Method for rapidly measuring content of furfural by high performance liquid chromatography

A high-performance liquid chromatography and rapid determination technology, which is applied in the field of rapid determination of furfural content by high-performance liquid chromatography, can solve the problems of toxicity, greater harm to laboratories and personnel, and short service life, so as to achieve accurate detection data and fast determination speed , good stability

Inactive Publication Date: 2014-01-01
SHANDONG LONGLIVE BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

However, the titration method is cumbersome and takes a long time, so it cannot be quickly determined in time to guide the actual production; although the gas chromatography method is fast, it cannot be used for a long time due to the high acidity of the furfural semi-finished product (aldehyde vapor condensate) and serious corrosion to the gas chromatography column. Poor stability; the high-pressure liquid chromatography C18 column method must use a highly volatile organic solution as the mobile phase, which has certain toxicity, and long-term use is harmful to the laboratory and personnel. short life

Method used

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  • Method for rapidly measuring content of furfural by high performance liquid chromatography
  • Method for rapidly measuring content of furfural by high performance liquid chromatography
  • Method for rapidly measuring content of furfural by high performance liquid chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Sampling: From the furfural production workshop, connect the sampler to the sampling port, open the cooling water valve, and open the aldehyde vapor sampling valve after passing the cooling water. After the aldehyde vapor is condensed, it is collected in the sampling cup and discarded before 1 minute sample, collect 50ml of sample after 1 minute, for the determination of furfural content.

[0027] (2) Preparation of standard curve: According to the solubility of furfural in aqueous solution, draw 10, 50, 100, 200, 500, and 1000 μl of pure furfural solution into 100.0ml volumetric flasks respectively, add mobile phase to the mark, and shake well , to get the furfural standard series, respectively containing furfural 0.16, 0.58, 1.16, 2.32, 5.8, 11.6mg / ml; the standard curve regression equation obtained is

[0028] y=4247272.6203x+152310.3247

[0029] R 2 =0.9999

[0030] The correlation coefficient meets the requirements, and the standard curve is shown in the att...

Embodiment 2

[0040] (1) Sampling: From the furfural production workshop, connect the sampler to the sampling port, open the cooling water valve, and open the aldehyde vapor sampling valve after passing the cooling water. After the aldehyde vapor is condensed, it is collected in the sampling cup and discarded before 1 minute sample, collect 80ml of sample after 1 minute, for the determination of furfural content.

[0041] (2) Preparation of standard sample: According to the solubility of furfural in aqueous solution, draw 1000 μl of pure furfural solution into a 100.0ml volumetric flask, add mobile phase to the mark, and shake well to obtain a furfural standard sample of 11.6 mg / ml.

[0042] (3) Liquid phase system: chromatographic column: BIO RAD Aminex HPX-87H (300*7.8mm); mobile phase: 0.005mol sulfuric acid solution; flow rate: 0.600mL / min; column temperature: 60°C; differential detector temperature: 45 ℃;

[0043] (4) Sample treatment: Use a refractometer to measure the concentration ...

Embodiment 3

[0055] The difference from Example 2 is that the mobile phase used is a sulfuric acid solution of 0.01mol / L; the detection column temperature is 55°C, and the temperature of the differential detector is 40°C; the resulting standard sample peak area is 55241030, and the sample peak area is 41902863 , the sample concentration is

[0056] C=41902863×11.6×10÷55241030=87.9913 mg / ml.

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Abstract

The invention provides a method for rapidly measuring the content of furfural by a high performance liquid chromatography. A chromatographic column adopted by the method is a polystyrene divinylbenzene resin chromatographic column; a mobile phase of the column is a sulfuric acid solution; the concentration of the sulfuric acid solution is 0.001-0.01mol / L; the detection temperature of the column is 55-65 DEG C; and the temperature of a differential detector is 40-55 DEG C. The method is high in measuring speed, can rapidly measure the content and the concentration of furfural in aldehyde steam, and can be used for semifinished product production control, and for guiding judgment of a reaction end point in a dehydration and cyclization technological process.

Description

technical field [0001] The invention relates to a method for quickly measuring furfural content by high performance liquid chromatography. Background technique [0002] Furfural is an important organic chemical raw material and chemical solvent widely used in petroleum industry, chemical industry, medicine, food, synthetic rubber, synthetic resin and other industries. Furfural, also known as furan formaldehyde, is a colorless and transparent liquid at room temperature, and has a bitter almond smell, and the industrial product is slightly pale yellow. It is easy to turn black in the air. The molecular weight is 96.09, the specific gravity is 1.16, and the melting point is -36.67°C. The boiling point is 161.67°C, the relative density is 1.1596 (20°C), the ignition point is 393°C, and the critical pressure is 5.5MPa. [0003] At present, there are sulfuric acid method, acetic acid method, hydrochloric acid method and inorganic salt method in the world to produce furfural. U...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/34G01N30/60G01N30/06
Inventor 王萍刘阳肖林覃树林崔艳
Owner SHANDONG LONGLIVE BIO TECH CO LTD
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