CN106867510A - A kind of method of the carbon quantum dot and its detection arsenite for detecting arsenite - Google Patents
A kind of method of the carbon quantum dot and its detection arsenite for detecting arsenite Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
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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"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
Abstract
The invention discloses a kind of carbon quantum dot for detecting arsenite and its method for detection arsenite.The present invention is the graphite mould carbon quantum dot of templated synthesis nitrogen sulfur doping with sodium citrate, urea and mercaptoethylmaine（g‑CNSQDs）, then use dithiothreitol (DTT)（DTT）Cultivated by hydro-thermal carries out surface graft modification to it, obtains the graphite mould fluorescent carbon quantum dot that a large amount of sulfydryls and amido are contained in surface（SH‑g‑CNSQDs‑NH2）, by the interaction between amido, sulfydryl and arsenite, by As（III）With SH g CNSQDs NH2With reference to making SH g CNSQDs NH2Fluorescence significantly increase, so as to realize the detection function of sub- low-concentration arsenic hydrochlorate.Fluorescent carbon quantum dot prepared by the present invention is free of heavy metal, and low production cost has no toxic side effect, simple to operate to water quality sample non-secondary pollution, to the As of low content（III）Water sample has sensitive irritability and selection detection property.
Description
Technical field
The present invention relates to a kind of carbon quantum dot for detecting arsenite and its method for detection arsenite, belong to table
Face chemistry and optical sensing technology field.
Background technology
Arsenic is a kind of nonmetallic substance of generally existing in natural environment, and it mostlys come from the earth's crust rock in natural resources
Organoarsenic pesticide and feed addictive, fossil fuel, industrial wastewater in stone and mineral matter, and manual resource etc., and to people
Class harm most serious are the arsenic pollutions for quoting water, and arsenic has carcinogenicity.Arsenic is the material paid close attention in problem of environmental pollution
One of composition, its high sensitivity and high selectivity detection technique in various environment is very important.In general, it is inorganic
The arsenic poison of the more organic arsenide of arsenide and zero-valent state is much bigger, and arsenite toxicity is especially big, therefore detection food
It is critically important with the arsenite in drinking water.In decades recently, arsenite detection method and technology are continued to develop, example
Such as chromatograph mass spectrum analysis method, Atomic absorption emission spectrometry, but these methods are present, and testing cost is expensive, detecting step is multiple
Miscellaneous, the detection and analysis shortcomings such as the time is more long and sample process is complicated so that As（III）Specific environment in many fields
Can not be widely used in detection.
Carbon quantum dot is also called carbon nano-particles, generally by carbon nanomaterial stripping, size degradation or the condensation of small molecule carbon source, carbon
Change and formed, according to differences such as preparation, passivation modes, its surface can be a class diameter with various functions groups such as carboxyl, amino
Environment-friendly Novel Carbon Nanomaterials less than 10 nm.In addition to there is similar optical property to semiconductor-quantum-point, also
With toxicity is low, good biocompatibility, it is easy to extensive synthesis and functional modification, carbon source and self property diversity, prepares
The advantage such as with low cost and reaction condition is gentle, in bio-imaging, biomarker, bio-sensing and organic matter, metal ion, the moon
Ion, large biological molecule, gas detection and the aspect such as photocatalysis degradation organic contaminant, Photocatalyzed Hydrogen Production are received and closed extensively
Note.However, as a kind of surface nature diversity and the environment-friendly carbon nano-particle for being easy to functionalization, carbon nano-quantum point
Also many functions have to be developed.And recently by the carbon quantum dot of the surface sulfydryl modification of extensive concern, because its is many excellent
Characteristic such as high-light-fastness, physical and chemical stability high, good bio-compatibility water-soluble, high, detection high is selective and sensitive
Property and low production cost, allow its turn into detection arsenite fluorescence probe.Have what is be modified using surface at present
Fluorescent carbon quantum dot detects the As in water by fluorescent quenching or enhancement effect（III）, but these quantum dots mostly contain weight
Metal, to low concentration（5-10ppb）As（III）The detection of water sample is insensitive.
