CN107389673A - A kind of assay method of organic matter hydroxyl value and application - Google Patents
A kind of assay method of organic matter hydroxyl value and application Download PDFInfo
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- CN107389673A CN107389673A CN201710604822.4A CN201710604822A CN107389673A CN 107389673 A CN107389673 A CN 107389673A CN 201710604822 A CN201710604822 A CN 201710604822A CN 107389673 A CN107389673 A CN 107389673A
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Abstract
The invention provides a kind of assay method of organic matter hydroxyl value and application; the amount that by calculating organic matter the hydroxyl of acylation reaction occurs for the assay method of organic matter hydroxyl value of the present invention; to determine the hydroxyl value of organic matter; wherein acylation reaction is carried out by the way of being heated to reflux; and using funnel as reflux; water circulation type condensation reflux unit need not be used, significantly reduces the waste of water resource；Using funnel as reflux, the loss of material in reaction vessel will not substantially be caused, even if partial material is lost in reflux course, because the measure and blank assay of sample are to use identical method, identical operates, the loss of material tested twice is essentially identical, and the decrement of the dosage of used alkali lye is also essentially identical, and follow-up calculating is not had an impact；The assay method program of organic matter hydroxyl value of the present invention is simple, easy to operate, as a result accurately, and can reduce the wasting of resources, can be effective for the hydroxy value measuring of surfactant.
Description
Technical field
The present invention relates to organic matter hydroxy value measuring method and technology field, in particular to a kind of survey of organic matter hydroxyl value
Determine method and application.
Background technology
Hydroxyl value (Hydroxyl value) refers to the amount of the material of the oh group in 100g materials.And generally industrial use
Hydroxyl value refer to the milligram number of the suitable potassium hydroxide (KOH) of hydroxyl in hydroxyl value (Hydroxyl value) 1g samples, with
MgKOH/g is represented.
Surfactant (surfactant), referring to add can make the interface state of its solution system that obvious become occur on a small quantity
The material of change.With fixed hydrophilic lipophilic group, aligned in the surface energy of solution.The molecular structure tool of surfactant
Have amphipathic：One end is hydrophilic radical, and the other end is hydrophobic grouping；Hydrophilic radical is often polar group, such as carboxylic acid, sulfonic acid, sulphur
Acid, amino or amido and its salt, hydroxyl, amide groups, ehter bond etc. can also be used as polar hydrophilic group；And hydrophobic grouping is often non-pole
Property hydrocarbon chain, such as 8 carbon atom above hydrocarbon chains.
Hydroxyl is as important polar hydrophilic group, and the surface-active of Surfactant, which has, to be significantly affected, and surface is lived
The size of property agent middle hydroxyl value, determine the height of its surface-active.
In correlation technique in the assay method of Surfactant middle hydroxyl value, water circulation type condensation reflux unit need to be used,
The problem of water resource waste, cumbersome in practical operation be present；In addition, Surfactant middle hydroxyl value in correlation technique
Potassium hydroxide-ethanol solution used in assay method has that preservation is easy to change, causes result inaccurate, uses
The term of validity is short, increases workload.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of assay method of organic matter hydroxyl value, and this method program is simple, operation
It is convenient, as a result accurately, and the wasting of resources can be reduced.
The second object of the present invention is the application for providing the assay method of above-mentioned organic matter hydroxyl value, and this method can be used
In the hydroxy value measuring of surfactant, program is simple, easy to operate, as a result accurately, energy-saving and emission-reduction.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
A kind of assay method of organic matter hydroxyl value, acylation reaction is carried out to sample using acylating reagent, hydrolysis, entered with alkali lye
Row colour developing titration；
Using identical method, sample is not added, carries out blank assay；
The consumption volume of alkali lye is recorded respectively, is calculated as follows to obtain the hydroxyl value of sample compound：
Wherein, X is hydroxyl value, and unit is mg alkali/g；
M is sample mass, unit g；
V0By the alkali lye volume that colour developing titration consumes in blank assay, unit mL；
V1Consumed alkali lye volume, unit mL are titrated to the addition of colour developing in the experiment of sample；
C be alkali lye concentration, unit mol/L；
M is, the quality of alkali in grams suitable with the alkali lye standard liquid that 1.00mL concentration is 1.000mol/L, single
Position is g；
The acylation reaction is carried out by the way of being heated to reflux, and funnel intercalation reaction container and fixation are held to reaction
Device is sealed, and acylation reaction is carried out using funnel as reflux.
