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关于辉光放电发射光谱分析校准的探讨 温州市工业科学研究院 张加民  蔡延奔
校准的定义 所谓校准就是仪器在一定的工作条件下,对一系列已知成分的标准样品进行检测,测得元素特征谱线强度与其在样品中的浓度之间的对应关系,经过回归计算得到校准工作曲线,然后利用这条校准工作曲线,根据对待测样品所测得的元素谱线强度来确定其在样品中的浓度
辉光放电发射光谱分析校准主要包括以下三个过程:   建立校准工作曲线 ; 校准工作曲线的标准化也称为再校准( recalibration )  最小校准 (minicalibration)
建立校准工作曲线:   一、建立校准工作曲线  1 、选择标准样品
标准样品选择原则:   2 、 标准样品的浓度覆盖范围要能满足实际待检测样品可能达到的范围要求   3 、 每个元素的数据点最少需六个以上   1 、选用有证标准物质,最好 CRM ;
需要增加标准样品数量 :   2 、 当元素含量覆盖范围很宽时; 3 、 当校准工作曲线线性不好时(如二次曲线或更高级次);  1 、 当标准样品中含有较高的干扰谱线比较丰富的元素时(如 Co 、 Mo 、 W 等);
RF 光源的辉光放电发射光谱仪主要有以下几个重要的光源参数:   氩气压力 RF 源设置功率 匹配器的两个初始值 Module 和 Phase 阳极直径 氩气吹扫时间 预积分时间 积分时间等
光学系统工作条件   ,[object Object],[object Object],[object Object]
环境条件: ,[object Object],[object Object],[object Object],[object Object],[object Object]
选择分析模式:   ,[object Object],[object Object],[object Object],[object Object],[object Object]
选择分析模式:   ,[object Object]
选择分析模式:   ,[object Object]
选择分析模式:   ,[object Object]
元素谱线的选择 ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
标准样品的表面处理 ,[object Object],[object Object]
标准工作曲线的修正 ,[object Object],[object Object],[object Object],[object Object],[object Object]
二、校准工作曲线的标准化 ( recalibration) ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
校准工作曲线再校准原理:
再校准修正关系式 :          ( 5 )
工作曲线再校准的优点 : ,[object Object],[object Object]
再校准工作曲线的缺点   : ,[object Object],[object Object]
再校准工作曲线的缺点   : ,[object Object]
再校准标样的选择 : ,[object Object],[object Object],[object Object]
最小校准 (mini-calibration): ,[object Object]
最小校准 (mini-calibration): ,[object Object],[object Object],[object Object],[object Object]
结 束 语 ,[object Object],[object Object]
[object Object]

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