Method for using HS-GC (headspace gas chromatography) external standard method to measure residual acrylic acid in acrylic polymer

An acrylic acid polymer and acrylic acid technology, applied in the field of analytical chemistry, can solve problems such as human and environmental hazards, impact of test results, and inability to quantitatively test, achieving good repeatability, high accuracy, and simple and easy methods

Inactive Publication Date: 2018-10-16
ZIBO LURUI FINE CHEM CO LTD
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, there will be a certain amount of acrylic acid residues in acrylic acid polymers. If the residual amount is not well controlled, it will cause certain harm to humans and the environment. According to literature reports, the current detection methods for acrylic acid residues in acrylic acid polymers mainly include chemical methods and ions. Chromatography, but these methods have large human errors, and the products and their by-products will affect the test results, so they cannot be quickly and effectively quantitatively tested

Method used

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  • Method for using HS-GC (headspace gas chromatography) external standard method to measure residual acrylic acid in acrylic polymer
  • Method for using HS-GC (headspace gas chromatography) external standard method to measure residual acrylic acid in acrylic polymer
  • Method for using HS-GC (headspace gas chromatography) external standard method to measure residual acrylic acid in acrylic polymer

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Embodiment 1

[0040] 1. Instrument Preparation

[0041] Adopt Agilent 7890B gas chromatograph, 7697A headspace sampler for headspace injection, equilibrate at 60°C for 15min; the chromatographic column is DB-WAX (or a chromatographic column with equivalent polarity), the column length is 30m, and the inner diameter of the column is 320μm. The initial column temperature is 130°C, keep it for 2min, then raise the temperature to 190°C at a rate of 20°C / min, keep it for 12min, the carrier gas flow rate is 1ml / min; 4:1, injection volume 1μl; hydrogen flame detector, the detection temperature is 260°C, the hydrogen flow rate is 40ml / min, and the air flow rate is 300ml / min.

[0042] 2. Drawing of standard curve

[0043]Preparation of acrylic acid standard solution: Accurately weigh 50.0mg of acrylic acid standard in a beaker, dilute with distilled water, transfer to a 500ml volumetric flask, dilute to the mark with distilled water, and prepare 100mg / L stock solution VI; accurately pipette 10.00ml...

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Abstract

The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for using an HS-GC (headspace gas chromatography) external standard method to measure the residual acrylic acid in a acrylic polymer. A headspace gas chromatographic instrument is adopted to conduct detection and external standard method quantitative analysis, wherein the gas chromatographicinstrument is an Agilent gas chromatography 7890B, the gas chromatography analysis conditions are that chromatographic columns are chromatographic columns with DB-WAX or polarity being equivalent, thelength of the columns is 30 m, the inner diameter of the columns is 320 microns, the initial column temperature is 130 DEG C, the temperature is maintained for 2 minutes, then the temperature is risen to be 190 DEG C at the ratio of 20 DEG C / min, the temperature is maintained for 12 minutes, and the flow rate of carrier gas is 1 ml / min. The method is high in precision, good in reproducibility, high in accuracy and good in repeatability, can achieve direct detection of samples, avoids influences of raw materials and by-products to the product peak, shortens the analysis time, is simple and practical, and convenient and reliable.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for measuring residual acrylic acid in acrylic acid polymers by using an HS-GC external standard method. Background technique [0002] Acrylic acid is a colorless clear liquid with a pungent odor. It is the simplest unsaturated carboxylic acid, consisting of a vinyl group and a carboxyl group. It is miscible with water, alcohol, ether and chloroform, flammable, highly corrosive and moderately toxic. On October 27, 2017, the list of carcinogens released by the International Agency for Research on Cancer of the World Health Organization was initially compiled for reference, and acrylic acid was included in the list of three types of carcinogens. [0003] Acrylic acid is an important raw material for organic synthesis. It is a vinyl monomer with a very fast polymerization rate. As an important chemical raw material, acrylic acid is widely used in s...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 谢瑞丽王艾德曹春晓段红英
Owner ZIBO LURUI FINE CHEM CO LTD
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