CN108226376A - A kind of detection method of phenols or amino benzenes compounds coupling value - Google Patents
A kind of detection method of phenols or amino benzenes compounds coupling value Download PDFInfo
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- CN108226376A CN108226376A CN201711488396.9A CN201711488396A CN108226376A CN 108226376 A CN108226376 A CN 108226376A CN 201711488396 A CN201711488396 A CN 201711488396A CN 108226376 A CN108226376 A CN 108226376A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention discloses a kind of phenols or the detection methods of amino benzenes compounds coupling value.The detection method includes the following steps：(1) single sweep polarographic wave aqueous solution is added in mixture A, forms mixture B；Mixture A is phenols or amino benzenes compounds sample, acetic acid, sodium acetate and water；(2) 2,4 diaminotoluene aqueous solutions are added in mixture B, you can.The detection method of the present invention is easy to operate, and detection error is small, raw materials used few, suitable for the detection of plant produced.
Description
Technical field
The present invention relates to a kind of phenols or the detection methods of amino benzenes compounds coupling value.
Background technology
The detection method for being presently used for phenols or amino benzenes compounds coupling value is to use the buret of jacketed, with weight
Nitrogen salt standard specimen direct titration is coupled component.Due to the unstable easy decomposition of diazol, so the detection method detection error is big, and adopt
With operating difficulties during buret jacketed.
Invention content
Technical problem solved by the invention is existing phenols or the detection method error of amino benzenes compounds coupling value
Greatly, the defects of operating difficulties, so as to provide the detection method of a kind of phenols or amino benzenes compounds coupling value.The detection of the present invention
Method is easy to operate, and detection error is small, raw materials used few.
The present invention is to solve above-mentioned technical problem by the following technical programs：
The present invention provides a kind of phenols or the detection methods of amino benzenes compounds coupling value, include the following steps：
(1) single sweep polarographic wave aqueous solution is added in mixture A, forms mixture B；The mixture A is
Phenols or amino benzenes compounds sample, acetic acid, sodium acetate and water；
(2) 2,4- diaminotoluene aqueous solutions are added in mixture B, you can.
In the present invention, the phenols or amino benzenes compounds sample are the common phenols in this field or amino benzenes compounds sample
Product, such as N- cyanoethyl-N- Acetoxyethyl aniline, form can be that the acetic acid of N- cyanoethyl-N- Acetoxyethyl aniline is molten
Liquid (yellowish-brown esterifying liquid).
In the present invention, those skilled in the art know, the acetic acid is preferably glacial acetic acid, and (mass fraction is 98% second
Acid).
In the present invention, the water can be water commonly used in the art, such as distilled water.
In the present invention, the concentration of the single sweep polarographic wave aqueous solution can be conventional, preferably 0.25mol/L.
In the present invention, the concentration of 2, the 4- diaminotoluenes aqueous solution can be conventional, preferably 0.1mol/L.
In the present invention, the phenols or amino benzenes compounds sample, the acetic acid, the sodium acetate, the water and described
The amount ratio of single sweep polarographic wave aqueous solution can be routine, preferably (0.4-0.5g)：(18-20mL)：(8.1-
8.2g)：(98-100mL)：(48-50mL)；More preferably, the quality of the phenols or amino benzenes compounds sample is 0.4639g.
In the present invention, the sodium acetate can be used in the form of sodium acetate aqueous solution, such as use a concentration of 2mol/L
Sodium acetate aqueous solution, preferably, the phenols or amino benzenes compounds sample, the acetic acid, the sodium acetate, the water and
The amount ratio of the single sweep polarographic wave aqueous solution is (0.4-0.5g)：(18-20mL)：(48-50mL)：(48-50mL)：
(48-50mL)。
In the present invention, 2, the 4- diaminotoluenes aqueous solution can be prepared by the method for this field routine, such as：By 2,
4- diaminotoluenes, water and concentrated hydrochloric acid are in mixing, constant volume.
Wherein, the water can be water commonly used in the art, such as distilled water.
Wherein, the amount ratio of 2, the 4- diaminotoluenes, the water and the concentrated hydrochloric acid can be conventional, preferably
12.2g：1000mL：75mL.
It wherein, can be with suitable water by 2, the 4- diaminotoluenes and institute when those skilled in the art know the mixing
Concentrated hydrochloric acid dissolving is stated, can be added during the constant volume needed for adding water to.
In the present invention, the single sweep polarographic wave aqueous solution can be made by the method for this field routine, such as：
Paranitroanilinum, water and concentrated hydrochloric acid below 0 DEG C are mixed, mixed later with sodium nitrite standard solution, at 5 DEG C
Below with starch potassium iodide paper detection in micro- blue, constant volume.
