HPLC analytical method for fine terephthalic acid products and produced residue
A technology of high performance liquid chromatography and purified terephthalic acid, which is applied in the direction of analyzing materials, material separation, and measuring devices, and can solve problems such as inability to detect impurities and complicated processes
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Embodiment 1
[0016] High performance liquid chromatograph from WATERS company in the United States, wavelength 240nm, Agilent ZORBAX SAX column (Φ4.6μm×250mm), 0.25mol / l ammonium dihydrogen phosphate buffer as mobile phase, equipped with 15% methanol for organic modification reagent, the flow rate is 1ml / min, and the column temperature is 20°C.
[0017] Prepare standard samples of eight acid components: p-carboxybenzaldehyde at a concentration of 5-50 mg / l, p-toluic acid at a concentration of 10-80 mg / l, benzoic acid at a concentration of 20-170 mg / l, terephthalic acid The concentration is 10-90mg / l, the concentration of phthalic acid is 10-100mg / l, the concentration of isophthalic acid is 20-150mg / l, the concentration of trimellitic acid is 20-140mg / l, and the concentration of trimellitic acid is 20~140mg / l, and draw the working curve.
[0018] Select a standard concentration point from the linear concentration of each acid component working curve, measure its recovery rate and standard ...
example 2
[0036] Example 2 Determination of residue components in the oxidation process stage of purified terephthalic acid
[0037] (1) Determination purpose: take the residue in the oxidation process stage of purified terephthalic acid for determination, and then test the reliability of the method.
[0038] (2) Reagent source: Standard samples are imported reagents provided by Bailingwei Chemical Reagent Company.
[0039] (3) Analytical conditions: using high performance liquid chromatography from WATERS, USA, with a detection wavelength of 240nm, an Agilent ZORBAX SAX column (Φ4.6μm×250mm), and 0.25mol / l ammonium dihydrogen phosphate buffer as the mobile phase. 15% methanol is used as a modifier, the flow rate is 0.5ml / min, and the column temperature is 18°C.
[0040] (4) Experimental procedure: Weigh 0.5g of the residue sample, add excess ammonia water to dissolve, and then adjust the pH to 6-7 with phosphoric acid, filter with suction, and dilute to a 100ml volumetric flask.
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example 3
[0043] Example 3 Determining the residue component of purified terephthalic acid washing process stage
[0044] (1) Determination purpose: take the residue of purified terephthalic acid washing process stage for determination, and then test the reliability of the method.
[0045] (2) Reagent source: Standard samples are imported reagents provided by Bailingwei Chemical Reagent Company.
[0046] (3) Analytical conditions: high-performance liquid chromatography from WATERS, USA, with a detection wavelength of 240nm, an Agilent ZORBAX SAX column (Φ4.6μm×250mm), and 0.30mol / l ammonium dihydrogen phosphate buffer as the mobile phase. 15% methanol is used as a modifier, the flow rate is 0.8ml / min, the column temperature is 18°C, and the sample is measured.
[0047] (4) Experimental procedure: Weigh 0.5g of the residue sample, add excess ammonia water to dissolve, and after it is completely dissolved, adjust the pH to 6-7 with phosphoric acid, suction filter, and dilute to a 100ml v...
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