CN108680541A - A kind of fluorescence molybdenum oxide quantum dot measurement determination of trace uranium(Ⅵ)Method - Google Patents
A kind of fluorescence molybdenum oxide quantum dot measurement determination of trace uranium(Ⅵ)Method Download PDFInfo
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- CN108680541A CN108680541A CN201810205403.8A CN201810205403A CN108680541A CN 108680541 A CN108680541 A CN 108680541A CN 201810205403 A CN201810205403 A CN 201810205403A CN 108680541 A CN108680541 A CN 108680541A
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- G—PHYSICS
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- 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
The invention discloses a kind of fluorescence molybdenum oxide quantum dots as indicator, and the method that the fluorescence intensity of front and back molybdenum oxide quantum dot carries out qualitative and quantitative analysis to uranium (VI) is added by uranium (VI).It is found in this method detection, most of metal ion does not generate interference to uranium (VI) detection;Simultaneously by quantitative detection, as a result, it has been found that, recovery of standard addition is 99.7 100.6%, illustrates that this method is accurate and reliable.
Description
Technical field
The present invention relates to technical field of analytical chemistry more particularly to a kind of fluorescence molybdenum oxide quantum dot to measure determination of trace uranium (VI)
Method.
Background technology
With being continuously increased for energy demand, the development and utilization of uranium resource is increasingly paid attention to by national governments.But
Uranium is also a kind of main natural radioactive element, has harm to human health.Therefore, it is necessary to nuclear facilities and uranium mine
Neighbouring environmental water sample is monitored to ensure the health of the mankind.Currently, the analysis method of determination of trace uranium includes mainly photometry, changes
Luminescence analysis, fluorescence method, optical colorimetry etc. are learned, wherein fluorescence method is because having high sensitivity, good selective, in uranium
Measurement in have good application prospect.
Invention content
Technical problems based on background technology, the present invention propose a kind of fluorescence molybdenum oxide quantum dot measurement determination of trace uranium
(VI) method.
Technical scheme is as follows:
In view of the deficiencies of the prior art, it is measured without multistep reaction, determination of trace uranium easy to operate the present invention provides a kind of
(VI) fluorescent method.
This method need to only use a kind of indicator of molybdenum oxide quantum dot, and front and back molybdenum oxide quantum dot is added by uranium (VI)
Fluorescence intensity to uranium (VI) carry out qualitative and quantitative analysis.
A kind of method that fluorescence molybdenum oxide quantum dot determination of trace uranium measures (VI), includes the following steps:
A, in nitric acid medium, pH 4.5-5.5 stand 1-5 points after molybdenum oxide quantum dot and mixing is added in uranium (VI)
Clock finally measures molybdenum oxide quantum dot with excitation wavelength 380-450nm, launch wavelength 525nm, excitation and transmite slit 10nm
Fluorescence;
B, the standard curve of uranyl nitrate ion is drawn;
C, according to the fluorescence and standard curve of the molybdenum oxide quantum dot of measurement, the content of determination of trace uranium (VI) is calculated.
The preparation method of the fluorescence molybdenum oxide quantum dot, includes the following steps:It weighs molybdenum disulfide powder and is put into burning
In cup, distilled water and 25-35% hydrogen peroxide is added, stands 25-35 minutes;After molybdenum disulfide fully dissolves, hydroxide is added
Sodium adjusts pH value of solution to 6.8-7.2, is centrifuged 8-15 minutes in 15000-17000r/min after the reaction was continued 2-4 hours, on gained
Clear liquid is molybdenum oxide quantum dot.
After molybdenum oxide quantum dot is added in uranium (VI), due to strong affinity of the uranium (VI) between oxygen atom, uranium (VI) can
It is incorporated into molybdenum oxide quantum dot surface, and then quenches the fluorescence of molybdenum oxide quantum dot, and works as a concentration of 1.04-16.64 μ of uranium (VI)
When M, good linear relationship is presented with uranium (VI) concentration in fluorescent quenching intensity, can carry out the qualitative and quantitative analysis of uranium (VI).
Preferably, when uranyl nitrate is 1.04-16.64 μM a concentration of, the fluorescence intensity of molybdenum oxide quantum dot and its concentration
Show good linear relationship, linear equation IF=1261.6-582.9log (c), coefficient R2=0.99.
Make sample detection with uranyl nitrate ion, experiment value is consistent with theoretical value.
The invention has the beneficial effects that:The present invention has investigated common metal ion in environmental water sample and has been done to this method
It disturbs, the results showed that, most of metal ion does not generate interference to uranium (VI) detection.Fe3+、Cu2+、Al3+、Ni2+、Th4+Though having one
Fixed interference, but after addition screening agent EDETATE DISODIUM, cysteine, citric acid, the interference of these metal ions can exclude substantially,
Therefore the present invention can carry out selective enumeration method to the uranium (VI) in environmental water sample.Finally, using the method for the present invention in water sample
Determination of trace uranium (VI) carried out quantitative detection, as a result, it has been found that, recovery of standard addition 99.7-100.6%, illustration method accurately may be used
It leans on.
