CN108956590A - Purposes of the Au nano particle/polyethyleneimine composite material in detection mercury ion - Google Patents

Purposes of the Au nano particle/polyethyleneimine composite material in detection mercury ion Download PDF

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CN108956590A
CN108956590A CN201810501307.8A CN201810501307A CN108956590A CN 108956590 A CN108956590 A CN 108956590A CN 201810501307 A CN201810501307 A CN 201810501307A CN 108956590 A CN108956590 A CN 108956590A
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solution
composite material
concentration
nano particle
polyethyleneimine
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卢小泉
汪天胜
王泽�
蒲贵强
张守婷
陕多亮
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Northwest Normal University
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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
    • G01N21/17—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
    • 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
    • G01N21/75—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
    • G01N2021/775—Indicator and selective membrane

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  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses purposes of the Au nano particle/polyethyleneimine composite material in detection mercury ion, detection process includes: addition Au nano particle/polyethyleneimine composite material, sample solution to be detected, H into the buffer solution of citric acid and disodium hydrogen phosphate2O2With 3,3', 5,5'- tetramethyl benzidine of color developing agent, the absorbance of solution, obtains Hg in sample solution after then the color of solution or measurement mix after record mixing2+Concentration.With existing Hg2+Detection method is compared, and the present invention can be achieved to Hg2+Inexpensive, fast and convenient quantitative, half-quantitative detection.