The content of the invention
Low concentration can be detected it is an object of the invention to provide one kind（5-10ppb）As（III）The carbon quantum dot of water sample.
The present invention is achieved by the following technical solutions：
A kind of carbon quantum dot for detecting arsenite（SH-g-CNSQDs-NH2）, its preparation method comprises the following steps：
（1）Prepare g-CNSQDs：
Sodium citrate, urea and mercaptoethylmaine and deionized water are mixed, solution A is obtained；Solution A is in 160-165 DEG C of 30 points of constant temperature
More than clock, obtain dark brown pulverulent solids as g-CNSQDs；
（2）Prepare SH-g-CNSQDs-NH2：
By DDT and g-CNSQDs and deionized water wiring solution-forming C；Solution C is small in 60-70 DEG C of hydro-thermal 20-24 under agitation
When, then dialyse more than 12 hours, collect solid；
The g-CNSQDs is the graphite mould carbon quantum dot of nitrogen sulfur doping；The DDT is dithiothreitol (DTT).
Above-mentioned carbon quantum dot, step（1）In, it is preferred that solution A was in 165 DEG C of constant temperature 30 minutes.
Above-mentioned carbon quantum dot, step（1）In, it is preferred that sodium citrate, urea and mercaptoethylmaine mass percent are 1:3:
3-8；It is furthermore preferred that sodium citrate, urea and mercaptoethylmaine mass percent are 1:3:5.
Above-mentioned carbon quantum dot, step（2）In, it is preferred that hydrothermal temperature is 65 DEG C.
Above-mentioned carbon quantum dot, step（2）In, it is preferred that the hydro-thermal time is 24h.
Above-mentioned carbon quantum dot, step（2）In, it is preferred that the mass ratio of DDT and g-CNSQDs is 1：2-5, it is furthermore preferred that
The mass ratio of DDT and g-CNSQDs is 1:4.
Above-mentioned carbon quantum dot, step（2）In, it is preferred that the g-CNSQDs is 2-6 relative to the consumption of deionized water:
24。
Above-mentioned carbon quantum dot, step（2）, it is preferred that first g-CNSQDs and deionized water are mixed, solution B is obtained；Again will
DTT is added in solution B, is uniformly mixing to obtain solution C.
Carbon quantum dot prepared by the present invention, is a kind of water miscible dark brown nanoscale solids particle powder, and particle diameter is
2-8nm, abbreviation SH-g-CNSQDs-NH2.SH-g-CNSQDs-NH prepared by the present invention2, surface contains a large amount of sulfydryls and amido,
By the interaction between amido, sulfydryl and arsenite（As (III) by the amido with graphite mould carbon quantum dot surface and
Sulfydryl is combined and is embedded into graphite mould carbon quantum dot）Make SH-g-CNSQDs-NH2Fluorescence significantly increase, it is low so as to realize
Concentration（5-10ppb）The detection function of arsenite.
One kind uses above-mentioned carbon quantum dot（SH-g-CNSQDs-NH2）The method for detecting arsenite,
By SH-g-CNSQDs-NH2With deionized water wiring solution-forming D, then with the hydrochloric acid-tromethamine buffer of 0.1mol/L
The pH value of solution D is adjusted to 7, solution E is obtained；
Arsenite aqueous liquid sample to be measured is mixed with solution E, solution F is obtained；
Solution F and solution E are carried out into fluorescence intensity comparative analysis with sepectrophotofluorometer；
The excitation wavelength of sepectrophotofluorometer is 280nm, launch wavelength is 350-550nm.
Above-mentioned detection method, it is preferred that SH-g-CNSQDs-NH in solution E2Mass content be 0.5-2%.
Beneficial effect：
Fluorescent carbon quantum dot prepared by the present invention is free of heavy metal, and low production cost has no toxic side effect, to water quality sample without
Secondary pollution, it is simple to operate, to detection As（III）With sensitive irritability and selectivity, it is not necessary to extra by large-scale inspection
Instrument is surveyed, step is simple, easy to operate, testing cost is cheap, sensitivity is high.
