CN103728410A - Measuring method for furfuraldehyde content of mixed solvent - Google Patents
Measuring method for furfuraldehyde content of mixed solvent Download PDFInfo
- Publication number
- CN103728410A CN103728410A CN201310644623.8A CN201310644623A CN103728410A CN 103728410 A CN103728410 A CN 103728410A CN 201310644623 A CN201310644623 A CN 201310644623A CN 103728410 A CN103728410 A CN 103728410A
- Authority
- CN
- China
- Prior art keywords
- furfural
- mixed solvent
- sodium hydroxide
- solution
- furfuraldehyde
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a measuring method for the furfuraldehyde content of a mixed solvent. The method comprises the following steps: (1) weighing 1-2 grams of furfuraldehyde sample according to a mass decrement method; (2) putting the weighed furfuraldehyde sample into an iodine flask in which 30 mL of oxammonium hydrochloride alcohol solution is added; screwing the cork and shaking up; placing for 15 minutes (holding temperature of 20-25 DEG C) for sufficient reaction; (3) titrating sodium hydroxide standard solution of 0.25 mol/L with a blue line leather head burette to a standard color (the color of the original oxammonium hydrochloride alcohol solution); (4) refilling a drop of an indicator when the sodium hydroxide standard solution approaches to the titration end point in order to observe the titration end point conveniently; (5) calculating weight percentage composition of the furfuraldehyde W (%). The measuring method has the benefits as follows: the bromophenol blue indicator is selected; through observation of the colors of the solution, volume of the sodium hydroxide standard solution which is needed to drop in is calculated; the furfuraldehyde content of the mixed solvent can be obtained simply and conveniently by utilizing calculation formulas; error is relatively small.
Description
Technical field
The invention belongs to solvent analysis technical field, especially relate to the assay method of furfural content in a kind of mixed solvent.
Background technology
In existing technology, before using mixed solvent, need to measure furfural content in mixed solvent.If assay method is incorrect, can have a strong impact on the quality of mixed solvent, even affect its use.
Summary of the invention
The assay method that the object of this invention is to provide furfural content in a kind of mixed solvent, the method can be simple and direct, quick and precisely, is applicable in mixed solvent except furfural the mixed solvent that other components do not react with oxammonium hydrochloride.
Technical scheme of the present invention is: the assay method of furfural content in a kind of mixed solvent, adopt Hydrochloride Hydroxylamine Oximation method, and the total carbonyls recording calculates its weight percentage by furfural, and its chemical equation is:
Process following steps:
(1) adopt decrement method to take furfural sample 1～2 g;
(2) the furfural sample taking is put into be added with 30 mL oxammonium hydrochloride ethanolic solutions determine iodine flask, tighten bottle stopper, shake up, place 15 min(and keep 20～25 ℃ of temperature), treat abundant reaction;
(3) use blue line leather point buret titration 0.25 mol/L standard solution of sodium hydroxide till identical with standard colors (former oxammonium hydrochloride ethanolic solution color);
(4) for the ease of observing titration end-point, while approaching terminal, add one of indicator.
(5) result is calculated: furfural weight percentage W(%) by under formula, calculate:
In formula:
W--furfural weight percentage in mixed solvent, unit: %;
M--titration standard solution of sodium hydroxide volumetric molar concentration, unit: mol/L;
V--sample consumes standard solution of sodium hydroxide volume, unit: mL;
G--furfural example weight, unit: g;
0.09608--the grams of every mM furfural.
Further, in described step (1), the weight of furfural sample is accurate to 0.0002g.
Further, in described step (2), the capacity of determining iodine flask is 100ml.
Further, in described step (2), the compound method of oxammonium hydrochloride ethanolic solution is for dissolving 50 g oxammonium hydrochlorides in 1000 mL distilled water, add 1000 mL ethanol, add again bromophenol blue indicator 2.5 mL, shake up, with 0.25 mol/L standard solution of sodium hydroxide, be transferred to yellow green (pH3.7～3.8).
Further, 0.4 g bromophenol blue is got in being formulated as of described bromophenol blue indicator, is dissolved in the 100ml volumetric flask that is added with 12 mL sodium hydroxide solutions, and wherein sodium hydroxide solution volumetric molar concentration is 0.05mol/L, then is diluted to 100 mL with 4 g/L ethanol.
