CN106442863A - Method for measuring content of furfural in corncobs - Google Patents
Method for measuring content of furfural in corncobs Download PDFInfo
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- CN106442863A CN106442863A CN201610913631.1A CN201610913631A CN106442863A CN 106442863 A CN106442863 A CN 106442863A CN 201610913631 A CN201610913631 A CN 201610913631A CN 106442863 A CN106442863 A CN 106442863A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
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Abstract
The invention relates to the technical field of biomass measurement, in particular to a method for measuring the content of furfural in corncobs. The method comprises the following steps: firstly, obtaining distillate of furfural and a to-be-measured liquid of a sample; then, measuring the content of furfural: the to-be-measured liquid is sucked with a pipette and put in a ground conical flask, ice water is added, a sodium bromate-sodium bromide solution is added when the temperature of a solution in the conical flask drops to 0 DEG C, the conical flask is corked quickly and placed in the dark for a period of time, a potassium iodide solution is added to the conical flask when the temperature of the solution is still kept at 0 DEG C, the conical flask is corked again and evenly shaken, a sodium thiosulfate solution is used for titration after placement for a period of time, a starch solution is added when the solution in the flask becomes light yellow, and titration is performed continuously until blue disappears; finally, a hydrochloric acid solution is sucked additionally, a blank test is performed in accordance with the operation, and a result is computed. The method is simple to operate and provides a detection basis for judgment of the quality of raw materials of the corncobs used in the furfural industry.
Description
Technical field
The present invention relates to living beings determination techniques field, the detection side of furfural content in more particularly to a kind of corncob
Method.
Background technology
Furfural, also known as furtural, are a kind of colourless to amber transparent oily liquids.The chemical property of furfural is active,
Numerous derivatives can be prepared by reactions such as oxidation, condensations, be a kind of important organic chemical industry's intermediate, be widely used in
The industry such as casting auxiliary material, synthetic plastic, medicine, agricultural chemicals；Furfural is fabulous organic solvent, for refining senior lubricant and bavin
Oil.Furfural has certain application in perfume synthesis, synthetic fibers and food additives field simultaneously；Furfural is by pentosan
Hydrolysis generates pentose under the action of an acid, then is formed by dehydration of pentoses cyclisation；The primary raw material producing furfural is corncob, corn
The agricultural wastes such as stalk；Furfural industry is GB/T 1926.1-2009 to the detection foundation of furfural product quality indicator at present,
And judging that the content of furfural in corncob does not have detection method, in corncob, the number of furfural content is that corncob quality is sentenced
One of disconnected index, its furfural content is higher, and corncob quality is better, and then prepares the unit consumption meeting of furfural using corncob hydrolysis
Low, single pot of yield height of furfural, and in corncob, furfural content assay method does not have the standard of unified standard it is impossible to learn corn
Furfural content in core, so the quality for corncob quality does not have reliable data to judge.Therefore how to design one kind
In detection corncob, the method for furfural content becomes the problem of this area urgent need to resolve.
Content of the invention
The present invention be directed to the deficiencies in the prior art it is proposed that in a kind of corncob furfural content detection method, the method
Easy and simple to handle, accurately, the Quality estimation of the corncob raw material using for furfural industry provides a kind of detection foundation to testing result.
For solving above-mentioned technical problem, the technical scheme that the present invention takes is：
The detection method of furfural content in a kind of corncob, according to embodiments of the invention, comprises the following steps：Step one：Chaff
The distillation of aldehyde：Weigh dry corncob sample 0.5g, be accurate to 0.1mg, insert in 500mL round-bottomed flask, add 10g chlorination
Sodium, installs condenser and separatory funnel, the hydrochloric acid 30mL of addition 12% is in described flask from separatory funnel on described flask
Distilled, to when altogether steaming 300mL distillate, checked whether the furfural in described sample has distilled with aniline acetate solution
Entirely, such as occur without redness then it represents that distillation finishes；
Step 2：Obtain sample prepare liquid：Distillate described in step one is moved in 500mL volumetric flask, molten with 12% hydrochloric acid
Liquid washs receiving bottle, and whole washing lotions are poured in described volumetric flask, is diluted to scale with 12% hydrochloric acid solution, after fully shaking up
Obtain prepare liquid；
Step 3：The mensure of furfural：With prepare liquid described in pipette, extract 40mL in 250mL ground conical flask, add 50g ice
Water, when the solution temperature in described conical flask is down to 0 DEG C, adds 5.0mL sodium bromate-sodium bromide solution, stoppers bottle stopper rapidly,
In the dark place a period of time, now when described solution temperature remains at 0 DEG C, add 2mL10% liquor kalii iodide in
In conical flask, again stopper bottle stopper and shake up, then place a period of time after titrated with 0.1mol/L hypo solution, when
When solution is changed into light yellow in bottle, add 0.5% starch solution 3mL, till continuing to be titrated to blue disappearance, finally separately draw 12%
Hydrochloric acid solution 40mL, enters line blank test by aforesaid operations；
Step 4：Result calculates：Computing formula is, wherein, X is in institute's test specimens
Furfural content, be expressed as %；The 0.1mol/L sodium thiosulfate standard solution volume that V1 is consumed by above-mentioned blank test, single
Position is mL；The 0.1mol/L sodium thiosulfate standard solution volume that V2 is consumed by described sample, unit is mL；C is thio sulphur
Sour sodium standard solution concentration, unit is mol/L；M is the absolute dry mass of described sample, and unit is g；0.048 is thio with 1.0mL
The suitable furfural quality of sulfuric acid sodium standard solution, 500 is coefficient.
