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Method for detecting organochlorine residues in azo dye product

An azo dye and organochlorine technology, which is used in measurement devices, material separation, and analysis of materials, etc., can solve the problems of inability to batch operation, extract many impurities, and result interference, and achieve the protection of the injection port and chromatographic column, and purification effects. Good, easy-to-operate effects

Inactive Publication Date: 2016-11-23
HANGZHOU JIHUA JIANGDONG CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the chlorotoluene compound is highly toxic, potentially teratogenic and carcinogenic to the human body, and has stable chemical properties and a wide range of pollution. Therefore, many countries and organizations have strictly restricted the use of chlorinated toluene compounds as dyeing carriers.
[0005] At present, the detection method of organochlorine mainly adopts the determination of polychlorobenzene in GB / T 24164 dye products and the determination of chlorinated toluene in GB / T24167 dye products. The pretreatment uses n-hexane as the extraction solvent and direct ultrasonic extraction. This method extracts a lot of impurities, which will interfere with the results
The detection of organic chlorine also adopts the determination of DIN 54232 textiles based on the adhesive content of chlorobenzene and chlorotoluene, using dichloromethane as the extraction solvent, direct ultrasonic extraction, and then direct sample injection with 0.45 μm polytetrafluoroethylene membrane filtration. The injection port and chromatographic column of the gas phase mass spectrometer cause relatively large pollution and cannot be operated in batches

Method used

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  • Method for detecting organochlorine residues in azo dye product
  • Method for detecting organochlorine residues in azo dye product
  • Method for detecting organochlorine residues in azo dye product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Sample preparation:

[0045] Weigh 0.5g of Disperse Orange 73 azo dye product (accurate to 0.0001g) and place the dye sample to be tested in a conical flask with a ground stopper.

[0046] (2) Reductive cracking:

[0047] Add 25mL citrate buffer solution (0.06mol / L aqueous solution, pH=6) to the Erlenmeyer flask, seal the Erlenmeyer flask and preheat it at 60°C for 30min, then add 10.0mL sodium dithionite solution (200g / L ), shake vigorously and keep at 60°C for 30 minutes, and shake it from time to time to fully restore it. After reduction, take out the Erlenmeyer flask, cool it down to room temperature quickly with cold water, and adjust the pH to 8 with anhydrous sodium carbonate solution (200g / L). (3) Extraction:

[0048]In a separatory funnel, extract with chloroform three times, using 30 mL of chloroform each time, centrifuge for 5 minutes during extraction, then let stand to separate layers, take the lower layer and put it into a round bottom flask.

[00...

Embodiment 2

[0055] (1) Sample preparation:

[0056] Weigh 0.5g of the disperse yellow 82 azo dye product (accurate to 0.0001g) and place the dye sample to be tested in a conical flask with a ground stopper.

[0057] (2) Reductive cracking:

[0058] Add 25mL citrate buffer solution (0.08mol / L aqueous solution, pH=6) to the Erlenmeyer flask, seal the Erlenmeyer flask and preheat it at 50°C for 40min, then add 10.0mL sodium dithionite solution (200g / L ), shake vigorously and keep it at 50°C for 40 minutes, and shake it from time to time to fully restore it. After reduction, take out the Erlenmeyer flask, cool it down to room temperature quickly with cold water, and adjust the pH to 9 with anhydrous sodium carbonate solution (200g / L).

[0059] (3) Extraction:

[0060] In a separatory funnel, extract with n-hexane 3 times, using 30 mL of n-hexane each time, centrifuge for 5 minutes during extraction, then let stand to separate layers, take the lower layer and put it into a round bottom flas...

Embodiment 3

[0066] (1) Sample preparation:

[0067] Weigh 0.5g of the disperse black ECO azo dye product (accurate to 0.0001g) and place the dye sample to be tested in a conical flask with a ground stopper.

[0068] (2) Reductive cracking:

[0069] Add 25mL citrate buffer solution (0.1mol / L aqueous solution, pH=6) into the Erlenmeyer flask, seal the Erlenmeyer flask and preheat it at 80°C for 20min, then add 10.0mL sodium dithionite solution (200g / L ), shake vigorously and keep it at 80°C for 20 minutes, and shake it from time to time to fully restore it. After reduction, take out the Erlenmeyer flask, cool it down to room temperature quickly with cold water, and adjust the pH to 8 with anhydrous sodium carbonate solution (200g / L).

[0070] (3) Extraction:

[0071] In a separatory funnel, extract with dichloromethane 3 times, using 30 mL of dichloromethane each time, centrifuge for 5 minutes during extraction, then let stand to separate layers, take the lower layer and put it into a ro...

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Abstract

The invention belongs to the technical field of detecting organic chlorine residues in azo dye products. In order to solve the problems existing in the detection method of organic chlorine, the invention provides a method for detecting organic chlorine residues in azo dye products, aiming at the detection of organic chlorine residues The pretreatment process has been improved to improve the accuracy of detection of organochlorine residues and reduce the large pollution to the inlet and chromatographic column of the gas phase mass spectrometer.

Description

technical field [0001] The invention belongs to the technical field of detection of organochlorine residues in azo dye products, and relates to a method for detecting organochlorine residues in azo dye products using gas phase mass spectrometry technology. Background technique [0002] Dye products (including dyes and auxiliaries) are mostly used to produce textiles and leather products used in people's daily life, which are closely related to people's health. However, dye products may produce harmful substances in the process of production and use, including organic chlorine, and cause harm to the human body through contact with the human body. Therefore, effective control of the content of harmful substances in dye products has become a task for people An urgent task ahead. Organochlorines include polychlorobenzenes and chlorinated toluenes. [0003] Polychlorobenzenes are a class of organic pollutants with stable chemical properties, wide pollution range and high toxici...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88G01N2030/025G01N2030/062G01N2030/884
Inventor 邵辉周萍萍孙岩峰陈美芬
Owner HANGZHOU JIHUA JIANGDONG CHEMICAL CO LTD
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