CN110196241A - A kind of selective enumeration method iron ion test paper and preparation method thereof - Google Patents
A kind of selective enumeration method iron ion test paper and preparation method thereof Download PDFInfo
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- CN110196241A CN110196241A CN201910421272.1A CN201910421272A CN110196241A CN 110196241 A CN110196241 A CN 110196241A CN 201910421272 A CN201910421272 A CN 201910421272A CN 110196241 A CN110196241 A CN 110196241A
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- test paper
- iron ion
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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Abstract
A kind of selective enumeration method iron ion test paper of the present invention and preparation method thereof; include the following steps: to sequentially add hydroquinone, polyethylene glycol -200, hexamethylene diisocyanate, water removal tetrahydrofuran, triethylene diamine in container; condensing reflux reaction is carried out under nitrogen protection; acetone is added after reaction and removes by-product, is filtered under diminished pressure and obtains final product;It takes final product to be dissolved in the mixed solution of acetonitrile and water, after final product all dissolution, non-blooming test paper is put into immersion in mixed solution, dry, pressing obtains selective enumeration method iron ion test paper.Material obtained by the present invention is for the method for other detection iron ions, and method is simple, and testing cost is low.For the reagent of other fluorescence detection iron ions, forming steps are simple, and stability is good, are capable of the presence of selective detection iron ion under various circumstances.
Description
Technical field
The present invention relates to a kind of test paper and preparation method thereof, in particular to a kind of selective enumeration method iron ion test paper and its system
Preparation Method belongs to metal ion detection field.
Background technique
Ferro element is widely present in nature, accounts for about the 5.1% of earth crustal mass.In human body, ferro element be also can not
Or one of scarce microelement, iron ion are mainly present in liver, spleen, in marrow in the form of hemoglobin.Absorb excessive iron
It will also result in body metabolism disorder, threaten human health.Thus it is guaranteed that the iron ion in drinking water containing debita spissitudo is very
It is necessary to.In industrial aspect, if iron ion is attached in metallic conduit or equipment, metallic conduit or equipment, shadow can be corroded
Ring its normal operation.Therefore, can have a kind of method of the iron ion in highly selective, highly sensitive detection varying environment is
It is very important.
The method of detection iron ion has very much, such as spectrophotometry, chromatography, electrochemical process etc. being capable of selective enumeration methods
The presence of iron ion, but it is complicated for operation, testing cost is excessively high the disadvantages of but limit its application.And fluorescence detection is with simple
Conveniently, the advantages that high sensitivity and by wide coverage.The Chinese patent of Publication No. CN106565679A discloses a kind of trivalent
Iron ion detection reagent and its preparation method and application, the reagent being capable of selective qualitative detection iron under aqueous environment
Ion.The Chinese patent of Publication No. CN108593616A also discloses a kind of reagent of fluorescence detection ferric ion, should
Reagent is made by the method for electrochemistry, equally can selective qualitative detection iron ion.
The above technology is disadvantageous in that jointly, although obtained reagent can selective detection various concentration not
With the iron ion of environment, but the obtained method of its reagent is sufficiently complex, and not recyclable and easily right as detection reagent itself
Sample pollutes.In addition to this, the stability of reagent also becomes a big problem.And there is not yet related iron ion Test paper
Report.
Summary of the invention
The present invention is simple in order to provide a kind of method, the low selective enumeration method iron ion test paper of testing cost and its preparation side
Method.
The object of the present invention is achieved like this:
A kind of preparation method of selective enumeration method iron ion test paper, includes the following steps:
Step 1: by hydroquinone, polyethylene glycol -200, hexamethylene diisocyanate, water removal tetrahydrofuran, triethylene
Diamines sequentially adds in container, and condensing reflux reaction is carried out under nitrogen protection, and acetone is added after reaction and removes by-product, subtracts
Press filtration obtains final product;
Step 2: taking final product to be dissolved in the mixed solution of acetonitrile and water, after final product all dissolution, by nothing
The test paper of fluorescence is put into immersion in mixed solution, dry, pressing obtains selective enumeration method iron ion test paper.