Specific embodiment
With reference to specific embodiment, the invention will be further described；Except as otherwise indicating, the number in embodiment
It is by weight.
Embodiment 1
The graphite mould carbon quantum dot of nitrogen sulfur doping（g-CNSQDs）Preparation：By 1 part of sodium citrate, 3 parts of urea and 5 parts of sulfydryl second
Amine is added in 24 parts of deionized waters, and obtaining solution after stirring is placed in reactor, in being heated 30 minutes at 160 DEG C, is obtained
To the powdered g-CNSQDs of dark brown solid.
Carbon quantum dot SH-g-CNSQDs-NH2Preparation:By 1 part of DDT（Dithiothreitol (DTT), similarly hereinafter）With 4 parts of g-CNSQDs
20 parts of deionized waters are added to, the solution being uniformly mixing to obtain is in hydro-thermal while stirring（65℃）Under the conditions of cultivate 24 hours, so
Dialyse 12 hours afterwards, obtain SH-g-CNSQDs-NH2。
The detection of arsenite in water sample：With the hydrochloric acid-tromethamine buffer and deionized water of 0.1mol/L by SH-
g-CNSQDs-NH2It is the aqueous solution E that 0.5%, pH value is 7 to be configured to mass fraction, takes 3ml for subsequent detection.By Asia to be measured
Arsenate aqueous liquid sample（Certain urban groundwater, arsenite content is 50ppb）1-2 drops are taken with glue head dropper instill solution E,
Shake up and obtain solution F, it is 350- that solution E, F are recorded into launch wavelength under 280nm excitation wavelengths with fluorescence spectrophotometry respectively
Fluorescence intensity under 550nm scopes.Result discovery, solution F（Contain arsenite）Peak fluorescence intensity be 318 (a.u, it is ultraviolet
Absorbance, similarly hereinafter), solution E（Do not contain arsenite）Peak fluorescence intensity is 78（a.u）, contrasting detection result solution F fluorescence
Intensity is apparently higher than solution E, and arsenite Detection results are obvious.
Embodiment 2
The graphite mould carbon quantum dot of nitrogen sulfur doping（g-CNSQDs）Preparation：By 1 part of sodium citrate, 3 parts of urea and 8 parts of sulfydryl second
Amine is added in 66 parts of deionized waters, and obtaining solution after stirring is placed in reactor, is heated 30 minutes at 160 DEG C, is obtained
To the powdered g-CNSQDs of dark brown solid.
Carbon quantum dot SH-g-CNSQDs-NH2Preparation:1 part of DDT and 5 part of g-CNSQDs is added to 20 parts of deionizations
Water, the solution being uniformly mixing to obtain is in hydro-thermal while stirring（65℃）Under the conditions of cultivate 24 hours, then dialyse 12 hours, obtain
SH-g-CNSQDs-NH2。
The detection of arsenite in water sample：With the hydrochloric acid-tromethamine buffer and deionized water of 0.1mol/L by SH-
g-CNSQDs-NH2It is the aqueous solution E that 1.5%, pH value is 7 to be configured to mass fraction, takes 4ml for subsequent detection.By Asia to be measured
Arsenate aqueous liquid sample（Certain urban drinking water, arsenite content is 5ppb）1-2 drops are taken with glue head dropper instill solution E,
Shake up and obtain solution F, it is 350- that solution E, F are recorded into launch wavelength under 280nm excitation wavelengths with fluorescence spectrophotometry respectively
Fluorescence intensity under 550nm scopes, as a result finds, solution F（Contain arsenite）Peak fluorescence intensity is 167 (a.u), and molten
Liquid E（Do not contain arsenite）Peak fluorescence intensity is 85（a.u）, solution F fluorescence intensities apparently higher than solution E, arsenite inspection
Survey effect obvious.
Embodiment 3
The graphite mould carbon quantum dot of nitrogen sulfur doping（g-CNSQDs）Preparation：By 1 part of sodium citrate, 3 parts of urea and 3 parts of sulfydryl second
Amine is added in 8 parts of deionized waters, and obtaining solution after stirring is placed in reactor, is heated 30 minutes at 160 DEG C, is obtained
The powdered g-CNSQDs of dark brown solid.
