CN107703129A - A kind of detection method of colouring agent aberration - Google Patents
A kind of detection method of colouring agent aberration Download PDFInfo
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- CN107703129A CN107703129A CN201710804606.4A CN201710804606A CN107703129A CN 107703129 A CN107703129 A CN 107703129A CN 201710804606 A CN201710804606 A CN 201710804606A CN 107703129 A CN107703129 A CN 107703129A
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Abstract
The present invention discloses a kind of detection method of colouring agent aberration, comprises the following steps：1) sample is dissolved in edta solution and acetone soln successively, filtered, gained supernatant is liquid to be extracted；2) acid solution and Silon are sequentially added in gained liquid to be extracted into step 1), washs above-mentioned gained mixed solution and filter, gained supernatant is solution to be measured；3) regulating step 2) in gained solution to be measured acid-base value, measure its chromatic value, gained chromatic value is the chromatic value of colouring agent.The application provides a kind of detection method of colouring agent aberration, and it extracts the pigment after colouring in Diammonium phosphate (DAP) and its chromatic value is tested, the fertilizer that screening is met demand is sold on the premise of eliminating metal ion and test result is disturbed.This method reappearance is higher, and test result is relatively stable.
Description
Technical field
The present invention relates to colouring agent detection field, and in particular to a kind of detection method of colouring agent aberration.
Background technology
In the production of Diammonium phosphate (DAP), due to mineral resources, phosphoric acid quality, production operation method, process conditions, degree of neutralization etc.
Influence, the diammonium phosphate product for preventing to produce usually is presented different colors, product occur from reaching preferable white
The changes such as part bleaches, inside and outside irregular colour is even flower phenomenon, is adversely affected.These colors are asked in fertilizer industry at this stage
It is a kind of conventional method to fertilizer coloring in the processing of topic.
And different batches are prepared the difference or different batches of ammonia and phosphoric acid degree of neutralization in Diammonium phosphate (DAP) and are prepared
The reasons such as the difference of toner chromatic value so that each batch produce Diammonium phosphate (DAP) after coloring chromatic value have it is certain inclined
Difference, the presentation quality of its product is influenceed, so as to influence to sell.Therefore, people survey to the chromatic value of Diammonium phosphate (DAP) after coloring
Examination, the fertilizer that screening is met demand are sold.And currently for the method for the chromatic value of Diammonium phosphate (DAP) after detection coloring
It is less, and the reappearance of method is relatively low, test result is unstable.
The content of the invention
In view of this, the application provides a kind of detection method of colouring agent aberration, and it is eliminating metal ion to test knot
On the premise of dried fruit is disturbed, extract the pigment after colouring in Diammonium phosphate (DAP) and its chromatic value is tested, screening, which is met, to be needed
The fertilizer asked is sold.This method reappearance is higher, and test result is relatively stable.
To solve above technical problem, technical scheme provided by the invention is a kind of detection method of colouring agent aberration, bag
Include following steps：
1) sample is dissolved in edta solution and acetone soln successively, filtered, gained supernatant is to treat
Extract solution；
2) acid solution and Silon are sequentially added in gained liquid to be extracted into step 1), washs above-mentioned gained mixing
Solution simultaneously filters, and gained supernatant is solution to be measured；
3) regulating step 2) in gained solution to be measured acid-base value, measure its chromatic value, gained chromatic value is colouring agent
Chromatic value.
Preferably, the volume ratio of edta solution and acetone soln is 2-5 in the step 1):1.
Preferably, in the step 2) acid solution in citric acid, oxalic acid, hydrochloric acid, sulfamic acid or tartaric acid
It is one or more.
Preferably, it is described add acid solution after solution pH value in the range of 4.0-6.0.
Preferably, the amount for Silon being added in the step 2) is 1.0-1.8g.
Preferably, detailed process is as follows in the step 2)：Into step 1) acidity is sequentially added in gained liquid to be extracted
Solution and Silon, after washing above-mentioned gained mixed solution 3-5 times using ethanol, then using water washing 2-3 times, gained is washed
Liquid filtering is washed, gained supernatant is solution to be measured.
Preferably, the volume fraction of the ethanol is 80-85%.
Preferably, step 3) the neutral and alkali conditioning agent in sodium acid carbonate, sodium hydroxide, ammoniacal liquor or calcium oxide one
Kind is a variety of.