The amount that by calculating organic matter the hydroxyl of acylation reaction occurs for the assay method of organic matter hydroxyl value of the present invention, comes true
Determine the hydroxyl value of organic matter, wherein acylation reaction is carried out by the way of being heated to reflux, and is not required to using funnel as reflux
Water circulation type condensation reflux unit is used, significantly reduces the waste of water resource；Using funnel as reflux, substantially
The loss of material in reaction vessel will not be caused, even if partial material is lost in reflux course, due to the measure and sky of sample
White experiment is to use identical method, and identical operation, the loss of material tested twice is essentially identical, used alkali lye
The decrement of dosage be also essentially identical, follow-up calculating is not had an impact；The assay method of organic matter hydroxyl value of the present invention
Program is simple, easy to operate, as a result accurately, and can reduce the wasting of resources.
Alternatively, the acylating reagent is mainly prepared by solvent and acid anhydrides.
Preferably, the preparation method of the acylating reagent includes solvent and acid anhydrides being sufficiently mixed uniformly.
Preferably, the volume ratio of the solvent and acid anhydrides is 4：1-2, preferably 4：1-1.5 more preferably 4：1.
Preferably, the solvent includes organic solvent, preferably pyridine.
Preferably, the acid anhydrides includes organic acid anhydride, preferably acetic anhydride.
Alternatively, the temperature of the acylation reaction is more than 96 DEG C, preferably 96-99 DEG C, more preferably 97 DEG C.
Alternatively, the temperature of the acylation reaction is more than 0.5h, preferably 1-2h, more preferably 1h.
Alternatively, after the completion of the hydrolysis includes acylation reaction, it is hydrolyzed after adding water.
Alternatively, the temperature of the hydrolysis is more than 96 DEG C, preferably 96-99 DEG C, more preferably 97 DEG C.
Alternatively, the time of the hydrolysis is more than 1min, preferably 1-10min, more preferably 5min.
Alternatively, the alkali lye includes the aqueous solution or alkali alcosol of alkali, preferably alkali alcosol.
Preferably, one or more, preferably potassium hydroxide in hydroxide of the alkali including alkali metal.
Preferably, the alcohol includes monohydric alcohol, preferably ethanol, more preferably ethanol,aldehyde free.
Preferably, the alkali lye is the ethanol solution of potassium hydroxide；
It is further preferred that the compound method of the ethanol solution of the potassium hydroxide includes, potassium hydroxide is soluble in water,
Diluted with ethanol, take supernatant to demarcate after standing, obtain the ethanol solution of potassium hydroxide.
It is highly preferred that the time of the standing is more than 24h.
It is further preferred that the ethanol solution of the potassium hydroxide at least carries out weekly 1 demarcation.
It is further preferred that the term of validity after the ethanol solution of the potassium hydroxide is prepared is no more than 6 weeks.
Preferably, the preparation method of the ethanol,aldehyde free includes：Metal simple-substance is added in absolute ethyl alcohol, is steamed after backflow
Evaporate, recovery cut obtains ethanol,aldehyde free.
It is further preferred that the metal simple-substance includes Al.
It is further preferred that the return time is more than 0.5h, preferably 0.5-2h, more preferably 1h.
Alternatively, it is described to carry out colour developing titration including adding developer in solution after hydrolyzing with alkali lye, dripped with alkali lye
It is fixed extremely to change colour.
