tube does not exceed 100 times; X fluorescence spectrometry is more suitable for field monitoring or soil samples nondestructive testing Easy to operate.