CN109030473A - Utilize the method for Nano silver grain detection mercury ion - Google Patents

Utilize the method for Nano silver grain detection mercury ion Download PDF

Info

Publication number
CN109030473A
CN109030473A CN201810605937.XA CN201810605937A CN109030473A CN 109030473 A CN109030473 A CN 109030473A CN 201810605937 A CN201810605937 A CN 201810605937A CN 109030473 A CN109030473 A CN 109030473A
Authority
CN
China
Prior art keywords
solution
nano
mercury ion
silver grain
grain detection
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810605937.XA
Other languages
Chinese (zh)
Inventor
姜翠凤
杨孟达
***
徒华健
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yangcheng Institute of Technology
Yancheng Institute of Technology
Original Assignee
Yangcheng Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yangcheng Institute of Technology filed Critical Yangcheng Institute of Technology
Priority to CN201810605937.XA priority Critical patent/CN109030473A/en
Publication of CN109030473A publication Critical patent/CN109030473A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • 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
    • G01N21/17—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
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • 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
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/7769—Measurement method of reaction-produced change in sensor

Landscapes

  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The present invention relates to Material Fields, in particular to a kind of method using Nano silver grain detection mercury ion.This method comprises: silver nano-particle solution, 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions and H2O2Solution mixing system obtains the first mixed solution；By the first mixed solution and Hg2+Solution mixing after 20-90 DEG C heating 10-40 minutes, with ultraviolet spectrometry spectrometer detection ion concentration of mercury；Wherein, silver nano-particle solution is by NaBH4Solution, Ag+It is made after solution and sodium citrate aqueous solution mixing.The preparation of this method silver nano-particle solution is simple, and required cost of material is lower.So that using the method for Nano silver grain detection mercury ion, cost is relatively low, and can quickly detect mercury ion.

