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建立丙体六六六纯度标准物质的定值及不确定度评定方法,成功研制了丙体六六六纯度标准物质。原料成分采用气相色谱-质谱法(GC-MS)、红外光谱法(IR)和核磁共振法(1H和13CNMR)进行准确定性。通过均匀性及稳定性考察并检验合格后,采用两种不同原理和精度的方法,即质量平衡法和差示扫描量热法(DSC)进行有机纯度定值。原料中的水分和灰分杂质分别用卡尔费休法、马弗炉灰化燃烧法进行测定。研制的丙体六六六纯度标准物质纯度为99.5%。对定值结果进行不确定度评估,得到扩展相对不确定度为0.4%(k=2)。通过比对分析和第三方实验室量值核验,进一步确保定值结果的准确、可靠。该纯度标准物质已被国家质量监督检验检疫总局批准为国家二级有证标准物质[编号GBW(E)061724],可作为测量和量值溯源标准,为相关部门提供服务。
To establish the method for the determination of the standard value and the degree of uncertainty of C66 standard purity materials, the C66 standard purity material has been successfully developed. The raw materials were identified by gas chromatography-mass spectrometry (GC-MS), infrared spectroscopy (IR) and nuclear magnetic resonance (1H and 13CNMR). After the homogeneity and stability were inspected and tested, two methods with different principles and accuracies, that is, mass balance method and differential scanning calorimetry (DSC), were used to determine the organic purity. Raw materials, water and ash impurities were measured by Karl Fischer method, muffle furnace ash combustion method. The purity of the C66 hexagonal purity standard developed was 99.5%. The uncertainty of rating result is evaluated, and the relative uncertainty of expansion is 0.4% (k = 2). Through the comparative analysis and third-party laboratory verification of values, to further ensure the accuracy of the results of the valuation and reliability. The purity of the standard material has been approved by the State General Administration of Quality Supervision, Inspection and Quarantine as a national standard two certified materials [No. GBW (E) 061724], can be used as a traceability and measurement standards for the relevant departments to provide services.