Preferably, the developer includes phenolphthalein.
Preferably, more than 30s is continued to changing colour with alkali-titration.
Alternatively, used reaction vessel has frosted mouth.
Preferably, the funnel is fixed by grinding port plug and reaction vessel.
Alternatively, external fixation device fixed funnel is passed through.
Preferably, the external fixation device includes clip.
A kind of application of the assay method of above-mentioned organic matter hydroxyl value, the assay method of the organic matter hydroxyl value are used for surface
The hydroxy value measuring of activating agent.
The inventive method can be used in the hydroxy value measuring of surfactant, and program is simple, easy to operate, as a result accurately, section
Can emission reduction.
Preferably, the surfactant is selected from nonionic surfactant, is preferably selected from the work of aliphatic non-ionic surface
Property agent and alicyclic nonionic surfactant, more preferably AEO.
Preferably, the scope of the organic matter hydroxyl value is 30-1000.
Compared with prior art, beneficial effects of the present invention are：
The amount that by calculating organic matter the hydroxyl of acylation reaction occurs for the assay method of organic matter hydroxyl value of the present invention, comes true
Determine the hydroxyl value of organic matter, wherein acylation reaction is carried out by the way of being heated to reflux, and is not required to using funnel as reflux
Water circulation type condensation reflux unit is used, significantly reduces the waste of water resource；Using funnel as reflux, substantially
The loss of material in reaction vessel will not be caused, even if partial material is lost in reflux course, due to the measure and sky of sample
White experiment is to use identical method, and identical operation, the loss of material tested twice is essentially identical, used alkali lye
The decrement of dosage be also essentially identical, follow-up calculating is not had an impact；The assay method of organic matter hydroxyl value of the present invention
Program is simple, easy to operate, as a result accurately, and can reduce the wasting of resources, can be effective for the hydroxy value measuring of surfactant.
Embodiment
Technical scheme is clearly and completely described below in conjunction with embodiment, but ability
Field technique personnel will be understood that following described embodiment is part of the embodiment of the present invention, rather than whole embodiments,
The present invention is merely to illustrate, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.Unreceipted actual conditions person in embodiment, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or instrument
Unreceipted production firm person, it is the conventional products that can be obtained by commercially available purchase.
The specific embodiment of the invention provides a kind of assay method of organic matter hydroxyl value, and sample is entered using acylating reagent
Row acylation reaction, hydrolysis, colour developing titration is carried out with alkali lye；
Using identical method, sample is not added, carries out blank assay；
The consumption volume of alkali lye is recorded respectively, is calculated as follows to obtain the hydroxyl value of sample compound：
Wherein, X is hydroxyl value, and unit is mg alkali/g；
M is sample mass, unit g；
V0By the alkali lye volume that colour developing titration consumes in blank assay, unit mL；
V1Consumed alkali lye volume, unit mL are titrated to the addition of colour developing in the experiment of sample；
C be alkali lye concentration, unit mol/L；
M is, the quality of alkali in grams suitable with the alkali lye standard liquid that 1.00mL concentration is 1.000mol/L, single
Position is g；
The acylation reaction is carried out by the way of being heated to reflux, and funnel intercalation reaction container and fixation are held to reaction
Device is sealed, and acylation reaction is carried out using funnel as reflux.
The amount that by calculating organic matter the hydroxyl of acylation reaction occurs for the assay method of organic matter hydroxyl value of the present invention, comes true
Determine the hydroxyl value of organic matter, wherein acylation reaction is carried out by the way of being heated to reflux, and is not required to using funnel as reflux
Water circulation type condensation reflux unit is used, significantly reduces the waste of water resource；Using funnel as reflux, substantially
The loss of material in reaction vessel will not be caused, even if partial material is lost in reflux course, due to the measure and sky of sample
White experiment is to use identical method, and identical operation, the loss of material tested twice is essentially identical, used alkali lye
The decrement of dosage be also essentially identical, follow-up calculating is not had an impact；The assay method of organic matter hydroxyl value of the present invention
Program is simple, easy to operate, as a result accurately, and can reduce the wasting of resources.
