CN107044961A - A kind of method of spectrophotometry silver ion - Google Patents
A kind of method of spectrophotometry silver ion Download PDFInfo
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- CN107044961A CN107044961A CN201710182569.8A CN201710182569A CN107044961A CN 107044961 A CN107044961 A CN 107044961A CN 201710182569 A CN201710182569 A CN 201710182569A CN 107044961 A CN107044961 A CN 107044961A
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
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Abstract
The present invention provides a kind of method of spectrophotometry silver ion, silver ion solution, aptamers silver ion solution, negative electricity nano-Au solution needed for first preparing respectively；Negative electricity nano-Au solution is added in aptamers silver ion solution, effect 5 minutes adds concentration and reunited for 0.2mol/L sodium chloride solution induction nanogold, then obtains standard liquid afterwards；Standard liquid is subjected to the sweep measuring of ultraviolet-visible absorption spectroscopy and standard curve is drawn；Then solution to be measured is prepared, gained solution to be measured is carried out to the scanning of ultraviolet-visible absorption spectroscopy, and establishing criteria curve calculates the concentration of silver ions in water sample to be measured.The inventive method is selectively good, with good reliability, so that detection sensitivity is higher, detection limit is low, and only need to complete detection operation using cheap and general spectrophotometer, entirely detect easy to operate quick, technical requirements to operating technology personnel are low, it is easy to extensive Implementation and application.
Description
【Technical field】
The invention belongs to analyze detection field, and in particular to a kind of method of spectrophotometry silver ion.
【Background technology】
Silver extensively, causes the generation of a large amount of silver ions in industrial wastewater, ion in the sector application such as electronics, plating, photosensitive
The silver-colored toxicity maximum of form, severe contamination environment and harm people's is healthy.At present, the World Health Organization (WHO) advises
The Cmax allowed in drinking water is 0.1mg/L (927nM), and Environmental Protection Agency (EPA) suggestion is to greatest extent
0.05mg/L(464nM).Therefore, the detection of silver ion to environmental protection and safeguard people it is healthy highly significant.
Conventional Silver detection technical method mainly has ICP-MS (ICP-MS), atomic spectroscopy, electrification
Method, XRF, colorimetric method and ultraviolet absorption spectroscopy etc..There are some defects in these methods：Detection process is complicated, consumption
Duration；It is superior using instrument and equipment costliness, and need to carry out complicated pretreatment, high is required to technical staff；Background signal height,
The low shortcoming of sensitivity.
And AAS is used for the inspection of silver ion because of the characteristics of inexpensively general etc. prominent with easy quick, instrument
Survey.But, the spectrophotometry Ag developed at present+Analysis method, its sensitivity is generally relatively low, and design principle
It is complex so that the precision of method is inadequate, so as to influence the degree of accuracy of detection, therefore, spectrophotometry silver ion
Technical method still suffer from challenging, further improve the sensitivity of analysis, develop simple and practical spectrophotometry
The technical method of low concentration silver ion be clearly practitioner institute urgently desirably.
【The content of the invention】
The technical problems to be solved by the invention are to provide a kind of method of spectrophotometry silver ion, with choosing
Selecting property is good and good reliability so that detection sensitivity is higher, detection limit is low, and need to only use cheap and general light splitting
Photometer can both complete detection operation.