The invention also includes features some in this way:
1, the hydroquinone is 5-10mM, polyethylene glycol -200 is 5-10mM, hexamethylene diisocyanate 5-
15mM, water removal tetrahydrofuran be 0.1-1mM, triethylene diamine 5-10mM;
2, the volume ratio of the acetonitrile and water is 1:1;
3, the condensing reflux reaction time is 6-9h, and reaction temperature is 75 DEG C.
A kind of selective enumeration method iron ion test paper, is prepared from the following steps:
Step 1: by hydroquinone, polyethylene glycol -200, hexamethylene diisocyanate, water removal tetrahydrofuran, triethylene
Diamines sequentially adds in container, and condensing reflux reaction is carried out under nitrogen protection, and acetone is added after reaction and removes by-product, subtracts
Press filtration obtains final product;
Step 2: taking final product to be dissolved in the mixed solution of acetonitrile and water, after final product all dissolution, by nothing
The test paper of fluorescence is put into immersion in mixed solution, dry, pressing obtains selective enumeration method iron ion test paper.
The hydroquinone is 5-10mM, polyethylene glycol -200 is 5-10mM, hexamethylene diisocyanate 5-15mM,
Remove water tetrahydrofuran be 0.1-1mM, triethylene diamine 5-10mM;
The volume ratio of the acetonitrile and water is 1:1;
The condensing reflux reaction time is 6-9h, and reaction temperature is 75 DEG C.
Compared with prior art, the beneficial effects of the present invention are:
Material obtained by the present invention is for the method for other detection iron ions, and method is simple, and testing cost is low.
For the reagent of other fluorescence detection iron ions, forming steps are simple, and stability is good, can select under various circumstances
Property detection iron ion presence.
Detailed description of the invention
Fig. 1 is selective enumeration method iron ion schematic diagram of the present invention.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.The present embodiment is based on the technical solution of the present invention
Implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to following realities
Apply example.
A kind of selective enumeration method ferric ion test paper and its preparation preparation method, preparation step are as follows:
Step 1, by hydroquinone (5-10mM), polyethylene glycol -200 (PEG-200) (5-10mM), two isocyanide of hexa-methylene
Acid esters (HDI) (5-15mM), water removal tetrahydrofuran (THF) (0.1-1mM), triethylene diamine (TEDA) (5-10mM) are successively added
In three-necked flask, 75 DEG C of condensing refluxes of nitrogen protection react 6-9h.Proper amount of acetone is added after reaction and removes by-product, decompression
Filtering obtains final product;
Step 2, appropriate product is taken to be dissolved in VAcetonitrile: VWaterIn the mixed solution of=1:1, to product all dissolution with mix it is molten
After liquid, non-blooming test paper is put into mixed solution and is soaked for a period of time, flattened after it is completely dried to get used in
Test paper.
Embodiment 1:
A kind of preparation method of selective enumeration method ferric ion test paper, preparation step are as follows:
Step 1, sequentially added in three-necked flask hydroquinone (8mM), PEG-200 (5.90mM), HDI (10mM),
TEDA (3mM), water removal THF (0.3mM) are successively added in three-necked flask, and the lower 75 DEG C of condensing refluxes of nitrogen protection react 8h.Reaction
After appropriate ether removal by-product is added, be filtered under diminished pressure and obtain final product;
Step 2,0.10g product is taken to be dissolved in 50mL VAcetonitrile: VWaterIn=1:1 mixed solution, all dissolved to product and mixed
After closing solution, non-blooming test paper is put into mixed solution and is soaked for a period of time, flattened after it is completely dried to get arriving
Test paper used.
Embodiment 2:
A kind of preparation method of selective enumeration method ferric ion test paper, preparation step are as follows:
Step 1, sequentially added in three-necked flask hydroquinone (8mM), PEG-200 (5.90mM), HDI (10mM),
TEDA (3mM), water removal THF (0.3mM) are successively added in three-necked flask, and the lower 75 DEG C of condensing refluxes of nitrogen protection react 8h.Reaction
After appropriate ether removal by-product is added, be filtered under diminished pressure and obtain final product;
Step 2,0.50g product is taken to be dissolved in 100mL VAcetonitrile: VWaterIn=1:1 mixed solution, all dissolved to product and mixed
After closing solution, non-blooming test paper is put into mixed solution and is soaked for a period of time, flattened after it is completely dried to get arriving
Test paper used.