According to embodiments of the invention, described step one also includes measuring the moisture of described sample it is preferred that adopting GB/
T1926.1-2009 is measured.
According to embodiments of the invention, the distillation speed in described step one distills out 30mL distillate for every 10min.
According to embodiments of the invention, described frozen water is made with distilled water, and described standing time is 5min.
Could be aware that from above-mentioned technical scheme, the beneficial effects of the present invention is：The method is easy and simple to handle, testing result
Accurately, the Quality estimation of the corncob raw material using for furfural industry provides a kind of detection foundation.
Specific embodiment
In order that those skilled in the art more fully understand technical scheme, with reference to specific embodiment to this
Invention is described in further detail.In general, the invention provides in a kind of corncob furfural content detection method, under
Face illustrates the feature of the present invention by the example below.
The invention provides in a kind of corncob furfural content detection method, according to embodiments of the invention, it is concrete
Step is as follows：
Step one：The distillation of furfural：Weigh dry corncob sample 0.5g, be accurate to 0.1mg, insert 500mL round-bottomed flask
In, separately take described sample to be measured moisture therein using GB/T1926.1-2009 simultaneously；Then add to described flask
10g sodium chloride, installs condenser and separatory funnel, the hydrochloric acid 30mL of addition 12% is in institute from separatory funnel on described flask
State and distilled in flask it is preferred that distillation speed distills out 30mL distillate for every 10min, evaporate to altogether steaming 300mL
When going out liquid, checking whether the furfural in described sample distills completely with aniline acetate solution, such as occurring without redness then it represents that distilling
Finish；
Step 2：Obtain sample prepare liquid：Distillate described in step one is moved in 500mL volumetric flask, molten with 12% hydrochloric acid
Liquid washs receiving bottle, and whole washing lotions are poured in described volumetric flask, is diluted to scale with 12% hydrochloric acid solution, after fully shaking up
Obtain prepare liquid；
Step 3：The mensure of furfural：With prepare liquid described in pipette, extract 40mL in 250mL ground conical flask, 50g is added to use
The frozen water that distilled water is made, when the solution temperature in described conical flask is down to 0 DEG C, adds 5.0mL sodium bromate-sodium bromide molten
Liquid, stoppers rapidly bottle stopper, places 5min in the dark, now when described solution temperature remains at 0 DEG C, adds 2mL10%
Liquor kalii iodide, in conical flask, again stoppers bottle stopper and shakes up, then is entered with 0.1mol/L hypo solution after placing 5min
Row titration, when solution is changed into light yellow in bottle, adds 0.5% starch solution 3mL, till continuing to be titrated to blue disappearance, finally
Another absorption 12% hydrochloric acid solution 40mL, enters line blank test by aforesaid operations；
Step 4：Result calculates：Computing formula is, wherein, X is in institute's test specimens
Furfural content, be expressed as %；The 0.1mol/L sodium thiosulfate standard solution volume that V1 is consumed by above-mentioned blank test, single
Position is mL；The 0.1mol/L sodium thiosulfate standard solution volume that V2 is consumed by described sample, unit is mL；C is thio sulphur
Sour sodium standard solution concentration, unit is mol/L；M is the absolute dry mass of described sample, and unit is g；0.048 is thio with 1.0mL
The suitable furfural quality of sulfuric acid sodium standard solution, 500 is coefficient.
Embodiment 1：Weigh dry corncob sample 0.5045g, be accurate to 0.1mg, separately materials by GB/ simultaneously
T1926.1-2009 measures moisture, inserts in 500mL round-bottomed flask, adds 10g sodium chloride, loads onto condenser on described flask
And separatory funnel, distillation speed distills out 30mL distillate for every 10min, add from separatory funnel 12% hydrochloric acid 30mL in
In described flask, to when altogether distilling out 300mL distillate, whether distill completely with aniline acetate solution inspection furfural, if not
Occur red then it represents that distillation finishes.