Description

Utilize the method for Nano silver grain detection mercury ion
Technical field
The present invention relates to Material Fields, in particular to a kind of method using Nano silver grain detection mercury ion.
Background technique
Mercury is a kind of heavy metal with very big toxicity, it can enter human body by food chain or environment, right The body of people causes extremely serious harm.And dimercurion (Hg2+) it is the most common existing way of mercury again.Thus, to Hg2 +It is quick detection it is all significant for environment and food safety and human health.
Some mercury detection methods commonly used in the prior art: including x ray fluorescence spectrometry, ICP-AES and Atomic absorption Spectroscopic methodology etc..However, existing above method presence is such as time-consuming, arduously, the defects of equipment expensive and complicated sample pretreatment. A new way is provided for mercury ion detecting based on the colorimetric determination of nano material, does not need expensive equipment, detection Time is also very fast.
What is separately had is some in the prior art using based on colorimetric determination mercury ion.
But this method is mostly used noble metal gold nano-material, it is contemplated that the price of drug needed for gold nano-material is prepared, The cost of this method greatly improves.
Therefore, a kind of method for developing cheap and easy, quick detection mercury ion is extremely urgent.
Summary of the invention
The purpose of the present invention is to provide a kind of methods of cheap and easy, quick detection mercury ion.
To achieve the goals above, technical solution used in the embodiment of the present invention is as follows:
A method of mercury ion is detected using Nano silver grain, comprising: silver nano-particle solution, 3,3', 5,5'- tetramethyls Base biphenyl amine aqueous solution and H2O2Solution mixing system obtains the first mixed solution；By the first mixed solution and Hg2+In 20- after solution mixing 90 DEG C heating 20-40 minutes, with ultraviolet spectrometry spectrometer detect ion concentration of mercury；Wherein, silver nano-particle solution is by NaBH4 Solution, Ag+It is made after solution and sodium citrate aqueous solution mixing.
The beneficial effects of the present invention are:
A kind of method using Nano silver grain detection mercury ion provided by the invention, comprising: silver nano-particle solution, 3, 3', 5,5'- tetramethyl biphenyl amine aqueous solutions and H2O2Solution mixing system obtains the first mixed solution；By the first mixed solution and Hg2+It is molten Liquid mixing after 20-90 DEG C heating 10-40 minutes, with ultraviolet spectrometry spectrometer detection ion concentration of mercury；Wherein, Nano silver grain Solution is by NaBH4Solution, Ag+It is made after solution and sodium citrate aqueous solution mixing.The preparation of this method silver nano-particle solution Simply, required cost of material is lower.So that using the method for Nano silver grain detection mercury ion, cost is relatively low, and can be fast The detection mercury ion of speed.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to institute in embodiment Attached drawing to be used is needed to be briefly described.
Fig. 1 is that the UV, visible light for the method for detecting mercury ion using Nano silver grain that 1-11 of the embodiment of the present invention is provided is inhaled Receive spectrogram；
Fig. 2 is the method Hg that mercury ion is detected using Nano silver grain that 1-11 of the embodiment of the present invention is provided2+Selectivity Experimental result.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is The conventional products that can be obtained by commercially available purchase.
In the description of the present invention, it should be noted that term " first ", " second " etc. are only used for distinguishing description, without It can be interpreted as indication or suggestion relative importance.
The method using Nano silver grain detection mercury ion of the embodiment of the present invention is specifically described below.
A kind of method using Nano silver grain detection mercury ion provided in an embodiment of the present invention, comprising:
S1, preparation silver nano-particle solution.
Silver nano-particle solution is by NaBH4Solution, Ag+It is made after solution and sodium citrate aqueous solution mixing.
Simple using silver nano-particle solution preparation, required cost of material is lower.So that being examined using Nano silver grain Cost is relatively low for the method for survey mercury ion, and can quickly detect mercury ion.
It is further alternative, in the present embodiment, above-mentioned Ag+Solution selects AgNO3Solution.
AgNO3Silver nitrate is a kind of clear crystal, soluble easily in water.Silver nitrate meets the graying black of organic matter, decomposites silver.It is pure Silver nitrate stablizes light, but since general product purity is inadequate, aqueous solution and solid are often saved in brown reagent bottle. Silver nitrate is heated to resolving into silver, nitrogen, oxygen and nitrogen dioxide at 440 DEG C.Aqueous solution and ethanol solution are in neutrality reindeer moss Reaction, pH is about 6.444 DEG C of boiling point (decomposition).It is oxidizing.It is light-exposed to gray or grey black in the presence of organic matter.Nitric acid With a series of reagents precipitation reaction or complexation reaction can occur for silver.
Silver nitrate is common in the extreme, is widely used, and in the prior art, is usually used in photographic emulsion, silver-plated, mirror processed, printing, doctor Medicine, examines chloride ion at dyeing hair, and bromide ion and iodide ion etc. are also used for electronics industry.
Silver nitrate is widely applied in the prior art, cheap.
In the present embodiment, select silver nitrate that can greatly reduce the cost of manufacture of silver nano-particle solution, Jin Erneng Enough it is effectively reduced the cost using Nano silver grain detection mercury ion.
Further, NaBH4Hydrogen in sodium borohydride has partial negative charge (the electronegativity ratio H of B is small), pure and mild amine - OH ,-NH- ,-NH in matter2In hydrogen all have more part positive charge, so the BH in sodium borohydride4Can with constitute these Dihydrogen bond is formed between the molecule of substance, therefore sodium borohydride can be dissolved in water, liquefied ammonia, pure and mild amine substance.
In the present embodiment, NaBH is selected4Solution preparation silver nano-particle solution can obtain the stable silver nanoparticle of performance Particle solution.