Application of the test paper in terms of detecting iron ion
That prepares same concentrations contains Li+, Na+, Mg2+, Al3+, K+, Ca2+, Co2+, Ni+, Cu2+, Zn2+, Ba2+And Fe3+'s
Solution.A small amount of solution is taken to be dripped on different test paper respectively.As a result as shown in Figure 1, under 365nm ultraviolet lamp, Fe is instilled3+Test paper
Fluorescent quenching, and the test paper fluorescence for instilling other ions does not have significant change.Therefore, the detection iron of the present invention property of can choose from
Son.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and saying herein
Bright General Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to above-mentioned realities
Example, those skilled in the art's announcement according to the present invention are applied, improvement and modification made without departing from the scope of the present invention all should
Within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of selective enumeration method iron ion test paper, characterized in that include the following steps:
Step 1: by hydroquinone, polyethylene glycol -200, hexamethylene diisocyanate, water removal tetrahydrofuran, triethylene diamine
It sequentially adds in container, condensing reflux reaction is carried out under nitrogen protection, acetone is added after reaction and removes by-product, depressurized
Filter obtains final product;
Step 2: taking final product to be dissolved in the mixed solution of acetonitrile and water, after final product all dissolution, by unstressed configuration
Test paper be put into mixed solution and impregnate, is dry, flattening and obtain selective enumeration method iron ion test paper.
2. the preparation method of selective enumeration method iron ion test paper according to claim 1, characterized in that the hydroquinone
It is 5-10mM for 5-10mM, polyethylene glycol -200, hexamethylene diisocyanate 5-15mM, water removal tetrahydrofuran are 0.1-
1mM, triethylene diamine 5-10mM.
3. the preparation method of selective enumeration method iron ion test paper according to claim 1 or 2, characterized in that the acetonitrile
Volume ratio with water is 1:1.
4. the preparation method of selective enumeration method iron ion test paper according to claim 1 or 2, characterized in that the condensation
Reflux time is 6-9h, and reaction temperature is 75 DEG C.
5. the preparation method of selective enumeration method iron ion test paper according to claim 3, characterized in that the condensing reflux
Reaction time is 6-9h, and reaction temperature is 75 DEG C.
6. a kind of selective enumeration method iron ion test paper, characterized in that be prepared from the following steps:
Step 1: by hydroquinone, polyethylene glycol -200, hexamethylene diisocyanate, water removal tetrahydrofuran, triethylene diamine
It sequentially adds in container, condensing reflux reaction is carried out under nitrogen protection, acetone is added after reaction and removes by-product, depressurized
Filter obtains final product;
Step 2: taking final product to be dissolved in the mixed solution of acetonitrile and water, after final product all dissolution, by unstressed configuration
Test paper be put into mixed solution and impregnate, is dry, flattening and obtain selective enumeration method iron ion test paper.
7. selective enumeration method iron ion test paper according to claim 6, characterized in that the hydroquinone be 5-10mM,
Polyethylene glycol -200 is 5-10mM, hexamethylene diisocyanate 5-15mM, water removal tetrahydrofuran are 0.1-1mM, triethylene
Diamines is 5-10mM.
8. selective enumeration method iron ion test paper according to claim 6 or 7, characterized in that the volume of the acetonitrile and water
Than for 1:1.
9. selective enumeration method iron ion test paper according to claim 6 or 7, characterized in that when the condensing reflux reacts
Between be 6-9h, reaction temperature be 75 DEG C.
10. selective enumeration method iron ion test paper according to claim 8, characterized in that the condensing reflux reaction time
For 6-9h, reaction temperature is 75 DEG C.
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CN103172829A (en) * | 2013-03-21 | 2013-06-26 | 中国科学技术大学 | Preparation method of fluorescent waterborne polyurethane emulsion based on chromophore in diisocyanate |
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