Preferably, scope of the pH value of solution to be measured in 7.0-7.5 after being adjusted in the step 3) using alkaline conditioner
It is interior.
Preferably, the detection method of a kind of colouring agent aberration, it is applied to diammonium hydrogen phosphate fertilizer coloring agent aberration
Detection in.
The invention provides a kind of detection method of colouring agent aberration, comprise the following steps：
1) sample is dissolved in edta solution and acetone soln successively, filtered, gained supernatant is to treat
Extract solution；
2) acid solution and Silon are sequentially added in gained liquid to be extracted into step 1), washs above-mentioned gained mixing
Solution simultaneously filters, and gained supernatant is solution to be measured；
3) regulating step 2) in gained solution to be measured acid-base value, measure its chromatic value, gained chromatic value is colouring agent
Chromatic value.
Sample is dissolved in edta solution and acetone soln by the present invention successively first, is filtered, gained supernatant
Liquid is liquid to be extracted；Wherein, the volume ratio of the edta solution and acetone soln is 2-5:1；Will in the present invention
The purpose that sample is dissolved in edta solution is that metal ion has certain color, ethylenediamine tetra-acetic acid molecule
In have two amino nitrogen atoms and four carboxylic oxygen atoms, the very strong coordination atom of its six complexing powers can be bonded with metal ion,
It can both be used as quadridentate ligand, can be used as sexidentate ligand again, and the ligancy of most metal ions is 4 or 6, because
This, in general, no matter metal ion is divalence, trivalent or other valence states, can be complexed with ethylenediamine tetra-acetic acid
Reaction, form 1：1 complex compound, and metal ion is sheltered, eliminate interference of the metal ion to measurement result.Wherein, the application
Also propose sample being dissolved in acetone soln, it is intended that eliminating influence of the organic impurities to measurement result, acetone is one
The good organic solvent of kind, both with fat-soluble, it may have water-soluble.Fat-soluble to wash impurity off, water solubility can make water solubility
Impurity wash away, and in organic solvent acetone boiling point than relatively low, it is readily volatilized fall, therefore, using acetone remove it is organic miscellaneous
The interference of confrontation measurement result.
Secondly, acid solution and Silon are sequentially added into gained liquid to be extracted, above-mentioned gained is washed using ethanol
After mixed solution 3-5 times, then using water washing 2-3 times, gained cleaning solution is filtered, gained supernatant is solution to be measured.Its
In, one or more of the acid solution in citric acid, oxalic acid, hydrochloric acid, sulfamic acid or tartaric acid, and control the pH of solution
In the range of 4.0-6.0.The purpose that the application proposes to add acid solution into gained liquid to be extracted is：1) solution is adjusted
Acid-base value, make the aobvious acidity of solution, extract pigment for lower step and prepare；2) the application proposes particularly preferred lemon in acid solution
Acid is used as acid regulator, the reason is that citric acid can be eliminated in diammonium hydrogen phosphate on the premise of other impurities are not introduced
The interference of part metals ion and ammonium ion to testing result.Wherein, the purpose of Silon is added into the extract solution of gained
It is, polyamide is to polymerize the high-molecular compound formed by amido link, and its amide groups can be with hydroxyl phenols, acids, quinones, nitre
Base class compound is adsorbed with Hydrogenbond, has preferable enrichment for water miscible pigment；Silon is in acidity
Under the conditions of, pigment can be adsorbed to its surface, and in the basic conditions, the pigment of eluting surface.Therefore, by adjusting solution
Acid-base value, pigment is adsorbed or eluted, and reach the purpose of measurement pigment chromatic value.Wherein, the application also proposes to use
Ethanol washs above-mentioned solution, it is intended that removing impurity.
Finally, the acid-base value of regulation gained solution to be measured, measures chromatic value, gained chromatic value is the colourity of colouring agent
Value, wherein, one or more of the alkaline conditioner in sodium acid carbonate, sodium hydroxide, ammoniacal liquor or calcium oxide, solution
PH value is in the range of 7.0-7.5.Wherein, the purpose for adjusting solution acid alkalinity is, in the basic conditions, makes adsorbed color
Element is fully eluted out, and so as to measure chromatic value, it is required to judge whether it meets.Wherein, alkaline conditioner is selected from sodium hydroxide,
The reason is that on the premise of foreign ion is not introduced, solution is adjusted to alkalescence condition, wherein, control the mesh of solution ph
Be, the application draws pH value in the range of 7.0-7.5 through test of many times, the elution best results of pigment.