Further, sodium citrate is stablized in room temperature and air, micro- in humid air to have dissolubility, produces in hot-air Raw weathering phenomenon.It is heated to 150 DEG C and loses the crystallization water.It is soluble easily in water, dissolve in glycerol, be insoluble in alcohols and other are organic molten Agent is crossed and is thermally decomposed, and micro- in a humid environment to have deliquescence, micro- in hot-air to have weathering, solution ph is about 8.
In the present embodiment, selection sodium citrate solution prepares silver nano-particle solution, further increases silver nanoparticle The stability of particle solution performance.
Further, NaBH4Solution, Ag+The volume ratio of solution and sodium citrate aqueous solution is 15:5:1.
Further, NaBH4Solution, Ag+Solution and sodium citrate aqueous solution are first by NaBH when mixing4Solution, Ag+ After solution mixing, after stirring 5-15 minutes, sodium citrate aqueous solution is added.
Specifically, in the present embodiment, optionally, 15ml 2mM NaBH is first produced4Solution (being prepared using ice water) is added It into 50ml round-bottomed flask, is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then it is added 1% sodium citrate aqueous solution of 1ml makes colloid-stabilised, stirring 20min.Sample save to 4 degrees Celsius it is spare, can be used two days.
S2, the first mixed solution of preparation.
By aforementioned silver nano-particle solution, 3,3' obtained, 5,5'- tetramethyl biphenyl amine aqueous solutions and H2O2Solution mixing system Obtain the first mixed solution.
3,3', 5,5'- tetramethyl benzidines (TMB) are white crystalline powder, odorless, tasteless, are insoluble in water, are soluble in The organic solvents such as acetone, ether, dimethyl sulfoxide, dimethylformamide.A kind of chromogen reagent of new type of safe.
Still optionally further, in this experiment, the selection of TMB solution is prepared with ethyl alcohol.
Further, silver nano-particle solution, 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions and H2O2The volume ratio of solution For 1:1:1:.
Further, the concentration of 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions is 5-12mmol/L；H2O2The concentration of solution is 0.2-100mmol/L。
Further, silver nano-particle solution, 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions and H2O2Solution mixing after also to The buffer that pH value is 3.6-5.6 is added in first mixed solution.
Further, buffer is selected from phosphoric acid, citric acid, carbonic acid, acetic acid, acetate, citrate, carbonate or phosphorus At least one of hydrochlorate.
S3、Hg2+Detection.
Further, by the first mixed solution and Hg2+Solution mixing after 20-90 DEG C heating 10-40 minutes, with ultraviolet point Photothermal spectroscopic analyzer detects ion concentration of mercury.
Since Nano silver grain itself has weaker peroxidase sample activity, TMB+H can be made2O2System is by colourless Become blue, characteristic peak occurs at 652nm in ultraviolet-visible absorption spectroscopy.Be added mercury ion after, due to mercury ion can and silver Nanoparticle reaction, to make its peroxidase sample increased activity, shows as, system is made to darken, and inhales at 652nm Enhancing is received, and the intensity of absorption value is directly proportional to ion concentration of mercury.So as to detect mercury ion.Again because of the atom of mercury ion Core is larger, and the combination of Nano silver grain is better than other metal ions, so, other common metal ions will not interfere mercury ion Measurement.Based on this, this method can it is simple, quickly, selectivity, sensitively detect mercury ion.Silver nano-grain used is not necessarily to Modification.
Feature and performance of the invention are described in further detail with reference to embodiments:
Embodiment 1
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH4Solution (being prepared using ice water) is added to It in 50ml round-bottomed flask, is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1ml is added 1% sodium citrate aqueous solution makes colloid-stabilised, stirring 20min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 10mM TMB, 100ul 50mM H2O2, silver nano-particle solution and 100ul Acetic acid-sodium acetate solution (pH=5.2) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 10min in 50 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 2
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 5min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 5mM TMB, 100ul 0.2mM H2O2, silver nano-particle solution and 100ul acetum (pH=3.6) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 20min in 20 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 3
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 15min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 12mM TMB, 100ul 50mM H2O2, silver nano-particle solution and 100ul citric acid solution (pH=5.6) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 40min in 90 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 4
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 8min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 8mM TMB, 100ul 40mM H2O2, silver nano-particle solution and 100ul phosphoric acid solution (pH=3.8) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 30min in 30 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 5
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 8min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 9mM TMB, 100ul 1mM H2O2, silver nano-particle solution and 100ul carbon acid solution (pH=4.0) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 15min in 40 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 6
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 8min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 9mM TMB, 100ul 4mM H2O2, silver nano-particle solution and 100ul carbon acid solution (pH=4.4) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 15min in 60 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 7
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 8min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 9mM TMB, 100ul 8mM H2O2, silver nano-particle solution and 100ul carbon acid solution (pH=4.6) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 15min in 70 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 8
