镍释放量标准物质的研制  

Development of Nickel Release Certified Reference Material

作　　者：许菲菲 姜士磊 柴明青 

机构地区：[1]义乌出入境检验检疫局,浙江义乌322000

出　　处：《化学分析计量》2016年第3期8-11,共4页Chemical Analysis And Meterage

基　　金：国家质检总局课题(2015IK298)

摘　　要：研制了镍释放量标准样品。以铜粉、锌粉、镍粉为原料,通过熔炼炉熔炼及模具加工制备镍释放量标准物质,采用能量色散荧光光谱法(EDX)确认镍含量。样品分装成200份,采用电感耦合等离子体光谱法(ICP)进行均匀性、稳定性检验和定值分析。从样品中随机抽取15份进行均匀性检验,经F检验表明在95%的置信区间范围内样品均匀性良好;在常温条件下,经过12个月长期试验稳定性考察,统计值t均小于临界值2.571,结果表明样品稳定性良好。镍释放量定值结果为1.121μg/(cm^2·week)。对镍释放量定值结果进行了不确定度评估,扩展不确定度为0.300μg/(cm^2·week)(k=1.96)。该镍释放量标准物质符合检测需要,可用于合金产品镍释放量检测的方法校正和质量控制。Nickel release certified reference material was developed. Nickel release certified reference material was made by melting copper powder,zinc powder and nickel powder with melting furnace. The nickel content was confirmed by energy dispersive fluorescence spectroscopy(EDX). Nickel release certified reference material was divided into 200 pieces. The homogeneity and stability testing and quantitative analysis method were evaluated by inductively coupled plasma spectrometry(ICP). According to analysis procedure of homogeneity,15 pieces of sample were randomly taken from 200 pieces,the sample homogeneity of inspection validated by F–test statistical methods within the 95% confidence interval was good. The stability inspection was carried on the long-term(12 months),and the results showed that statistics t values were less than critical value 2.571,the results indicated that the period for nickel release of storage was 12 months at room temperature. The certified value of the reference material of nickel release was 1.121 μg/(cm^2· week) with the relative expanded uncertainty of 0.300 μg/(cm^2· week)(k=1.96). The reference material can conform to the technical requirement of the certified reference material, it is suitable for the method validation and quality control regarding nickel release.

关 键 词：镍释放量标准物质 均匀性 稳定性 不确定度 

分 类 号：O656[理学—分析化学]