Further, 0.25 mol/L standard solution of sodium hydroxide in described step (4) is to prepare and demarcate with reference to GB 601 prescriptive procedures.
Advantage and good effect that the present invention has are: owing to adopting technique scheme, the method can simple and direct, quick and precisely be measured furfural content in mixed solvent, and error is less; Select bromophenol blue indicator, by observing the color of solution, and then draw the volume of the standard solution of sodium hydroxide that need to splash into, utilize computing formula can draw furfural content in mixed solvent, simple, convenient; Be convenient to observe titration end-point, when approaching terminal, add one of indicator, reduced measuring error.
Embodiment
Technical scheme of the present invention is: the assay method of furfural content in a kind of mixed solvent, adopt Hydrochloride Hydroxylamine Oximation method, furfural is reacted with oxammonium hydrochloride ethanolic solution, wherein take bromophenol blue as indicator, under optimal conditions, reacted solution splashes into standard solution of sodium hydroxide, its solution colour and standard colors (former oxammonium hydrochloride ethanolic solution color) compare, when both solution colours are identical, and then can calculate its weight percentage of furfural by the volumescope of standard solution of sodium hydroxide, be applicable in mixed solvent except furfural, the mixed solvent that other components do not react with oxammonium hydrochloride, its chemical equation is:
1. instrument
Common laboratory equipment and instrument:
Determine iodine flask: 100 mL; Blue line leather point buret: Xue Shi alkali formula, 50 mL; Volumetric flask: 100ml, 1500ml.
2. reagent and solution
(1) choose 95% ethanol (GB 679);
(2) preparation of bromophenol blue (HG 3-1224) indicator:
Take 0.4 g bromophenol blue, be dissolved in the 100ml volumetric flask that is added with 12 mL sodium hydroxide solutions, wherein the volumetric molar concentration of sodium hydroxide solution is 0.05 mol/L, then is diluted to 100 mL with 4 g/L ethanol.
(3) preparation of NaOH (GB 629):
With reference to GB 601 prescriptive procedures, prepare and demarcate, be mixed with 0.25 mol/L standard solution of sodium hydroxide.
(4) preparation of oxammonium hydrochloride (HG 3-967):
Take 50 g oxammonium hydrochlorides, be dissolved in the 1500ml volumetric flask that is added with 1000 mL distilled water, add 1000 mL ethanol, wherein the concentration of ethanol is 25 g/L, add again bromophenol blue indicator 2.5 mL, shake up, with 0.25 mol/L standard solution of sodium hydroxide, be transferred to yellow green (pH3.7～3.8).
3. test procedure
(1) adopt decrement method to take furfural sample 1～2 g;
(2) the furfural sample taking is put into be added with 30 mL oxammonium hydrochloride ethanolic solutions determine iodine flask, tighten bottle stopper, shake up, place 15 min(and keep 20～25 ℃ of temperature);
(3) use blue line leather point buret titration 0.25 mol/L standard solution of sodium hydroxide till identical with standard colors (former oxammonium hydrochloride ethanolic solution color);
(4) for the ease of observing titration end-point, while approaching terminal, add one of indicator.
4. result is calculated
Furfural weight percentage W(%) by under formula, calculate:
In formula:
W--furfural weight percentage in mixed solvent, unit: %;
M--titration standard solution of sodium hydroxide volumetric molar concentration, unit: mol/L;
V--sample consumes standard solution of sodium hydroxide volume, unit: mL;
G--furfural example weight, unit: g;
0.09608--the grams of every mM furfural.
5. furfural content detection example in mixed solvent:
In this table, list 6 groups of different pieces of informations of furfural in mixed solvent, phenol and dimethylbenzene, adopt this method, obtained respectively the content that furfural accounts for mixed solvent, specific as follows:
Experimental data shows, the furfural weight percentage error that adopts this method to measure is controlled at 0.005, shows the difference that this method does not have conspicuousness, and this method is feasible.
Above one embodiment of the present of invention are had been described in detail, but described content is only preferred embodiment of the present invention, can not be considered to for limiting practical range of the present invention.All equalization variations of doing according to the present patent application scope and improvement etc., within all should still belonging to patent covering scope of the present invention.
