CN103487536A - Method for rapidly measuring content of furfural by high performance liquid chromatography - Google Patents
Method for rapidly measuring content of furfural by high performance liquid chromatography Download PDFInfo
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- CN103487536A CN103487536A CN201310450879.5A CN201310450879A CN103487536A CN 103487536 A CN103487536 A CN 103487536A CN 201310450879 A CN201310450879 A CN 201310450879A CN 103487536 A CN103487536 A CN 103487536A
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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
The present invention relates to the method for high-efficient liquid phase color spectrum quick test furfural content.
Background technology
Furfural is a kind of important Organic Chemicals and chemical solvent that is widely used in the industries such as petroleum industry, chemical industry, medicine, food and synthetic rubber, synthetic resin.Furfural has another name called furtural, under normal temperature, is water white liquid, and the semen armeniacae amarae flavor is arranged, and it is faint yellow that industrial goods show slightly.Easily blackening in air.Molecular weight 96.09, proportion 1.16, fusing point-36.67 ℃.161.67 ℃ of boiling points, relative density 1.1596(20 ℃), 393 ℃ of burning-points, emergent pressure 5.5MPa.
The method of producing in the world furfural at present has sulfuric acid process, method of acetic acid, salt acid system, inorganic salts method.Take plant as raw material, is current unique industrialized preparing process through acidic hydrolysis furfural processed.China furfural production producer 95% adopts the sulfuric acid catalysis method.At present, acidic hydrolysis is produced furfural technique and is divided single stage method and two-step approach, and development two-step approach furfural production technology, be the inevitable development trend of furfurol industry.No matter be single stage method or two-step approach, the yield of furfural is the highest can only reach 70% left and right, and some technical matterss need to be studied and explore.Therefore furfural production technology also needs further improvement, and in this development in the furfural semi-manufacture mensuration of furfural content be absolutely necessary.
At present, the production technology of furfural mainly contains traditional one-step technology and just started in recent years and explores, and studies hotter two-step approach production technology.No matter be the one-step method production process that pentosan hydralysis and cyclodehydration one step complete, still first hydrolysis, the two-step approach production technology of cyclodehydration again after the separation of slag liquid.Gained aldehyde vapour condensed fluid is acidic materials.How furfural content in aldehyde vapour condensed fluid is carried out to Fast Measurement, judge the terminal of cyclodehydration with measurement result, and then guidance production is an important subject in this field.The assay method of furfural content mainly contains traditional titrimetry, vapor-phase chromatography, high pressure liquid chromatography C18 post method.But the titrimetry complex steps, use duration, Fast Measurement is to instruct actual production in time; Although the vapor-phase chromatography speed, because furfural semi-manufacture (aldehyde vapour condensed fluid) acidity is high, to the gas chromatographic column seriously corroded, can not be used and poor stability for a long time; High pressure liquid chromatography C18 post method must adopt organic mobile phase that is dissolved as that volatility is stronger that certain toxicity is arranged, and long-term use is larger to laboratory and personnel's harm, and, because sample acidity is large, chromatographic column filler runs off serious, and serviceable life is short.
Summary of the invention
In order to overcome the above problems this patent, to have invented a kind of acid resistance of selecting strong, the HPX-87H Hydrogen post of stable, long service life, prepare the diluted acid mobile phase that a kind of volatility is little, and sample is carried out to fast processing can be simultaneously for furfural semi-manufacture and finished product content, carry out the detection method of fast accurate mensuration.
The method of high-efficient liquid phase color spectrum quick test furfural content, step comprises that making, liquid phase systems, the Sample Dilution of sampling, typical curve are processed and loading is measured, the chromatographic column that the method adopts is polystyrene divinylbenzene resin chromatography post, the post mobile phase is sulfuric acid solution, the sampler of sample liquid band cooling tube obtains, and mobile phase is diluted sample as sample diluting liquid; Described sulfuric acid solution concentration is 0.001-0.01mol/L, and the detection column temperature is 55-65 ℃, differential detector temperature: 40-55 ℃.
Described sulfuric acid solution preferred concentration is 0.005mol/L.
The preferred column temperature of described detection is 60 ℃.
The preferred temperature of described differential detecting device is 45 ℃.
The step of this detection method that following the present invention adopts.
(1) sampling: the cyclodehydration operation in suitability for industrialized production, at cyclodehydration tank aldehyde steam pipe road design aldehyde vapour sample tap.During sampling, first sampler is connected with sample tap, opens water quench, after opening aldehyde vapour sample cock and making the condensation of aldehyde vapour, be collected in sampling cup, discard first 1 minute sample in cup, collect after 1 minute more than sample 50ml, for the mensuration of furfural content.