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 8min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 9mM TMB, 100ul 10mM H2O2, silver nano-particle solution and 100ul carbon acid solution (pH=4.8) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 15min in 60 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 9
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 8min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 9mM TMB, 100ul 40mM H2O2, silver nano-particle solution and 100ul carbon acid solution (pH=5.0) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 15min in 80 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 10
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 8min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 9mM TMB, 100ul 50mM H2O2, silver nano-particle solution and 100ul carbon acid solution (pH=5.4) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 15min in 80 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Embodiment 11
A kind of method using Nano silver grain detection mercury ion provided in this embodiment, comprising:
1. the preparation of silver nano-particle solution: first producing 15ml 2mM NaBH450ml is added in solution (being prepared using ice water) Round-bottomed flask is placed on blender, then instills 5ml 1mM AgNO3Solution is vigorously stirred 10min.Then 1% lemon of 1ml is added Lemon acid sodium aqueous solution makes colloid-stabilised, stirring 8min.Sample is saved to 4 degrees Celsius, can be used two days.
2. preparing the first mixed liquor: by 100ul 9mM TMB, 100ul 0.5mM H2O2, silver nano-particle solution and 100ul carbon acid solution (pH=5.4) is mixed to prepare the first mixed liquor.
3.Hg2+Detection: by the Hg of 100ul the first mixed liquor and various concentration2+(0 0.001 0.005 0.01 0.02 0.03 0.04 0.05 0.06 0.08 0.1 0.15 0.2mM) solution heats 15min in 55 DEG C of water-bath, use ultraviolet spectrometry Spectrometer carries out detection Hg2+Concentration.
Experimental example:
1, the variation of solution colour after observation embodiment 1-11 reacts.
It has been observed that in embodiment 1-11, the solution after reaction is relative to the solution colour before reaction after mercury ion is added It deepens, therefore can significantly detect mercury ion.Wherein, the degree maximum that darkens in embodiment 1, detection effect is most It is good.
2, ultraviolet spectrometry spectral detection result.
The method that embodiment 1-11 is provided illustrates to implement in ultraviolet-visible absorption spectroscopy in 652nm influx and translocation everywhere The method that example 1-11 is provided can quickly detect mercury ion.
Testing result is shown in Fig. 1.Along ordinate, it is followed successively by the corresponding curve of spectrum of embodiment 1-11 from the top down.
3、Hg2+Selectivity experiment.
Other interfering ions, testing result such as Fig. 2 is added in the scheme that embodiment 1-11 is provided.Along ordinate, from On be followed successively by Hg downwards2+Detection curve；Ni+Detection curve；Cu2+Detection curve；Cr2+Detection curve；Al3+Detection curve；Mn2+ Detection curve；Fe3+Detection curve；K+Detection curve；Na+Detection curve；Zn2+Detection curve；Ca2+Detection curve；Pb2+Detection Curve.
From figure 2 it can be seen that Hg2+The sensitivity of detection is significantly greater than other interfering ions.Therefore,
The method that embodiment 1-11 is provided can delicately detect Hg2+。
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of method using Nano silver grain detection mercury ion characterized by comprising
Silver nano-particle solution, 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions and H2O2Solution mixing system obtains the first mixed solution；
By first mixed solution and Hg2+Solution mixing after 20-90 DEG C heating 10-40 minutes, with ultraviolet spectrometry spectrometer Detect ion concentration of mercury；
Wherein, the silver nano-particle solution is by NaBH4Solution, Ag+It is made after solution and sodium citrate aqueous solution mixing.
2. utilizing the method for Nano silver grain detection mercury ion as described in claim 1, which is characterized in that
The silver nano-particle solution, 3,3', 5, the 5'- tetramethyl biphenyl amine aqueous solution and the H2O2Solution mixing after also to The buffer that pH value is 3.6-5.6 is added in first mixed solution.
3. utilizing the method for Nano silver grain detection mercury ion as claimed in claim 2, which is characterized in that
The buffer is in phosphoric acid, citric acid, carbonic acid, acetic acid, acetate, citrate, carbonate or phosphate It is at least one.
4. utilizing the method for Nano silver grain detection mercury ion as described in claim 1, which is characterized in that
When preparing first mixed solution, the concentration of described 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions is 5-12mmol/L.
5. utilizing the method for Nano silver grain detection mercury ion as claimed in claim 4, which is characterized in that
When preparing first mixed solution, the H2O2The concentration of solution is 0.2-100mmol/L.
6. utilizing the method for Nano silver grain detection mercury ion as claimed in claim 5, which is characterized in that
When preparing first mixed solution, the silver nano-particle solution, 3,3', 5, the 5'- tetramethyl biphenyl amine aqueous solution And the H2O2The volume ratio of solution is 1:1:1:.
7. utilizing the method for Nano silver grain detection mercury ion as described in claim 1, which is characterized in that
Heating is using heating water bath.
8. utilizing the method for Nano silver grain detection mercury ion as described in claim 1, which is characterized in that
The Ag+Solution is selected from AgNO3Solution.
9. utilizing the method for Nano silver grain detection mercury ion as described in claim 1, which is characterized in that
The NaBH4Solution, the Ag+The volume ratio of solution and the sodium citrate aqueous solution is 15:5:1.
10. utilizing the method for Nano silver grain detection mercury ion as claimed in claim 9, which is characterized in that
The NaBH4Solution, the Ag+Solution and the sodium citrate aqueous solution are first by the NaBH when mixing4Solution, The Ag+After solution mixing, after stirring 5-15 minutes, the sodium citrate aqueous solution is added.
CN201810605937.XA 2018-06-13 2018-06-13 Utilize the method for Nano silver grain detection mercury ion Pending CN109030473A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810605937.XA CN109030473A (en) 2018-06-13 2018-06-13 Utilize the method for Nano silver grain detection mercury ion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810605937.XA CN109030473A (en) 2018-06-13 2018-06-13 Utilize the method for Nano silver grain detection mercury ion

