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Method for Improving the Accuracy of Determination of Molecular Weight of Water-Soluble Polymer by Gel Chromatography

A water-soluble polymer, gel chromatography technology, applied in the field of water treatment, can solve problems such as inability to obtain, interfere with inverted peaks, and continuous peaks, and achieve the effects of improving accuracy, avoiding interference and inverted peaks, and simple operation steps.

Active Publication Date: 2017-02-08
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, water-soluble polymers are generally liquid products, containing more than 40% of water, and may contain organic solvents, residual initiators, monomers and other substances. The determination of molecular weight and its distribution by gel filtration chromatography may be difficult due to too much interference. If it is large, there will be inverted peaks, continuous peaks, etc., and it will not be possible to obtain effective and accurate results.

Method used

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  • Method for Improving the Accuracy of Determination of Molecular Weight of Water-Soluble Polymer by Gel Chromatography
  • Method for Improving the Accuracy of Determination of Molecular Weight of Water-Soluble Polymer by Gel Chromatography
  • Method for Improving the Accuracy of Determination of Molecular Weight of Water-Soluble Polymer by Gel Chromatography

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Take 2g of commercially available polyacrylic acid (PAA), adjust its pH to 7.5 with 10mol / L NaOH solution, and convert PAA into salt; take 50mL of methanol in a beaker, and drop the sample converted into salt into methanol, while Stir, the precipitated solid is the sample to be tested; let it stand for 10 minutes and pour out the methanol, add new methanol to the precipitate and stir and wash again, repeat three times; put the precipitate in a vacuum drying oven at 70°C to dry to constant weight, Cool for later use; determine the molecular weight and its distribution using gel chromatography.

[0023] The molecular weight and molecular weight distribution results of PAA are shown in Table 1 before and after using the method of the present invention, and the spectrogram is shown in figure 1 and figure 2 . As can be seen from the spectrograms, the PAA spectrograms processed by the method of the present invention are significantly improved, the baseline is stable, the p...

Embodiment 2

[0027] Take 2g of commercially available AA-MA copolymer, adjust its pH to 8 with 10mol / L NaOH solution, and convert the polymer into salt; take 50mL of methanol in a beaker, and drop the sample converted into salt into methanol, Stir at the same time, the precipitated solid is the sample to be tested; let it stand for 10 minutes and pour out the methanol, add new methanol to the precipitate and stir and wash again, repeat three times; put the precipitate in a 70°C vacuum drying oven and dry to constant weight , cooled for later use; use gel chromatography to determine the molecular weight and its distribution.

[0028] The molecular weight and molecular weight distribution results of the AA-MA copolymer are shown in Table 2 before and after using the method of the present invention, and the spectrogram is shown in image 3 and Figure 4 . As can be seen from the spectrogram, the AA-MA copolymer processed by the method of the present invention is significantly improved, the ...

Embodiment 3

[0032] Take 2g of commercially available AA-AMPS multi-polymer copolymer, adjust its pH to 9 with 10mol / L NaOH solution, and convert the polymer into salt; take 50mL of methanol in a beaker, and drop the sample converted into salt into methanol drop by drop , stirring at the same time, the precipitated solid is the sample to be tested; let stand for 10 minutes and pour out the methanol, add new methanol to the precipitate and stir and wash again, repeat three times; put the precipitate in a vacuum drying oven at 70°C and dry until constant Weight, cooled for later use; use gel chromatography to determine the molecular weight and its distribution.

[0033] The results of molecular weight and molecular weight distribution of AA-AMPS multi-polymer copolymer before and after using the method of the present invention are shown in Table 3, and the spectrogram is shown in Figure 5 and Figure 6 . As can be seen from the spectrogram, the AA-AMPS multi-component copolymer processed ...

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Abstract

The invention discloses a method for improving the accuracy of the molecular weight of a water-soluble polymer by determination of a gel chromatography. The method is characterized by adopting the following steps: (1) converting a water-soluble polymer into salt, namely weighing a proper amount of water-soluble polymer, adjusting the pH value to 7-9 by using NaOH or KOH, and enabling the water-soluble polymer to be completely converted into a corresponding sodium salt or potassium salt; (2) carrying out purification, namely taking a proper amount of polar precipitating agent which is selected from methyl alcohol, acetone, dioxane, methylbenzene and petroleum ether, dripping the sodium salt or the potassium salt of the water-soluble polymer into the precipitating agent in a dropwise manner while stirring, thus obtaining precipitated solid which is firstly viscous and then becomes powdery gradually, and purifying for three times repeatedly; drying till constant weight, and cooling for spare use, thus obtaining a water-soluble polymer sample to be tested; and (3) carrying out determination on the molecular weight and the distribution of the molecular weight by using the gel chromatography, namely taking sodium polyacrylate as a standard product, adopting a NaNO3 aqueous solution as a flow phase, and carrying out gel chromatographic analysis with the sampling amount of 50-100muL.

Description

technical field [0001] The invention belongs to the technical field of water treatment, and relates to a method for improving the accuracy of gel chromatography for determining the molecular weight of water-soluble polymers; in particular, a method for improving the accuracy of gel chromatography for determining the molecular weight and distribution of low-molecular-weight water-soluble polymers. Background technique [0002] As a class of functional chemicals, water-soluble polymers are widely used in the field of water treatment technology and play a very important role. The molecular weight and distribution of water-soluble polymers are a key factor affecting product performance. In recent years, my country's water treatment agent industry has developed rapidly, but in contrast, my country's product quality control level lags behind, especially for water-soluble polymers, the monitoring of industrial product quality is still only solid content, limit viscosity, density, e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/88
Inventor 侯洋靳晓霞孙继赵迎秋王会
Owner CNOOC TIANJIN CHEM RES & DESIGN INST