Liquid phase chromatographic analysis method for 3-nitro or 4-nitrophthalic acid and impurities thereof
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A technology of nitrophthalic acid and high-performance liquid chromatography, which is applied in the direction of analyzing materials, separating materials, measuring devices, etc., to achieve the effect of accurate results and simple operation
Inactive Publication Date: 2005-06-29
NANJING UNIV
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It is very meaningful to realize the separation and accurate quantification of these three compounds, but there is
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[0023] 1.1 Instrument
[0024] Varian 5060 type high performance liquid chromatograph (U.S. Varian company), is equipped with Rheodyne7725i six-port sampling valve (U.S. Rheodyne company); Waters 486 type ultraviolet-visible spectrophotometric detector (U.S. Waters company); JS-3050 chromatographic workstation ( Dalian Jiangshen Separation Science and Technology Company); the chromatographic recorder is a Type 3066 pen recorder (Sichuan Instrument No. 4 Factory); the PHS-3D type pH meter (Shanghai Sanxin Instrument Factory) for solution pH measurement is equipped with a pH composite electrode ( Shanghai Precision Scientific Instrument Co., Ltd).
[0025] 1.2 Drugs and reagents
[0026] Phthalic acid, 3-nitrophthalic acid, 4-nitrophthalic acid reference substance (99.0%); methanol (chromatographically pure); glacial acetic acid (analytical pure); perchloric acid (excellent pure) ; The mobile phase water used in the experiment was commercially available Wahaha purified water, ...
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Abstract
It is a high effective liquid chromatogram analysis method of a mixture composed of three-nitryl phthalandione, four-nitryl phthalandione and phthalandione. Its conditions are the following: chromatogram of Kromasil C#-[18]ú¼5ª–mú¼150í‡4.6mm(I.D.); flow phase of carbinol to acetic acid liquid (0.1mol/Lú¼pH2.89) with volume proportion as 10í† 90; flow speed of 1.0mL/min; column temperature as thirty degrees; sample-in volume: 10ª–L; test wavelength: 254nm; accuracy: 0.2aufs.
Description
technical field [0001] The present invention relates to the analysis method of 3-nitrophthalic acid and 4-nitrophthalic acid. Background technique [0002] 3-Nitrophthalic acid (3-NPA) and 4-Nitrophthalic acid (4-NPA) are important basic chemical intermediates, such as phthalocyanine dyes Synthetic starting materials for polymers [See: Achar, Bappalige N., Fohlen George M., Parker John A, (National Research Council, Washington; United States National Aeronautics and Space Administration) U.S. Pat. Appl. US 440,656 27 May 1983, Appl. 10 Nov 1982; 30pp.]. They are usually prepared from phthalic acid (o-Phthalic acid, o-PA) through nitration reaction to generate a mixture of two nitro derivatives, and then separated [Ref: Pitra Josef, Zoula Vaciav, Czech.CS 190 , 202 (Cl.C07C79 / 46), 15Sep 1981, Appl.77 / 4,983, 27 Jul 1977; 2pp.; Odle, Roy Ray (General Electric Co.) PCT Int.Appl.WO 8502,615 (Cl.C07D307 / 89), 20 Jun 1985, US Appl.559,575,08 Dec 1983; 18pp.], so 3-nitrophthalic ...
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