The present invention is to solve above-mentioned technical problem by the following technical programs：A kind of spectrophotometry silver ion
Method, this method comprises the following steps：
(1) preparation of standard curve：
A, take silver ion aptamers compound concentration be 1 × 10-7Mol/L silver ion adaptation liquid solution, it is stand-by；Preparing one is
The silver ion solution of row various concentrations, it is stand-by；
B, take each silver ion solution of preparation to be adapted to liquid solution with silver ion to be mixed in equal volume respectively, and at room temperature
Effect 10 minutes, obtains aptamers-silver ion solution；
C, to be separately added into gained aptamers-silver ion solution concentration be 1.7 × 10-8Mol/L negative electricity nanogold is molten
Liquid, effect 5 minutes adds concentration and reunited for 0.2mol/L sodium chloride solution induction nanogold, then obtains standard liquid afterwards；Its
In, negative electricity nano-Au solution：Aptamers-silver ion solution：The volume ratio of sodium chloride solution is 4：4：1；
D, the scanning by standard liquid progress uv-visible absorption spectra, while bioassay standard solution is 620nm in wavelength
With the absorbance at 520nm, i.e. A620And A520, and calculate absorbance ratio A620/A520；
E, using the concentration of the silver ion solution of standard liquid as abscissa, with the absorbance ratio A of gained620/A520For
Ordinate, draws standard curve；
(2) concentration of silver ions in water sample to be measured is determined：
F, take water sample to be measured and through 0.22 μm of membrane filtration, then the chlorine in cleared water sample to be measured is boiled in heating, then cools down
Sample to be tested is produced to room temperature；Then the silver ion solution described in sample to be tested alternative steps b is taken, and according to step b, step
C operations then obtain solution to be measured；
G, the scanning that gained solution to be measured is carried out to uv-visible absorption spectra, while determining solution to be measured and being in wavelength
Absorbance at 620nm and 520nm, calculates its absorbance ratio A620/A520, finally by absorbance ratio A620/A520
It is compared with the standard curve of above-mentioned drafting, calculates the concentration of silver ions in water sample to be measured.
Further, in the step a, the specific process for preparation of silver ion adaptation liquid solution is：Take silver ion aptamers
And using pH value to be dissolved for 7.5 Tris-HCl cushioning liquid, compound concentration is 1 × 10-7Mol/L silver ion aptamers are molten
Liquid.
A kind of beneficial effect of the method for spectrophotometry silver ion of the present invention is：
The inventive method is selectively good, with good reliability so that detection sensitivity is higher, detection limit is low, and
Using when, only need using cheap and general spectrophotometer complete detection operation, entirely detect it is easy to operate quickly, it is right
The technical requirements of operating technology personnel are low, it is easy to extensive Implementation and application.
【Brief description of the drawings】
With reference to the accompanying drawings in conjunction with the embodiments to further description of the present invention.
Fig. 1 is the canonical plotting in the embodiment of the present invention 1.
Fig. 2 is the spectrogram of the uv-visible absorption spectra in the embodiment of the present invention 2.
Fig. 3 is electron microscope of the mixed liquor I under transmission electron microscope in the embodiment of the present invention 2.
Fig. 4 is electron microscope of the mixed liquor II under transmission electron microscope in the embodiment of the present invention 2.
Fig. 5 is the schematic diagram of the selective analysis result in the embodiment of the present invention 3.
【Embodiment】
A kind of method of spectrophotometry silver ion of the invention is further described with reference to following examples.
It should be noted that test method described in following each embodiments, is then conventional method unless otherwise specified；
Reagent, solution for being used etc., unless otherwise specified, are commercially obtained；And the silver used in following embodiments
The sequence of ion aptamers is 5 '-CCT CCC TCC TTT TCC ACC CAC C-3 ' (its nucleotide sequence such as SEQ ID
NO：Shown in 1), it is purchased from Beijing Ding Guo Bioisystech Co., Ltd.
Preparing for negative electricity nano-Au solution employed in following each embodiments is as follows：Take gold chloride (HAuCl4·4H2O,
AR, Au content>47.8%, Chemical Reagent Co., Ltd., Sinopharm Group) and be dissolved in secondary deionized water preparing 0.01%
W/w gold chloride stock solution is HAuCl4Solution, is put in 4 DEG C of refrigerators and preserves；Take 50mL 0.01%w/w HAuCl4Solution
Boiling is heated to, afterwards under strong stirring, 2.8mL 1% sodium citrate solution is added into whirlpool rapidly, obtains mixed solution,
And keep the mixed solution to stop heating after seething with excitement 10 minutes, it is 1.7 × 10 that then stirring, which is cooled to room temperature and produces concentration,- 8Mol/L negative electricity nano-Au solution, gained negative electricity nano-Au solution is put in brown reagent bottle, and is preserved in 4 DEG C of refrigerators
It is standby.And the particle diameter of the negative electricity nanogold in negative electricity nano-Au solution is 13nm.
