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Liquid phase chromatographic analysis method for 3-nitro or 4-nitrophthalic acid and impurities thereof

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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is very meaningful to realize the separation and accurate quantification of these three compounds, but there is no report on the separation and determination of these three compounds by high performance liquid chromatography.

Method used

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  • Liquid phase chromatographic analysis method for 3-nitro or 4-nitrophthalic acid and impurities thereof
  • Liquid phase chromatographic analysis method for 3-nitro or 4-nitrophthalic acid and impurities thereof
  • Liquid phase chromatographic analysis method for 3-nitro or 4-nitrophthalic acid and impurities thereof

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Embodiment Construction

[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 ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/26G01N30/84
Inventor 练鸿振王惟汉李丹妮
Owner NANJING UNIV
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