Publications (1)

Publication Number Publication Date
CN109030473A true CN109030473A (en) 2018-12-18

Family

ID=64609209

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810605937.XA Pending CN109030473A (en) 2018-06-13 2018-06-13 Utilize the method for Nano silver grain detection mercury ion

Country Status (1)

Country Link
CN (1) CN109030473A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109900691A (en) * 2019-04-04 2019-06-18 青岛大学 The test paper of rapid mercury detection ion, preparation method and applications
CN109900690A (en) * 2019-04-04 2019-06-18 青岛大学 A kind of green quickly detects the colloidal sol preparation method and applications of sulphion
CN111337485A (en) * 2020-03-19 2020-06-26 江苏科技大学 Hexavalent chromium colorimetric detection method based on silver nanocluster nanoenzyme
CN113884458A (en) * 2020-07-03 2022-01-04 吉林化工学院 Method for detecting mercury ions by nano silver particles based on green synthesis

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5527524A (en) * 1986-08-18 1996-06-18 The Dow Chemical Company Dense star polymer conjugates
EP0913689A1 (en) * 1997-04-17 1999-05-06 Eicom Corporation Method for detecting s-nitroso compound
CN103808717A (en) * 2014-02-14 2014-05-21 哈尔滨师范大学 Method for detecting mercury ions by adopting colorimetric method
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
CN104458704A (en) * 2014-12-24 2015-03-25 中国科学院合肥物质科学研究院 Method for detecting low-concentration mercury ions based on DNA modified SERS substrate
CN105675793A (en) * 2014-11-20 2016-06-15 中国科学院青岛生物能源与过程研究所 Peroxidase-imitating material and application thereof
CN105675519A (en) * 2016-04-01 2016-06-15 江南大学 Mercury ion detection method
CN106546585A (en) * 2016-11-09 2017-03-29 江南大学 Mercury ion, total mercury and organomercurial detection method and detection kit
US9719975B1 (en) * 2016-03-03 2017-08-01 King Fahd University Of Petroleum And Minerals Mercury detection in water-based compositions

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5527524A (en) * 1986-08-18 1996-06-18 The Dow Chemical Company Dense star polymer conjugates
EP0913689A1 (en) * 1997-04-17 1999-05-06 Eicom Corporation Method for detecting s-nitroso compound
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
CN103808717A (en) * 2014-02-14 2014-05-21 哈尔滨师范大学 Method for detecting mercury ions by adopting colorimetric method
CN105675793A (en) * 2014-11-20 2016-06-15 中国科学院青岛生物能源与过程研究所 Peroxidase-imitating material and application thereof
CN104458704A (en) * 2014-12-24 2015-03-25 中国科学院合肥物质科学研究院 Method for detecting low-concentration mercury ions based on DNA modified SERS substrate
US9719975B1 (en) * 2016-03-03 2017-08-01 King Fahd University Of Petroleum And Minerals Mercury detection in water-based compositions
CN105675519A (en) * 2016-04-01 2016-06-15 江南大学 Mercury ion detection method
CN106546585A (en) * 2016-11-09 2017-03-29 江南大学 Mercury ion, total mercury and organomercurial detection method and detection kit

