罗丹明B纯度标准物质的研制

以商购罗丹明B为原料,进行重结晶提纯,制备罗丹明B纯度标准物质。采用红外光谱(IR)、高分辨质谱和核磁共振谱(NMR)进行定性分析。样品分装400瓶后,依据国家《一级标准物质研制技术规范》,采用液相色谱-二极管阵列法对随机抽取的15瓶样品进行均匀性检验,经F检验表明,在95%的置信区间范围内,样品均匀性良好。在室温下,经过30个月稳定性考察,结果表明样品稳定性良好。标准物质经国内8家具有分析资质的实验室进行协同定值,定值结果为99.0%,扩展不确定度为1.0%(k=2)。该标准物质达到了国家标准物质的技术要求,可用于有关罗丹明B的分析方法校正和质量控制。

Development of Rhodamine B Certiifed Reference Material

Rhodamine B certified reference material was developed. Raw material was recrystallized for preparation of Rhodamine B by business purchased. The structure of RhodamineB certified reference material was comfirmed by infrared spectroscopy (IR),high resolution mass spectral and nuclear magnetic resonance (NMR). The homogeneity testing were evaluated by liquid chromatography with diode array detector detector (LC–DAD). According to analysis procedure of homogeneity,15 bottles of sample were randomly taken from 400 bottles,and the results were validated byF–test statistical method. The test results indicated that the homogeneity was good in the 95% confidence interval. The stability inspection was carried at room temperature for 30 months. The results indicated that the stability was good. A cooperative certification was conducted by eight qualified laboratories. The certified purity value of the reference material of Rhodamine B was 99.0% with relative expaned uncertainty of 1.0%(k=2). The reference material can meet the technical requirement of the certified reference material, it can be used for the method validation and quality control regarding Rhodamine B.