CN110044885A - One kind exempting from instrument Hg2+Quantitative detecting method - Google Patents
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- CN110044885A CN110044885A CN201910314816.4A CN201910314816A CN110044885A CN 110044885 A CN110044885 A CN 110044885A CN 201910314816 A CN201910314816 A CN 201910314816A CN 110044885 A CN110044885 A CN 110044885A
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Abstract
The invention discloses one kind to exempt from instrument Hg2+Quantitative detecting method.Utilize Hg2+Inhibit the reaction rate of redox reaction between nanogold seed catalyst reducing agent and gold chloride to extend the mechanism that red nano gold solution forms the time.Hg2+Concentration and red nano gold solution formation time are proportional.Signal (the formation time of red solution) reading is carried out by using the cheap small-sized time set such as mobile phone and equipment, can be achieved with nanomolar range Hg2+Portable quantitative detection.The method of the present invention have it is easy to operate, low in cost, without the use of specialty analysis instrument and equipment, be suitable for Hg2+Field assay and immediately detection outstanding advantages of.This method can directly be applied in the numerous areas such as medical diagnosis, environmental monitoring, food safety Hg in all kinds of solution samples2+Simple, economic, quick, sensitive, the special portable qualitative and quantitative detection of analyte.
Description
Technical field
The invention belongs to nanochemistry field of sensing technologies, and in particular to one kind exempts from instrument Hg2+Quantitative detecting method.
Background technique
Mercury ion (Hg2+) it is one of the heavy metal ion with serious physiological-toxicity.Hg2+It can be in animal and plant body
Interior accumulation, and be gradually enriched with by food chain, concentration can be thousands of or even million times be increased, final to threaten the mankind strong
Health, for example, can the serious systems such as insulting neural, mucocutaneous, uropoiesis and reproduction, even result in death." the Chinese people
Republic's Law on Environmental Protection " prepared Drinking Water and farmland irrigating water water standard in provide Hg2+Content must not surpass
Cross 0.001 mg/L.To ensure the Hg in food, water and environment2+Human health and life security are not influenced, to food, water and ring
Trace Hg in border2+It is significant to carry out quantitative detection.Existing Hg2+Detection technique mainly includes inductively coupled plasma body
Mass spectrography, atomic absorption spectrography (AAS), atomic emission spectrometry, atomic fluorescence spectrometry etc..However, the generally existing behaviour of these methods
Make that complex steps are time-consuming, cannot be used for the problems such as field assay.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide one kind to exempt from instrument Hg2+Quantitative detecting method.
Thinking of the invention: studies have shown that in the presence of the colourless weak solution of nanometer gold seeds of the partial size less than 10 nm,
The reducing agents such as sodium citrate can quickly restore gold chloride in-situ preparation red nano gold solution.It is a discovery of the invention that in Hg2+In the presence of
Under, by with nanogold Seed Development gold amalgam, the reaction rate of above-mentioned redox reaction can be significantly inhibited, greatly prolonged
The formation time of long red nano gold solution.Hg2+It is proportional that with red nano gold solution the time is formed in situ in concentration.Pass through
Atomic Absorption Spectrometer, electrochemical analyser, fluorescence spectrophotometer are replaced using the cheap small-sized time set such as mobile phone, wrist-watch and equipment
Photometer measuring method, Chemiluminescence Apparatus, ultraviolet-uisible spectrophotometer etc. it is expensive and lack portability analysis instrument carry out letter
Number (be formed in situ red nano gold solution the time required to) reads, the portable Hg of low cost can be realized2+Accurate quantitative analysis.
Specific steps are as follows:
Step 1: by Hg2+Water sample, colourless nano-Au solution hybrid reaction.
Step 2: aqueous solution of chloraurate and reducing agent aqueous solution are continuously added.
Step 3: the color change of visual observation mixed solution, while using portable small-sized timing device record from also
Former agent aqueous solution has been added to mixed solution is presented red required time, the time and Hg completely2+Concentration be positively correlated, from
And realize Hg2+Timing quantitative detection.