The positive achievement that the present invention obtains is：
On the premise of eliminating metal ion and test result disturbed, pigment after extraction coloring in Diammonium phosphate (DAP) and to it
Chromatic value is tested, and the fertilizer that screening is met demand is sold.This method reappearance is higher, and test result is more
It is stable.
Embodiment
In order that those skilled in the art more fully understands technical scheme, with reference to specific embodiment pair
The present invention is described in further detail.
Diammonium hydrogen phosphate fertilizer is a kind of critically important fertilizer, because it is simultaneously containing two kinds of nitrogen, phosphorus nutrients, Ji Hushi
For being widely used in various crops and soil, it can not only be used as base manure but also can be used in top dressing, and conduct
During the base fertilizer of complex fertilizer, being mixed with other fertilizer ginseng has good compatibility.China's phosphate rock resource has compared with horn of plenty
According to the statistical result of US Geological Survey in data, based on reserves and reserves basis, the phosphorus ore in China in 2002 has been verified
Total resources is only second to Morocco, occupies the 2nd, the world.By 2007, shared high-concentration phosphate compound fertilizerses manufacturing enterprise 100 of China
Family, phosphate fertilizer production are risen to 16,230,000 tons of phosphorus pentoxides of 06 year by 4,560,000 tons of phosphorus pentoxides of 1991, are only second to U.S.
State, the 2nd is occupied in the world, consumption figure is the first in the nation.This also means that China plays this local products high-concentration phosphate compound fertilizerses
For the key player of agriculture stimulation treatment.
Pure diammonium hydrogen phosphate is a kind of white crystal or in powdered, and the phosphoric acid hydrogen in chemical fertilizer industry production
Two ammoniums, due to various aspects, the finished product produced typically is unable to reach preferable white, but with the phosphorus used
There are many color problems in the reasons such as sour source difference.Such as khaki, brown color, celadon, furvous, ash is presented in color
Concentration color occurs in the diammonium hydrogen phosphate product produced in the different color of the depth, or even production in one day sometimes；Separately
Outer product there is also bleach, it is local bleach, the inside and outside change such as irregular colour flower phenomenon.
The reason for causing diammonium hydrogen phosphate color problem comes from different aspects, mainly has：
1) phosphorus ore source
Phosphorus ore for producing phosphoric acid is different, in the phosphoric acid liquid that wet production comes out contained impurity in phosphoric acid and ammonia and
In course of reaction, a series of compound can be formed, these complicated compounds are general jelly, to the physics of ammonium phosphate slip
The influence of property and color is very big, so as to which when carrying out the production of diammonium hydrogen phosphate, the difference of color can be presented in the product of output
It is different.
2) phosphoric acid quality
The industrial ardealite containing substantial amounts of active silica and difficult precipitation in used phosphoric acid liquid of ammophos
Deng impurity, these materials not only make phosphoric acid liquid be not easy to clarify in time, but also easily form substantial amounts of colloid molecules group, in phosphoric acid and
In the reaction of ammonia, it will the intermolecular adhesion of heavy damage diammonium hydrogen phosphate, decline the intensity of Diammonium phosphate (DAP) particle, influence
The appearance color of diammonium phosphate product.
3) the production operation method and process conditions of Diammonium phosphate (DAP)
Such a influence essentially consists in the influence of initial start-up process and neutralization reaction condition on production color.Traditional original
Beginning starting method can usually make neutralize slip in neutralization chamber or longer or oversize neutralizing tower residence time, with ammonifying process
Carry out, sour degree of neutralization is also improved constantly, and the impurity in phosphoric acid sequentially forms the substantial amounts of white molten thing of Chinese holly, and the silicon dissolved in acid also can
Silica gel is formed in N-process, and then makes the color of finished product Diammonium phosphate (DAP) grey, it is uneven.Neutralization reaction condition pair
The influence of product colour is mainly manifested in when reaction temperature is high, and sour concentration is high, and neutralization chamber liquid level is low, and the residence time is short, all can
Make diammonium phosphate slurry color burn, on the contrary, will then cause slurry color thin out or even greyish white.
