A kind of assay method of polyethylene glycol content in polycarboxylate superplasticizer macromonomer

A technology of polyethylene glycol and water reducing agent, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of reducing sample volume, short inspection cycle and good reproducibility

Active Publication Date: 2017-06-27
SICHUAN SEDAR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method with high sensitivity, strong specificity, short detection period and accurate analysis results for the determination of polyethylene glycol in the macromonomer of the water reducing agent. Drawbacks of the polyethylene glycol method

Method used

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  • A kind of assay method of polyethylene glycol content in polycarboxylate superplasticizer macromonomer
  • A kind of assay method of polyethylene glycol content in polycarboxylate superplasticizer macromonomer
  • A kind of assay method of polyethylene glycol content in polycarboxylate superplasticizer macromonomer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Method validation test

[0026] 1. Instruments and reagents:

[0027] Shimadzu LC-20AT liquid chromatograph, labsolutions LC workstation; ME204E electronic analytical balance (Mettler Toledo)

[0028] Superplasticizer macromonomer sample; polyethylene glycol 4000 reference substance (Agilent); acetonitrile (Thermo Fisher); laboratory water is ultrapure water

[0029] 2. Methods and results

[0030] 2.1 Chromatographic conditions: chromatographic column is GLInterSutain-C 18 (4.6mm*250mm*5μm), the mobile phase is acetonitrile:water (45:55), the flow rate is 1mL / min, the column temperature is 35°C, the injection volume is 5μL, and the number of theoretical plates is not low based on polyethylene glycol in 2000.

[0031] 2.2 Preparation of the reference substance solution: Weigh 20 mg of polyethylene glycol 4000 to a 50 ml measuring bottle, accurately weigh it, add mobile phase to dissolve and dilute to the mark to obtain the reference substance solution.

[0032] 2.3...

Embodiment 2

[0042] Comparative test with chemical method

[0043] 1. Instruments and reagents:

[0044] Shimadzu LC-20AT liquid chromatograph, labsolutions LC workstation; ME204E electronic analytical balance (Mettler Toledo).

[0045] Macromonomer samples of water-reducing agents from 5 different companies; polyethylene glycol 4000 reference substance (Agilent); acetonitrile (Thermo Fisher); laboratory water was ultrapure water.

[0046] 2. Methods and results

[0047] 2.1 Chromatographic conditions: chromatographic column is GLInterSutain-C 18(4.6mm*250mm*5μm), the mobile phase is acetonitrile: water (45:55), the flow rate is 1mL / min, the column temperature is 35°C, the injection volume is 5μL, and the number of theoretical plates is not low based on polyethylene glycol in 2000.

[0048] 2.2 Preparation of reference substance solution: Weigh 20 mg of polyethylene glycol 4000 into a 50 ml measuring bottle, weigh accurately, add mobile phase to dissolve and dilute to the mark to obtai...

Embodiment 3

[0054] Blank sample comparison test

[0055] 1. Instruments and reagents:

[0056] Shimadzu LC-20AT liquid chromatograph, labsolutions LC workstation; ME204E electronic analytical balance (Mettler Toledo)

[0057] Superplasticizer macromonomer, acetonitrile (Thermo Fisher), methanol (Thermo Fisher) laboratory water is ultrapure water

[0058] 2. Methods and results

[0059] 2.1 Chromatographic condition 1: chromatographic column is GLInterSutain-C 18 (4.6mm*250mm*5μm), the mobile phase is acetonitrile: water (45:55), the flow rate is 1mL / min, the column temperature is 35°C, the injection volume is 5μL, and the number of theoretical plates is not low based on polyethylene glycol in 2000.

[0060] 2.2 Chromatographic conditions 2: The chromatographic column is GLInterSutain-C18 (4.6mm*250mm*5μm), the mobile phase is methanol:water (45:55), the flow rate is 1mL / min, the column temperature is 35°C, the injection volume is 5μL, the theoretical The number of plates is not less ...

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Abstract

The invention discloses a method for determining the content of polyethylene glycol in a macromonomer of a polycarboxylate water reducer. Adopt HPLC method to detect, adopt standard curve method or external standard method to quantify, wherein, chromatographic column is C18 post; Mobile phase is the mixed solution of acetonitrile and water, and its weight percent example is acetonitrile: water=30~60:70~40. The invention adopts the HPLC method, uses acetonitrile / water as the mobile phase, reduces the sample injection volume, eliminates the influence of the solvent peak on the detection of the polyethylene glycol content, and is targeted at the polycarboxylate superplasticizer macromonomer The polyethylene glycol content in the medium provides a detection method, which has important practical significance. The method is accurate, simple, and the inspection period is short, about half an hour, which can provide a reference for the quality control of the superplasticizer macromonomer.

Description

technical field [0001] The invention relates to a method for measuring polyethylene glycol content in polycarboxylate superplasticizer macromonomers, in particular to a method which can effectively avoid the influence of solvent peaks on polyethylene glycol content detection by using HPLC. Background technique [0002] Polycarboxylate high-performance water reducer is a concrete superplasticizer (water reducer) with the most cutting-edge technology, the highest technology content, the best application prospect and the best comprehensive performance in the world. Polycarboxylate high-performance water reducer is a compound product of carboxylic acid grafted multi-polymer and other effective additives. The performance comparison with similar products at home and abroad shows that the polycarboxylate high-performance water reducer has reached the current international advanced level in terms of technical performance indicators and cost performance. Polycarboxylate superplastic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 杨海君杨成武
Owner SICHUAN SEDAR CHEM
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