无自身标准样品GC-FID法测定标准物质中有机杂质含量

Determination of the Components of Organic Impurity in Reference Material Without the Self-RM by GC–FID

建立了一种标准物质中有机杂质的无自身标准样品准确定值的GC–FID方法。以与待测有机杂质结构相似的物质作为参考物质校准GC–FID响应信号,采用有效碳数法计算待测杂质的质量响应值Si,检测出样品中该有机杂质的准确含量。以癸二酸二正丁酯纯度标准物质为例,用该法对其中有机杂质总量进行定值,定值结果为0.29%,U=0.07%(k=2)。定值不确定度主要来源于Si和检测重复性。

The method was established for determining the components of organic impurity without the self-reference material （ RM ） by GC-FID. The signal of GC-FID was caliberated with the compound whose structure was similar with the organic impurity to be determined, and after the mass response（Si） of GC-FID of the impurity counted by ECN, the components of impurity in sample were determined. DBS purity RM as the example, the sum of organic impurities in DBS RM was （0.29 ± 0.07）% （k=2）. The major sources ofuncertainty of measurement were Si and the repeatability.