Distillate is moved in 500mL volumetric flask, washs receiving bottle with a small amount of 12% hydrochloric acid solution, and whole washing lotions are fallen
Enter in volumetric flask, scale is diluted to 12% hydrochloric acid solution, after fully shaking up, obtain prepare liquid.
With pipette, extract 40mL prepare liquid in 250mL ground conical flask, add the frozen water that 50g distilled water is made,
When solution temperature is down to 0 DEG C in conical flask, adds 5.0mL sodium bromate-sodium bromide solution, stopper rapidly bottle stopper, put in the dark
Put 5min, now solution temperature remains at 0 DEG C, add 2mL10% liquor kalii iodide in conical flask, again stopper bottle stopper and shake
Even, place 5min 0.1mol/L hypo solution and titrate, when solution is changed into light yellow, add 0.5% starch solution
3mL, continues till being titrated to blue disappearance；Finally separately draw 12% hydrochloric acid solution 40mL, enter line blank test by aforesaid operations.
Recording sample moisture is 9.3%, V1=5.40mL, V2=3.23mL, is calculated furfural content through described computing formula
For 25.81%, concrete calculating process is as follows：
.
Embodiment 2：Weigh dry corncob sample 0.5082g, be accurate to 0.1mg, separately materials by GB/ simultaneously
T1926.1-2009 measures moisture, inserts in 500mL round-bottomed flask, adds 10g sodium chloride, loads onto condenser on described flask
And separatory funnel, distillation speed distills out 30mL distillate for every 10min, add from separatory funnel 12% hydrochloric acid 30mL in
In described flask, to when altogether distilling out 300mL distillate, whether distill completely with aniline acetate solution inspection furfural, if not
Occur red then it represents that distillation finishes.
Distillate is moved in 500mL volumetric flask, washs receiving bottle with a small amount of 12% hydrochloric acid solution, and whole washing lotions are fallen
Enter in volumetric flask, scale is diluted to 12% hydrochloric acid solution, after fully shaking up, obtain prepare liquid.
With pipette, extract 40mL prepare liquid in 250mL ground conical flask, add the frozen water that 50g distilled water is made,
When solution temperature is down to 0 DEG C in conical flask, adds 5.0mL sodium bromate-sodium bromide solution, stopper rapidly bottle stopper, put in the dark
Put 5min, now solution temperature remains at 0 DEG C, add 2mL10% liquor kalii iodide in conical flask, again stopper bottle stopper and shake
Even, place 5min 0.1mol/L hypo solution and titrate, when solution is changed into light yellow, add 0.5% starch solution
3mL, continues till being titrated to blue disappearance；Finally separately draw 12% hydrochloric acid solution 40mL, enter line blank test by aforesaid operations.
Recording sample moisture is 33%, V1=5.40mL, V2=3.70mL, being calculated furfural content through described computing formula is
20.07%, concrete calculating process is as follows：
.
Embodiment 3：Weigh dry corncob sample 0.5128g, be accurate to 0.1mg, separately materials by GB/ simultaneously
T1926.1-2009 measures moisture, inserts in 500mL round-bottomed flask, adds 10g sodium chloride, loads onto condenser on described flask
And separatory funnel, distillation speed distills out 30mL distillate for every 10min, add from separatory funnel 12% hydrochloric acid 30mL in
In described flask, to when altogether distilling out 300mL distillate, whether distill completely with aniline acetate solution inspection furfural, if not
Occur red then it represents that distillation finishes.
Distillate is moved in 500mL volumetric flask, washs receiving bottle with a small amount of 12% hydrochloric acid solution, and whole washing lotions are fallen
Enter in volumetric flask, scale is diluted to 12% hydrochloric acid solution, after fully shaking up, obtain prepare liquid.
With pipette, extract 40mL prepare liquid in 250mL ground conical flask, add the frozen water that 50g distilled water is made,
When solution temperature is down to 0 DEG C in conical flask, adds 5.0mL sodium bromate-sodium bromide solution, stopper rapidly bottle stopper, put in the dark
Put 5min, now solution temperature remains at 0 DEG C, add 2mL10% liquor kalii iodide in conical flask, again stopper bottle stopper and shake
Even, place 5min 0.1mol/L hypo solution and titrate, when solution is changed into light yellow, add 0.5% starch solution
3mL, continues till being titrated to blue disappearance；Finally separately draw 12% hydrochloric acid solution 40mL, enter line blank test by aforesaid operations.
Recording sample moisture is 48.6%, V1=5.40mL, V2=3.0mL, is calculated furfural content through described computing formula
For 28.08%, concrete calculating process is as follows：
.
The beneficial effects of the present invention is：The method is easy and simple to handle, and testing result accurately, is the corn that furfural industry uses
The Quality estimation of core raw material provides a kind of detection foundation.