Claims (6)
1. an assay method for furfural content in mixed solvent, is characterized in that: adopt Hydrochloride Hydroxylamine Oximation method, the total carbonyls recording calculates its weight percentage by furfural, and its chemical equation is:
Process following steps:
(1) adopt decrement method to take furfural sample 1～2 g;
(2) the furfural sample taking is put into be added with 30 mL oxammonium hydrochloride ethanolic solutions determine iodine flask, tighten bottle stopper, shake up, place 15 min(and keep 20～25 ℃ of temperature), treat abundant reaction;
(3) use blue line leather point buret titration 0.25 mol/L standard solution of sodium hydroxide till identical with standard colors (former oxammonium hydrochloride ethanolic solution color);
(4) for the ease of observing titration end-point, while approaching terminal, add one of indicator;
(5) result is calculated: furfural weight percentage W(%) by under formula, calculate:
In formula:
W--furfural weight percentage in mixed solvent, unit: %;
M--titration standard solution of sodium hydroxide volumetric molar concentration, unit: mol/L;
V--sample consumes standard solution of sodium hydroxide volume, unit: mL;
G--furfural example weight, unit: g;
0.09608--the grams of every mM furfural.
2. the assay method of furfural content in a kind of mixed solvent according to claim 1, is characterized in that: in described step (1), the weight of furfural sample is accurate to 0.0002g.
3. the assay method of furfural content in a kind of mixed solvent according to claim 1, is characterized in that: 0.25 mol/L standard solution of sodium hydroxide in described step (4) is to prepare and demarcate with reference to GB 601 prescriptive procedures.
4. the assay method of furfural content in a kind of mixed solvent according to claim 1, is characterized in that: in described step (2), the capacity of determining iodine flask is 100ml.
5. the assay method of furfural content in a kind of mixed solvent according to claim 1, it is characterized in that: in described step (2), the compound method of oxammonium hydrochloride ethanolic solution is for dissolving 50 g oxammonium hydrochlorides in 1000 mL distilled water, add 1000 mL ethanol, add again bromophenol blue indicator 2.5 mL, shake up, with 0.25 mol/L standard solution of sodium hydroxide, be transferred to yellow green (pH3.7～3.8).
6. the assay method of furfural content in a kind of mixed solvent according to claim 5, it is characterized in that: 0.4 g bromophenol blue is got in being formulated as of described bromophenol blue indicator, be dissolved in the 100ml volumetric flask that is added with 12 mL sodium hydroxide solutions, wherein sodium hydroxide solution volumetric molar concentration is 0.05mol/L, then is diluted to 100 mL with 4 g/L ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310644623.8A CN103728410A (en) | 2013-12-05 | 2013-12-05 | Measuring method for furfuraldehyde content of mixed solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310644623.8A CN103728410A (en) | 2013-12-05 | 2013-12-05 | Measuring method for furfuraldehyde content of mixed solvent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103728410A true CN103728410A (en) | 2014-04-16 |
Family
ID=50452574
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310644623.8A Pending CN103728410A (en) | 2013-12-05 | 2013-12-05 | Measuring method for furfuraldehyde content of mixed solvent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103728410A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105300978A (en) * | 2015-11-18 | 2016-02-03 | 北京市政路桥建材集团有限公司 | Method for detecting whether warm mix asphalt contains oil-soluble amine surfactant warm mix agent |
| CN105754643A (en) * | 2014-12-19 | 2016-07-13 | 中国石油天然气股份有限公司 | Hydrocarbon oil type scale remover preparation method, hydrocarbon oil type scale remover and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4514503A (en) * | 1982-09-01 | 1985-04-30 | Morton Norwich Products | Reagent and process for detecting furfural in petroleum products |
| SU1665288A1 (en) * | 1989-04-11 | 1991-07-23 | Донецкий научный центр гигиены труда и профилактики травматизма | Method of analysis of furfuryl alcohol in air |
| CN1697971A (en) * | 2004-03-01 | 2005-11-16 | 三菱化学株式会社 | Method of determining impurity in acrylic acid |
| CN1790013A (en) * | 2004-12-16 | 2006-06-21 | 雅安三九药业有限公司 | Method for simultaneous determination of protocatechuic acid content and 5-hydroxymethyl furfural content in pulse-activating injection |