(2) making of typical curve: the solubleness according to furfural in aqueous solution, use liquid chromatogram mobile phase to prepare the furfural standard solution of a series of concentration, cross 0.2um-0.5um organic film, in preparation, machine is measured, the drawing standard curve.Draw regression equation, and related coefficient.
(3) liquid phase systems:
Polystyrene divinylbenzene resin chromatography post: BIO RAD Aminex HPX-87H(300*7.8mm); Mobile phase: 0.005mol sulfuric acid solution; Flow velocity: 0.600mL/min; Column temperature: 60 ℃; Differential detector temperature: 45 ℃; Sampling volume is 20 μ L
(4) sample preparation: with refractometer, furfural content in sample is carried out to thick side, add the mobile phase dilution, by certain extension rate, sample is diluted, control furfural content in 1% effect, accurately record extension rate.Cross the 0.2um organic film after dilution, in preparation, machine is measured.
(5) upper machine is measured: after chromatogram is stable, the sample feeding volume is 20 μ L, is measured, and calculates content.
The present invention is a kind of method for Fast Measurement furfural finished product, semi-manufacture furfural content, has the following advantages:
(1) high performance liquid chromatography HPX-87H method is measured the content of furfural in the furfural semi-manufacture, mobile phase used is the 0.005M aqueous sulfuric acid, with vapor-phase chromatography and high performance liquid chromatography C18 post method, compares, and operates fairly simple, good stability, and mobile phase cleanliness without any pollution.
(2) high performance liquid chromatography HPX-87H method chromatographic column is durable in use, belongs to sour post, is applicable to measuring the sample containing acid, can effectively detect the content of furfural in the furfural semi-manufacture.
(3) the method finding speed is fast, but furfural content and concentration in Fast Measurement aldehyde vapour can be used for the semi-manufacture production control, instruct the judgement of reaction end in the cyclodehydration technological process.
(4) in typical curve preparation and Sample Dilution process, dilution is all used the mobile phase under the current color spectral condition, has avoided the appearance of solvent peak, has reduced the impact of solvent peak on each component characteristics peak in sample, detects data more accurate.
The accompanying drawing explanation
The typical curve of Fig. 1 embodiment of the present invention;
The HPLC collection of illustrative plates that Fig. 2 furfural detects; Numeral material appearance time wherein, the highest peak value is furfural sample liquid peak value.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
(1) sampling: from the furfural production workshop, sampler is connected with sample tap, opens cooling water valve, open aldehyde vapour sample cock after logical chilled water, aldehyde vapour, after condensation, is collected in sampling cup, discard first 1 minute sample in cup, collect sample 50ml after 1 minute, for the mensuration of furfural content.
(2) making of typical curve: the solubleness according to furfural in aqueous solution, draw respectively furfural sterling solution 10,50,100,200,500,1000 μ l in the 100.0ml volumetric flask, respectively add mobile phase to scale, after shaking up, obtain the furfural standard series, respectively containing furfural 0.16,0.58,1.16,2.32,5.8,11.6mg/ml; The typical curve regression equation that obtains surveying is
y=4247272.6203x+152310.3247
R
2=0.9999
Related coefficient meets the demands, and typical curve is shown in accompanying drawing 1.
(3) liquid phase systems: chromatographic column: BIO RAD Aminex HPX-87H(300*7.8mm); Mobile phase: 0.005mol sulfuric acid solution; Flow velocity: 0.600mL/min; Column temperature: 60 ℃; Differential detector temperature: 45 ℃;
(4) sample preparation: with refractometer, furfural content in sample is carried out to thick side, measure furfural content greatly about 10% left and right, add 10 times of mobile phase dilutions.Cross the 0.2um organic film after dilution, in preparation, machine is measured.
(5) upper machine is measured: after chromatogram is stable, the sample feeding volume is 20 μ L, is measured, and calculates content.
The HPLC testing result is as follows, and spectrogram is shown in accompanying drawing 2.
Working sample peak area y=41982870, according to regression equation y=4247272.6203x+152310.3247
Calculating concentration x=8.84885mg/ml;
The Sample Dilution multiple is 10 times, so these semi-manufacture furfural content is 88.4885mg/ml.
(1) sampling: from the furfural production workshop, sampler is connected with sample tap, opens cooling water valve, open aldehyde vapour sample cock after logical chilled water, aldehyde vapour, after condensation, is collected in sampling cup, discard first 1 minute sample in cup, collect sample 80ml after 1 minute, for the mensuration of furfural content.
(2) standard sample is made: the solubleness according to furfural in aqueous solution, draw furfural sterling solution 1000 μ l in the 100.0ml volumetric flask, and add mobile phase to scale, after shaking up, obtain furfural standard sample 11.6mg/ml.
