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Detection method of content of halohydrocarbon organic substances in shoe-making treatment agent

A detection method, a halogenated hydrocarbon technology, is applied in the field of detection of halogenated hydrocarbon organic content in shoe-making treatment agents, which can solve problems such as unclear and unnoticed toxicity of shoe treatment agents, and achieve strong specificity and high efficiency. The effect of high precision and sensitivity

Inactive Publication Date: 2015-01-21
GUANGDONG DONGGUAN QUALITY SUPERVISION TESTING CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the past, people mainly focused on the detection of toxic and harmful substances in shoe materials and shoe adhesives, but did not pay attention to the detection of toxicity of shoe treatment agents. Even most people did not know that there is such a process in the shoe industry, so there is Not related to the detection method of the halogenated hydrocarbon content in the treatment agent for shoemaking

Method used

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  • Detection method of content of halohydrocarbon organic substances in shoe-making treatment agent
  • Detection method of content of halohydrocarbon organic substances in shoe-making treatment agent
  • Detection method of content of halohydrocarbon organic substances in shoe-making treatment agent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Extraction of halogenated hydrocarbons in the treatment agent

[0031] Weigh 1.0g (accurate to 0.1mg) of the treatment agent sample to be tested, add 10mL, 5mL and 5mL of ethyl acetate to the sample in turn for extraction, then mix evenly on a vortex mixer, ultrasonically extract for 30min and centrifuge, Finally, the three extracts were mixed and diluted with ethyl acetate to 25.0 mL for analysis.

[0032] 2) Gas chromatography-mass spectrometry analysis

[0033] Gas chromatography-mass spectrometry was used for analysis, and the chromatographic column was a 5% phenyl / 95% methyl polysiloxane capillary column with a specification of 30m×0.25mm×0.25μm; the temperature of the inlet was 230°C; The bombardment ionization source is 70eV, the ion source temperature is 250°C, the quadrupole temperature is 150°C, and the GC-MS interface temperature is 280°C; the column oven adopts a temperature program, and the initial temperature is 30°C for 12 minutes, and then the temper...

Embodiment 2

[0048] 1) Extraction of halogenated hydrocarbons in the treatment agent

[0049] Weigh 2.0g of the treatment agent sample to be tested (accurate to 0.1mg), add 10mL, 5mL and 5mL of methanol to the sample in turn for extraction, mix uniformly on a vortex mixer for 10min, ultrasonically extract for 30min and centrifuge, and then three The extracts were mixed, diluted with ethyl acetate to 25.0 mL, and the supernatant was taken for analysis.

[0050] 2) Gas chromatography-mass spectrometry analysis

[0051] Using gas chromatography-mass spectrometry, the chromatographic column is a 5% phenyl / 95% methyl polysiloxane capillary column (30m×0.25mm×0.25μm); the temperature of the injection port is 230°C; the electron bombardment ionization source is 70eV , the ion source temperature is 250°C, the quadrupole temperature is 150°C, and the GC-MS interface temperature is 280°C; the column oven adopts a temperature program, and the initial temperature is 30°C for 12 minutes, and then the ...

Embodiment 3

[0060] 1) Extraction of halogenated hydrocarbons in the treatment agent

[0061] Weigh 5g of the sample to be tested (accurate to 0.001mg), add 15mL, 10mL, 5mL, 5mL and 5mL of acetone to extract five times, mix evenly on a vortex mixer for 20min, ultrasonically extract for 30min and centrifuge, and then The five extracts were mixed, diluted with acetone to 50.0mL, and then analyzed.

[0062] 2) Gas chromatography-mass spectrometry analysis

[0063] Using gas chromatography-mass spectrometry, the chromatographic column is a 5% phenyl / 95% methyl polysiloxane capillary column (30m×0.25mm×0.25μm); the temperature of the injection port is 230°C; the electron bombardment ionization source is 70eV , the ion source temperature is 250°C, the quadrupole temperature is 150°C, and the GC-MS interface temperature is 280°C; the column oven adopts a temperature program, and the initial temperature is 30°C for 12 minutes, and then the temperature is raised to 150°C at 10°C / min for 5 minutes,...

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Abstract

The invention provides a detection method of content of halohydrocarbon organic substances in a shoe-making treatment agent. The method includes following steps: (1) weighing a to-be-detected sample and employing reagents, including ethyl acetate, methanol, acetone or isopropyl-ketone as an extraction liquid; (2) performing analysis through a gas chromatography-mass spectrometer; (3) preparing a mass-concentration-known standard mixed solution including dichloromethane, 1,1-dichloroethane, 1,2-dichloroethane, trichloromethane, 1,1,1-trichloroethane, 1,1,2-trichloroethane and carbon tetrachloride, performing gas chromatographic-mass spectrometer analysis, and drawing a standard curve according to a detected peak area of the standard mixed solution and corresponding concentrations; and (4) determining categories of the halohydrocarbon organic substances existing in the to-be-detected sample through a mass spectrum, and finding out or calculating the corresponding concentration on the standard curve according the peak area of the compounds through an external standard method. The detection method can enable halohydrocarbon to be separated from other components well and has a high accuracy.

Description

technical field [0001] The invention relates to a method for detecting the content of halogenated hydrocarbon organic matter (dichloromethane, dichloroethane, chloroform, trichloroethane, carbon tetrachloride) in a treatment agent for shoemaking. Background technique [0002] As an important organic solvent and product intermediate, organic halogenated hydrocarbons are widely used in many industries and can be used to extinguish fires. Toxic organic substances are often carcinogenic, teratogenic, and mutagenic substances. Chlorinated hydrocarbons mainly include dichloromethane, dichloroethane, chloroform, trichloroethane, and carbon tetrachloride. Dichloromethane is a colorless liquid with strong dissolving power and a large amount of application, among which the consumption of cleaning agent and chemical industry accounts for 20% of its total consumption. Dichloroethane includes 1,1-dichloroethane and 1,2-dichloroethane. It is a colorless or light yellow transparent highly...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 石葆莹王玉峰赖毅东欧海龙覃毅磊赵历
Owner GUANGDONG DONGGUAN QUALITY SUPERVISION TESTING CENT