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Measuring method for content of metal elements in polymer resin

A metal element and determination method technology, applied in the field of chemical analysis, can solve the problems of large errors in the measurement results of metal element content, achieve the effects of small sample size, ensure safe production, and improve accuracy

Active Publication Date: 2013-01-16
CHNA ENERGY INVESTMENT CORP LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims to provide a method for determining the content of metal elements in polymer resins to solve the problem of large errors in the measurement results of metal elements in the prior art

Method used

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  • Measuring method for content of metal elements in polymer resin
  • Measuring method for content of metal elements in polymer resin
  • Measuring method for content of metal elements in polymer resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Microwave digestion of polypropylene resin:

[0049] Weigh 0.1053g of a polypropylene resin sample and place it in a microwave digestion tank, add 8ml of concentrated nitric acid and 2ml of hydrogen peroxide in sequence, cover the inner cover and explosion-proof membrane, and lock the outer cover. Then put it into the digester for digestion. The digestion program is pressure 40bar, power 800 watts, temperature program rises to 200°C for 30 minutes, detects the temperature and pressure of the digestion tank in real time, and the digestion program ends after 20 minutes of heat preservation. When the temperature drops to about room temperature, turn on the digestion instrument and take out the digestion tank. Transfer the acid solution into a polytetrafluoroethylene beaker, heat to remove the acid until a wet salt-like substance is obtained, add a small amount of hydrogen peroxide after cooling, and continue to remove the acid until there is no large amount of bubbles when...

Embodiment 2

[0065] Microwave digestion of polyethylene resin:

[0066] Weigh 0.1538g of a polyethylene resin sample and place it in a microwave digestion tank, add 6ml of concentrated nitric acid, 2ml of concentrated hydrochloric acid and 2ml of hydrogen peroxide in sequence, cover the inner cover and explosion-proof membrane, and lock the outer cover. Then put it into the digester for digestion. The digestion program is pressure 25bar, power 500 watts, and programmed temperature rise to 180°C for 25 minutes. The temperature and pressure of the digestion tank are detected in real time. After 10 minutes of heat preservation, the digestion program ends. When the temperature drops to about room temperature, turn on the digestion instrument and take out the digestion tank. Transfer the acid solution into a polytetrafluoroethylene beaker, heat the acid until it is nearly dry, add a small amount of hydrogen peroxide after cooling, and continue to rinse the acid until there is no large amount of...

Embodiment 3

[0078] Microwave digestion of polypropylene resin:

[0079]Weigh 0.2000g of a polypropylene resin sample and place it in a microwave digestion tank, add 7ml of concentrated nitric acid and 3.5ml of concentrated sulfuric acid in sequence, cover the inner cover and explosion-proof membrane, and lock the outer cover. Then put it into the digester for digestion. The digestion program is a pressure of 50 bar, a power of 300 watts, and a programmed temperature rise of 40 minutes to 220 ° C. The temperature and pressure of the digestion tank are detected in real time. After 15 minutes of heat preservation, the digestion program ends. When the temperature drops to about room temperature, the digestion instrument is turned on, and the digestion tank is taken out. Transfer the acid solution into a polytetrafluoroethylene beaker, heat to remove the acid until nearly dry, add a small amount of hydrogen peroxide after cooling, and continue to remove the acid until there are no large bubble...

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Abstract

The invention provides a measuring method for content of metal elements in polymer resin. The measuring method includes the steps of firstly, establishing a standard curve of concentration and light absorbance of different metal elements on an atomic absorption spectrograph; secondly, adding digestion liquid into polymer resin to be measured to obtain mixture A, and digesting the mixture A by a microwave digestion method to obtain acid fluid A; thirdly, heating the acid fluid A to allow residual matter to be a wet salt state, and performing constant volume by deionized water to prepare solution A to be measured; and fourthly, measuring the solution A to be measured by the atomic absorption spectrograph to obtain light absorbance of the metal elements in the solution A to be measured, acquiring concentration Ci of the metal elements of the solution A to be measured according to the standard curve of concentration and light absorbance, and calculating to acquire content of the metal elements in the polymer resin to be measured. The polymer resin is digested by the microwave digestion method, metal is free of loss in treatment process, and accuracy of measurement is increased.

Description

technical field [0001] The invention relates to the field of chemical analysis, in particular to a method for determining the content of metal elements in polymer resins. Background technique [0002] In the process of polymer synthesis, it generally needs to be carried out under the catalysis of the catalyst. The main catalyst in the catalyst is the metal element supported on the carrier, and the catalyst is often mixed in the polymer as the polymerization reaction proceeds. Therefore, by measuring the polymerization The metal content in the product can indirectly obtain the catalyst content in the polymerization process of these products, so as to further study the performance of the catalyst. [0003] Traditionally, heat digestion is used for sample processing of polymer resins, that is, a certain amount of polymer is weighed into a crucible, and the crucible is placed on a gas lamp or an electric furnace and slowly heated until the polymer begins to decompose, and the re...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N1/44
Inventor 张维斌徐颖王涛周茂侠
Owner CHNA ENERGY INVESTMENT CORP LTD
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