4) degree of neutralization
What degree of neutralization represented is the neutralization Chengdu of ammonia and phosphoric acid, during real reaction, ammonia and phosphatase reaction generation phosphorus
MAP continues to react generation Diammonium phosphate (DAP), or even triammonium phosphate people with ammonia a sour ammonium simultaneously, but triammonium phosphate is extremely unstable,
Become Diammonium phosphate (DAP) with regard to ammonia can be released at normal temperatures, therefore control the degree of neutralization of reaction to be allowed in certain scope, generate
Material be MAP and the mixture of Diammonium phosphate (DAP).Different shapes is presented with the difference of degree of neutralization in impurity in phosphoric acid
State.
To sum up, at this stage in fertilizer industry to being a kind of conventional side to fertilizer coloring in the processing of these color problems
Method.And different batches are prepared the difference or different batches of ammonia and phosphoric acid degree of neutralization in Diammonium phosphate (DAP) and colouring agent color are prepared
The reasons such as the difference of angle value so that the chromatic value that each batch produces Diammonium phosphate (DAP) after coloring has certain deviation, influences
The presentation quality of its product, so as to influence to sell.Therefore, people are tested the chromatic value of Diammonium phosphate (DAP) after coloring, screening
The fertilizer for being met demand is sold.And the method for the chromatic value of Diammonium phosphate (DAP) is less after being coloured currently for detection, and
The reappearance of method is relatively low, and test result is unstable.In view of this, the application provides a kind of detection method of colouring agent aberration,
It is on the premise of eliminating metal ion and test result is disturbed, pigment after extraction coloring in Diammonium phosphate (DAP) and to its chromatic value
Tested, the fertilizer that screening is met demand is sold.This method reappearance is higher, and test result is relatively stable.
Sample is dissolved in edta solution and acetone soln by the present invention successively first, is filtered, gained supernatant
Liquid is liquid to be extracted；Wherein, the volume ratio of the edta solution and acetone soln is 2-5:1；Will in the present invention
The purpose that sample is dissolved in edta solution is that metal ion has certain color, ethylenediamine tetra-acetic acid molecule
In have two amino nitrogen atoms and four carboxylic oxygen atoms, the very strong coordination atom of its six complexing powers can be bonded with metal ion,
It can both be used as quadridentate ligand, can be used as sexidentate ligand again, and the ligancy of most metal ions is 4 or 6, because
This, in general, no matter metal ion is divalence, trivalent or other valence states, can be complexed with ethylenediamine tetra-acetic acid
Reaction, form 1：1 complex compound, and metal ion is sheltered, eliminate interference of the metal ion to measurement result.Wherein, the application
Also propose sample being dissolved in acetone soln, it is intended that eliminating influence of the organic impurities to measurement result, acetone is one
The good organic solvent of kind, both with fat-soluble, it may have water-soluble.Fat-soluble to wash impurity off, water solubility can make water solubility
Impurity wash away, and in organic solvent acetone boiling point than relatively low, it is readily volatilized fall, therefore, using acetone remove it is organic miscellaneous
The interference of confrontation measurement result.
Secondly, acid solution and Silon are sequentially added into gained liquid to be extracted, above-mentioned gained is washed using ethanol
After mixed solution 3-5 times, then using water washing 2-3 times, gained cleaning solution is filtered, gained supernatant is solution to be measured.Its
In, one or more of the acid solution in citric acid, oxalic acid, hydrochloric acid, sulfamic acid or tartaric acid, and control the pH of solution
In the range of 4.0-6.0.The purpose that the application proposes to add acid solution into gained liquid to be extracted is：1) solution is adjusted
Acid-base value, make the aobvious acidity of solution, extract pigment for lower step and prepare；2) the application proposes particularly preferred lemon in acid solution
Acid is used as acid regulator, the reason is that citric acid can be eliminated in diammonium hydrogen phosphate on the premise of other impurities are not introduced
The interference of part metals ion and ammonium ion to testing result.Wherein, the purpose of Silon is added into the extract solution of gained
It is, polyamide is to polymerize the high-molecular compound formed by amido link, and its amide groups can be with hydroxyl phenols, acids, quinones, nitre
Base class compound is adsorbed with Hydrogenbond, has preferable enrichment for water miscible pigment；Silon is in acidity
Under the conditions of, pigment can be adsorbed to its surface, and in the basic conditions, the pigment of eluting surface.Therefore, by adjusting solution
Acid-base value, pigment is adsorbed or eluted, and reach the purpose of measurement pigment chromatic value.Wherein, the application also proposes to use
Ethanol washs above-mentioned solution, it is intended that removing impurity.