(3) liquid phase systems: chromatographic column: BIO RAD Aminex HPX-87H(300*7.8mm); Mobile phase: 0.005mol sulfuric acid solution; Flow velocity: 0.600mL/min; Column temperature: 60 ℃; Differential detector temperature: 45 ℃;
(4) processing of sample: with refractometer, furfural content in sample is carried out to thick side, measure furfural content greatly about 10% left and right, add 10 times of mobile phase dilutions.Cross the 0.2um organic film after dilution, in preparation, machine is measured.
(5) upper machine is measured: after chromatogram is stable, the sample feeding volume is 20 μ L, is measured, and calculates content.
The standard specimen peak area of surveying is 55341050, and the sample peak area is 41982860, is calculated as follows:
In formula: C
samplethe content of furfural in-furfural semi-manufacture, unit: mg/mL;
C
markthe content of furfural in-standard specimen, unit: mg/mL;
A
samplethe chromatographic peak area of furfural in-furfural semi-manufacture;
A
markthe chromatographic peak area of furfural in-standard specimen;
The half-finished dilution gfactor of f-furfural.
, the concentration of sample is
C=41982860×11.6×10÷55341050=87.9999mg/ml。
Embodiment 3
From the different of embodiment 2, be: the sulfuric acid solution that the mobile phase that is employing is 0.01mol/L; Detecting column temperature is 55 ℃, 40 ℃ of differential detector temperatures, and the standard specimen peak area of gained is 55241030, and the sample peak area is 41902863, and sample concentration is
C=41902863×11.6×10÷55241030=87.9913mg/ml。
From the different of embodiment 2, be: the sulfuric acid solution that the mobile phase that is employing is 0.001mol/L; Detecting column temperature is 65 ℃, 55 ℃ of differential detector temperatures, and the standard specimen peak area of gained is 55243030, and the sample peak area is 41963863, and sample concentration is
C=41963863×11.6×10÷55243030=88.116mg/ml。
Claims (4)
1. the method for high-efficient liquid phase color spectrum quick test furfural content, step comprises that making, liquid phase systems, the Sample Dilution of sampling, typical curve are processed and loading is measured, it is characterized in that: the chromatographic column that the method adopts is polystyrene divinylbenzene resin chromatography post, the post mobile phase is sulfuric acid solution, the sampler of sample liquid band cooling tube obtains, and mobile phase is diluted sample as sample diluting liquid; Described sulfuric acid solution concentration is 0.001-0.01mol/L, and the detection column temperature is 55-65 ℃, differential detector temperature: 40-55 ℃.
2. the method for claim 1, it is characterized in that: described sulfuric acid solution concentration is 0.005mol/L.
3. the method for claim 1, it is characterized in that: described detection column temperature is 60 ℃.
4. the method for claim 1, it is characterized in that: described differential detector temperature is 45 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104122343A (en) * | 2014-07-07 | 2014-10-29 | 河南省科学院能源研究所有限公司 | Method for gas chromatographic quantitative detection on furfural prepared through hydrochloric acid method |
| CN104614451A (en) * | 2014-12-08 | 2015-05-13 | 宁波北仑大港科技创新服务中心 | Methyl 3-(2-(2-hydroxyethoxy)ethoxy)propanoate modification agent detection method |
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| WO2013102027A1 (en) * | 2011-12-28 | 2013-07-04 | E. I. Du Pont De Nemours And Company | Process for the production of furfural |
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| JPH04337456A (en) * | 1991-05-15 | 1992-11-25 | Meidensha Corp | Method for analyzing furan and furan derivative |
| WO2013102027A1 (en) * | 2011-12-28 | 2013-07-04 | E. I. Du Pont De Nemours And Company | Process for the production of furfural |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104122343A (en) * | 2014-07-07 | 2014-10-29 | 河南省科学院能源研究所有限公司 | Method for gas chromatographic quantitative detection on furfural prepared through hydrochloric acid method |
| CN104122343B (en) * | 2014-07-07 | 2016-02-24 | 河南省科学院能源研究所有限公司 | A kind of gas chromatography quantitative detecting method to furfural prepared by hydrochloric acid method |
| CN104614451A (en) * | 2014-12-08 | 2015-05-13 | 宁波北仑大港科技创新服务中心 | Methyl 3-(2-(2-hydroxyethoxy)ethoxy)propanoate modification agent detection method |
| CN104614451B (en) * | 2014-12-08 | 2016-08-17 | 宁波北仑大港科技创新服务中心 | A kind of diethylene glycol methyl propionate detection method |
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