Wherein, the concentrated hydrochloric acid is concentrated hydrochloric acid commonly used in the art, and the mass fraction of the concentrated hydrochloric acid is preferably
36-38%.
Wherein, the water can be water commonly used in the art, such as distilled water.
Wherein, the concentration of the sodium nitrite standard solution can be conventional, such as 0.5mol/L；The sodium nitrite standard is molten
Liquid can be prepared by conventional method, such as：Sodium nitrite, sodium hydroxide, natrium carbonicum calcinatum and water are mixed, constant volume；
It wherein, can be with suitable water by the sodium nitrite, the sodium hydroxide and institute when those skilled in the art know the mixing
Natrium carbonicum calcinatum dissolving is stated, can be added during the constant volume needed for adding water to；The sodium nitrite, the hydroxide
The amount ratio of sodium, the natrium carbonicum calcinatum and the water can be conventional, preferably 36g：0.5g：1g：1000mL.
Wherein, the amount ratio of the paranitroanilinum, the water, the concentrated hydrochloric acid and the sodium nitrite standard solution can
For routine, preferably 50g：50mL：12mL：25mL.
Wherein, those skilled in the art know, if using starch potassium iodide after being mixed with the sodium nitrite standard solution
Test paper detection is not in micro- blue, then needs to continue that sodium nitrite is added dropwise, until starch potassium iodide paper is in three points of micro- blue and holding
Clock is colour-fast, later constant volume.
Wherein, those skilled in the art know, the single sweep polarographic wave aqueous solution being prepared need to be stored in
In ice-water bath.
In the present invention, the addition can be titration, and preferably using fat tripe suction pipe, the titration is carried out to Huang for the titration
Color；The detection of the titration preferably carries out profit circle experiment using H- acid.
In the present invention, those skilled in the art know that step (1) and step (2) preferably carry out at 0-5 DEG C.
In the present invention, those skilled in the art know coupling value can be calculated by the following formula：
Coupling value=(V0-V1) × C × 0.352 × 100%/G,
Wherein, the volume of 2,4- diaminotoluene aqueous solutions that V0 is consumed by blank assay；
The volume of 2,4 di amino toluene aqueous solution that V1 is consumed for titration sample；
C is 2,4 di amino toluene concentration of aqueous solution；
G is example weight.
Wherein, the difference of the step of those skilled in the art know, the blank assay and above-mentioned detection method is only
It is：Sample to be tested is added without in the blank assay.
In the present invention, the balance for weighing sample can be conventional use of balance, preferably electronic balance, the electricity
The precision of sub- balance is 0.1mg.
Without prejudice to the field on the basis of common sense, above-mentioned each optimum condition can be combined arbitrarily each preferably to get the present invention
Embodiment.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is：
The detection method of the present invention is easy to operate, and detection error is small, raw materials used few, suitable for the detection of plant produced.
Specific embodiment
It is further illustrated the present invention below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.Test method without specific conditions in the following example, according to conventional methods and conditions or according to quotient
Product specification selects.
Agents useful for same, instrument, single sweep polarographic wave and blank assay are as described below in following embodiment.
Agents useful for same：The single sweep polarographic wave of 0.25mol/L, concentrated hydrochloric acid, the sodium nitrite standard of 0.5mol/L are molten
Liquid, starch potassium iodide paper, anhydrous sodium acetate (anhydrous sodium acetate), the 2,4 di amino toluene aqueous solution of 0.1mol/L, H- acid.
Instrument：250mL brown volumetric flasks, 250mL whites volumetric flask, 400mL beakers, straight type dropper, the fat tripes of 25mL
The fat tripe suction pipe of suction pipe, 50mL, 50mL browns acid buret, electronic balance, 50mL graduated cylinders, 100mL graduated cylinders, magnetic stirring apparatus.
The preparation of single sweep polarographic wave aqueous solution：
The paranitroanilinum 50g weighed adds distilled water 50mL, concentrated hydrochloric acid 12mL to be cooled in 250mL brown volumetric flasks
0 DEG C hereinafter, disposably add in the sodium nitrite standard solution (about 25mL) of theoretical amount 0.5mol/L.
5 DEG C are maintained at hereinafter, with starch potassium iodide paper detection terminal in micro- blue, otherwise should continue that nitrous acid is added dropwise
Sodium, until starch potassium iodide paper in micro- blue and keep three minutes it is colour-fast, be then diluted with water to scale and shake up and be placed on
It is preserved in cryostat water.
The preparation of sodium nitrite standard solution：
Weigh 36g sodium nitrites, 0.5g NaOH and 1g anhydrous Nas2CO3Water is dissolved in, and is diluted to 1000mL.