Colourless nano-Au solution in the step 1 is the solution containing nanometer gold seeds, wherein the grain of nanometer gold seeds
The solution is diluted to using deionized water colourless by diameter less than 10 nm, this nanometer of gold seeds can be catalyzed the chlorine of subsequent addition
Redox reaction between auric acid and reducing agent, quickly generating appearance is red nano-Au solution.
Hg in the step 12+Water sample and colourless nano-Au solution hybrid reaction, Hg2+Gold can be formed with nanogold
Amalgam, gold amalgam cannot be catalyzed the redox reaction between the gold chloride and reducing agent of subsequent addition, so that it is molten to extend mixing
Liquid ultimately forms the time that appearance is red nano-Au solution.
Gold chloride can be restored and be generated in the presence of nanometer gold seeds are as catalyst by the reducing agent in the step 2
Nanogold, nanometer gold seeds concentration is bigger, and the quantity and rate that nanogold generates are all bigger, and mixed solution ultimately forms appearance and is
The time of red nano-Au solution is also shorter.
The portable small-sized timing device is miniature electric timer, electronic watch, mechanical watch, mobile phone and has meter
One of hand-held type miniature equipment of Shi Gongneng.
With existing Hg2+Detection method is compared, and of the invention has the prominent advantages that:
1) entire Hg2+Operation in analytic process is extremely simple (mixing step for only relating to four kinds of solution).
2) change of naked-eye observation solution colour is only needed, and can be into using the cheap small-sized timing device such as mobile phone, wrist-watch
The portable quantifiable signal of row is read, to also be able to achieve Hg while greatly reducing analysis cost2+Field assay and immediately
Detection.
3) present invention can directly be applied to all kinds of molten in the numerous areas such as medical diagnosis, environmental monitoring, food safety
Hg in liquid sample2+Simple, economic, quick, sensitive, the special qualitative and quantitative detection of analyte.
Detailed description of the invention
Fig. 1 is to exempt from instrument Hg used in the embodiment of the present invention2+The schematic illustration of quantitative detecting method.
Marked in the figure: 1- test tubes；2- colourless solution；3- nanometers of gold seeds；4-Hg2+；5-Hg2+With nanometer gold seeds
The gold amalgam of formation；6- gold chloride；7- reducing agent；8- mobile phone；9- larger size nanogold；10- contains larger size nanogold
Red solution.
Fig. 2 is to exempt from instrument Hg using of the invention in the embodiment of the present invention 12+Quantitative detecting method analyzes 50 nM Hg2+Sample
Signal time value (time) obtained by this solution is compared with blank sample (blank) gained blank time value.Time value is mobile phone
The autoreduction agent aqueous solution of record has been added to mixed solution is presented the red required time completely.
Fig. 3 is to exempt from instrument Hg using of the invention in the embodiment of the present invention 22+Quantitative detecting method analyzes a series of concentration models
It encloses for the Hg of 0.9 ~ 1000 nM2+Gained signal time value (t when sampleHg2+) blank time value (t in Fig. 2 is individually subtractedblank)
Time difference (t) and Hg2+Log value (the LogC of concentrationHg2+) between working curve.Time value is the autoreduction of mobile phone record
Agent aqueous solution is added to mixed solution is presented the red required time completely.
Specific embodiment
Following embodiment will be further described the present invention, but not thereby limiting the invention.
Embodiment 1:
Exempt from instrument Hg using of the invention2+Quantitative detecting method analyzes 50 nM Hg2+Sample solution and blank sample (blank,
Without Hg2+Resistivity be 18.2 M Ω cm ultrapure water).