A kind of concrete operations of the method for spectrophotometry silver ion of the invention of embodiment 1
(1) preparation of standard curve：
A, take silver ion aptamers and use pH value for 7.5 Tris-HCl cushioning liquid dissolve, compound concentration be 1 ×
10-7Mol/L silver ion adaptation liquid solution, it is stand-by；Using secondary deionized water dissolving silver nitrate, (Aladdin chemical reagent is limited
Company) with compound concentration it is respectively 1.0 × 10-10、5.0×10-10、 1.0×10-9、5.0×10-9、1.0×10-8、5.0×
10-8、8.0×10-8Mol/L silver ion solution, it is stand-by；
B, take each concentration silver ion solution of preparation to be adapted to liquid solution with silver ion to be mixed in equal volume respectively, and in room
The lower effect of temperature 10 minutes, obtains aptamers-silver ion solution；
C, to be separately added into gained aptamers-silver ion solution concentration be 1.7 × 10-8Mol/L negative electricity nanogold is molten
Liquid, effect 5 minutes adds concentration and reunited for 0.2mol/L sodium chloride solution induction nanogold, then obtains standard liquid afterwards；Its
In, negative electricity nano-Au solution：Aptamers-silver ion solution：The volume ratio of sodium chloride solution is 4：4：1；
D, the scanning by standard liquid progress uv-visible absorption spectra, while bioassay standard solution is 620nm in wavelength
With the absorbance at 520nm, i.e. A620And A520, and calculate absorbance ratio A620/A520；
E, using the concentration of the silver ion solution of standard liquid as abscissa, with the absorbance ratio A of gained620/A520For
Ordinate, draws standard curve (as shown in Figure 1)；
(2) concentration of silver ions in water sample to be measured is determined：
F, take water sample to be measured and through 0.22 μm of membrane filtration, then the chlorine in cleared water sample to be measured is boiled in heating, then cools down
Sample to be tested is produced to room temperature；Then the silver ion solution described in sample to be tested alternative steps b is taken, and according to step b, step
C operations then obtain solution to be measured, specifically：Take sample to be tested to be adapted to liquid solution with silver ion to be mixed in equal volume respectively, and
Act on 10 minutes at room temperature, obtain aptamers-silver ion solution；It is separately added into the gained aptamers-silver ion solution dense
Spend for 1.7 × 10-8Mol/L negative electricity nano-Au solution, acts on 5 minutes, concentration is added afterwards molten for 0.2mol/L sodium chloride
Liquid induction nanogold reunite, then solution to be measured；Wherein, negative electricity nano-Au solution：Aptamers-silver ion solution：Sodium chloride is molten
The volume ratio of liquid is 4：4：1；
G, the scanning that gained solution to be measured is carried out to uv-visible absorption spectra, while determining solution to be measured and being in wavelength
Absorbance at 620nm and 520nm, calculates its absorbance ratio A620/A520, finally by absorbance ratio A620/A520
It is compared with the standard curve of above-mentioned drafting, calculates the concentration of silver ions in water sample to be measured.
The feasibility analysis of the inventive method of embodiment 2
In order to verify that negative electricity nanogold can actually be used to carry out uv-visible absorption spectra measure silver ion, applicant
Following experiment is carried out.
