水的饱和辛醇溶水分标准物质的研制.PDFVIP

生 物 工 程 学 报 Chin J Biotech 2011, March 25; 27(3): 510−515 journals.im.ac.cn Chinese Journal of Biotechnology ISSN 1000-3061 cjb@im.ac.cn ©2011 CJB, All rights reserved. 生物能源系统分析与方法 水的饱和辛醇溶液水分标准物质的研制 王海峰，马康，张伟，李占元 中国计量科学研究院，北京 100013 摘 要: 生物燃料的国家标准规定了产品的技术指标和相应的检测方法。水的饱和辛醇溶液的水分标准物质，用于生 物燃料水分测量时仪器的校准和方法的验证，能够保障测量结果的准确可靠和等效一致。该标准物质采用卡尔· 费休库 仑法、卡尔· 费休容量法和定量核磁共振等三种不同原理的方法定值。通过方法研究和改进，实现了库仑法和容量法的 一致；通过引入新的核磁共振方法，提高了结果的准确性。最终标准物质的水分量值为4.76 ％，扩展不确定度为0.09 ％。 关键词: 水分，标准物质，不确定度，卡尔· 费休库仑法，卡尔· 费休·容量法，核磁共振 The water content reference material of water saturated octanol Haifeng Wang, Kang Ma, Wei Zhang, and Zhanyuan Li National Institute of Metrology , Beijing 100013, China Abstract: The national standards of biofuels specify the technique specification and analytical methods. A water content certified reference material based on the water saturated octanol was developed in order to satisfy the needs of the instrument calibration and the methods validation, assure the accuracy and consistency of results in water content measurements of biofuels. Three analytical methods based on different theories were employed to certify the water content of the reference material, including Karl Fischer coulometric titration, Karl Fischer volumetric titration and quantitative nuclear magnetic resonance. The consistency of coulometric and volumetric titration was achieved through the improvement of methods. The accuracy of the certified result was improved by the introduction of the new method of quantitative nuclear magnetic resonance. Finally, the certified value of reference material is 4.76% with an expanded uncertainty of 0.09%. Keywords: water content, reference materials, uncertainty, Karl Fischer coulometry, Karl Fischer v