Finally, the acid-base value of regulation gained solution to be measured, measures chromatic value, gained chromatic value is the colourity of colouring agent
Value, wherein, one or more of the alkaline conditioner in sodium acid carbonate, sodium hydroxide, ammoniacal liquor or calcium oxide, solution
PH value is in the range of 7.0-7.5.Wherein, the purpose for adjusting solution acid alkalinity is, in the basic conditions, makes adsorbed color
Element is fully eluted out, and so as to measure chromatic value, it is required to judge whether it meets.Wherein, alkaline conditioner is selected from sodium hydroxide,
The reason is that on the premise of foreign ion is not introduced, solution is adjusted to alkalescence condition, wherein, control the mesh of solution ph
Be, the application draws pH value in the range of 7.0-7.5 through test of many times, the elution best results of pigment.
Wherein, sample value of chromatism is calculated as follows shown in formula：
△ E --- sample total color difference value；
L1、a1、b1--- colour photometer determination sample reading；
L0、a0、b0--- standard sample value of chromatism.
Wherein, the concept of standard sample value of chromatism is introduced in above formula, thinks the influence for eliminating mother liquor to institute's colour examining difference.
Technical scheme provided by the invention is a kind of detection method of colouring agent aberration, is comprised the following steps：
1) it is 2-5 that sample is dissolved in volume ratio successively:In 1 edta solution and acetone soln, filtering, institute
It is liquid to be extracted to obtain supernatant；
2) acid solution and 1.0-1.8g Silon are sequentially added in gained liquid to be extracted into step 1), used
After 80-85% ethanol washs above-mentioned gained mixed solution 3-5 times, then using water washing 2-3 times, gained cleaning solution is filtered,
Gained supernatant is solution to be measured；
3) regulating step 2) in gained solution to be measured acid-base value, measure its chromatic value, gained chromatic value is colouring agent
Chromatic value.
Wherein, one or more of the acid solution in citric acid, oxalic acid, hydrochloric acid, sulfamic acid or tartaric acid；
Wherein, it is described add acid solution after solution pH value in the range of 4.0-6.0；Wherein, it is described to be adjusted using alkaline conditioner
Save the acid-base value of solution to be measured, one kind in sodium acid carbonate, sodium hydroxide, ammoniacal liquor or calcium oxide of the alkaline conditioner or
A variety of, the pH value of solution to be measured is in the range of 7.0-7.5 after the regulation.
Below in conjunction with embodiments of the invention, technical scheme is clearly and completely described, it is clear that
Described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on the implementation in the present invention
Example, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, is belonged to
The scope of protection of the invention.
Embodiment 1：
A kind of detection method of colouring agent aberration, comprises the following steps：
1) sample is dissolved in volume ratio successively for 2：In 1 edta solution and acetone soln, filtering, gained
Supernatant is liquid to be extracted；
2) citric acid and 1.5g Silons are sequentially added in gained liquid to be extracted into step 1), is washed using 85% ethanol
After washing above-mentioned gained mixed solution 3 times, then using water washing 3 times, gained cleaning solution is filtered, gained supernatant is to be measured molten
Liquid；
3) acid-base value of solution to be measured is adjusted using sodium hydroxide, the pH value for making solution after regulation is 7.2, measures its colourity
Value, gained chromatic value is the chromatic value of colouring agent.
Wherein, solution ph is adjusted to 5.0 after adding citric acid in step 2).
By a kind of above-mentioned detection method of colouring agent aberration, the detection applied to diammonium hydrogen phosphate fertilizer coloring agent aberration
In.
Value of chromatism is considered as standard aberration, the data obtained L as obtained by the above method in the application0：29.34；a0：
21.30；b0：11.89.
Embodiment 2：
It is measured using method in embodiment 1, the colour difference of sample is calculated by formula for gained chromatic value, probes into
Needed for whether the fertilizer meets, at the same time, by repeatedly testing the reappearance and stability of test this method, the data obtained is such as
Shown in table 1：
Table 1
In table 1, sequence number 1 and sequence number 2 are the test result of sample under equal conditions in embodiment 1, pass through colour difference
Test result understand that the method for testing has higher a reappearance and stability, sequence number 3 is to take different samples by calculating sample
The colour difference of product, probe into needed for whether the fertilizer meet, by experimental data, its colour difference meets institute no more than 2.5
Need.
