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Method for quickly measuring content of 3,4-benzopyrene in coal tar and coal pitch

A technology for rapid determination of coal tar, applied in the field of chemical detection and analysis, can solve problems such as incompatibility, and achieve the effects of less organic solvent consumption, fewer processing steps, and high accuracy

Inactive Publication Date: 2019-05-31
SINOSTEEL ANSHAN RES INST OF THERMO ENERGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] As we all know, there are many components in coal tar and coal tar pitch, and the domestic and foreign standards used to determine 3,4-benzopyrene so far (such as GB / T22509-2008 "Determination of 3,4-benzopyrene in animal and vegetable oils and fats Phase High Performance Liquid Chromatography", HJ478-2009 "Determination of Water Quality Polycyclic Aromatic Hydrocarbons by Liquid-Liquid Extraction and Solid Phase Extraction High Performance Liquid Chromatography", ZEK01-08 "Determination of 3,4-Benzene Content in Plastics", etc. ) in the components of the substances to be measured are relatively simple, so although its assay method is simple and easy, it is not suitable for the determination of 3,4-benzopyrene in coal tar products

Method used

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  • Method for quickly measuring content of 3,4-benzopyrene in coal tar and coal pitch
  • Method for quickly measuring content of 3,4-benzopyrene in coal tar and coal pitch
  • Method for quickly measuring content of 3,4-benzopyrene in coal tar and coal pitch

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Mix the low-temperature coal tar fully and evenly, accurately weigh it to 1.0000g and put it into the extraction column, use acetone as the extraction solvent, control the pressure of the pump in the extraction device to 4Mpa, and the extraction speed to 1mL / min, extract the 3,4 - Dilute the benzopyrene solution to 20ml.

[0076] The 3,4-benzopyrene standard solution of 0.1mg / L, 1mg / L, 10mg / L, 100mg / L, 1000mg / L, and the 3,4-benzopyrene solution after constant volume were analyzed by gas chromatography. The conditions are: the detector adopts a hydrogen flame ionization (FID) detector, and the chromatographic column adopts an SE-54 (30m×0.25mm×0.32μm) gas chromatographic column.

[0077] The temperature programming process is as follows: initial temperature 80°C, retention time 0min, heating rate 8°C / min, final temperature 260°C, retention time 5min; carrier gas is high-purity argon; pre-column pressure 100kpa; injection volume 1μL ; The inlet temperature is 260°C; the ...

Embodiment 2

[0080] Slowly heat the coal tar pitch with a softening point of 45°C to a liquid state in an oil bath and mix well, accurately weigh 0.5000g and put it into the extraction column, use acetone as the extraction solvent, the pressure of the pump in the extraction device is 3Mpa, the extraction speed 0.8mL / min, the extracted 3,4-benzopyrene solution was adjusted to 20ml.

[0081] The 10mg / L, 100mg / L, 1000mg / L, 10000mg / L 3,4-benzopyrene standard solution and the 3,4-benzopyrene solution after constant volume were analyzed by gas chromatography, and the chromatographic conditions were: detector A hydrogen flame ionization (FID) detector is used; the chromatographic column is SE-54 (50m×0.25mm×0.32μm) gas chromatographic column.

[0082] The temperature programming process is: initial temperature 100°C, retention time 2min, heating rate 5°C / min, final temperature 275°C, retention time 10min; carrier gas is high-purity argon; column pre-pressure is 120kpa; injection volume is 0.5 μL...

Embodiment 3

[0085] Crush the imported high-temperature asphalt with a softening point of 230°C, grind it in a mortar, and sieve it with a 200-mesh sieve until it is completely sieved; accurately weigh 0.5000g and put it into the extraction column, using cyclohexane as the extraction solvent , the pressure of the pump in the extraction device was 6Mpa, the extraction speed was 0.8mL / min, and the volume of the extracted 3,4-benzopyrene solution was adjusted to 20ml.

[0086] The 3,4-benzopyrene standard solution of 0.1mg / L, 1mg / L, 10mg / L, 100mg / L, 1000mg / L, and the 3,4-benzopyrene solution after constant volume were analyzed by gas chromatography. The conditions are: the detector adopts a hydrogen flame ionization (FID) detector; the chromatographic column adopts a SE-54 (50m×0.25mm×0.32μm) gas chromatographic column.

[0087] The temperature programming process is as follows: initial temperature 120°C, retention time 3min, heating rate 10°C / min, final temperature 320°C, retention time 15mi...

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Abstract

The invention relates to a method for quickly measuring the content of 3,4-benzopyrene in coal tar and coal pitch. The method comprises the steps of (1) preprocessing a sample to be measured, (2) extracting 3,4-benzopyrene in the sample to be measured by using a high-pressure extraction device, (3) preparing a standard solution and drawing a standard working curve, (4) measuring, and (5) calculating. In the present invention, after the sample to be measured is dissolved / milled, the 3,4-benzopyrene in the sample to be measured is extracted by the high-pressure extraction device, the content isquantitatively analyzed by using gas chromatography, and the method of the invention has the advantages of simple operation, rapidity, low detection cost and high accuracy.

Description

technical field [0001] The invention relates to the technical field of chemical detection and analysis, in particular to a method for quickly measuring the content of 3,4-benzopyrene in coal tar and coal tar pitch. Background technique [0002] In the process of coal tar processing, the residue after distillation to remove the liquid fraction is called coal tar pitch, which is the main component of coal tar, accounting for about 50% to 60% of the total; the main components of coal tar pitch are polycyclic, The composition of polycyclic aromatic hydrocarbons and their derivatives is very complex, and the difference in raw coal and processing technology will also lead to differences in composition. At room temperature, coal tar pitch is a black lump, shiny, smelly, flammable and toxic when molten. Coal tar pitch has poor climate stability and contains many harmful components, especially carcinogenic polycyclic aromatic hydrocarbons such as 3,4-benzopyrene, which are one of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 陈雪武全宇李强生杨桦孙刚屈滨刘书林臧娜张金柱于秀明
Owner SINOSTEEL ANSHAN RES INST OF THERMO ENERGY CO LTD
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