Method for quantitatively analyzing adsorption capacity of stone powder to polycarboxylic superplasticizer by ultraviolet derivative spectroscopy

A technology of derivative spectroscopy and quantitative analysis, applied in the field of building materials, can solve the problems of high TOC test cost, test uncertainty, affecting the normal progress of research work, etc., to achieve the effect of easy understanding and simple operation

Inactive Publication Date: 2018-11-23
NINGBO UNIVERSITY OF TECHNOLOGY
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Problems solved by technology

[0003] At present, the test methods for the adsorption capacity of polycarboxylate superplasticizers by stone powder mainly include total organic carbon analysis (TOC), gel permeation chromatography (GPC), and ultraviolet-visible spectrophotometry (UV). The test cost is high and the sample processing is complicated. UV technology is mature, easy to operate, fast and accurate, and the test cost is cheap
The existing UV method for determining the concentration of polycarboxylate superplasticizers is as follows: Ma Baoguo, Yang Hu, Tan Hongbo, etc. Adsorption characteristics of cement and clay minerals on different superplasticizers [J]. Journal of Silicates, 2013, 41 (03 ): 328-333. In the article, it is believed that the UV spectrophotometer scanning confirms that the polycarboxylate superplasticizer solution has no characteristic absorption wavelength; Duan Jianping, Lu Shenghua, Gao Ruijun, Li Di, Cao Qiang. Spectrophotometric determination of polycarboxylate superplasticizer Research on [J]. Modern Chemical Industry, 2011, 31 (03): 89-92. It is believed that if there is no conjugation effect, this absorption is weak in the ultraviolet region and is easily affected by free inorganic ions, especially in molar It is not easy to determine its content when the concentration is low, which brings uncertainty to the test and seriously affects the normal progress of research work

Method used

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  • Method for quantitatively analyzing adsorption capacity of stone powder to polycarboxylic superplasticizer by ultraviolet derivative spectroscopy
  • Method for quantitatively analyzing adsorption capacity of stone powder to polycarboxylic superplasticizer by ultraviolet derivative spectroscopy
  • Method for quantitatively analyzing adsorption capacity of stone powder to polycarboxylic superplasticizer by ultraviolet derivative spectroscopy

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Embodiment 1

[0027] A UV derivative spectral quantitative analysis method of stone powder on the adsorption capacity of polycarboxylate water reducer, specifically comprising the following steps:

[0028] (1) In the No.35-PCs solution with a volume of 30 ml and a concentration of 0.4 mg / mL, add stone powder with a mass of 3 g, shake well, and oscillate at a frequency of 30 r / min in a constant temperature water bath to obtain a suspension; After 30 min, the suspension was centrifuged to obtain a supernatant; then the supernatant was filtered with a 0.45 μm pinhole filter to obtain a test sample solution for use. Among them, the No.35-PCs solution is self-synthesized by using α-methallyl polyethylene glycol macromonomer (HPEG) with a molecular weight of 3500 and acrylic acid provided by Shanghai Fujia Fine Chemical Co., Ltd. ; The stone powder is the tuff rock powder after the undisturbed ash discharged by the sandstone industry in Ningbo area is ground by a ball mill, and the passing rate o...

Embodiment 2

[0036] A UV derivative spectral quantitative analysis method of stone powder on the adsorption capacity of polycarboxylate water reducer, specifically comprising the following steps:

[0037] (1) In the No.30-PCs solution with a volume of 30 ml and a concentration of 2 mg / mL, add stone powder with a mass of 3 g, shake well, and vibrate at a frequency of 30 r / min in a constant temperature water bath to obtain a suspension; 30 After 1 min, the suspension was centrifuged to obtain a supernatant; then the supernatant was filtered with a 0.45 μm pinhole filter to obtain a test sample solution for later use. Among them, the No.30-PCs solution is α-methallyl polyethylene glycol macromonomer (HPEG) with a molecular weight of 3000 provided by Shanghai Fujia Fine Chemical Co., Ltd., acrylic acid, etc. Synthesized by itself; the stone powder is the tuff rock powder after the undisturbed ash discharged by the sand and gravel industry in Ningbo area is ground by a ball mill, and the passin...

Embodiment 3

[0045] A UV derivative spectral quantitative analysis method of stone powder on the adsorption capacity of polycarboxylate water reducer, specifically comprising the following steps:

[0046] (1) In the No.24-PCs solution with a volume of 30 ml and a concentration of 0.4 mg / mL, add stone powder with a mass of 3 g, shake well, and oscillate at a frequency of 30 r / min in a constant temperature water bath to obtain a suspension; After 30 min, the suspension was centrifuged to obtain a supernatant; then the supernatant was filtered with a 0.45 μm pinhole filter to obtain a test sample solution for use. Among them, the No.24-PCs solution is α-methallyl polyethylene glycol macromonomer (HPEG) with a molecular weight of 2400 provided by Shanghai Fujia Fine Chemical Co., Ltd., acrylic acid, etc. Synthesized by itself; the stone powder is the tuff rock powder after the undisturbed ash discharged by the sand and gravel industry in Ningbo area is ground by a ball mill, and the passing ra...

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Abstract

The invention discloses a method for quantitatively analyzing the adsorption capacity of stone powder to polycarboxylic superplasticizer (PCs) by ultraviolet derivative spectroscopy. The method comprises the following steps: (1) establishing an absorption spectrum curve of a standard solution by using an ultraviolet visible spectrophotometer; (2) performing second derivative processing of the absorption spectrum curve to extract the ultraviolet characteristic peaks of carboxylic acid of PCs; (3) collecting absorbance A of the solution at the characteristic peaks after blank zero adjustment ofthe spectral curve taking the stone powder and the deionized water system as reference, fitting the relationship formula between the absorbance A and PCs concentrations C by a data statistics method,as working curve, extracting the slope characteristic parameters of the working curve; and (4) according to Langerbeer's law A=KC, determining the change of PCs concentrations by the change of the absorbance values of a filtrate before and after adding stone powder to obtain the adsorption capacity of stone powder to PCs with different side chain lengths. The method is simple in operation, fast inanalysis process, accurate and cheap, and does not require color development.

Description

technical field [0001] The invention belongs to the field of building materials, and in particular relates to a UV derivative spectrum quantitative analysis method for the adsorption amount of polycarboxylate superplasticizers by stone powder. Background technique [0002] Polycarboxylate superplasticizers (abbreviated as PCs) have high water reducing rate, low shrinkage ratio and almost no Cl - with SO 4 2- It has become an indispensable and important material for the preparation of high-durability concrete. The performance of polycarboxylate superplasticizer is mainly adsorbed on the surface of cement particles or hydration products through the negatively charged main chain, forming an adsorption layer with a certain thickness, and destroying the flocculation between cement particles through the effect of steric hindrance and electrostatic repulsion The structure ensures the rheology of the fresh concrete. However, river sand resources in many areas are almost exhauste...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N21/33
CPCG01N21/31G01N21/33
Inventor 温小栋冯蕾陈锡芹张振亚王赛赛蔡伟
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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