Embodiment 3：
A kind of detection method of colouring agent aberration, comprises the following steps：
1) sample is dissolved in volume ratio successively for 4：In 1 edta solution and acetone soln, filtering, gained
Supernatant is liquid to be extracted；
2) citric acid and 1.8g Silons are sequentially added in gained liquid to be extracted into step 1), is washed using 80% ethanol
After washing above-mentioned gained mixed solution 5 times, then using water washing 2 times, gained cleaning solution is filtered, gained supernatant is to be measured molten
Liquid；
3) acid-base value of solution to be measured is adjusted using sodium hydroxide, the pH value for making solution after regulation is 7.5, measures its colourity
Value, gained chromatic value is the chromatic value of colouring agent.
Wherein, solution ph is adjusted to 6.0 after adding citric acid in step 2).
By a kind of above-mentioned detection method of colouring agent aberration, the detection applied to diammonium hydrogen phosphate fertilizer coloring agent aberration
In.
Value of chromatism is considered as standard aberration, the data obtained L as obtained by the above method in the application0：28.89；a0：
21.53；b0：11.60.
Embodiment 4：
It is measured using method in embodiment 3, the colour difference of sample is calculated by formula for gained chromatic value, probes into
Needed for whether the fertilizer meets, at the same time, by repeatedly testing the reappearance and stability of test this method, the data obtained is such as
Shown in table 2：
Table 2
In table 2, sequence number 1 and sequence number 2 are the test result of sample under equal conditions in embodiment 1, pass through colour difference
Test result understand that the method for testing has higher a reappearance and stability, sequence number 3 is to take different samples by calculating sample
The colour difference of product, probe into needed for whether the fertilizer meet, by experimental data, its colour difference meets institute no more than 2.5
Need.
Comparative example 1：
A kind of detection method of colouring agent aberration, comprises the following steps：
1) sample is dissolved in successively and adds citric acid and 1.5g Silons, above-mentioned gained is washed using 85% ethanol and mixed
After closing solution 3 times, then using water washing 3 times, gained cleaning solution is filtered, gained supernatant is solution to be measured；
2) acid-base value of solution to be measured is adjusted using sodium hydroxide, the pH value for making solution after regulation is 7.2, measures its colourity
Value, gained chromatic value is the chromatic value of colouring agent.
Wherein, solution ph is adjusted to 5.0 after adding citric acid in step 1).
By a kind of above-mentioned detection method of colouring agent aberration, the detection applied to diammonium hydrogen phosphate fertilizer coloring agent aberration
In.
Value of chromatism is considered as standard aberration, the data obtained L as obtained by the above method in the application0：29.25；a0：
22.11；b0：11.20.
Comparative example 2：
Tested using method in comparative example 1, the colour difference of sample is calculated by formula for gained chromatic value, probes into
Needed for whether the fertilizer meets, at the same time, by repeatedly testing the reappearance and stability of test this method, the data obtained is such as
Shown in table 3：
Table 3
In table 3, sequence number 1 and sequence number 2 are the test result of sample under equal conditions in comparative example 1, pass through colour difference
Test result understand that the method for testing has higher a reappearance and stability, sequence number 3 is to take different samples by calculating sample
The colour difference of product, probe into needed for whether the fertilizer meet, by experimental data, its colour difference meets institute no more than 2.5
Need.
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch and also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of detection method of colouring agent aberration, it is characterised in that comprise the following steps：
1) sample is dissolved in edta solution and acetone soln successively, filtered, gained supernatant is as to be extracted
Liquid；
2) acid solution and Silon are sequentially added in gained liquid to be extracted into step 1), washs above-mentioned gained mixed solution
And filter, gained supernatant is solution to be measured；
3) regulating step 2) in gained solution to be measured acid-base value, measure its chromatic value, gained chromatic value is the color of colouring agent
Angle value.
A kind of 2. detection method of colouring agent aberration according to claim 1, it is characterised in that second two in the step 1)
The volume ratio of amine tetrem acid solution and acetone soln is 2-5:1.
3. a kind of detection method of colouring agent aberration according to claim 1, it is characterised in that acid in the step 2)
One or more of the solution in citric acid, oxalic acid, hydrochloric acid, sulfamic acid or tartaric acid.
4. a kind of detection method of colouring agent aberration according to claim 1, it is characterised in that added in the step 2)
The pH value of solution is in the range of 4.0-6.0 after acid solution.
5. a kind of detection method of colouring agent aberration according to claim 1, it is characterised in that added in the step 2)
The amount of Silon is 1.0-1.8g.
