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Gas chromatography detection method of 9,9-bis(4-amino-3-chlorophenyl)fluorene in polyimide film

A technology of polyimide film and detection method, which is applied in the field of chromatographic analysis, can solve problems such as health hazards, toxicity of aquatic organisms, and unreported analysis methods, and achieve improved accuracy, low detection limit and quantification limit, good symmetry

Active Publication Date: 2022-04-12
GUANGZHOU GRG METROLOGY & TEST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, polyimide materials have excellent performance in industry, but the residual 9,9-bis(4-amino-3-chlorophenyl)fluorene will bring harm to people's health. Studies have confirmed that this compound is harmful to skin It has a strong irritant effect on eyes and eyes, and has persistent toxicity to aquatic organisms. Therefore, a suitable analysis method should be established to determine the content of 9,9-bis(4-amino-3-chlorophenyl)fluorene in the product. It is necessary to measure
However, most of the current research on 9,9-bis(4-amino-3-chlorophenyl)fluorene is about the synthesis and application of it and related derivatives, while the residual 9,9-bis( The analysis method of 4-amino-3-chlorophenyl) fluorene content has not been reported

Method used

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  • Gas chromatography detection method of 9,9-bis(4-amino-3-chlorophenyl)fluorene in polyimide film
  • Gas chromatography detection method of 9,9-bis(4-amino-3-chlorophenyl)fluorene in polyimide film
  • Gas chromatography detection method of 9,9-bis(4-amino-3-chlorophenyl)fluorene in polyimide film

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Experimental program
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Effect test

Embodiment 1

[0045] 1. Take the polyimide film sample, cut it into pieces until the sample size is less than or equal to 2mm×2mm, accurately weigh 1g sample (accurate to 0.1mg) and put it into the sample bottle, add 10mL of toluene to it, and tighten the bottle cap Put the sample bottle into an ultrasonic cleaner, and ultrasonicate at 60°C for 70min. Take 1 mL of the cooled extract and filter it through a 0.22 μm filter membrane to obtain the sample to be tested.

[0046] 2. Set the inlet temperature of the gas chromatograph to 290°C, the column flow rate to 1.5mL / min, and set the temperature rise program as follows: set the initial temperature to 180°C, and then raise the temperature to 320°C at a heating rate of 35°C / min And keep it for 6min.

[0047] 3. Use the mass spectrometer as the detector, and set the working conditions of the mass spectrometer as follows: select the electron bombardment ion source, ion source temperature: 230°C, quadrupole temperature: 150°C, scan range m / z: 100...

Embodiment 2

[0050] 1. Take the film sample, cut it into pieces until the size of the sample is less than or equal to 2mm×2mm, accurately weigh 1g of the sample (accurate to 0.1mg) and put it into the sample bottle, add 10mL of toluene to it, tighten the cap and put the sample bottle Put it into an ultrasonic cleaner, and ultrasonicate at 60°C for 70min. Take 1 mL of the cooled extract and filter it through a 0.22 μm filter membrane to obtain the sample to be tested.

[0051] 2. Set the inlet temperature of the gas chromatograph to 280°C, the column flow rate to 1.4mL / min, and set the temperature rise program as follows: set the initial temperature to 150°C, and then raise the temperature to 320°C at a heating rate of 25°C / min And keep it for 8 minutes.

[0052] 3. Use the mass spectrometer as the detector, and set the working conditions of the mass spectrometer as follows: select the electron bombardment ion source, ion source temperature: 230°C, quadrupole temperature: 150°C, scan range...

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Abstract

The invention relates to the field of chromatographic analysis, and in particular to a gas chromatography detection method for 9,9-bis(4-amino-3-chlorophenyl)fluorene in polyimide films. The present invention performs a programmed temperature rise on the gas chromatograph, sets the initial temperature to 120°C to 180°C, and then raises the temperature to 310°C to 330°C at a heating rate of 25°C / min to 35°C / min and maintains it for 6min to 8min, which can effectively The content of 9,9-bis(4-amino-3-chlorophenyl)fluorene in the extract obtained after extraction pre-treatment was analyzed to determine the content of 9,9-bis(4-amino-3-chlorophenyl) in the film. phenyl)fluorene content. The obtained chromatographic peaks have sharp peak shapes, good symmetry, small baseline fluctuations, and no drift. The analysis method of the present invention has high sensitivity and accuracy, low detection limit and quantitation limit, early retention time of chromatographic peaks, high analysis efficiency, and can quickly obtain analysis results.

Description

Technical field [0001] The invention relates to the field of chromatographic analysis, and in particular to a gas chromatography detection method for 9,9-bis(4-amino-3-chlorophenyl)fluorene in polyimide films. Background technique [0002] 9,9-bis(4-amino-3-chlorophenyl)fluorene, as an important monomer raw material, is commonly used in industry to synthesize polymers such as polyimide, polyamide, and polyurethane. Among them, poly Imide is the most common. Polyimide has excellent thermal stability, chemical solvent resistance, good mechanical properties and electrical properties. It is mainly used in aerospace, microelectronics, machinery, automobiles, etc. in the form of films and molded parts. modern industrial field. However, polyimide materials have excellent industrial properties, but the residual 9,9-bis(4-amino-3-chlorophenyl)fluorene in them can cause harm to people's health. Studies have confirmed that this compound is harmful to the skin. It has a strong irritat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 李支薇钟琳张兰兰杨文宇严洪连
Owner GUANGZHOU GRG METROLOGY & TEST CO LTD
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