Description

Purposes of the Au nano particle/polyethyleneimine composite material in detection mercury ion
Technical field
The present invention relates to Au nano particle/polyethyleneimine composite material purposes.
Background technique
Heavy metal ion has the features such as serious toxicity, strong bioaccumulation, non-natural degradation and complicated source, right Ecological environment and human health do great damage.Mercury ion (the Hg generated by various natural origins and industrial waste2+) wide It is general to be considered most dangerous one of pollutant.Toxicologic study confirms Hg2+To brain, kidney, central nervous system, immune system It causes greatly to damage with endocrine system, in recent years, detects toxic Hg in aquatic system2+Content cause the pass of people Note.Therefore, a kind of efficiently convenient cheap analysis method is developed for Hg2+Highly sensitive, highly selective detection, have weight The realistic meaning wanted.
Currently, to Hg2+Detection depend on micro- spectrum analysis (MS), atomic absorption method (AAS), atomic fluorescence method (AFS), inductively coupled plasma body method (ICP), X fluorescence spectrum (XRF), Inductively coupled plasma-mass spectrometry (ICP-MS) and electricity Chemical method (CV).Although the detection precision of these methods is high, the instrument of these analysis methods is more expensive, running cost With height, to the more demanding of testing conditions, the pre-treatment of sample is more troublesome, and whole process is more time-consuming, causes discomfort For large-scale field quick detection.
Summary of the invention
It is an object of the invention to the statuses according to above-mentioned background technique, provide a kind of Au nano particle/polyethyleneimine The purposes of amine composite material, to realize to Hg2+Inexpensive, fast and convenient quantitative, half-quantitative detection.
In order to solve the above-mentioned technical problems, the present invention provides the following technical solutions:
Au nano particle/polyethyleneimine composite material is in detection Hg2+In purposes.
Au nano particle/polyethyleneimine the composite material can be by including the following steps to be made: by polyethyleneimine Ethanol solution and sodium chloraurate ethanol solution after mixing, be added sodium borohydride, reduction generate Au nano particle/poly- second Alkene imines composite material.
Preferably, the mass ratio of sodium chloraurate and polyethyleneimine is 1:1~10, and preferably mass ratio is 1:5.
Preferably, the weight average molecular weight of the polyethyleneimine is 20000~30000, more preferably polyethyleneimine Weight average molecular weight is 25000.
Hg is detected with Au nano particle/polyethyleneimine composite material2+The step of include:
To in the buffer solution of citric acid and disodium hydrogen phosphate be added Au nano particle/polyethyleneimine composite material, to Sample solution, the H of detection2O2With 3,3', 5,5'- tetramethyl benzidine of color developing agent, the color or survey of solution after then record mixes The absorbance of solution, obtains Hg in sample solution after fixed mixing2+Concentration.
Using above-mentioned same steps to the Hg of series of concentrations2+Standard solution is detected, and standard corresponding with concentration is made The standard curve of color picture or concentration and absorbance.By standard color picture or standard curve, sample to be detected is judged Product Solution H g2+Concentration.
Preferably, the pH of the buffer solution of the citric acid and disodium hydrogen phosphate is 3.5~4.5, and more preferably pH is 4.
Preferably, by addition H2O2Afterwards, H in solution2O2Concentration be 0.05~0.55mol/L, preferably concentration is 0.50mol/L。
Preferably, after by 3,3', 5,5'- tetramethyl benzidine of color developing agent is added, 3,3', 5,5'- tetramethyls join in solution The concentration of aniline is 0.05~0.25mmol/L, and preferably concentration is 0.20mmol/L.
Preferably, after by Au nano particle/polyethyleneimine composite material is added, Au nano particle/polyethylene in solution Concentration of the imines composite material in terms of Au is 0.1~1 μm of ol/L, and preferably concentration is 0.5 μm of ol/L.
Preferably, absorbance of the solution at 652nm after measurement mixing, detection temperature are 35 DEG C.
Au nano particle of the present invention/PEI composite material detects Hg2+Principle: in the buffering of citric acid and disodium hydrogen phosphate In solution, since citrate has weak reproducibility, by Hg2+It is reduced to Hg0, Hg after reduction0It is compound to be attached to Au/PEI Au nano grain surface in material, forms Au-Hg alloy, which is catalyzed H2O2OH is generated, OH is by seizing color developing agent The electronics of TMB makes TMB become oxTMB, and the color of solution becomes blue from colourless, to realize to Hg2+Detection.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is that the TEM of Au/PEI composite material of the present invention schemes.
Fig. 2 is ultraviolet-visible spectrogram of the present invention detection solution within the scope of 500-750nm.
Fig. 3 is the optimum results of testing conditions of the present invention, in which: a is the optimum results for detecting temperature；B is the excellent of pH value Change result；C is the optimum results of TMB concentration；D is H2O2The optimum results of concentration.