The preparation of 2,4 di amino toluene aqueous solution：
It weighs 2.4- diaminotoluenes 12.2g and fills 300mL distilled water and 75ml concentrated hydrochloric acids in 1000mlL beakers in advance
Middle dissolving, is diluted with water to 1000mL, left undisturbed overnight, and clarification is moved into brown bottle and stored.
Blank test：
20mL glacial acetic acids (glacial acetic acid), 50mL anhydrous sodium acetates (2mol/L), 50mL distillations are added in into 400mL beakers
With 5 DEG C of ice water cooling hereinafter, adding 50ml single sweep polarographic waves again, 0.1mol/L is used after being stirred 30 minutes at 0-5 DEG C for water
The titration of 2,4- diaminotoluenes aqueous solution, and do profit circle experiment, with H- acid in colourless, single sweep polarographic wave is in yellow
Only.
Using above-mentioned 2.4- diaminotoluenes standard solution
Embodiment 1
In the present embodiment, sample to be tested is yellowish-brown esterifying liquid (acetum of N- cyanoethyl-N- Acetoxyethyl aniline).
Sample 0.4639g is weighed, adds 20mL glacial acetic acid, 50mL sodium acetates, 50mL distillations are water-cooled to 5 DEG C hereinafter, adding again
50mL single sweep polarographic waves use the water-soluble drop of 2,4 di amino toluene of 0.1mol/L after being stirred 30 minutes at 0-5 DEG C
It is fixed, and profit circle experiment is done, it is in colourless with H- acid, until single sweep polarographic wave is in yellow.
Embodiment 2-4
Amount of samples in embodiment 2-4 is respectively 0.4392g, 0.4407g, 0.4640g, remaining operation and condition and reality
It is identical to apply example 1.
Comparative example 1
In this comparative example, sample to be tested is yellowish-brown esterifying liquid (acetum of N- cyanoethyl-N- Acetoxyethyl aniline).
Detection method is as follows：
Sample 4.9381g is weighed, constant volume is diluted with 100mL glacial acetic acid, uses the single sweep polarographic wave in embodiment 1
Aqueous solution is titrated, and is done and moistened circle experiment, and with H- acid in yellow, single sweep polarographic wave is in colourless for terminal.
Comparative example 2-4
Amount of samples in comparative example 2-4 is respectively 4.0324g, 4.3125g, 4.8167g, remaining operation and condition with it is right
Ratio 1 is identical.
Effect example 1
The coupling value of embodiment 1-4 calculates according to the following equation：
Coupling value=(V0-V1) × C × 0.352 × 100%/G
Wherein, the volume of 2,4- diaminotoluene aqueous solutions that V0--- blank assays are consumed；
The volume of 2,4 di amino toluene aqueous solution that V1--- titration samples are consumed；
C---2,4- diaminotoluene concentration of aqueous solution；
G--- example weights.
The coupling value of comparative example 1-4 calculates according to the following equation：
Coupling value=V × C × 0.352 × 100%/G
Wherein, V is the volume of single sweep polarographic wave aqueous solution；
C is the concentration of single sweep polarographic wave aqueous solution；
G--- example weights.
It the results are shown in Table 1.
The coupling value of table 1 embodiment 1-4 and comparative example 1-4
Although specific embodiments of the present invention have been described above, it will be appreciated by those of skill in the art that this is only
For example, protection scope of the present invention is to be defined by the appended claims.Those skilled in the art without departing substantially from
Under the premise of the principle and substance of the present invention, many changes and modifications may be made, but these change and
Modification each falls within protection scope of the present invention.
Claims (10)
1. the detection method of a kind of phenols or amino benzenes compounds coupling value, which is characterized in that it includes the following steps：
(1) single sweep polarographic wave aqueous solution is added in mixture A, forms mixture B；The mixture A is phenols
Or amino benzenes compounds sample, acetic acid, sodium acetate and water；
(2) 2,4- diaminotoluene aqueous solutions are added in mixture B, you can.
2. detection method as described in claim 1, which is characterized in that the phenols or amino benzenes compounds sample are N- cyanogen second
Base-N- Acetoxyethyl aniline；
And/or the acetic acid is glacial acetic acid；
And/or the water is distilled water；
And/or a concentration of 0.25mol/L of the single sweep polarographic wave aqueous solution；
And/or a concentration of 0.1mol/L of 2, the 4- diaminotoluenes aqueous solution；
And/or the phenols or amino benzenes compounds sample, the acetic acid, the sodium acetate, the water and the p-nitrophenyl
The amount ratio of amine diazonium salt solution is (0.4-0.5g)：(18-20mL)：(8.1-8.2g)：(98-100mL)：(48-50mL).