The silver ion aptamers solution effects 5 minutes that 200 μ L negative electricity nano-Au solutions and 200 μ L embodiments 1 prepare are taken, it
After add sodium chloride solution, resulting solution is used as mixed liquor I；It is 8.0 × 10 to take concentration-8Mol/L silver ions and 200 μ L are implemented
The silver ion aptamers solution effects of the preparation of example 1 10 minutes, add 200 μ L negative electricity nano-Au solutions effect 5 minutes, then afterwards
Sodium chloride solution is added, resulting solution is used as mixed liquor II；Mixed liquor I, mixed liquor II is taken to carry out uv-visible absorption spectra
Scanning, determines the two absorbance at different wave length, measurement result such as Fig. 2：As shown in Figure 2, mixed liquor II is compared to mixed
Liquid I is closed, the spectrogram of its uv-visible absorption spectra there occurs obvious change；Mixed liquor I, mixed liquor II are distinguished simultaneously
It is placed under transmission electron microscope and is observed, then electron microscope of the mixed liquor I under transmission electron microscope is as shown in figure 3, mixed liquor II is in transmission
Electron microscope under Electronic Speculum is as shown in figure 4, comparison diagram 3 and Fig. 4 is understood, the form of mixed liquor I, mixed liquor II under transmission electron microscope etc.
With obvious difference.
Therefore, understood with reference to Fig. 2 to Fig. 4, coordinate silver ion aptamers can actually be to determine using negative electricity nanogold
Silver ion.
The selectivity analysis of the inventive method of embodiment 3
Ag is investigated by testing+、Hg2+、Ba2+、Ni2+、Pb2+、Cu2+、Cd2+、Mg2+、Ca2+、 Zn2+、Al3+、Fe3+It is right respectively
The inventive method (concrete operations of embodiment 1) is the response of system, so as to investigate the choosing that the inventive method is determined to silver ion
Selecting property.In experiment, the corresponding bulk concentration that is adapted to of each metal ion is 1 × 10-7mol/L；Other control metal ion (Hg2+、
Ba2+、Ni2+、Pb2+、 Cu2+、Cd2+、Mg2+、Ca2+、Zn2+、Al3+、Fe3+) concentration is identical with concentration of silver ions, be 5.0 ×
10-8Mol/L, remaining experiment condition is identical；Then experimental result is as shown in figure 5, compared to other metal ion absorbance ratios, silver
Ion shows a notable big absorbance ratio, so as to indicate this method to Ag+With good selectivity.
Embodiment 4 carries out water sample analysis using the inventive method
In order to verify the reliability of the inventive method practical application, Min River water and running water are sampled respectively and (respectively take three
Water sample, respectively running water 1, running water 2, running water 3, Min River water 1, Min River water 2 and Min River water 3), then using the present invention
Method is that the concrete operations of embodiment 1 carry out the measure of silver ion in water sample, and carries out the rate of recovery using standard addition method simultaneously
Experiment, experimental result sees below table 1.
Silver ion measurement result in the water sample of table 1
Via table 1 test result indicates that, the inventive method has the preferable degree of accuracy and precision, and the rate of recovery is
95.0%~103%, RSD are between 2.2%~4.6%, and analysis time is short, further, since the inventive method only needs to determine
Absorbance, then during practical operation, can both have been realized, so that the inventive method is used for by cheap general spectrophotometer
Can quickly and easily it be carried out during Silver detection in water sample.
To sum up, the inventive method is selectively good, with good reliability so that detection sensitivity is higher, detection limit is low,
And when applying, only need to complete detection operation using cheap and general spectrophotometer, entirely detect easy to operate fast
Speed, the technical requirements to operating technology personnel are low, it is easy to extensive Implementation and application.