Description of the drawings
Fig. 1:Molybdenum oxide quantum dot excitation and emission spectra figure;
Fig. 2:The fluorescence spectra of molybdenum oxide quantum dot and the interaction of various concentration uranyl ion;
Fig. 3:The working curve of uranyl ion;
Fig. 4:The interference figure of common metal ion.
Specific implementation mode
Embodiment:
Selective oxidation molybdenum quantum dot of the present invention studies its reacting with uranium (VI), explores the best of reaction as indicator
Condition measures the content of determination of trace uranium (VI), obtains preferable effect.
Embodiment 1
A kind of method that fluorescence molybdenum oxide quantum dot determination of trace uranium measures (VI), includes the following steps:Accurately weigh 100.0mg
Molybdenum disulfide powder is put into beaker, and 2mL distilled water and 30% hydrogen peroxide of 8mL is added, and stands 30 minutes.Wait for that molybdenum disulfide fills
After dividing dissolving, sodium hydrate regulator solution pH to 7.0 is added, is centrifuged 10 minutes in 16000r/min after the reaction was continued 3 hours, institute
It is molybdenum oxide quantum dot to obtain supernatant.
Embodiment 2
A kind of method that fluorescence molybdenum oxide quantum dot determination of trace uranium measures (VI), includes the following steps:Accurately weigh 100.0mg
Molybdenum disulfide powder is put into beaker, and 2mL distilled water and 25% hydrogen peroxide of 8mL is added, and stands 25 minutes.Wait for that molybdenum disulfide fills
After dividing dissolving, sodium hydrate regulator solution pH to 6.8 is added, is centrifuged 15 minutes in 15000r/min after the reaction was continued 4 hours, institute
It is molybdenum oxide quantum dot to obtain supernatant.
Embodiment 3
A kind of method that fluorescence molybdenum oxide quantum dot determination of trace uranium measures (VI), includes the following steps:Accurately weigh 100.0mg
Molybdenum disulfide powder is put into beaker, and 2mL distilled water and 35% hydrogen peroxide of 8mL is added, and stands 35 minutes.Wait for that molybdenum disulfide fills
After dividing dissolving, sodium hydrate regulator solution pH to 7.2 is added, is centrifuged 8 minutes in 17000r/min after the reaction was continued 2 hours, institute
It is molybdenum oxide quantum dot to obtain supernatant.
The configuration of 66.0mg/L uranyl nitrates:The accurate uranium standard solution for measuring 1.0mL 6.6g/L is in 100mL volumetric flasks
In, a certain amount of distilled water is added and with nitric acid tune pH to 4.5, last constant volume.
Fluorescence molybdenum oxide quantum dot determination of trace uranium measures the selection of each parameter of (VI):
1, the selection of excitation wavelength and launch wavelength
First, excitation and the transmitting situation of molybdenum oxide quantum dot have been investigated.As shown in Figure 1, when keeping excitation and emitting narrow
When seam is 10nm, change the excitation wavelength of molybdenum oxide quantum dot, can be obtained with excitation wavelength red shift and the transmitting light of gradual red shift
Spectrogram.When excitation wavelength is 380-450nm, the fluorescent emission intensity of molybdenum oxide quantum dot is stronger, meets and measures uranium (VI)
Demand.
2, the selection of system acidity
It is 10nm with excitation wavelength 405nm, excitation and transmite slit, measures uranyl nitrate ion and molybdenum oxide quantum dot
The front and back fluorescence intensity of effect.As shown in table 1, using nitric acid as medium, when pH is 4.5, uranyl ion and molybdenum oxide quantum
The fluorescence intensity for selecting mixed liquor is minimum, illustrates the quenching best results of uranyl nitrate ion pair molybdenum oxide quantum dot at this time.
Table 1:The fluorescence intensity of mixed liquor under different pH
:3, the standard curve of uranyl nitrate ion
In order to better illustrate the molybdenum oxide quantum dot change in fluorescence situation front and back with uranium (VI) interaction, nitric acid is selected
Uranyl ion is sample, excitation wavelength 405nm.It can be observed from fig. 2 that after uranyl nitrate is added, molybdenum oxide quantum dot
Fluorescence significantly reduces, and fluorescence reduces degree and enhances with the increase of uranyl nitrate concentration.Therefore, according to molybdenum oxide quantum dot
Fluorescence intensity can establish the working curve of uranyl nitrate, as shown in figure 3, when uranyl nitrate is 1.04-16.64 μM a concentration of, oxygen
It is in good linear relationship, linear equation I to change the fluorescence intensity of molybdenum quantum dot and its concentrationF=1261.6-582.9log
(c), coefficient R2=0.99.