6. a kind of detection method of colouring agent aberration according to claim 1, it is characterised in that specific in the step 2)
Process is as follows：Acid solution and Silon are sequentially added in gained liquid to be extracted into step 1), is washed using ethanol above-mentioned
After gained mixed solution 3-5 times, then using water washing 2-3 times, gained cleaning solution is filtered, gained supernatant is to be measured molten
Liquid.
A kind of 7. detection method of colouring agent aberration according to claim 6, it is characterised in that the volume integral of the ethanol
Number is 80-85%.
A kind of 8. detection method of colouring agent aberration according to claim 1, it is characterised in that the step 3) neutral and alkali
One or more of the conditioning agent in sodium acid carbonate, sodium hydroxide, ammoniacal liquor or calcium oxide.
9. a kind of detection method of colouring agent aberration according to claim 1, it is characterised in that used in the step 3)
The pH value of solution to be measured is in the range of 7.0-7.5 after alkaline conditioner regulation.
10. a kind of detection method of colouring agent aberration according to claim 1-9, it is characterised in that it is applied to phosphoric acid
In the detection of the ammonium fertilizer colouring agent aberration of hydrogen two.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710804606.4A CN107703129B (en) | 2017-09-08 | 2017-09-08 | Method for detecting chromatic aberration of colorant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710804606.4A CN107703129B (en) | 2017-09-08 | 2017-09-08 | Method for detecting chromatic aberration of colorant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107703129A true CN107703129A (en) | 2018-02-16 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071673A (en) * | 1991-10-18 | 1993-05-05 | 默克专利股份有限公司 | Pigment |
| CN101644681A (en) * | 2008-08-05 | 2010-02-10 | 潘华 | Method for quickly detecting food synthetic pigment and detection box of food synthetic pigment |
| CN101861366A (en) * | 2007-11-15 | 2010-10-13 | 惠普发展公司，有限责任合伙企业 | Polymer encapsulated pigments |
| CN102279178A (en) * | 2010-06-10 | 2011-12-14 | 东北农业大学 | Method for analyzing and testing body cell content in raw milk |
| CN103091314A (en) * | 2013-01-16 | 2013-05-08 | 深圳市计量质量检测研究院 | Rapid detection method for water-soluble azo dyes in foods |
| CN105115965A (en) * | 2015-07-27 | 2015-12-02 | 南昌大学 | Soft drink synthetic pigment fast detection method and kit |
| CN106370748A (en) * | 2016-08-25 | 2017-02-01 | 浙江省农业科学院 | Test method and sample pretreatment method of flouroquinolone medicine in organic fertilizer |
-
2017
- 2017-09-08 CN CN201710804606.4A patent/CN107703129B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071673A (en) * | 1991-10-18 | 1993-05-05 | 默克专利股份有限公司 | Pigment |
| CN101861366A (en) * | 2007-11-15 | 2010-10-13 | 惠普发展公司，有限责任合伙企业 | Polymer encapsulated pigments |
| CN101644681A (en) * | 2008-08-05 | 2010-02-10 | 潘华 | Method for quickly detecting food synthetic pigment and detection box of food synthetic pigment |
| CN102279178A (en) * | 2010-06-10 | 2011-12-14 | 东北农业大学 | Method for analyzing and testing body cell content in raw milk |
| CN103091314A (en) * | 2013-01-16 | 2013-05-08 | 深圳市计量质量检测研究院 | Rapid detection method for water-soluble azo dyes in foods |
| CN105115965A (en) * | 2015-07-27 | 2015-12-02 | 南昌大学 | Soft drink synthetic pigment fast detection method and kit |
| CN106370748A (en) * | 2016-08-25 | 2017-02-01 | 浙江省农业科学院 | Test method and sample pretreatment method of flouroquinolone medicine in organic fertilizer |
Non-Patent Citations (5)
| Title |
|---|
| 何世杰: "影响磷酸二铵产品颜色的因素分析", 《磷肥与复肥》 * |
| 朱洪法: "《生活化学品与健康》", 30 April 2013, 金盾出版社 * |
| 李晓莉: "《分析化学》", 31 May 2017, 中国轻工业出版社 * |
| 经久艳: "磷酸二铵专用着色剂的制备与研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 谢汪洋: "磷酸二铵存储过程中外观质量变化的研究与应用", 《中国优秀硕士学位论文全文数据库 工程科技I辑 2015年期》 * |
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