Preparation of aquatic fulvic acid standard sample and preparation of those guarantee data

水生黄腐酸标准样品的制备及保证数据的准备

• 批准号: 13460033
• 负责人: YONEBAYASHI Koyo
• 金额: $ 6.27万
• 依托单位: Kyoto Prefectural University
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (B)
• 财政年份: 2001
• 资助国家: 日本
• 起止时间: 2001 至 2002
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-13460033/
• 关键词: aquatic fulvic acid; aquatic standard sample; DAX-8 resin; lake Biwa lake water; ^<13>C-NMR; ^1H-NMR; HP-SEC; pyrolysis mass spetrometry; ^1H-NMR

"Humic substances" which exist in natural water are high molecular compounds chemically synthesized from degradation products of the plankton remains and organisms. Recently, the environmental pollution by hazardous organic compounds has been indicated. In aqueous environment, these noxious organic substances adsorb, distribute and are solubilized to the humic substances. It is important to examine the interaction between noxious organic substance and humic substances in order to study the dynamics of noxious organic substance in the environment. However, it is known that chemical property of humic substances in aqueous environment completely differ from all purchased humic substances, since it was extracted from the peat. As a representative aqueous environmental sample of Japan, Lake Biwa lake water was chosen, and aquatic fulvic acid standard sample was prepared at Kita-Komatsu lake shore station of the environmental standard point of Lake Biwa. The automatic concentration system fo … More r aquatic humic substances which consisted of giant column (φ50 cm, 20 Kg of DAX-8 resin), 3 kind connection filter columns (10,1.0,0.45μm), acid mixing column, and diaphragm pump was constructed. The pH of lake water was prepared under 2 with the automatic injection of hydrochloric acid into the filtered lake water. The humic substances were adsorbed on DAX-8 resin column by the elution of the lake water. We dealt with the lake water of about 300 tons in the period from middle October to early November 2001 and in the period from middle April to early May 2002. DAX8 resin which adsorbed the humic substances was brought back in the laboratory, the alkaline elution was done, the humic substance was recovered, and the fulvic acid was separated from humic acid as pH 1.2. By repeating and dissolving process which adsorbed to the small column again, the fulvic acid was refined, and Lake Biwa fulvic acid standard sample (2001 Autumn sample about 18 g, 2002 Spring sample : about 15 g) was obtained. Elemental analysis, functional group analysis (carboxyl group, phenolic group, carbonyl group, total hydroxyl group), ^<13>C-NMR and ^1H-NMR measurements, acid-base titration, molecular weight distribution measurement (HP-SEC), thermal decomposition mass spectrometric analysis, fluorescence analysis were carried out on the aquatic standard samples. Less

天然水体中的“腐殖物质”是由浮游生物和生物体的降解产物经化学反应合成的高分子化合物。近年来，有害有机物对环境的污染已引起人们的关注。在水环境中，这些有毒有机物吸附、分布并溶解于腐殖物质中。研究有毒有机物与腐殖物质之间的相互作用对研究有毒有机物在环境中的动态变化具有重要意义。然而，众所周知，由于腐殖物质是从泥炭中提取的，因此在水环境中的腐殖物质的化学性质与所有购买的腐殖物质完全不同。选择日本有代表性的水体环境样品-日本琵琶湖湖水，在日本琵琶湖环境标准点的北小松湖海岸站制备水中富里酸标准样品。自动浓缩系统 ...更多信息 建立了一个由巨型柱（φ50 cm，DAX-8树脂20 Kg）、3种连通过滤柱（10、1.0、0.45 μm）、酸混柱和隔膜泵组成的分离水中腐殖物质的实验装置。通过向过滤后的湖水中自动注入盐酸，将湖水的pH调节到2以下。用DAX-8树脂柱对湖水中的腐殖物质进行吸附。我们在2001年10月中旬至11月初和2002年4月中旬至5月初处理了约300吨湖水。将吸附腐殖酸的DAX 8树脂带回实验室，进行碱洗脱，回收腐殖酸，在pH 1.2时将富里酸与腐殖酸分离。通过重复溶解过程，使其再次吸附到小柱上，对富里酸进行精制，得到了琵琶湖富里酸标准样品（2001年秋样约18 g，2002年春样约15 g）。对水产品标准样品进行了元素分析、官能团分析（羧基、酚基、羰基、总羟基）、~ <13>1H-NMR和~ 1C-NMR测定、酸碱滴定、分子量分布测定（HP-SEC）、热分解质谱分析、荧光分析。少