Carbon quantum dot SH-g-CNSQDs-NH2Preparation:1 part of DDT and 2 part of g-CNSQDs is added to 24 parts of deionizations
Water, the solution being uniformly mixing to obtain is in hydro-thermal while stirring（65℃）Under the conditions of cultivate 24 hours, then dialyse 12 hours, obtain
SH-g-CNSQDs-NH2。
The detection of arsenite in water sample：With the hydrochloric acid-tromethamine buffer and deionized water of 0.1mol/L by SH-
g-CNSQDs-NH2It is the aqueous solution E that 2%, pH value is 7 to be configured to mass fraction, takes 5ml for subsequent detection.By arsenous to be measured
Acid salt aqueous solution sample（Industrial wastewater, arsenite content is about 100ppb）1-2 drops are taken with glue head dropper and instill solution E, shake
Even to obtain solution F, it is 350- that solution E, F are recorded into launch wavelength under 280nm excitation wavelengths with fluorescence spectrophotometry respectively
Fluorescence intensity under 550nm scopes, as a result finds, solution F（Contain arsenite）Peak fluorescence intensity is 466 (a.u), and molten
Liquid E（Do not contain arsenite）Peak fluorescence intensity is 97（a.u）, solution F fluorescence intensities apparently higher than solution E, arsenite inspection
Survey effect obvious.
Embodiment 4
The SH-g-CNSQDs-NH prepared using embodiment 12And testing conditions, the water sample of detection is changed into containing except As
（III）（50ppb）Outward, also comprising Br−, PO4 2−, NO3−, NO2−, F−, Co2+, Ni2+, Li2+, Fe2+, Mg2+, Zn2+,
K+, As (V), Se (IV), Cu2+, Rb2+, Sr2+, Ca2+18 kinds of industrial wastewaters of metallic element（18 kinds of metallic elements contain
Amount is no less than 50ppb）, detection method result discovery solution F（Contain arsenic III and other 18 kinds of metallic elements）Fluorescence
Intensity remains unchanged apparently higher than solution E, and without generation fluorescent quenching phenomenon.Illustrate detection of the detection method to arsenite
With selectivity and selectivity, arsenite Detection results are good.
Embodiment 5
The SH-g-CNSQDs-NH prepared using embodiment 32, testing conditions with embodiment 1, by the water sample of detection change into containing
Except As（III）（100ppb）Outward, also comprising F−, Co2+, Ni2+, Li2+, Fe2+,K+, As (V), Mg2+, Zn2+, Cu2+,
Rb2+, Sr2+, Br−, PO4 2−, NO3−, NO2−,Ca2+18 kinds of industrial wastewaters of metallic element（The content of 18 kinds of metallic elements is equal
It is 200ppb）, the detection method result finds that the fluorescence intensity of solution F remains unchanged apparently higher than solution E, and no generation fluorescence
Quenching phenomenon.Illustrate that detection of the method to arsenite has selectivity and selectivity, arsenite Detection results are good.
Embodiment 6
The SH-g-CNSQDs-NH prepared using embodiment 32, testing conditions with embodiment 1, by the water sample of detection change into containing
Except As（III）（10ppb）Outward, also comprising Br−, PO4 2−, NO3−, NO2−, F−, Co2+, Ni2+, Fe2+, Mg2+, K+,
As (V), Cu2+,Sr2+, Ca2+18 kinds of rivers of metallic element（The content of 18 kinds of metallic elements is 20ppb）, testing result hair
The fluorescence intensity of existing solution F remains unchanged apparently higher than solution E, without generation fluorescent quenching phenomenon.Explanation the method is to arsenous
The detection of hydrochlorate has selectivity and selectivity, detects sensitive, and Detection results are good.
