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生物质化学工程 ›› 2010, Vol. 44 ›› Issue (4): 8-12.

• 论文 • 上一篇    下一篇

2,3,4-三甲氧基苯甲醛标准样品的制备和定值研究

张亮亮1,2, 陈笳鸿1, 汪咏梅1,2, 吴冬梅1,2, 徐曼1, 吴在嵩1   

  1. 1. 中国林业科学研究院, 林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局, 林产化学工程重点开放性实验室;江苏省生物质能源与材料重点实验室, 江苏 南京 210042;2. 中国林业科学研究院, 林业新技术研究所, 北京 100091
  • 收稿日期:2010-04-14 修回日期:1900-01-01 出版日期:2010-07-30 发布日期:2010-07-30
  • 通讯作者: 陈笳鸿,研究员,主要从事植物资源化学利用研究;E-mail:chen-jiahong@163.com。

Study on Preparation and Certification of Reference Substance of 2,3,4-Trimethoxybenzaldehyde

ZHANG Liang-liang1,2, CHEN Jia-hong1, WANG Yong-mei1,2, WU Dong-mei1,2, XU Man1, WU Zai-song1   

  1. 1. Institute of Chemical Industry of Forest Products, CAF;National Engineering Lab. for Biomass Chemical Utilization;Key and Open Lab. on Forest Chemical Engineering, SFA;Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China;2. Institute of New Technology of Forestry, CAF, Beijing 100091, China
  • Received:2010-04-14 Revised:1900-01-01 Online:2010-07-30 Published:2010-07-30

摘要: 研究了2,3,4-三甲氧基苯甲醛标准样品的制备、均匀性和稳定性及其定值试验。标准样品采用工业级2,3,4-三甲氧基苯甲醛产品经亚硫酸氢钠加成反应和乙醇重结晶相结合的方法制备。测得熔点为37.8~39.6℃,经红外光谱和核磁共振分析结构与2,3,4-三甲氧基苯甲醛相吻合。标准样品的含量测定采用气相色谱面积归一化法,并通过了均匀性检验和稳定性检验(6个月)。经定值检测,2,3,4-三甲氧基苯甲醛标准样品的含量值为99.48%,不确定度(99%置信率)为0.07%。

关键词: 4-三甲氧基苯甲醛, 标准样品, 定值

Abstract: Preparation, homogeneity, stability and certification of reference substance of 2,3,4-trimethoxybenzaldehyde were studied. The reference substance of 2,3,4-trimethoxybenzaldehyde was prepared from an industrial grade product of 2,3,4-trimethoxybenzaldehyde by NaHSO3 addition reaction followed by re-crystallization in ethanol. The melting point of product was 37.8-39.6℃. The structure was conformed by IR and NMR spectra. The content of 2,3,4-trimethoxybenzaldehyde in reference substance was measured by gas chromatographic area normalization. The reference substance of 2,3,4-trimethoxybenzaldehyde passed the test of homogeneity, and it was stable during 6 months at least. Through valuation test, 2,3,4-trimethoxybenzaldehyde content of the reference substance was 99.48% with uncertainty of 0.07% and confidence coefficient of 99%.

Key words: 4-trimethoxybenzaldehyde, standard sample, certification

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