Above the detection method of furfural content in a kind of corncob provided by the present invention is described in detail, herein
In apply embodiment the step of the application be set forth, the explanation of above example is only intended to help and understands the application
Method and its core concept；Simultaneously for one of ordinary skill in the art, according to the thought of the application, it is being embodied as
All will change in mode and range of application, in sum, this specification content should not be construed as the restriction to the application.
Claims (4)
1. in a kind of corncob the detection method of furfural content it is characterised in that comprising the following steps：
Step one：The distillation of furfural：Weigh dry corncob sample 0.5g, be accurate to 0.1mg, insert 500mL round-bottomed flask
In, add 10g sodium chloride, condenser and separatory funnel are installed on described flask, add 12% hydrochloric acid from separatory funnel
30mL is distilled in described flask, to when altogether steaming 300mL distillate, is checked in described sample with aniline acetate solution
Furfural whether distill completely, such as occur without redness then it represents that distillation finish；
Step 2：Obtain sample prepare liquid：Distillate described in step one is moved in 500mL volumetric flask, molten with 12% hydrochloric acid
Liquid washs receiving bottle, and whole washing lotions are poured in described volumetric flask, is diluted to scale with 12% hydrochloric acid solution, after fully shaking up
Obtain prepare liquid；
Step 3：The mensure of furfural：With prepare liquid described in pipette, extract 40mL in 250mL ground conical flask, add 50g ice
Water, when the solution temperature in described conical flask is down to 0 DEG C, adds 5.0mL sodium bromate-sodium bromide solution, stoppers bottle stopper rapidly,
In the dark place a period of time, now when described solution temperature remains at 0 DEG C, add 2mL10% liquor kalii iodide in
In conical flask, again stopper bottle stopper and shake up, then place a period of time after titrated with 0.1mol/L hypo solution, when
When solution is changed into light yellow in bottle, add 0.5% starch solution 3mL, till continuing to be titrated to blue disappearance, finally separately draw 12%
Hydrochloric acid solution 40mL, enters line blank test by aforesaid operations；
Step 4：Result calculates：Computing formula is, wherein, X is in institute's test specimens
Furfural content, be expressed as %；The 0.1mol/L sodium thiosulfate standard solution volume that V1 is consumed by above-mentioned blank test, single
Position is mL；The 0.1mol/L sodium thiosulfate standard solution volume that V2 is consumed by described sample, unit is mL；C is thio sulphur
Sour sodium standard solution concentration, unit is mol/L；M is the absolute dry mass of described sample, and unit is g；0.048 is thio with 1.0mL
The suitable furfural quality of sulfuric acid sodium standard solution, 500 is coefficient.
2. in corncob according to claim 1 the detection method of furfural content it is characterised in that described step one is also wrapped
Include the moisture measuring described sample it is preferred that being measured using GB/T1926.1-2009.
3. in corncob according to claim 1 the detection method of furfural content it is characterised in that in described step one
Distillation speed distills out 30mL distillate for every 10min.
4. in corncob according to claim 1 furfural content detection method it is characterised in that described frozen water distillation
Water is made, and described standing time is 5min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610913631.1A CN106442863A (en) | 2016-10-20 | 2016-10-20 | Method for measuring content of furfural in corncobs |
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| CN201610913631.1A CN106442863A (en) | 2016-10-20 | 2016-10-20 | Method for measuring content of furfural in corncobs |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110823751A (en) * | 2019-11-11 | 2020-02-21 | 安徽理工大学 | Method for determining content of catalyst sodium bisulfate in furfural residues |
-
2016
- 2016-10-20 CN CN201610913631.1A patent/CN106442863A/en active Pending
Non-Patent Citations (6)
| Title |
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| 中华人民共和国国家质量监督检验检疫总局等: "GB/T1926.1-2009 工业糠醛", 《中华人民共和国标准》 * |
| 吴树新等: "固体酸催化剂SO42-/TiO2催化木糖脱水制备糠醛的新方法", 《河北师范大学学报自然科学版》 * |
| 吴楠等: "《制浆造纸厂化验室化验检验方法》", 30 June 2009, 中国轻工业出版社 * |
| 岳丽清等: "三苯基磷在玉米芯制备糠醛中的应用", 《化工进展》 * |
| 李凭力: "木糖制备糠醛的工艺", 《化学工业与工程》 * |
| 贾眉等: "三种化学分析法测定糠醛含量试验", 《林产化学与工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110823751A (en) * | 2019-11-11 | 2020-02-21 | 安徽理工大学 | Method for determining content of catalyst sodium bisulfate in furfural residues |
| CN110823751B (en) * | 2019-11-11 | 2021-12-24 | 安徽理工大学 | Method for determining content of catalyst sodium bisulfate in furfural residues |
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