In a kind of preferred embodiment of the present invention, the acylating reagent is mainly prepared by solvent and acid anhydrides.
Preferably, the preparation method of the acylating reagent includes solvent and acid anhydrides being sufficiently mixed uniformly.
The acylating reagent is preferably matching while using.
Preferably, the volume ratio of the solvent and acid anhydrides is 4：1-2, preferably 4：1-1.5 more preferably 4：1.
The dosage of acid anhydrides can be suitably excessive, can guarantee that the abundant progress of acylation reaction, excessive acid anhydrides has no effect on
Result of calculation it is accurate.
Preferably, the solvent includes organic solvent, preferably pyridine, and pyridine can both make solvent, and and can promotes reaction.
Preferably, the acid anhydrides includes organic acid anhydride, preferably acetic anhydride.
The acylation reaction activity of acid anhydrides is higher, and conventional is acetic anhydride.
In a kind of preferred embodiment of the present invention, the temperature of the acylation reaction is more than 96 DEG C, preferably 96-
99 DEG C, more preferably 97 DEG C.
In a kind of preferred embodiment of the present invention, the temperature of the acylation reaction is more than 0.5h, preferably 1-
2h, more preferably 1h.
Using specified temp and time, contribute to the abundant progress of acylation reaction, improve the accuracy of measurement result.
In a kind of preferred embodiment of the present invention, after the completion of the hydrolysis includes acylation reaction, carried out after adding water
Hydrolysis.
In a kind of preferred embodiment of the present invention, the temperature of the hydrolysis is more than 96 DEG C, preferably 96-99
DEG C, more preferably 97 DEG C.
In a kind of preferred embodiment of the present invention, the time of the hydrolysis is more than 1min, preferably 1-
10min, more preferably 5min.
Using specified temp and time, contribute to the abundant progress of hydrolysis, excessive acid anhydrides is fully hydrolyzed, improve and survey
Determine the accuracy of result.
In a kind of preferred embodiment of the present invention, the alkali lye includes the aqueous solution or alkali alcosol of alkali, excellent
Elect alkali alcosol as.
Preferably, one or more, preferably potassium hydroxide in hydroxide of the alkali including alkali metal.
Preferably, the alcohol includes monohydric alcohol, preferably ethanol, more preferably ethanol,aldehyde free.
Prepare to obtain alkali alcosol using ethanol,aldehyde free, can effectively overcome and potassium hydroxide-second is used in correlation technique
Alcoholic solution there is a situation where preserve it is easy to change, cause result inaccurate, it is short using the term of validity, increase workload the problem of.
Preferably, the alkali lye is the ethanol solution of potassium hydroxide；
It is further preferred that the compound method of the ethanol solution of the potassium hydroxide includes, potassium hydroxide is soluble in water,
Diluted with ethanol, take supernatant to demarcate after standing, obtain the ethanol solution of potassium hydroxide.
It is highly preferred that the time of the standing is more than 24h.
It is further preferred that the ethanol solution of the potassium hydroxide at least carries out weekly 1 demarcation.
It is further preferred that the term of validity after the ethanol solution of the potassium hydroxide is prepared is no more than 6 weeks.
Ethanol solution of the concentration for 0.5N potassium hydroxide is used in the specific embodiment of the invention, its compound method bag
Include：28g potassium hydroxide is dissolved in 30ml deionized waters, is diluted to 1000ml with ethanol,aldehyde free, is placed 24 hours, export upper strata is clear
Liquid is placed in brown bottle, demarcation.The standard liquid is demarcated once for one week, the term of validity six weeks.Concentration values during actual calculating
It is defined by the concentration value demarcated recently.
