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Method for analyzing content of cyclopentane and extraction agent by gas chromatography

A gas chromatographic analysis and extractant technology, applied in the field of gas chromatographic analysis of cyclopentane and extractant content, can solve the problems of large gap in response factor and inaccurate measurement, and achieve low detection limit, good precision and high recovery rate high effect

Pending Publication Date: 2022-03-08
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the technical problems existing at present, the present invention has set up a kind of gas chromatography internal standard method to measure cyclopentane and extractant composition in extractive distillation process, and this method is accurate and reliable, solves simple area normalization method because each component is in Analytical technical problems of inaccurate determination of cyclopentane and extractant caused by large gap of response factors in gas chromatography

Method used

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  • Method for analyzing content of cyclopentane and extraction agent by gas chromatography
  • Method for analyzing content of cyclopentane and extraction agent by gas chromatography
  • Method for analyzing content of cyclopentane and extraction agent by gas chromatography

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Experimental program
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Effect test

Embodiment 1

[0046] 1.1 Experimental instruments and reagents:

[0047] (1) Gas chromatography: 7890B, Agilent, equipped with hydrogen flame ionization detector, equipped with G4513A autosampler; capillary column: HP-INNOWax (30m×0.25mm×0.25μm), 40-260°C, Agilent ;

[0048](2) Reagents: cyclopentane (mass fraction 98.08%), methanol, N,N-dimethylformamide, ethylene glycol, isopropanol, analytically pure;

[0049] 1.2 Steps for setting gas chromatograph detection conditions, gas chromatograph detection conditions include the following parameters:

[0050] a) The instrument used is an Agilent 7890B gas chromatograph equipped with a hydrogen flame ionization detector, and the chromatographic column is Agilent HP-INNOWax (30m×0.25mm×0.25μm), 40-260°C;

[0051] b) Heating program: keep at 45°C for 6 minutes, raise the temperature to 250°C at a rate of 25°C / min, and hold for 5 minutes;

[0052] c) Carrier gas: nitrogen, with a purity greater than 99.999%;

[0053] d) Inlet temperature: 250°C;...

Embodiment 2

[0070] The instrument used, the detection conditions are set, the standard solution configured, and the standard curve drawn are all the same as in Example 1;

[0071] Determination and calculation of samples

[0072] Sample preparation steps: accurately weigh 0.9542 g of rich solvent sample (solvent at the bottom of extractive distillation tower) and 80.5 mg of internal standard - isopropanol in a 10ml volumetric flask, and then accurately weigh poor solvent sample (extraction solvent Recover tower bottom solvent) 0.7339g and internal standard-isopropanol 82.2mg, dilute with methanol to the mark, mix evenly to obtain sample solution, transfer to chromatographic bottle for gas phase detection. Record the ratio of the peak area of ​​each component in the sample to the internal standard, and calculate the contents of cyclopentane, N,N-dimethylformamide, and ethylene glycol in the sample according to the standard curve regression equation in 1.4. The contents of cyclopentane, N,...

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Abstract

The invention belongs to the technical field of analysis, and particularly relates to a method for analyzing the content of cyclopentane and an extracting agent by gas chromatography, which adopts an internal standard method, takes isopropanol as an internal standard substance and performs quantitative analysis according to the peak area of a target compound. The method comprises the following specific steps: preparing and detecting a standard solution, drawing a standard curve by an internal standard method, preparing and detecting a solution to be detected, and determining the content of cyclopentane and an extracting agent in the solution to be detected. The method is simple and convenient to operate, good in precision, high in recovery rate and low in detection limit, plays an important guiding role in calculating material balance, overcomes the defect that the content accuracy of each component is poor due to different response factors of each substance in the conventional area normalization method, can accurately calculate the content of each component, and has a good application prospect. And the method is not influenced by moisture in a sample and unstable state of an instrument.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to a method for analyzing the contents of cyclopentane and extractant by gas chromatography. Background technique [0002] Cyclopentane is an environmentally friendly refrigerant and has become one of the products replacing chlorofluorocarbons. It is widely used in fluorine-free refrigerators, freezers, cold storage, pipeline insulation and other fields. At the same time, it is an excellent polyurethane foaming agent, and it can also be used as a solvent for solution polymerization of polyisoprene rubber and a solvent for cellulose ether and a standard substance for chromatographic analysis. It has a good market prospect. At present, the purity of cyclopentane processed by petroleum equipment is generally about 70-80%, and its impurities mainly include isopentane, n-pentane, 3-methylpentane, n-hexane and 2.2-dimethylbutane. Through product component analysis, 2,2-dimet...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8634G01N2030/045
Inventor 董淑杰张晓阳杨丽吕印美王岳华赵红波崔丽华李霞付鹿韩立霞
Owner CHAMBROAD CHEM IND RES INST CO LTD
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