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Method for determining content of metal elements in polyvinylidene fluoride resin

A polyvinylidene fluoride resin and metal element content technology, which is applied in the field of fluoropolymer analysis and detection, can solve the problems of inability to eliminate organic interference, affect the accuracy of analysis results, high cost and maintenance costs, and achieve instrument cost and maintenance costs Low, stable and reliable results, low detection limit effect

Inactive Publication Date: 2020-12-29
JUHUA GROUP TECH CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This sample injection method effectively avoids the complicated sample pretreatment process. The disadvantage of this method is that the content of metal elements in the reagent blank of this analysis method is relatively high, and the external standard method cannot eliminate the interference of organic substances in the matrix, which affects the analysis results. The accuracy of the solution; the concentration of the prepared solution is too high, the viscosity is high, the instrument is difficult to absorb liquid, and it is easy to cause analysis errors; the MS detector is easily affected by the argon plasma generated by the ionization of the carrier gas argon and some substances with the same molecular weight in the matrix. Interference causes analysis errors; coupled with the high cost and maintenance costs of ICP-MS instruments, it is not easy to popularize

Method used

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  • Method for determining content of metal elements in polyvinylidene fluoride resin
  • Method for determining content of metal elements in polyvinylidene fluoride resin
  • Method for determining content of metal elements in polyvinylidene fluoride resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Preparation of PVDF resin sample solution: Accurately weigh 2.0058g sample, add 20mL THF, then add 80mL NMP, heat and stir on a metal bath at 60°C for 120min until the sample dissolves, and obtain a PVDF resin sample solution. The used solvent THF:NMP=1:4 (volume ratio) was used as a blank.

[0037] (2) Preparation of standard addition method standard solution: respectively pipette 5 equal parts of 10.0mL PVDF resin sample solution prepared in the above step (1) into a 25mL volumetric flask, from the prepared 1.0mg / mL K, Mg, Al, Pipette 0.0mL, 0.1mL, 0.2mL, 0.5mL, 1.0mL from the mixed standard solution of Cd, Cr, Fe, Cu, Ni, Mn, Pb, Na, Ca into the sample solution in sequence, and use THF:NMP=1: 4 (volume ratio) of mixed solvents to constant volume, to prepare series concentration standard addition method standard solutions.

[0038] (3) Set the ICP-OES instrument parameters: turn on the ICP-OES instrument to preheat, and perform optical initialization after the pr...

Embodiment 2

[0048] (1) Preparation of PVDF resin sample solution: Accurately weigh 3.0820g sample, add 500mL DMF, heat and stir on a metal bath at 80°C for 60min until the sample dissolves, and obtain a PVDF resin sample solution. The used solvent DMF was used as a blank.

[0049] (2) Preparation of standard addition method standard solution: respectively pipette 5 equal parts of 50.0mL PVDF resin sample solution prepared in the above step (1) into a 100mL volumetric flask, from the prepared 1.0mg / mL K, Mg, Al, Pipette 0.0mL, 1.0mL, 2.0mL, 5.0mL, and 10.0mL from the mixed standard solution of Cd, Cr, Fe, Cu, Ni, Mn, Pb, Na, and Ca into the PVDF resin sample solution, and dilute to volume with solvent DMF , to prepare a series of concentration standard addition method standard solutions.

[0050] (3) Set the ICP-OES instrument parameters: turn on the ICP-OES instrument to preheat, and perform optical initialization after the prism temperature is stable, and set the instrument parameters: ...

Embodiment 3

[0057] (1) Preparation of PVDF resin sample solution: Accurately weigh 0.1009g sample, add 40mL DMF and 10mL TEP, heat and stir on a metal bath at 90°C for 40min until the sample dissolves, and obtain a PVDF resin sample solution. The used solvent DMF:TEP=4:1 (volume ratio) was used as a blank.

[0058] (2) Preparation of standard addition method standard solution: pipette 4 equal parts of 10.0mL PVDF resin sample solution prepared in the above step (1) into a 25mL volumetric flask, and prepare 1.0mg / mL of K, Mg, Al, Pipette 0.0mL, 0.05mL, 0.2mL, and 0.5mL from the mixed standard solution of Cd, Cr, Fe, Cu, Ni, Mn, Pb, Na, and Ca into the PVDF resin sample solution in sequence, and use DMF:TEP=4:1 (volume ratio) of the mixed solvent to constant volume to prepare a series of concentration standard addition method standard solutions.

[0059] (3) Set the ICP-OES instrument parameters: turn on the ICP-OES instrument to preheat, and perform optical initialization after the prism ...

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Abstract

The invention discloses a method for determining the content of metal elements in polyvinylidene fluoride resin. The method comprises the following steps of heating and dissolving a polyvinylidene fluoride resin sample by using an organic solvent, and analyzing the metal element content of the polyvinylidene fluoride resin sample by using an inductively coupled plasma emission spectrometer (ICP-OES) in an organic system direct sample injection mode. The method specifically comprises the following steps of (1) preparing a polyvinylidene fluoride resin sample solution; (2) preparing a standard solution by a standard addition method; (3) setting analysis conditions of the inductively coupled plasma emission spectrometer; and (4) measuring the content of metal elements in the sample. The analysis method is high in precision, low in detection limit, capable of rapidly carrying out qualitative and quantitative detection on the inorganic metal elements in the sample, easy to operate, rapid inanalysis, stable and reliable in result, low in instrument cost and maintenance cost and easy to popularize and apply.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection of fluorine-containing polymers, and in particular relates to a method for determining the content of metal elements in polyvinylidene fluoride resin. Background technique [0002] Polyvinylidene fluoride (PVDF) resin is a homopolymer of 1,1-difluoroethylene (VDF) or a copolymer of VDF and other fluorine-containing vinyl monomers. PVDF resin is a thermoplastic with excellent performance, which is widely used in petrochemical, construction, food, water treatment, electrical and electronic and fluorocarbon coatings and other fields. In special application areas such as tap water pipelines, food packaging materials, and storage and transportation of high-purity chemicals in the semiconductor industry, the requirements for the content of metal elements in PVDF resin are relatively high. Therefore, it can quickly and accurately determine the content of impurity metal elements in PVDF res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/44
CPCG01N21/73G01N1/44
Inventor 郑红梅叶林谭慧钟军张庆华王濛琪
Owner JUHUA GROUP TECH CENT
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