Preferably, the preparation method of the ethanol,aldehyde free includes：Metal simple-substance is added in absolute ethyl alcohol, is steamed after backflow
Evaporate, recovery cut obtains ethanol,aldehyde free.
It is further preferred that the metal simple-substance includes Al.
It is further preferred that the return time is more than 0.5h, preferably 0.5-2h, more preferably 1h.
Ethanol,aldehyde free is prepared using ad hoc approach, method is simple, prepares to obtain the alcohol of alkali using the obtained aldehyde-free ethanol
Solution, it can effectively overcome in correlation technique and that preservation is easy to change be present using potassium hydroxide-ethanol solution, cause to tie
Fruit is inaccurate, short using the term of validity, increase workload the problem of.
The preparation method of ethanol,aldehyde free includes in the specific embodiment of the invention：5g aluminium will be added in 1000mL absolute ethyl alcohols
Piece, flow back one hour, distill immediately, recovery cut is standby in brown bottle.
It is described to carry out colour developing titration with alkali lye and include after hydrolyzing molten in a kind of preferred embodiment of the present invention
Developer is added in liquid, with alkali-titration to discoloration.
Preferably, the developer includes phenolphthalein.
Preferably, more than 30s is continued to changing colour with alkali-titration.
In a kind of preferred embodiment of the present invention, used reaction vessel has frosted mouth.
Preferably, the funnel is fixed by grinding port plug and reaction vessel.
In a kind of preferred embodiment of the present invention, pass through external fixation device fixed funnel.
Preferably, the external fixation device includes clip.
The funnel used in the specific embodiment of the invention is for the heat resistant glass triangular funnel with grinding port plug, bore
60mm, lower pipe range 60mm, its lower nozzle are stretched under the liquid level in reaction vessel or on the liquid level in reaction vessel, but
The set-up mode of funnel in Specimen Determination and blank assay should be made to keep identical.
A kind of application of the assay method of above-mentioned organic matter hydroxyl value, the assay method of the organic matter hydroxyl value are used for surface
The hydroxy value measuring of activating agent.
The inventive method can be used in the hydroxy value measuring of surfactant, and program is simple, easy to operate, as a result accurately, section
Can emission reduction.
Preferably, the surfactant is selected from nonionic surfactant, is preferably selected from the work of aliphatic non-ionic surface
Property agent and alicyclic nonionic surfactant, more preferably AEO.
Preferably, the scope of the organic matter hydroxyl value is 30-1000.
Embodiment 1
A kind of assay method of AEO hydroxyl value, comprises the following steps：
1. weighing sample m (being accurate to 0.0002g) in 250mL drying iodine flask, the acetyl newly configured is accurately pipetted
Changing reagent 3mL, (volume ratio of pyridine and acetic anhydride is 2：1, it is a certain amount of using preceding preparation, take 3mL to add), frosted mouth will be carried
Small funnel be positioned over bottleneck, stepped up with clip, be put into and keep in 96 DEG C of constant temperature glycerol bath, iodine flask bottom is immersed about
1cm is deep, is heated to reflux 0.5h.Taking-up is cooled to room temperature, adds 2mL water, shakes up, place into 96 DEG C of glycerol bath and hydrolyze
1min.Taking-up is cooled to room temperature, and funnel inside and outside wall, and iodine flask inwall are rinsed with 50mL absolute ethyl alcohols.Phenolphthalein 3 is added to drip,
Blush, which is titrated to, with the ethanol standard liquid of the potassium hydroxide of demarcation continues 30 seconds.Read the volume of standard liquid consumption.
2. blank assay：It is to be added without sample using with step 1 identical method, difference, reads standard liquid consumption
Volume.
