Method for measuring content of dimethylbenzene oxidation products by using HPLC external standard method

An oxidation product, xylene technology, applied in the field of analysis, can solve the problems of difficult separation, reduced analysis accuracy, interference of qualitative and quantitative analysis of ortho, meta, and terephthalic acid, and achieves the effect of simple and easy method and short analysis time.

Inactive Publication Date: 2018-04-13
CHAMBROAD CHEM IND RES INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The above-mentioned series of oxidation products produced during the oxidation of xylene have similar polarity and properties, and there are isomers, which are difficult to separate, so they will interfere with the qualitative and quantitative analysis of o-, m-, and terephthalic acids.
[0004] According to literature data, there are few research reports on the analysis and detection of xylene oxidation products at present, and some analysis methods for single oxide systems use polarography, capillary electrophoresis, capillary micellar electrokinetic chromatography, etc., but none of them can be completely analyzed. Analysis of xylene oxidation products and various by-products. Although gas chromatography is commonly used to analyze benzene series, high boiling point substances are easy to accumulate in the chromatographic column, which reduces column efficiency and analysis accuracy. Liquid chromatography is based on group analysis. The partition coefficients of the mobile phase and the stationary phase are different to separate them. It is suitable for the analysis of organic compounds with high boiling points, non-volatile and different polarities. Therefore, the above methods cannot be effectively applied to the content of xylene oxidation products.

Method used

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  • Method for measuring content of dimethylbenzene oxidation products by using HPLC external standard method
  • Method for measuring content of dimethylbenzene oxidation products by using HPLC external standard method
  • Method for measuring content of dimethylbenzene oxidation products by using HPLC external standard method

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Effect test

Embodiment 1

[0045] There is a batch of samples of xylene oxidation products with unknown concentration, the ratio of o-, m-, and terephthalic acid is about 1:1:1, the content of the three needs to be determined, and the detection is carried out by high-performance liquid chromatography and external standard method Quantitative analysis, the specific steps include:

[0046] (1) Preparation of standard solution: Accurately weigh 10.0mg, 20.0mg, 30.0mg, 40.0mg, 50.0mg of each standard sample of phthalic acid, isophthalic acid, and terephthalic acid into 5 beakers, and add 10mL dimethyl sulfoxide to dissolve the sample, transfer it completely to a 100mL volumetric flask, add methanol to dissolve and mix, and set the volume to the mark to obtain mixed standard solutions I, II, III, IV, V, and its phthalic acid , isophthalic acid, and terephthalic acid are 100.0mg / L, 200.0mg / L, 300.0mg / L, 400.0mg / L, and 500.0mg / L respectively;

[0047] (2) Preparation of sample solution: Accurately weigh three...

Embodiment 2

[0054] There are a batch of samples of xylene oxidation products with unknown concentrations. The ratio of o-, m-, and terephthalic acid is about 1:1:2. It is necessary to measure the content of the three, and use high-performance liquid chromatography for detection and external standard method Quantitative analysis, the specific steps include:

[0055] (1) Preparation of standard solution: Accurately weigh 10.0mg, 20.0mg, 30.0mg, 40.0mg, 50.0mg of each standard sample of phthalic acid, isophthalic acid, and terephthalic acid into 5 beakers, and add 10mL dimethyl sulfoxide (DMSO), to dissolve the sample, transfer it completely to a 100mL volumetric flask, add methanol to dissolve and mix, and set the volume to the mark to obtain mixed standard solutions I, II, III, IV, V, and its adjacent The concentrations of phthalic acid, isophthalic acid and terephthalic acid are 100.0mg / L, 200.0mg / L, 300.0mg / L, 400.0mg / L, 500.0mg / L respectively;

[0056] (2) Preparation of sample solutio...

Embodiment 3

[0061] There are a batch of samples of xylene oxidation products with unknown concentrations. The ratio of o-, m-, and terephthalic acid is about 1:2:1. It is necessary to measure the content of the three, and use high-performance liquid chromatography for detection and external standard method Quantitative analysis, the specific steps include:

[0062] (1) Preparation of standard solution: Accurately weigh 10.0mg, 20.0mg, 30.0mg, 40.0mg, 50.0mg of each standard sample of phthalic acid, isophthalic acid, and terephthalic acid into 5 beakers, and add 10mL dimethyl sulfoxide to dissolve the sample, transfer it completely to a 100mL volumetric flask, add methanol to dissolve and mix, and set the volume to the mark to obtain mixed standard solutions I, II, III, IV, V, and its phthalic acid , isophthalic acid, and terephthalic acid are 100.0mg / L, 200.0mg / L, 300.0mg / L, 400.0mg / L, and 500.0mg / L respectively;

[0063] (2) Preparation of sample solution: Accurately weigh three parts o...

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Abstract

The invention discloses a method for measuring content of dimethylbenzene oxidation products by using an HPLC external standard method. According to the method, a high performance reversed-phase liquid chromatograph instrument is adopted, a C18 silica gel chromatographic column is taken as a separation column, an ultraviolet visible absorption detector is adopted, methanol and an acid aqueous solution are taken as mobile phases, phthalate, isophthalic acid and terephthalic acid are taken as standard samples, a concentration-peak area standard curve of a target component is drawn by using the external standard method so as to obtain a linear regression equation, and contents of the phthalate, isophthalic acid and terephthalic acid are calculated by using the regression equation. Through adoption of the method, three main products with similar polarity and four byproducts including 3-formylbenzoic acid, benzoic acid, paratoluic acid and p-tolualdehyde can be separated effectively, and the method takes short time in analysis, is easy and feasible, and is convenient and reliable.

Description

technical field [0001] The invention belongs to the technical field of analysis, and relates to a quantitative analysis method for phthalic acid, isophthalic acid, and terephthalic acid, in particular to a method for determining phthalic acid, isophthalic acid, and isophthalic acid in xylene oxidation products by using an HPLC external standard method. Formic acid, terephthalic acid content method. Background technique [0002] During the oxidation process of xylene, three main products of phthalic acid, isophthalic acid and terephthalic acid will be produced, and by-products such as 3-formylbenzoic acid, p-toluic acid, p-tolualdehyde and benzoic acid will be produced at the same time and intermediate products. Among them, phthalic acid can be used in the manufacture of fuels, resins, drugs and plasticizers. Isophthalic acid and terephthalic acid can also be used in polyester resins, synthetic fibers and plasticizers. All three are important chemical raw materials and hav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 崔丽华马韵升陈梅梅王岳华吕印美邢丽莉付鹿刘清钊韩立霞许晓莲王珊珊
Owner CHAMBROAD CHEM IND RES INST CO LTD
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