4, the influence of coexisting ion
Interference of the common metal ion to this method in environmental water sample is investigated, as shown in figure 4, most of metal ion pair
Uranium (VI) detection does not generate interference.Fe3+、Cu2+、Al3+、Ni2+、Th4+Though there is certain interference, screening agent EDETATE SODIUM is added
After salt, cysteine, citric acid, the interference of these metal ions can exclude substantially, therefore the present invention can be in environmental water sample
Uranium (VI) carries out selective enumeration method.
Test case:
Uranium in water sample (VI) content is detected using molybdenum oxide quantum dot:
Water sample:Tap water --- carry out running water pipe in self-test environment;
Lake water --- it is derived from the lake water on detection environment periphery, upper layer water sample is drawn after clarification;
Blank:Because considering that uranyl ion content is extremely low in conventional environment water sample, so the water sample of acquisition is done blank sample.
Instrument:USB-4000FL fluorimeters, excitation wavelength 405nm, launch wavelength 525nm, excitation and transmite slit 10nm.
Concrete operation step:
1) in 1.5mL centrifuge tubes, molybdenum oxide quantum dot, 20 μ L water samples and the 160 μ L pH of 20 μ L 1mg/mL are added
4.5 nitric acid acidifying water reacts 5 minutes after mixing, is then measured in USB-4000FL fluorimeters and read the fluorescence at 525nm
Intensity I0。
2) in another 1.5mL centrifuge tubes, the molybdenum oxide quantum dot of 20 μ L 1mg/mL, the nitric acid of 31.5 μM of 20 μ L is added
The nitric acid acidifying water of uranyl, 20 μ L water samples and 140 μ L pH 4.5 reacts 5 minutes after mixing, then in USB-4000FL fluorescence
Meter measures and reads the fluorescence intensity I at 525nm1。
3) according to the I measured1Numerical value, according to equation c=10(I F-1261.6)/582.9Calculate corresponding uranium content.
Tap water and lake water are determined with this method, the fluorescence intensity I0 at 520nm is respectively 1718.5 and 1717.4,
It is essentially identical with laboratory distilled water blank control fluorescence intensity, illustrate that the uranyl ion in two kinds of acquired water samples is extremely low,
This method cannot detect.After 3.15 μM of uranyl nitrate being separately added into tap water and lake water sample, the fluorescence intensity that measures
I1Respectively 971.7 and 969.5, according to equation c=10(I F-1261.6)/582.9The concentration that uranyl ion is calculated is respectively
3.142 and 3.17 μM, detailed results are shown in Table 2.
Table 2:Uranium content analysis result in water sample
Table 2 statistics indicate that, uranyl ion content that can be in Accurate Determining environmental water sample using the method for the present invention, mark-on reclaims
Rate 99.7%-100.6%, relative standard deviation are less than 5%, illustrate that detection method accuracy is good.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of method that fluorescence molybdenum oxide quantum dot measures determination of trace uranium (VI), which is characterized in that with fluorescence molybdenum oxide quantum dot
As indicator, the fluorescence intensity that front and back molybdenum oxide quantum dot is added by uranium (VI) carries out qualitative and quantitative point to uranium (VI)
Analysis.
2. the method that fluorescence molybdenum oxide quantum dot as described in claim 1 measures determination of trace uranium (VI), which is characterized in that including with
Lower step:
A, in nitric acid medium, pH 4.5-5.5 stand 1-5 minutes, most after molybdenum oxide quantum dot and mixing is added in uranium (VI)
The fluorescence of molybdenum oxide quantum dot is measured with excitation wavelength 380-450nm, launch wavelength 525nm, excitation and transmite slit 10nm afterwards;
B, the standard curve of uranyl nitrate ion is drawn;
C, according to the fluorescence and standard curve of the molybdenum oxide quantum dot of measurement, the content of determination of trace uranium (VI) is calculated.
3. the method that fluorescence molybdenum oxide quantum dot as claimed in claim 2 measures determination of trace uranium (VI), which is characterized in that work as nitric acid
When uranyl is 1.04-16.64 μM a concentration of, the fluorescence intensity of molybdenum oxide quantum dot is in good linear relationship with its concentration, linearly
Equation is IF=1261.6-582.9log (c), coefficient R2=0.99.
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CN110609023A (en) * | 2019-09-03 | 2019-12-24 | 东华理工大学 | Preparation method of dopamine-modified molybdenum oxide quantum dot and application of dopamine-modified molybdenum oxide quantum dot in trace uranium detection |
CN110882690A (en) * | 2019-11-07 | 2020-03-17 | 武汉科技大学 | Silicon dioxide nanosphere supported molybdenum oxide quantum dot catalyst and preparation method thereof |
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CN110882690A (en) * | 2019-11-07 | 2020-03-17 | 武汉科技大学 | Silicon dioxide nanosphere supported molybdenum oxide quantum dot catalyst and preparation method thereof |
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