Method for quantitatively detecting residual hydroxyethyl acrylate in process of polymer synthesis
A technology of hydroxyethyl acrylate and synthesis process, applied in measurement devices, instruments, scientific instruments, etc., can solve problems such as self-polymerization, molecular chain breakage, affecting precision, etc., and achieve improved sensitivity, high sensitivity and high accuracy. Effect
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Embodiment 1
[0045] Choice of wavelength and mobile phase
[0046] Wavelength: Take hydroxyethyl acrylate, dissolve it in methanol, and conduct full-wavelength scanning of ultraviolet light in the wavelength range of 190-400nm. The results show that it has a large absorption in the range of 200-220nm and a maximum absorption at 205nm;
[0047] Mobile phase A: 0.01-0.1mol / L phosphate solution (preparation of 0.01-0.1mol / L phosphoric acid solution, preferably 0.05mol / L, adjust pH to 4.0-7.0, preferably 7.0 with sodium hydroxide);
[0048] Mobile phase B: select common mobile phase methanol (chromatographically pure) as mobile phase B, select 200±10nm as the detection wavelength, preferably 205nm.
Embodiment 2
[0050] Main chromatographic conditions
[0051] Mobile phase ratio: mobile phase A: mobile phase B = 70:30, isocratic elution;
[0052] Flow rate: 1.0ml / min;
[0053] Column temperature: 30°C;
[0054] Detection wavelength: 205nm;
[0055] Injection volume: 20 μL.
[0056] Preparation of the test solution: Take the mixed liquid of the water reducer, dissolve it in ultrapure water to prepare a 1g / L polycarboxylate water reducer solution, and filter it through a 0.22μm water filter membrane for use.
[0057] Preparation of hydroxyethyl acrylate standard reference solution: Accurately weigh hydroxyethyl acrylate, dissolve it in ultrapure water and configure it to 200×10 -5 mol / L solution, and filtered through a 0.22 μm water filter membrane for use.
[0058] Get need testing solution and standard reference substance solution sample injection respectively, collect chromatogram (such as image 3 , Figure 4 ), calculate the content of hydroxyethyl acrylate in the polycarboxyla...
Embodiment 3
[0061] Verification test
[0062] According to the chromatographic conditions of Example 2, methodological verification was carried out from aspects of specificity, precision, linearity, detection limit and quantification limit, stability, and the results are as follows:
[0063] (1) Specificity:
[0064] Take the test solution (polycarboxylate superplasticizer) and hydroxyethyl acrylate standard reference solution respectively, and inject them sequentially. As a result of the test, the peak of the solvent is 1.5-1.8min, and the retention time of hydroxyethyl acrylate is 3.1-3.4min. The polycarboxylate superplasticizer has a good separation effect on the peak of the test product solution, and does not interfere with the standard reference substance of hydroxyethyl acrylate, and the retention time of the peak of acrylic acid is consistent. This method is feasible and specific.
[0065] (2) Precision:
[0066] Take the standard reference substance solution of hydroxyethyl acr...
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