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谁知道液态NMR测定腐殖酸的方法

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发表于 2008-5-27 12:05:47 | 显示全部楼层 |阅读模式

1、我用二甲基亚砜溶解后测定,根本无峰,可能是溶解性太少。

有资料说用2.7ml的重水+0.3ml5N的NaOH溶解300mgHA,离心过滤后,62.8MHZ,sweepwidth:20-30KHZ条件下测定。不知可行不?氢氧化钠对测定没干扰吗,是不是也要用氘代氢氧化钠?

2、河南附近哪里有做固态核磁的?如何收费?实在不行我想做个固态核磁测HA。

谁能帮个忙吗?我的毕业论文就需要这个数据,否则无法毕业了。

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EMAIL:astdy@126.com

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发表于 2008-5-27 15:15:26 | 显示全部楼层

 

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看来你查文献还不充分,NMR测定腐殖酸方面的文章还不少,中文的可查燃料化学学报,距现在大约有20多年。

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发表于 2008-5-27 15:21:55 | 显示全部楼层
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发表于 2008-5-27 15:23:06 | 显示全部楼层

Differences in Humic Acid Characteristics as Determined by Carbon-13 Nuclear Magnetic Resonance, Scanning Electron Microscopy, and Infrared Analysis

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An investigation was conducted on the usefulness of 13C nuclear magnetic resonance (NMR) spectroscopy in the characterization of humic acids (HA) isolated from selected soils. Soil samples for extraction of HA were collected from Indonesia, USA, and Argentina. The analyses were conducted by liquid 13C NMR, scanning electron microscopy (SEM), infrared (IR), and chemical analysis. The NMR spectra indicated that all HA samples had in common aliphatic, polysaccharide, aromatic, and carboxyl groups. However, the NMR signals for the chemical groups were different in intensities, producing a distinctive spectrum for each HA studied. The NMR analysis demonstrated that HA from the tropical region soils were highly aliphatic in nature, with a combined carbohydrate and polysaccharide C content of 59.5 to 67.6%. On the other hand, HA from the seven temperate region soils contained more COOH and aromatic C. The highest aromatic C concentration together with the strongest NMR signals for aromaticity were exhibited by HAs of the Mascotte (Ultic Haplaquod) and the Argentina (suborder unknown) soil. The differences in NMR spectra were accompanied by differences in SEM micrographs and IR spectra. A significant correlation was noted between NMR and especially IR spectra. Humic acid samples with strong NMR signals for aromatic C exhibited IR spectra with strong bands at 1240 cm–1, whereas HA with weak NMR signals for aliphatic C had IR spectra with weak bands at 2980 to 2900 cm–1. Therefore, IR spectroscopy can also be an important tool in the characterization of humic matter when used in conjunction with 13C NMR.

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' f3 n' Z2 B% m) i; H5 ]: e http://soil.scijournals.org/cgi/content/abstract/52/1/125
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发表于 2008-5-28 02:16:36 | 显示全部楼层
 据我所知Celan老师几十年前就做过。
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