3. the calculation formula of hydroxyl value：
Wherein, X is hydroxyl value, unit mgKOH/g；
M is sample mass, unit g；
V0By the ethanol standard liquid volume of the potassium hydroxide that colour developing titration consumes in blank assay, unit mL；
V1To with the addition of the ethanol standard liquid volume that colour developing in the experiment of sample titrates consumed potassium hydroxide, unit
For mL；
C be potassium hydroxide ethanol standard liquid demarcation concentration, unit mol/L；
The ethanol standard liquid for the potassium hydroxide that M is with 1.00mL concentration is 1.000mol/L is suitable, in grams
The quality of alkali, unit g.
Embodiment 2
A kind of assay method of AEO hydroxyl value, comprises the following steps：
1. weighing sample m (being accurate to 0.0002g) in 250mL drying iodine flask, the acetyl newly configured is accurately pipetted
Changing reagent 3mL, (volume ratio of pyridine and acetic anhydride is 4：1.5, it is a certain amount of using preceding preparation, take 3mL to add), frosted will be carried
The small funnel of mouth is positioned over bottleneck, is stepped up with clip, is put into the constant temperature glycerol bath for being kept for 99 DEG C, iodine flask bottom is immersed about
1cm is deep, is heated to reflux 2h.Taking-up is cooled to room temperature, adds 2mL water, shakes up, place into 99 DEG C of glycerol bath and hydrolyze 10min.
Taking-up is cooled to room temperature, and funnel inside and outside wall, and iodine flask inwall are rinsed with 50mL absolute ethyl alcohols.Add phenolphthalein 3 to drip, with demarcation
The ethanol standard liquid of potassium hydroxide be titrated to blush and continue 30 seconds.Read the volume of standard liquid consumption.
2. blank assay：It is to be added without sample using with step 1 identical method, difference, reads standard liquid consumption
Volume.
3. the calculation formula of hydroxyl value：
Wherein, X is hydroxyl value, unit mgKOH/g；
M is sample mass, unit g；
V0By the ethanol standard liquid volume of the potassium hydroxide that colour developing titration consumes in blank assay, unit mL；
V1To with the addition of the ethanol standard liquid volume that colour developing in the experiment of sample titrates consumed potassium hydroxide, unit
For mL；
C be potassium hydroxide ethanol standard liquid demarcation concentration, unit mol/L；
The ethanol standard liquid for the potassium hydroxide that M is with 1.00mL concentration is 1.000mol/L is suitable, in grams
The quality of alkali, unit g.
Embodiment 3
A kind of assay method of AEO hydroxyl value, comprises the following steps：
1. weighing sample m (being accurate to 0.0002g) in 250mL drying iodine flask, the acetyl newly configured is accurately pipetted
Changing reagent 3mL, (volume ratio of pyridine and acetic anhydride is 4：1, it is a certain amount of using preceding preparation, take 3mL to add), frosted mouth will be carried
Small funnel be positioned over bottleneck, stepped up with clip, be put into and keep in 97 DEG C of constant temperature glycerol bath, iodine flask bottom is immersed about
1cm is deep, is heated to reflux 1h.Taking-up is cooled to room temperature, adds 2mL water, shakes up, place into 97 DEG C of glycerol bath and hydrolyze 5min.
Taking-up is cooled to room temperature, and funnel inside and outside wall, and iodine flask inwall are rinsed with 50mL absolute ethyl alcohols.Add phenolphthalein 3 to drip, with demarcation
The ethanol standard liquid of potassium hydroxide be titrated to blush and continue 30 seconds.Read the volume of standard liquid consumption.
2. blank assay：It is to be added without sample using with step 1 identical method, difference, reads standard liquid consumption
Volume.
3. the calculation formula of hydroxyl value：
Wherein, X is hydroxyl value, unit mgKOH/g；
M is sample mass, unit g；
V0By the ethanol standard liquid volume of the potassium hydroxide that colour developing titration consumes in blank assay, unit mL；
V1To with the addition of the ethanol standard liquid volume that colour developing in the experiment of sample titrates consumed potassium hydroxide, unit
For mL；
C be potassium hydroxide ethanol standard liquid demarcation concentration, unit mol/L；
The ethanol standard liquid for the potassium hydroxide that M is with 1.00mL concentration is 1.000mol/L is suitable, in grams
The quality of alkali, unit g.