3. detection method as described in claim 1, which is characterized in that the sodium acetate is sodium acetate aqueous solution；
And/or the quality of the phenols or amino benzenes compounds sample is 0.4639g.
4. detection method as claimed in claim 3, which is characterized in that a concentration of 2mol/L of the sodium acetate aqueous solution；
And/or the phenols or amino benzenes compounds sample, the acetic acid, the sodium acetate, the water and the p-nitrophenyl
The amount ratio of amine diazonium salt solution is (0.4-0.5g)：(18-20mL)：(48-50mL)：(48-50mL)：(48-50mL).
5. detection method as claimed in claim 1 or 2, which is characterized in that 2, the 4- diaminotoluenes aqueous solution is under
Step is stated to be made：By 2,4- diaminotoluenes, water and concentrated hydrochloric acid in mixing, constant volume.
6. detection method as claimed in claim 5, which is characterized in that the water is distilled water；
And/or the amount ratio of 2, the 4- diaminotoluenes, the water and the concentrated hydrochloric acid is 12.2g：1000mL：75mL.
7. detection method as claimed in claim 1 or 2, which is characterized in that the single sweep polarographic wave aqueous solution passes through
Following methods are made：
Paranitroanilinum, water and concentrated hydrochloric acid below 0 DEG C are mixed, mixed later with sodium nitrite standard solution, below 5 DEG C
With starch potassium iodide paper detection in micro- blue, constant volume.
8. detection method as claimed in claim 7, which is characterized in that the mass fraction of the concentrated hydrochloric acid is 36-38%；
And/or the water is distilled water；
And/or a concentration of 0.5mol/L of the sodium nitrite standard solution；
And/or the paranitroanilinum, the water, the concentrated hydrochloric acid and the sodium nitrite standard solution amount ratio be
50g：50mL：12mL：25mL；
And/or the sodium nitrite standard solution is made by following step：By sodium nitrite, sodium hydroxide, natrium carbonicum calcinatum
It is mixed with water, constant volume.
9. detection method as claimed in claim 8, which is characterized in that the sodium nitrite, the sodium hydroxide, described anhydrous
The amount ratio of sodium carbonate and the water is 36g：0.5g：1g：1000mL.
10. detection method as described in claim 1, which is characterized in that described to be incorporated as titrating；The titration is inhaled using fat tripe
Pipe；The titration is carried out to yellow；The detection of the titration carries out profit circle experiment using H- acid；
And/or step (1) and step (2) carry out at 0-5 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113290002A (en) * | 2021-04-01 | 2021-08-24 | 浙江汇翔新材料科技股份有限公司 | Method for measuring yellow brown esterified liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091382A (en) * | 2013-01-15 | 2013-05-08 | 云南烟草科学研究院 | Determination method for content of total volatile alkali in cigarette smoke |
| CN104090017A (en) * | 2014-07-25 | 2014-10-08 | 重庆紫光国际化工有限责任公司 | Method for determining content of formaldehyde in glycolonitrile product |
| CN105445264A (en) * | 2015-12-02 | 2016-03-30 | 浙江闰土研究院有限公司 | Quick detection method for reaction degrees in dyestuff synthesis coupling reaction |
-
2017
- 2017-12-29 CN CN201711488396.9A patent/CN108226376A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091382A (en) * | 2013-01-15 | 2013-05-08 | 云南烟草科学研究院 | Determination method for content of total volatile alkali in cigarette smoke |
| CN104090017A (en) * | 2014-07-25 | 2014-10-08 | 重庆紫光国际化工有限责任公司 | Method for determining content of formaldehyde in glycolonitrile product |
| CN105445264A (en) * | 2015-12-02 | 2016-03-30 | 浙江闰土研究院有限公司 | Quick detection method for reaction degrees in dyestuff synthesis coupling reaction |
Non-Patent Citations (3)
| Title |
|---|
| 夏玉宇: "《化验员实用手册》", 31 March 1999, 化学工业出版社 * |
| 张志贤等: "《有机官能团定量分析》", 31 July 1990, 化学工业出版社 * |
| 陈亚庆: "《有机中间体的工业分析法》", 31 January 1997, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113290002A (en) * | 2021-04-01 | 2021-08-24 | 浙江汇翔新材料科技股份有限公司 | Method for measuring yellow brown esterified liquid |
| CN113290002B (en) * | 2021-04-01 | 2022-07-29 | 浙江汇翔新材料科技股份有限公司 | Method for measuring yellow brown esterified liquid |
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Application publication date: 20180629 |