甲醇中丙烯酸乙酯溶液标准物质制备

Preparation of reference material of ethyl acrylate solution in methanol

研制特征量值为1000μg/mL甲醇中丙烯酸乙酯溶液标准物质。分别利用气相色谱-质谱联用法、核磁共振波谱法和红外光谱法对丙烯酸乙酯标准品原料进行定性确认。采用质量平衡法对主成分含量进行量值核验,丙烯酸乙酯标准品纯度(质量分数)为99.842%,扩展不确定度为0.3%,量值在证书给出的不确定度范围内,因此采用证书标识量值作为原料标准值,证书中标识的不确定度作为原料不确定度。以丙烯酸乙酯标准品为原料,采用重量-容量法制备溶液标准物质,分别采用F检验和t检验对标准物质进行均匀性和稳定性检验,并对其定值结果的不确定度进行评定。结果表明,该标准物质均匀性和稳定性良好,有效期为12月,定值结果的相对扩展不确定度为2%(k=2),可用于环境样品中丙烯酸乙酯分析方法的确认和评价以及仪器校准与检测质量控制。

The reference material of ethyl acrylate solution in methanol with characteristic value of 1000μg/mL was prepared.The materials were qualitatively checked by gas chromatography-mass spectrometry,nuclear magnetic resonance spectroscopy and infrared spectroscopy,the structure and quantity of ethyl acrylate were confirmed by mass balance method,the purity of principal component was 99.842%with the extended uncertainty of 0.3%,which showed that the quantity value of standard product of ethyl acrylate was within the range of uncertainty,so the certificate identification quantity value might be as the standard value of raw materials,and the uncertainty identified in the certificate was the uncertainty of raw materials.Using ethyl acrylate standard material as raw material,the solution standard material was prepared by weight-capacity method,and its uniformity and stability were investigated by F test and t test,the test results showed that the uniformity and stability of the reference material were all satisfied,which supported that the validity period was 12 months The uncertainty of the fixed value was evaluated,and the relative extended uncertainty of the fixed value is 2%(k=2).It can be used for the confirmation and evaluation of analytical methods for ethyl acrylate in environmental samples,as well as for instrument calibration and detection quality control.