The method of various embodiments of the present invention is respectively adopted, carries out the measure of identical AEO sample hydroxyl value,
And the results contrast being measured respectively with GB/T 7384-1996 method successively, acquired results are as shown in table 1：
The AEO hydroxy value measuring result of the present invention of table 1
It can be seen from Table 1 that using the inventive method with being connect using the measurement result obtained by GB/T 7384-1996
Closely, deviation is in the range of 5 ‰, and the inventive method program is simple, easy to operate, as a result accurately, and can reduce the wasting of resources,
Using funnel as reflux, it is not necessary to using water circulation type condensation reflux unit, significantly reduce the waste of water resource；Adopt
By the use of funnel as reflux, it will not substantially cause the loss of material in reaction vessel, even if partial material is in reflux course
Middle loss, because the measure and blank assay of sample are to use identical method, identical operation, the loss of material tested twice
It is essentially identical, the decrement of the dosage of used alkali lye is also essentially identical, and follow-up calculating is not had an impact；This
Outside, the ethanol solution of potassium hydroxide is prepared using ethanol,aldehyde free, can effectively overcome and potassium hydroxide-second is used in correlation technique
Alcoholic solution there is a situation where preserve it is easy to change, cause result inaccurate, it is short using the term of validity, increase workload the problem of.This hair
Bright method can be used in the hydroxy value measuring of the organic matters such as surfactant, can be fast and convenient obtain accurate result, have aobvious
The progress of work.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that various embodiments above is only used
To illustrate technical scheme, rather than its limitations；It will be understood by those within the art that：Without departing substantially from this hair
In the case of bright spirit and scope, the technical scheme described in foregoing embodiments can be modified, or to wherein
Some or all of technical characteristic carries out equivalent substitution；And these are changed or are replaced, the essence of appropriate technical solution is not made
Depart from the scope of various embodiments of the present invention technical scheme；It is, therefore, intended that include belonging to the present invention in the following claims
In the range of all these substitutions and modifications.
Claims (10)
1. a kind of assay method of organic matter hydroxyl value, it is characterised in that acylation reaction, water are carried out to sample using acylating reagent
Solution, colour developing titration is carried out with alkali lye；
Using identical method, sample is not added, carries out blank assay；
The consumption volume of alkali lye is recorded respectively, is calculated as follows to obtain the hydroxyl value of sample compound：
<mrow>
<mi>X</mi>
<mo>=</mo>
<mfrac>
<mrow>
<mo>(</mo>
<msub>
<mi>V</mi>
<mn>0</mn>
</msub>
<mo>-</mo>
<msub>
<mi>V</mi>
<mn>1</mn>
</msub>
<mo>)</mo>
<mo>&CenterDot;</mo>
<mi>c</mi>
<mo>&CenterDot;</mo>
<mi>M</mi>
</mrow>
<mi>m</mi>
</mfrac>
<mo>&times;</mo>
<mn>1000</mn>
<mo>;</mo>
</mrow>
Wherein, X is hydroxyl value, and unit is mg alkali/g；
M is sample mass, unit g；
V0By the alkali lye volume that colour developing titration consumes in blank assay, unit mL；
V1Consumed alkali lye volume, unit mL are titrated to the addition of colour developing in the experiment of sample；
C be alkali lye concentration, unit mol/L；
M is, the quality of alkali in grams suitable with the alkali lye standard liquid that 1.00mL concentration is 1.000mol/L, and unit is
g；
The acylation reaction is carried out by the way of being heated to reflux, and funnel intercalation reaction container and fixation are sealed to reaction vessel
Mouthful, acylation reaction is carried out using funnel as reflux.