SEQUENCE LISTING
<110>Fujian University of Technology
<120>A kind of method of spectrophotometry silver ion
<130> 10000
<160> 1
<170> PatentIn version 3.3
<210> 1
<211> 22
<212> DNA
<213>Artificial sequence
<400> 1
cctccctcct tttccaccca cc 22
Claims (2)
1. a kind of method of spectrophotometry silver ion, it is characterised in that：This method comprises the following steps：
(1) preparation of standard curve：
A, take silver ion aptamers compound concentration be 1 × 10-7Mol/L silver ion adaptation liquid solution, it is stand-by；Preparation is a series of not
It is stand-by with the silver ion solution of concentration；
B, take each silver ion solution of preparation to be adapted to liquid solution with silver ion to be mixed in equal volume respectively, and act at room temperature
10 minutes, obtain aptamers-silver ion solution；
C, to be separately added into gained aptamers-silver ion solution concentration be 1.7 × 10-8Mol/L negative electricity nano-Au solution, makees
With 5 minutes, concentration was added afterwards and is reunited for 0.2mol/L sodium chloride solution induction nanogold, then obtains standard liquid；Wherein, bear
Electric nano-Au solution：Aptamers-silver ion solution：The volume ratio of sodium chloride solution is 4：4：1；
D, by standard liquid carry out uv-visible absorption spectra scanning, while bioassay standard solution wavelength be 620nm and
Absorbance at 520nm, i.e. A620And A520, and calculate absorbance ratio A620/A520；
E, using the concentration of the silver ion solution of standard liquid as abscissa, with the absorbance ratio A of gained620/A520For vertical seat
Mark, draws standard curve；
(2) concentration of silver ions in water sample to be measured is determined：
F, take water sample to be measured and through 0.22 μm of membrane filtration, the chlorine in cleared water sample to be measured is boiled in then heating, is cooled to room
Temperature produces sample to be tested；Then the silver ion solution described in sample to be tested alternative steps b is taken, and according to step b, step c behaviour
Then obtain solution to be measured；
G, the scanning by gained solution progress uv-visible absorption spectra to be measured, while it is 620nm to determine solution to be measured in wavelength
With the absorbance at 520nm, its absorbance ratio A is calculated620/A520, finally by absorbance ratio A620/A520With it is above-mentioned
The standard curve of drafting is compared, and calculates the concentration of silver ions in water sample to be measured.
2. a kind of method of spectrophotometry silver ion according to claim 1, it is characterised in that：In the step a,
Silver ion adaptation liquid solution specific process for preparation be：Take silver ion aptamers and use pH value to be buffered for 7.5 Tris-HCl
Solution dissolves, and compound concentration is 1 × 10-7Mol/L silver ion adaptation liquid solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108535203A (en) * | 2018-04-03 | 2018-09-14 | 金川集团股份有限公司 | The derivative spectrophotometric detecting method of saccharin sodium in a kind of pure Ni solution |
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| CN106290319A (en) * | 2016-08-04 | 2017-01-04 | 福建工程学院 | A kind of method of silver ion in chemiluminescence detection water sample |
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2017
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507952A (en) * | 2011-10-11 | 2012-06-20 | 中国科学院长春应用化学研究所 | Method for detecting protein and metal ions |
| CN104251827A (en) * | 2013-06-28 | 2014-12-31 | 中国科学院大连化学物理研究所 | Method for determining concentration of mercury ions or silver ions in solution |
| CN104596959A (en) * | 2015-01-22 | 2015-05-06 | 中国科学院化学研究所 | Method for detecting potassium ion concentration based on DNA enzymes |
| CN106290319A (en) * | 2016-08-04 | 2017-01-04 | 福建工程学院 | A kind of method of silver ion in chemiluminescence detection water sample |
Non-Patent Citations (1)
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| 欧丽娟: "基于滚环DNA扩增和纳米金的生物传感技术研究", 《中国博士学位论文全文数据库 医药卫生科技辑》 * |
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| CN108535203A (en) * | 2018-04-03 | 2018-09-14 | 金川集团股份有限公司 | The derivative spectrophotometric detecting method of saccharin sodium in a kind of pure Ni solution |
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Application publication date: 20170815 |