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
JUNLING DUAN: "Facile colorimetric detection of Hg2þ based on anti-aggregation", 《BIOSENSORS AND BIOELECTRONICS》 *
LI LI: "A colorimetric silver nanoparticle-based assay for Hg(II)", 《MICROCHIM ACTA》 *
孙宗招: "基于银纳米材料催化与荧光特性的传感技术", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
张丹慧: "《贵金属/石墨烯纳米复合材料的合成及性能》", 31 December 2015 *
邱罡: "显色分光光度法在汞(Ⅱ )测定中的应用", 《光谱实验室》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109900691A (en) * 2019-04-04 2019-06-18 青岛大学 The test paper of rapid mercury detection ion, preparation method and applications
CN109900690A (en) * 2019-04-04 2019-06-18 青岛大学 A kind of green quickly detects the colloidal sol preparation method and applications of sulphion
CN109900691B (en) * 2019-04-04 2021-11-19 青岛大学 Test paper for rapidly detecting mercury ions, preparation method and application thereof
CN111337485A (en) * 2020-03-19 2020-06-26 江苏科技大学 Hexavalent chromium colorimetric detection method based on silver nanocluster nanoenzyme
CN113884458A (en) * 2020-07-03 2022-01-04 吉林化工学院 Method for detecting mercury ions by nano silver particles based on green synthesis

Similar Documents

Publication Publication Date Title
CN109030473A (en) Utilize the method for Nano silver grain detection mercury ion
Feng et al. Determination of arsenic, antimony, selenium, tellurium and bismuth in nickel metal by hydride generation atomic fluorescence spectrometry
Gabbay et al. Rapid spectrophotometric micro-determination of nitrites in water
Park et al. Optical ascorbic acid sensor based on the fluorescence quenching of silver nanoparticles
Rajamanikandan et al. β-Cyclodextrin protected gold nanoparticle based cotton swabs as an effective candidate for specific sensing of trace levels of cyanide
Apak et al. Colorimetric sensors and nanoprobes for characterizing antioxidant and energetic substances
CN104198417B (en) Method for testing heavy metal arsenic in compound food additive
Park et al. Spectrofluorimetric method for determination of aluminium with chromotropic acid and its application to water samples
Leong Spectrophotometric determination of uranium (VI) with chromazurol S and cetylpyridinium bromide
CN108827897A (en) The method for detecting mercury ion
CN110186909B (en) Microwave digestion and ICP-OES (inductively coupled plasma-optical emission spectrometry) test of heavy metal elements in leather product
Tiwari A new spectrophotometric method for the determination of ascorbic acid using leuco malachite green
Fernandez-de Cordova et al. Determination of Trace Amounts of Cobalt at sub-μg 1− 1Level by Solid Phase Spectrophotometry
Sánchez et al. Spectrofluorimetric determination of reserpine by oxidation with cerium (IV) sulfate
Zatar et al. Spectrophotometric determination of cobalt with di-2-pyridyl ketone benzoylhydrazone
Hossain et al. A Rapid Spectrofluorometric Method for the Determination of Aluminum at Nano-trace Levels in Some Real, Environmental, Biological, Hemodialysis, Food, Pharmaceutical, and Soil Samples Using 2′, 3, 4′, 5, 7-Pentahydroxyflavone
Lv et al. A stable and sensitive Au metal organic frameworks resonance Rayleigh scattering nanoprobe for detection of SO32–in food based on fuchsin addition reaction
Kleszczewska et al. Spectrometric assay of reaction of L-ascorbic acid with promethazine occuring in quantitative determination of vitamin C
Mori et al. New And sensitive spectrophotometric determination of gold (III) with N, N-dimethyl-p-phenylenediamine and potassium persulfate
Sawicki et al. A Comparison of Methods for Spot Test Detection and Spectrophotometric Determination of Glyoxal.
Bhardwaj et al. Complexation of Norfloxacin with Some Transition Metal Ions-A Spectrophotometric Study
CN108436097A (en) A kind of preparation method of nano-class silver colloidal solution
Smith et al. Potentiometric and spectrophotometric methods for determination of tungsten and vanadium in heteropoly compounds
Watanabe et al. Fluorophotometric determination of trace amounts of atmospheric ozone
CN113125407B (en) Cr (chromium)6+Ion rapid detection method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20181218

RJ01 Rejection of invention patent application after publication