As shown in Figure 1, the specific steps of the present embodiment are as follows: step 1, under environment temperature, in the plastics examination of 1 1.5 mL
100 μ L, 50 nM Hg is sequentially added in pipe2+Sample solution (mercuric chloride solution) and the colourless nanogold kind of 100 μ L, 20 nM
Sub- solution (10 nm of partial size；Nanogold seed solution stock solution is prepared by reduction of sodium citrate gold chloride, and then uses resistivity
For 18.2 M Ω cm ultrapure water be diluted to it is colourless), and shake test tube make solution be uniformly mixed, react 20 s；Step 2, after
The sodium citrate aqueous solution of continuous 5 mM of aqueous solution of chloraurate and 100 μ L for sequentially adding 100 μ L, 30 mM, and shake test tube
It is uniformly mixed solution, reacts 20 s；Step 3, the color change of the above-mentioned mixed solution of naked-eye observation, while being remembered using mobile phone
It records and the red required time (time) is presented completely to mixed solution from sodium citrate aqueous solution addition.
According to identical step, by 50 nM Hg2+Sample solution changes blank sample, i.e. ultrapure water (resistivity 18.2 into
M Ω cm), and record to be added from sodium citrate aqueous solution to mixed solution using mobile phone and the red required time is presented completely.
Figure it is seen that detecting the resulting blank time value of blank sample only 5 min, and detect 50 nM Hg2+Sample
The resulting signal time value of solution significantly extends, and is up to 32 min.This is because in the presence of colourless nanogold seed solution, lemon
Lemon acid sodium can quickly restore gold chloride in-situ preparation red nano gold solution；And in Hg2+In the presence of, by with nanometer gold seeds
Gold amalgam is formed, the reaction rate of above-mentioned redox reaction can be significantly inhibited, greatly extend the shape of red nano gold solution
At the time.Contrast and experiment in Fig. 2 shows of the invention to exempt from instrument Hg2+Quantitative detecting method is practical.
Embodiment 2:
Exempt from instrument Hg using of the invention2+Quantitative detecting method analytical concentration range is the Hg of 0.9 ~ 1000 nM2+Sample solution.
As shown in Figure 1, each Hg in the present embodiment2+The specific steps of sample analysis are as follows: step 1, under environment temperature, 1
The a certain concentration Hg of 100 μ L is sequentially added in the plastic test tube of a 1.5 mL2+Sample solution (mercuric chloride solution) and 100 μ L
The colourless nanogold seed solution of 20 nM (10 nm of partial size；Nanogold seed solution stock solution is by reduction of sodium citrate gold chloride system
It is standby, so using resistivity be 18.2 M Ω cm ultrapure water be diluted to it is colourless), and shake test tube make solution be uniformly mixed,
React 20 s；Step 2 continues the sodium citrate for 5 mM of aqueous solution of chloraurate and 100 μ L for sequentially adding 100 μ L, 30 mM
Aqueous solution, and shaking test tube is uniformly mixed solution, reacts 20 s；The color of step 3, the above-mentioned mixed solution of naked-eye observation becomes
Change, while red (letter of required time is presented completely to mixed solution from sodium citrate aqueous solution addition using mobile phone record
Number time value, tHg2+).By the t of all samplesHg2+Blank time value (the t in embodiment 1 is individually subtractedblank) resulting time
Difference (t) is to Hg2+Log value (the LogC of concentrationHg2+) mapping (Fig. 3), that is, it completes to exempt from instrument Hg2+Quantitative detection.
From the figure 3, it may be seen that with Hg2+The increase of concentration, corresponding signal time value and the blank time value in embodiment 1
Difference, i.e. t value are gradually increased.This is because as Hg in sample2+When concentration is larger, inhibit citric acid in same time
Sodium-gold chloride redox reaction rate performance is stronger, so that it is longer to make to be formed the time of red nano gold solution, with blank
The difference (t) of time value is bigger.In addition, Fig. 3 is shown, gained t value and Hg are measured using mobile phone2+The Log value of concentration
(LogCHg2+) good linear relationship is presented in the concentration range of 1.9 ~ 500 nM.