Claims (9)
1. a kind of carbon quantum dot for detecting arsenite, it is characterised in that its preparation method is comprised the following steps：
（1）Prepare g-CNSQDs：
Sodium citrate, urea and mercaptoethylmaine and deionized water are mixed, solution A is obtained；Solution A is in 160-165 DEG C of 30 points of constant temperature
More than clock, obtain dark brown pulverulent solids as g-CNSQDs；
（2）Prepare SH-g-CNSQDs-NH2：
By DDT and g-CNSQDs and deionized water wiring solution-forming C；Solution C is small in 60-70 DEG C of hydro-thermal 20-24 under agitation
When, then dialyse more than 12 hours, collect solid；
The g-CNSQDs is the graphite mould carbon quantum dot of nitrogen sulfur doping；The DDT is dithiothreitol (DTT).
2. carbon quantum dot according to claim 1, it is characterised in that step（1）In, solution A was in 165 DEG C of constant temperature 30 minutes.
3. carbon quantum dot according to claim 1 or claim 2, it is characterised in that step（1）In, sodium citrate, urea and sulfydryl second
Amine mass percent is 1:3:3-8.
4. carbon quantum dot according to claim 3, it is characterised in that step（2）In, hydrothermal temperature is 65 DEG C, hydro-thermal time
It is 24h.
5. carbon quantum dot according to claim 4, it is characterised in that step（2）In, the mass ratio of DDT and g-CNSQDs is
1：2-5.
6. carbon quantum dot according to claim 5, it is characterised in that step（2）In, the g-CNSQDs is relative to deionization
The consumption of water is 2-6:24.
7. carbon quantum dot according to claim 6, it is characterised in that step（2）, first g-CNSQDs and deionized water are mixed
Close, obtain solution B；DTT is added in solution B again, is uniformly mixing to obtain solution C.
8. the method that carbon quantum dot described in a kind of use claim 1-7 any one detects arsenite, it is characterised in that
By SH-g-CNSQDs-NH2With deionized water wiring solution-forming D, then with the hydrochloric acid-tromethamine buffer of 0.1mol/L
The pH value of solution D is adjusted to 7, solution E is obtained；
Arsenite aqueous liquid sample to be measured is mixed with solution E, solution F is obtained；
Solution F and solution E are carried out into fluorescence intensity comparative analysis with sepectrophotofluorometer；
The excitation wavelength of sepectrophotofluorometer is 280nm, launch wavelength is 350-550nm.
9. detection method according to claim 8, it is characterised in that SH-g-CNSQDs-NH in solution E2Mass content be
0.5-2%。
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| CN108007907A (en) * | 2017-12-04 | 2018-05-08 | 广东上风环保科技有限公司 | The preparation method of carbon quantum dot and the method for detecting mercury content based on carbon quantum dot |
| CN108489954A (en) * | 2018-05-17 | 2018-09-04 | 南昌大学 | Alkaline phosphatase and arsenate detection method based on double transmitting fluorescence probes |
| CN108579671A (en) * | 2018-01-23 | 2018-09-28 | 辽宁大学 | It is a kind of to be used for heavy metal ion adsorbed carbon quantum dot and its preparation method and application |
| CN115403069A (en) * | 2022-08-01 | 2022-11-29 | 云南昱粼水环境治理有限责任公司 | Preparation method and application of novel photocatalyst bismuth oxysalt and coated fiber |
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| CN108007907A (en) * | 2017-12-04 | 2018-05-08 | 广东上风环保科技有限公司 | The preparation method of carbon quantum dot and the method for detecting mercury content based on carbon quantum dot |
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| CN108489954A (en) * | 2018-05-17 | 2018-09-04 | 南昌大学 | Alkaline phosphatase and arsenate detection method based on double transmitting fluorescence probes |
| CN108489954B (en) * | 2018-05-17 | 2021-01-12 | 瑞金盛源环保科技有限责任公司 | Alkaline phosphatase and arsenate radical detection method based on dual-emission fluorescent probe |
| CN115403069A (en) * | 2022-08-01 | 2022-11-29 | 云南昱粼水环境治理有限责任公司 | Preparation method and application of novel photocatalyst bismuth oxysalt and coated fiber |
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