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High performance liquid chromatography detection method for 9,9-bis(4-amino-3-chlorphenyl)fluorene in polyimide film

A technology of polyimide film and high-performance liquid chromatography, which is applied in the field of chromatographic analysis, can solve the problems of unreported analysis methods, health hazards, aquatic organism toxicity, etc., achieve good symmetry, improve accuracy, and detect The effect of low limit and limit of quantitation

Active Publication Date: 2021-03-05
GUANGZHOU GRG METROLOGY & TEST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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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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  • High performance liquid chromatography detection method for 9,9-bis(4-amino-3-chlorphenyl)fluorene in polyimide film
  • High performance liquid chromatography detection method for 9,9-bis(4-amino-3-chlorphenyl)fluorene in polyimide film

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Embodiment 1

[0047] 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 acetonitrile to it, tighten the bottle 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.

[0048] 2. Set the column temperature of the HPLC to 40°C, the detection wavelength to 200nm, select water and acetonitrile as the mobile phase, and set the volume ratio of water to acetonitrile to 0.4:0.6, and the flow rate of the mobile phase to 1.5mL / min. Then take 10 μL of the sample to be tested and inject it for isocratic elution.

[0049] At the end of the analysis, a liquid chromatography peak was obtained. The retention time of 9,9-bis(4-amino-3-chlorophenyl)fluorene was 6.68min. According to accurate q...

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Abstract

The invention relates to the field of chromatographic analysis, particularly to a high performance liquid chromatography detection method for 9,9-bis(4amino 3chlorphenyl) fluorene in a film. Accordingto the method, water and acetonitrile are selected as mobile phases to efficiently analyze the content of 9,9-bis(4amino 3chlorphenyl) fluorene in an extraction liquid obtained through extraction pretreatment so as to determine the content of a to-be-detected substance in a film; the obtained chromatographic peak is sharp in peak pattern, good in symmetry, small in baseline fluctuation and free of drifting phenomenon; and the proper detector wavelength is selected, the obtained chromatographic peak signal intensity is proper, analysis and calculation are facilitated, errors are reduced, and the accuracy is improved. The analysis method disclosed by the invention is high in sensitivity and accuracy, low in detection limit and quantification limit, early in chromatographic peak appearance retention time, high in analysis efficiency and capable of quickly obtaining an analysis result.

Description

technical field [0001] The invention relates to the field of chromatographic analysis, in particular to a high performance liquid chromatography detection method for 9,9-bis(4-amino-3-chlorophenyl)fluorene in a polyimide film. Background technique [0002] 9,9-bis(4-amino-3-chlorophenyl)fluorene, as an important monomer raw material, is commonly used in the industry to synthesize high molecular polymers such as polyimide, polyamide and polyurethane, among which 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 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...

Claims

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Application Information

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