Claims (1)
1. one kind exempts from instrument Hg2+Quantitative detecting method, it is characterised in that specific steps are as follows:
Step 1: by Hg2+Water sample, colourless nano-Au solution hybrid reaction；
Step 2: aqueous solution of chloraurate and reducing agent aqueous solution are continuously added；
Step 3: the color change of visual observation mixed solution, while autoreduction agent is recorded using portable small-sized timing device
Aqueous solution has been added to mixed solution is presented red required time, the time and Hg completely2+Concentration be positively correlated, thus real
Existing Hg2+Timing quantitative detection；
Colourless nano-Au solution in the step 1 is the solution containing nanometer gold seeds, and wherein the partial size of nanometer gold seeds is small
In 10 nm, and using deionized water the solution is diluted to colourless, this nanometer of gold seeds can be catalyzed the gold chloride of subsequent addition
Redox reaction between reducing agent, quickly generating appearance is red nano-Au solution；
Hg in the step 12+Water sample and colourless nano-Au solution hybrid reaction, Hg2+Gold amalgam can be formed with nanogold,
Gold amalgam cannot be catalyzed the redox reaction between the gold chloride and reducing agent of subsequent addition, so that it is final to extend mixed solution
Form the time that appearance is red nano-Au solution；
Gold chloride can be restored in the presence of nanometer gold seeds are as catalyst and generate nanometer by the reducing agent in the step 2
Gold, nanometer gold seeds concentration is bigger, and the quantity and rate that nanogold generates are all bigger, and mixed solution ultimately forms appearance as red
Nano-Au solution time it is also shorter；
The portable small-sized timing device is miniature electric timer, electronic watch, mechanical watch, mobile phone and has timing function
One of the hand-held type miniature equipment of energy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910314816.4A CN110044885A (en) | 2019-04-18 | 2019-04-18 | One kind exempting from instrument Hg2+Quantitative detecting method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910314816.4A CN110044885A (en) | 2019-04-18 | 2019-04-18 | One kind exempting from instrument Hg2+Quantitative detecting method |
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| Publication Number | Publication Date |
|---|---|
| CN110044885A true CN110044885A (en) | 2019-07-23 |
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| CN201910314816.4A Pending CN110044885A (en) | 2019-04-18 | 2019-04-18 | One kind exempting from instrument Hg2+Quantitative detecting method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442513A (en) * | 2016-11-24 | 2017-02-22 | 桂林理工大学 | Instrument-free bivalent copper ion detection method based on timing strategy |
| CN106680232A (en) * | 2017-03-21 | 2017-05-17 | 中国科学院长春光学精密机械与物理研究所 | Reagent composition and reagent solution for detecting Hg<2+> in aqueous solution, preparation method of reagent solution and detection method |
| CN106932390A (en) * | 2017-03-28 | 2017-07-07 | 桂林理工大学 | Hg based on analyte catalytic polymerization2+Colorimetric detection method |
| CN108828047A (en) * | 2018-07-02 | 2018-11-16 | 北京师范大学 | A method of detection Mercury in Water Body ion |
-
2019
- 2019-04-18 CN CN201910314816.4A patent/CN110044885A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106442513A (en) * | 2016-11-24 | 2017-02-22 | 桂林理工大学 | Instrument-free bivalent copper ion detection method based on timing strategy |
| CN106680232A (en) * | 2017-03-21 | 2017-05-17 | 中国科学院长春光学精密机械与物理研究所 | Reagent composition and reagent solution for detecting Hg<2+> in aqueous solution, preparation method of reagent solution and detection method |
| CN106932390A (en) * | 2017-03-28 | 2017-07-07 | 桂林理工大学 | Hg based on analyte catalytic polymerization2+Colorimetric detection method |
| CN108828047A (en) * | 2018-07-02 | 2018-11-16 | 北京师范大学 | A method of detection Mercury in Water Body ion |
Non-Patent Citations (2)
| Title |
|---|
| JUANHUA YANG ET AL: "Analyte-triggered autocatalytic amplification combined with gold nanoparticle probes for colorimetric detection of heavy-metal ions", 《CHEMCOMM》 * |
| 刘广力等: "基于聚乙烯醇/金纳米棒复合凝胶膜的Hg2+传感器构建及应用", 《分析科学学报》 * |
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Application publication date: 20190723 |