氮化硼化学成分标准物质研制

Preparation of chemical composition reference materials for boron nitride

研制3种氮化硼化学成分标准物质。以硼酸和三聚氰胺为原料,采用湿化学法合成固体前驱物,分别在空气和氮气气氛下高温热处理,制得质量分数为95%~99%的氮化硼候选物。随机抽取12瓶分装好的样品进行均匀性检验,组内和组间无显著性系统差异,样品均匀性良好。采用直线拟合法进行短期稳定性和长期稳定性检验,拟合直线斜率均小于临界值,样品稳定性良好。通过8家实验室采用两种不同原理的方法进行协作定值,统计评定出标准值和不确定度,定值组分包括总氮、总硼、氧化硼、铁、钙、钠,其中总氮质量分数为53.8%~55.9%,总硼质量分数为41.8%~43.7%,氧化硼质量分数为0.105%~2.37%,基本覆盖了常规氮化硼的纯度范围。该系列标准物质能够满足氮化硼相关产品的测量质量控制和测试需求。

Three chemical composition reference materials for boron nitride were developed.The solid precursor was synthesized by wet chemical method,using boric acid and melamine as raw materials.The boron nitride candidates with purity of 95%-99%were prepared by high-temperature heat treatment of the previous drive materials in air and nitrogen atmosphere respectively.The uniformity test and the short-term/long-term stability test showed that the measured values were all less than critical values,indicating good uniformity and stability of the samples.Eight laboratories participated in the collaborative certified value research using two different principles,and the determination results and corresponding uncertainties were obtained.The calibration components were total nitrogen,total boron,boron oxide,iron,calcium and sodium.The mass fraction of total nitrogen ranged from 53.8%to 55.9%,the mass fraction of total boron ranged from 41.8%to 43.7%,and the mass fraction of boron oxide ranged from 0.105%to 2.37%,basically covering the purity range of conventional boron nitride.This series of reference materials can meet the measurement quality control and testing requirements of boron nitride products.