Method for determining components of medium and low-temperature coal tar on basis of mixed internal standard method

A technology of low-temperature coal tar and internal standard method, which is applied in the direction of measuring devices, material separation, and analysis of materials, can solve the problems of weak quantitative analysis ability and achieve the effect of convenient qualitative analysis

Inactive Publication Date: 2019-01-04
榆林煤化工产业促进中心
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  • Application Information

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Problems solved by technology

[0005] In order to solve the existing technical problem of weak quantitative analysis ability of gas chromatography / mass spectrometry for medium and low temperature coal tar, the present invention provides a method for quantitative analysis of medium and low temperature coal tar components based on the mixed internal standard method. The method is A fast, simple and classified method for determining the relative content of each component of coal tar

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  • Method for determining components of medium and low-temperature coal tar on basis of mixed internal standard method
  • Method for determining components of medium and low-temperature coal tar on basis of mixed internal standard method

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Embodiment 1

[0035] Example 1: The method of the present invention for determining the components of medium and low temperature coal tar based on the mixed internal standard method is suitable for medium and low temperature coal tar, clear oil of medium and low temperature coal tar, and heavy oil of medium and low temperature coal tar.

[0036] Detect the components of medium and low temperature coal tar provided by Yulin Coal Chemical Industry Promotion Center (known to contain five components)

[0037] 1. Sample preparation

[0038] Accurately weigh 1,3,5-tri-tert-butylbenzene (purity greater than 99.5%, the same below) triphenylene, methyl nonadecanate, 2,4-dichlorobenzoic acid, 4-bromobenzaldehyde each 1mg Dissolved in acetone (analytical grade), 10mL volumetric flask to constant volume, configured into a mixed standard solution of 1mg / ml; accurately weigh 1mg of medium and low temperature coal tar (provided by Yulin Coal Chemical Industry Promotion Center), dissolve in 1ml of acetone,...

Embodiment 2

[0058] Example 2: Accuracy experiment, respectively take 0.01mg / ml, 0.5mg / ml, 1mg / ml, 2mg / ml, 5mg / ml, 10mg / ml, 20mg / ml mixed standard solution, and 1mg medium and low temperature coal tar The mixture dissolved in 1ml of acetone was measured by the same method as in Example 1, and the results showed that the linear range was 0.02mg / ml-10mg / ml. In this linear range, the accuracy of the method is high.

[0059] Control test: Take the acetone solution of methyl nonadecanoate with a concentration of 10mg / ml, and dilute it 10 times, 100 times, 1000 times, 10000 times respectively, that is, the final concentrations are 0.01mg / ml, 0.001mg / ml, 0.0001 mg / ml, 0.00001mg / ml, sample injection respectively, near the detection limit, that is, when S / N=3, the detection concentration is determined to be 0.00001mg / ml, indicating that the detection limit of this method is very low, and it is a gas phase 10-100 times that of chromatography.

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Abstract

The invention relates to a method for determining components of medium and low-temperature coal tar on the basis of a mixed internal standard method. The method comprises the steps as follows: 1) selection of internal standard substances: selecting multiple internal standard substances according to components of to-be-detected medium and low-temperature coal tar; 2) preparation of a standard liquid: preparing the internal standard substances selected in the step 1) into standard liquids, and mixing the liquids together to form a mixed standard liquid; 3) preparation of a to-be-determined sample liquid: preparing a sample liquid from a to-be-detected sample and adding the sample liquid to the mixed standard liquid; 4) analyzing and detecting a sample through gas chromatography-mass spectrometry; 5) data analysis and sample identification: performing calculation according to original chromatographic data and mass spectrometric data obtained through detection to obtain the content of eachcomponent in the medium and low-temperature coal tar. The method solves the technical problem about weak analysis capacity for the medium and low-temperature coal tar, and the method can determine the relative content of each component in coal tar quickly and simply in a classified manner.

Description

technical field [0001] The invention relates to a qualitative and quantitative analysis method for medium and low temperature coal tar, wherein the mixed internal standard method is used to determine its composition and content, in particular, it is a method for analyzing the composition and quantitative analysis of medium and low temperature coal tar by using different internal standard substances Methods. Background technique [0002] Coal tar is one of the products produced by coal pyrolysis. Coal pyrolysis is divided into low temperature pyrolysis (500-600°C), medium-temperature pyrolysis (700-800°C), high-temperature pyrolysis (950-1050°C), Under different pyrolysis conditions, the density of coal tar is usually between 0.95-1.10g. / cm3, with a special odor, and it is a black viscous liquid at room temperature. Coal tar is an organic mixture dominated by aromatic hydrocarbons. It contains more than 10,000 kinds of compounds, of which about 200 can be extracted. At prese...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72
CPCG01N30/02G01N30/72
Inventor 周秋成
Owner 榆林煤化工产业促进中心
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