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Method for detecting benzo (a) pyrene in medium and high-temperature coal pitch

A detection method, the technology of coal tar pitch, applied in the field of environmental detection, can solve the problems of benzo[a]pyrene loss, miscellaneous peak interference, etc., and achieve the effect of improving repeatability, increasing the degree of chromatography, and reducing the degree of decomposition or reaction

Active Publication Date: 2015-01-28
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Zhang Qiumin et al. used ordinary glass chromatography columns to separate medium-temperature coal tar pitch, and used gas chromatography combined with the empirical formula of relative correction factor to calculate the content of benzo(a)pyrene in medium-temperature coal tar pitch to be 1.01%. The sampling process is easy to cause the loss of benzo[a]pyrene, and there are many interference peaks when qualitative judgment is made by retention time

Method used

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  • Method for detecting benzo (a) pyrene in medium and high-temperature coal pitch
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  • Method for detecting benzo (a) pyrene in medium and high-temperature coal pitch

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Effect test

Embodiment 1

[0034] A chromatography column device, which includes a column head 1 with a standard frosted port, a water inlet 3, a water outlet 5, a control valve 4, and a chromatography tube 7, which is characterized in that the top of the chromatography tube 7 is connected with a standard frosted port The column head 1, the lower end of the chromatographic tube 7 is equipped with a control valve 4, the bottom end of the chromatographic tube 7 is the discharge port 6, and the outer side of the chromatographic tube 7 between the column head 1 with the standard frosted port and the control valve 4 has a thermal insulation Pipe 2, water outlet 6 is arranged at the upper end of insulation pipe 2, and water inlet 3 is arranged at the lower end, and chromatographic tube 7 is a color-changing glass material.

[0035] 1. Working curve drawing: take benzo(a)pyrene standard mother liquor, and prepare benzo(a)pyrene with concentrations of 2.4mg / L, 3mg / L, 4.8mg / L, 6mg / L and 8mg / L respectively with cycl...

Embodiment 2

[0038] 1. The working curve is the working curve in Example 1.

[0039] 2. Sample treatment: Accurately weigh 2.404g of high-temperature coal tar pitch sample ground into 80-100 mesh, wrap it with filter paper and put it into a Soxhlet extractor, add organic solvent cyclohexane to the round bottom flask at the bottom of the extractor, and extract to After the reflux liquid is colorless, concentrate the extract at low temperature and reduced pressure to 1ml, and load the sample onto the photosensitive temperature-controlled glass chromatography column 1. The chromatography column 1 is filled with activated 80-100 mesh silica gel and neutral alumina Fill from the bottom to the neck of the column, the silica gel is placed in the upper layer, and the neutral alumina is placed in the lower layer. The column size is 90cm×2cm, and the neutral alumina content is 20wt%. The temperature of the column is controlled by a constant temperature circulating water pump during the chromatograph...

Embodiment 3

[0041] 1. The working curve is the working curve in Example 1.

[0042] 2. Sample treatment: Weigh 4.000g and grind it into 80-100 mesh medium-temperature coal tar pitch sample, wrap it with filter paper and put it into a Soxhlet extractor, add the organic solvent cyclohexane to the round bottom flask at the bottom of the extractor, and extract to reflux After the solution was colorless, the extract was concentrated at low temperature and reduced pressure to 1ml, and loaded onto the photosensitive temperature-controlled glass chromatography column 1. The chromatography column 1 was made of activated 80-100 mesh silica gel and neutral alumina. The bottom is filled to the neck of the column, the silica gel is placed in the upper layer, and the neutral alumina is placed in the lower layer. The column size is 100cm×2cm, and the neutral alumina content is 30wt%. The temperature of the column is controlled by a constant temperature circulating water pump during the chromatography pr...

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Abstract

The invention discloses a method for detecting benzo (a) pyrene in medium and high-temperature coal pitch. The method comprises the steps of firstly constructing a standard working curve for analyzing benzo (a) pyrene, performing Soxhlet extraction on a medium or high-temperature coal pitch sample, performing chromatography on concentrated liquid in a photosensitive temperature control type glass chromatographic column to obtain a sample, and analyzing the sample by a UV1601 ultraviolet visible spectrophotometer to obtain the content of benzo (a) pyrene in the medium and high-temperature coal pitch. The method has the advantages of accuracy and visibility.

Description

technical field [0001] The invention belongs to the field of environmental detection, in particular to a method for detecting benzo(a)pyrene in medium and high temperature coal tar pitch. Background technique [0002] Benzo(a)pyrene, abbreviated as BaP, is a kind of polycyclic aromatic hydrocarbons. It has the spectroscopic optical properties and light instability of PAH. It is also a kind of organic compound with strong carcinogenic effect. The representative of polycyclic aromatic hydrocarbons is listed as one of the key detection items of environmental pollution by most countries. Coal tar pitch is widely used in electrode materials and carbon products, and has been gradually used in paving roads and producing anti-corrosion coatings in recent years. The wide use of coal products has led to an increase in the production of medium and high temperature coal tar pitches year by year, and medium and high temperature coal tar pitches contain more polycyclic carcinogenic aroma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/33G01N1/28G01N1/40
Inventor 任真席云龙冯瑜郭建平李玉霞赵永红
Owner CHINA RES INST OF DAILY CHEM IND
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