-
2013
- 2013-12-05 CN CN201310644623.8A patent/CN103728410A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4514503A (en) * | 1982-09-01 | 1985-04-30 | Morton Norwich Products | Reagent and process for detecting furfural in petroleum products |
| SU1665288A1 (en) * | 1989-04-11 | 1991-07-23 | Донецкий научный центр гигиены труда и профилактики травматизма | Method of analysis of furfuryl alcohol in air |
| CN1697971A (en) * | 2004-03-01 | 2005-11-16 | 三菱化学株式会社 | Method of determining impurity in acrylic acid |
| CN1790013A (en) * | 2004-12-16 | 2006-06-21 | 雅安三九药业有限公司 | Method for simultaneous determination of protocatechuic acid content and 5-hydroxymethyl furfural content in pulse-activating injection |
Non-Patent Citations (1)
| Title |
|---|
| 中国标准出版社: "《中国林业标准汇编 林产化工与林特产品卷》", 31 August 1998 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754643A (en) * | 2014-12-19 | 2016-07-13 | 中国石油天然气股份有限公司 | Hydrocarbon oil type scale remover preparation method, hydrocarbon oil type scale remover and application thereof |
| CN105754643B (en) * | 2014-12-19 | 2017-05-10 | 中国石油天然气股份有限公司 | Hydrocarbon oil type scale remover preparation method, hydrocarbon oil type scale remover and application thereof |
| CN105300978A (en) * | 2015-11-18 | 2016-02-03 | 北京市政路桥建材集团有限公司 | Method for detecting whether warm mix asphalt contains oil-soluble amine surfactant warm mix agent |
| CN105300978B (en) * | 2015-11-18 | 2018-02-09 | 北京市政路桥建材集团有限公司 | Containing oil soluble amine surfactants warm-mixing agent detection method in a kind of warm-mixed asphalt |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103115920B (en) | The assay method of iron calcium ratio in a kind of iron-calcium core-spun yarn | |
| CN102323133A (en) | Method for measuring total iron content in directly-reduced iron | |
| CN103344636A (en) | Method for determination of aluminum and alumina in steel slag | |
| CN104020157A (en) | Method for measuring elemental niobium content of titanium-niobium alloy | |
| CN103901018B (en) | Fireworks and firecrackers magnesium in pyrotechnic composition main constituent and aluminum content tests method | |
| CN103940946B (en) | A kind of gravimetric titrimetry device and titration method with titration protection assembly | |
| CN104198484A (en) | Method for testing fluorine content in solution | |
| CN108152444A (en) | Method for detecting content of free nitric acid in bismuth nitrate solution | |
| CN103344667B (en) | Lubricating oil moisture calorimetric titration rapid assay methods | |
| CN103728410A (en) | Measuring method for furfuraldehyde content of mixed solvent | |
| CN103645274B (en) | Measure the method for chloride ion content in cold-rolling emulsion | |
| CN104422685A (en) | Method for determining content of metal aluminum in ladle slag modifying agent | |
| CN103954729B (en) | A kind of method measuring acid number in oil-immersed power transformer insulating paper | |
| CN104713876A (en) | Method for determining free oxalic acid in mono-oxalate lithium borate | |
| CN108362824A (en) | The assay method of carbonate and bicarbonate radical in a kind of containing borate brine | |
| CN102288605A (en) | Method for rapidly determining iron content in concentrated sulphuric acid | |
| CN108267444A (en) | A kind of chelated acid is to the test method of the sequestering power of metal calcium ion | |
| CN101995381A (en) | Method for measuring cobalt in cobalt-containing material by using 5-Cl-PADAB photometry | |
| CN105866102B (en) | A method of lanthanum element content in lead or metal is measured with plasma emission spectrum | |
| CN109254111A (en) | A kind of detection method and preparation method thereof of Water soluble fertilizer nitrate nitrogen content | |
| CN102141562B (en) | Method for analyzing purity of 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration | |
| CN108226375A (en) | Boric acid assay method in aqueous solution containing boric acid and zinc sulfate | |
| CN103412028B (en) | Method for testing content of sodium oxide in silica sol | |
| CN104280368A (en) | Method for efficiently and accurately detecting main content of industrial magnesium oxide | |
| CN103592411B (en) | A kind of method of testing of capsule core release amount of concrete chemical self-repair microcapsule |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140416 |
|
| RJ01 | Rejection of invention patent application after publication |