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Method for measuring organic acid and ester of centrifuge waste water in cis-anhydride production process with liquid phase chromatography

A production process and liquid chromatography technology, applied in the field of chemical analysis, can solve problems such as difficult accurate quantification, inability to measure at the same time, low solubility, etc., and achieve the effect of simple determination method, good reproducibility and high sensitivity

Active Publication Date: 2008-10-08
SINOPEC LANZHOU GASOLINEEUM CHEM IND CORP
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Problems solved by technology

However, since maleic acid and fumaric acid are isomers, it is difficult to separate them in chromatography; in addition, in general, maleic acid, fumaric acid, orthophthalic acid The solubility of diformic acid in water is small, and it is difficult to quantify accurately
And because the sample background of the gas chromatography analysis method is completely different from that of the spectrophotometry analysis method, maleic acid, fumaric acid, phthalic acid and dibutyl phthalate cannot be analyzed by the same analysis method. Simultaneous determination

Method used

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  • Method for measuring organic acid and ester of centrifuge waste water in cis-anhydride production process with liquid phase chromatography
  • Method for measuring organic acid and ester of centrifuge waste water in cis-anhydride production process with liquid phase chromatography
  • Method for measuring organic acid and ester of centrifuge waste water in cis-anhydride production process with liquid phase chromatography

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Embodiment Construction

[0025] (1) Preparation of standard sample solution

[0026] Weigh 0.01 g (accurate to ±0.0001 g) of standard substances of maleic acid, fumaric acid, phthalic acid and dibutyl phthalate, respectively, and prepare 4 to 5 standards with different concentrations. solution, set aside. In order to ensure that the detection signal is within the optimal response value range of the instrument (20%-80% of full scale), the concentration range of the standard sample solution in this experiment is 0.05-5 mg / ml.

[0027] (2) Chromatographic analysis conditions

[0028] Instrument and chromatographic column: Agilent HP1090 or Shimadzu SCL-10AVP liquid chromatograph, matching diode array detector and data processing system, Agilent C18 chromatographic column.

[0029] Mobile phase: water / methanol / ethyl acetate were mixed at an initial mass ratio of 10 / 20 / 70, and gradient elution was adopted.

[0030] Raw materials: methanol (chromatographically pure), ethyl acetate (chromatographically pu...

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Abstract

The invention relates to a detecting method for the organic acid and ester in centrifugal waste water in the cis-butenedioic anhydride production process through liquid chromatography, the method uses Agilent C18 chromatographic column as the analytical column, water, methanol, and acetidin are mixed in a certain proportion as mobile phase, the flow velocity is 1.0mL / min, the column temperature is 40 DEG C, the operating time is 25min, the sample volume is 20muL, an external standard method quantificationally analyzes the organic acid and ester in the cis-butenedioic anhydride waste water through liquid chromatography, the linearly dependent coefficient is more than 0.9969. The invention carries out the effective quantitative analysis for the organic acid and ester in centrifugal waste water in the cis-butenedioic anhydride production process, the detecting method is simple and has good reproducibility; the detecting result is accuracy, the sensitivity is high, which acts a positive pushing effect for enhancing the product quality and lowing product cost of the cis-butenedioic anhydride.

Description

technical field [0001] The invention belongs to the field of chemical analysis, and relates to maleic acid, fumaric acid, phthalic acid and dibutyl phthalate in centrifuged wastewater in the process of producing maleic anhydride with butane as raw material analysis method. Background technique [0002] Maleic anhydride, referred to as maleic anhydride, is an important organic chemical raw material and fine chemical product, mainly used in the production of unsaturated polyester resin, alkyd resin, coating, ink, lubricating oil additive, agricultural chemicals, paper application Adhesives, textile permanent finishing agents, surfactants and other fields. In addition, a series of important fine chemical products such as tetrahydrofuran, maleic acid, fumarate and tetrahydroanhydride can also be produced with maleic anhydride as raw material. [0003] Maleic anhydride is produced by catalytic oxidation of butane. Maleic acid, fumaric acid, phthalic acid and dibutyl phthalate (h...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/86G01N30/02
Inventor 马翠芳杨慧明李延顾惠新武克锋
Owner SINOPEC LANZHOU GASOLINEEUM CHEM IND CORP
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