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Chromatographic Separation of Water-Soluble Organic Compounds and Determination of Benzene Ring Numbers in Components

A water-soluble organic matter and determination method technology, applied in the field of environmental analytical chemistry, can solve the problems of poor separation effect, inability to effectively determine the content of different components, long separation time, etc., and achieve the separation required by simple operation and basically consistent separation results , The effect of high sample demand

Active Publication Date: 2019-03-19
CHINESE RES ACAD OF ENVIRONMENTAL SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Existing studies have focused on the fact that there are many hydrophobic organic substances in the environment, and the concentration range of organic solvent methanol or acetonitrile in the elution phase is 20% to 90%. Compared with hydrophobic organic pollutants in the environment, water-soluble organic substances are more hydrophilic. Strong, in the chromatographic separation process using the above ratio of organic solvents, the separation effect is not good
It is very important to determine the proportion of the organic phase in the chromatographic separation eluent. If the proportion of the organic phase in the eluent is too high, the peak time of different water-soluble organic components is close, and the separation effect is poor; if the proportion of the organic phase in the eluent is too low, the separation Long time and high column pressure reduce the service life of the separation column, so it is very important to reasonably determine the proportion of the organic phase in the eluent; in addition to the proportion of the eluent, the injection volume and sample concentration are also very important. Too little, the chromatographic detector cannot detect, the injection is too high, exceeds the detector range, and cannot effectively determine the content of different components

Method used

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  • Chromatographic Separation of Water-Soluble Organic Compounds and Determination of Benzene Ring Numbers in Components
  • Chromatographic Separation of Water-Soluble Organic Compounds and Determination of Benzene Ring Numbers in Components
  • Chromatographic Separation of Water-Soluble Organic Compounds and Determination of Benzene Ring Numbers in Components

Examples

Experimental program
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Embodiment 1

[0042]Sample preparation: extract and prepare humic acid from the compost sample, dilute the humic acid sample with pH=8.0 phosphate buffer, adjust its DOC to 20 mg / L for sample injection.

[0043] Sample injection: Inject 20 μL of sample into the chromatographic system using an autosampler.

[0044] Sample elution: In Agilent's chromatographic separation system, acetonitrile-ammonium acetate mixed solution was used for elution, the injection volume ratio of acetonitrile in the fixed elution solution was 5%, and the elution time was 5 minutes.

[0045] Sample detection and humic acid composition analysis: adjust the excitation wavelength of the fluorescence detector to 240nm, and the emission wavelength to 300-500nm, and detect the separated components. The result is as figure 1 shown. It can be seen from the figure that composted humic acid is separated into 5 components with different emission wavelengths through the chromatographic column. The 5 components not only have s...

Embodiment 2

[0049] Sample preparation: Prepare a mixed sample of water-soluble organic matter and adjust its DOC to 80mg / L.

[0050] Sample injection: inject the prepared water-soluble organic solution into the chromatographic system with an injection volume of 40 μL.

[0051] Sample elution: In Agilent's chromatographic separation system, acetonitrile-ammonium acetate mixture was used for elution, the injection volume ratio of acetonitrile in the elution solution was 5%, and the elution time was 12 minutes. The sample is detected by a fluorescence detector with an excitation of 230nm and an emission wavelength of 280-520nm, and the results are as follows: image 3 shown. It can be seen from the figure that 11 components of water-soluble organic matter are separated by the C18 column, and the fluorescence signals of 11 components are relatively strong, and the separation is good. From left to right, the maximum emission fluorescence peak of component 1 is located at greater than 450nm, ...

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Abstract

The invention provides a chromatographic separation and benzene ring number determination method for water-soluble organic matters. The method comprises the steps of preparing a water-soluble organic solution, adding the prepared water-soluble organic solution into a chromatographic column, subjecting the water-soluble organic solution to concentration / gradient elution through a fixed organic phase, detecting components obtained through the elution process by means of a fluorescence detector, and determining the number of benzene ring functional groups in each of different components according to the position of a maximum fluorescence peak in the emission spectrum of the separated components. The chromatographic separation and benzene ring number determination method has the advantages of small demanded sample quantity, good separation effect and accurate determination of benzene ring functional groups.

Description

technical field [0001] The invention belongs to the field of environmental analysis chemistry, and in particular relates to the chromatographic separation of water-soluble organic matter and a method for determining the number of benzene rings in the separated components. Background technique [0002] Water-soluble organic matter is a general term for a large class of organic mixtures, which contain various organic components. In order to accurately characterize its composition, researchers used various grouping techniques to separate and analyze its composition on the basis of reducing the complexity of organic matter composition. Currently commonly used grouping techniques include resin method, chromatography and grouping by molecular weight. Chromatographic grouping has become a common method for the separation and characterization of organic matter due to its advantages such as low sample requirement, fast separation speed, and online monitoring. [0003] In chromatogr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/74
CPCG01N30/02G01N30/74
Inventor 何小松席北斗高如泰虞敏达张慧李丹檀文炳黄彩红
Owner CHINESE RES ACAD OF ENVIRONMENTAL SCI
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