2. the assay method of a kind of organic matter hydroxyl value according to claim 1, it is characterised in that the acylating reagent is main
It is prepared by solvent and acid anhydrides；
Preferably, the preparation method of the acylating reagent includes solvent and acid anhydrides being sufficiently mixed uniformly；
Preferably, the volume ratio of the solvent and acid anhydrides is 4：1-2, preferably 4：1-1.5 more preferably 4：1；
Preferably, the solvent includes organic solvent, preferably pyridine；
Preferably, the acid anhydrides includes organic acid anhydride, preferably acetic anhydride.
A kind of 3. assay method of organic matter hydroxyl value according to claim 1, it is characterised in that the temperature of the acylation reaction
Spend for more than 96 DEG C, preferably 96-99 DEG C, more preferably 97 DEG C；
Preferably, the temperature of the acylation reaction is more than 0.5h, preferably 1-2h, more preferably 1h.
4. the assay method of a kind of organic matter hydroxyl value according to claim 1, it is characterised in that the hydrolysis includes being acylated
After the completion of reaction, it is hydrolyzed after adding water；
Preferably, the temperature of the hydrolysis is more than 96 DEG C, preferably 96-99 DEG C, more preferably 97 DEG C；
Preferably, the time of the hydrolysis is more than 1min, preferably 1-10min, more preferably 5min.
5. the assay method of a kind of organic matter hydroxyl value according to claim 1, it is characterised in that the alkali lye includes alkali
The aqueous solution or alkali alcosol, preferably alkali alcosol；
Preferably, one or more, preferably potassium hydroxide in hydroxide of the alkali including alkali metal；
Preferably, the alcohol includes monohydric alcohol, preferably ethanol, more preferably ethanol,aldehyde free.
6. the assay method of a kind of organic matter hydroxyl value according to claim 5, it is characterised in that the alkali lye is hydroxide
The ethanol solution of potassium；
Preferably, the compound method of the ethanol solution of the potassium hydroxide includes, and potassium hydroxide is soluble in water, dilute with ethanol
Release, take supernatant to demarcate after standing, obtain the ethanol solution of potassium hydroxide；
Preferably, the time of the standing is more than 24h；
Preferably, the ethanol solution of the potassium hydroxide at least carries out weekly 1 demarcation；
Preferably, the term of validity after the ethanol solution of the potassium hydroxide is prepared is no more than 6 weeks.
A kind of 7. assay method of organic matter hydroxyl value according to claim 5, it is characterised in that the system of the ethanol,aldehyde free
Preparation Method includes：Metal simple-substance is added in absolute ethyl alcohol, is distilled after backflow, recovery cut obtains ethanol,aldehyde free；
Preferably, the metal simple-substance includes Al；
Preferably, the return time is more than 0.5h, preferably 0.5-2h, more preferably 1h.
8. the assay method of a kind of organic matter hydroxyl value according to claim 1, it is characterised in that described to be shown with alkali lye
Color titration includes adding developer in solution after hydrolyzing, with alkali-titration to discoloration；
Preferably, the developer includes phenolphthalein；
Preferably, more than 30s is continued to changing colour with alkali-titration.
A kind of 9. assay method of organic matter hydroxyl value according to claim 1, it is characterised in that used reaction vessel
With frosted mouth；
Preferably, the funnel is fixed by grinding port plug and reaction vessel；
Preferably, external fixation device fixed funnel is passed through；
It is further preferred that the external fixation device includes clip.
10. the application of the assay method of a kind of organic matter hydroxyl value as described in claim 1-9 is any, it is characterised in that described
The assay method of organic matter hydroxyl value is used for the hydroxy value measuring of surfactant；
Preferably, the surfactant is selected from nonionic surfactant, is preferably selected from aliphatic nonionic surfactant
With alicyclic nonionic surfactant, more preferably AEO；
Preferably, the scope of the organic matter hydroxyl value is 30-1000.
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