Fig. 4 is Hg of the present invention2+Selective experimental result of the detection method to 16 metal ion species.
Fig. 5 is Hg of the present invention2+Interference--free experiments result of the detection method to 16 metal ion species.
Fig. 6 is Hg of the present invention2+The linear graph of detection method.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
1, the preparation and characterization of Au/PEI composite material
By 1g PEI, (polyethyleneimine, weight average molecular weight: 25000) being dissolved in 100mL dehydrated alcohol, takes 2.5mL above-mentioned Solution adds 20mL dehydrated alcohol in 100mL round-bottomed flask, under magnetic agitation, is slowly added to 5mL dissolved with 5mg gold chloride The ethanol solution of sodium stirs 2 hours, adds 1mL dissolved with the ethanol solution of 10mg sodium borohydride, after persistently stirring 4 hours, revolves Turn to evaporate most solvent, washes off excessive PEI and sodium borohydride with petroleum ether/ethyl alcohol, then remove stone with a small amount of ethyl alcohol Oily ether, is placed in that allow ethyl alcohol to volatilize naturally at room temperature dry, is finally scattered in the deionized water of 1mL and is saved, passes through ICP-MS The content for measuring Au in Au nano particle/polyethyleneimine composite material is 10mmol/L, the transmission electricity of Au/PEI composite material Mirror such as Fig. 1, the left side are the transmission electron microscope picture of Au/PEI composite material, and illustration is the particle diameter distribution of Au nano particle, partial size master It will be in 3.6 ± 0.4nm；Right figure is high power transmission electron microscope picture, and the spacing of lattice of Au nano particle is 0.23nm as we know from the figure, brilliant Face is 200 faces.
2, the visible absorption spectra of solution
Two identical quartz colorimetric utensils are taken, the volume of solution is all 2mL in cuvette when measuring below, in one successively Addition citric acid and disodium hydrogen phosphate buffer solution (25mmol/L, 1850 μ L), Au/PEI composite material solution (100 μm of ol/L, 10 μ L), Hg2+(1.0mmol/L, 20 μ L), TMB (20mmol/L, 20 μ L), H2O2(10mol/L, 100 μ L) are not added in another Hg2+As control, absorption spectrum of two cuvettes between 500-750nm is scanned using UV-vis spectrometer, as a result such as Fig. 2 It is shown.From figure 2 it can be seen that added with Hg2+Cuvette in solution occur maximum absorption band at 652nm, and not plus Hg2+ Cuvette in solution do not absorbed within the scope of 500-750nm, therefore, the present invention is using 652nm as Hg2+Quantitative detection is most Good absorbing wavelength.
3、Hg2+The optimization of testing conditions:
(1) optimization of temperature: in cuvette, sequentially add citric acid and disodium hydrogen phosphate buffer solution (25mmol/L, 1850 μ L), Au/PEI composite material solution (100 μm of ol/L, 10 μ L), Hg2+(1.0mmol/L, 20 μ L), TMB (20mmol/L, 20 μ L) and H2O2(10mol/L, 100 μ L), in the different temperatures of 20-45 DEG C (20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C) Absorbance of the lower measurement solution at 652nm, as a result as shown in Figure 3a, the absorbance of solution is maximum when temperature is 35 DEG C, therefore selects Selecting optimum temperature is 35 DEG C.
(2) optimization of pH value: compound concentration 25mmol/L, pH be respectively 2,2.5,3,3.5,4,4.5,5,5.5,6, 6.5, the buffer solution of 7 citric acid and disodium hydrogen phosphate, then be sequentially added into the buffer solution (1850 μ L) of different pH Au/PEI composite material solution (100 μm of ol/L, 10 μ L), Hg2+(1.0mmol/L, 20 μ L), TMB (20mmol/L, 20 μ L) and H2O2(10mol/L, 100 μ L).Temperature measures under different pH absorbance of the solution at 652nm with the variation feelings of pH at 35 DEG C Condition.As a result as shown in Figure 3b, the absorbance of solution is maximum when pH is 4, therefore selects Optimal pH for 4.
(3) optimization of TMB concentration: being 4 in pH, under the conditions of temperature is 35 DEG C, in 1850 μ L citric acids and disodium hydrogen phosphate In buffer solution, Au/PEI composite material solution (100 μm of ol/L, 10 μ L), Hg are sequentially added2+(1.0mmol/L, 20 μ L), H2O2(10mol/L, 100 μ L) and various concentration (0,0.05,0.10,0.15,0.20,0.25mmol/L, by the concentration after addition Calculate) TMB, measure cuvette in absorbance of the solution at 652nm, as a result as shown in Figure 3c, TMB concentration is in solution The absorbance of solution is maximum when 0.20mmol/L, therefore selecting best TMB concentration is 0.20mmol/L.
(4)H2O2The optimization of concentration: being 4 in pH, under the conditions of temperature is 35 DEG C, in 1850 μ L citric acids and disodium hydrogen phosphate In buffer solution, Au/PEI composite material solution (100 μm of ol/L, 10 μ L), Hg are sequentially added2+(1.0mmol/L, 20 μ L), TMB (20mmol/L, 20 μ L) and various concentration (0,0.05,0.10,0.15,0.20,0.25,0.30,0.35,0.40,0.45, 0.50,0.55mol/L, by the concentration calculation after addition) H2O2.As a result as shown in Figure 3d, H in solution2O2Concentration is The absorbance of solution is maximum when 0.50mol/L, therefore selects best H2O2Concentration is 0.50mol/L.
To sum up, the optimum reaction condition of detection method are as follows: the concentration of citric acid and disodium hydrogen phosphate buffer solution For 25mmol/L, pH 4, temperature is 35 DEG C, and the concentration of TMB is 0.20mmol/L, H2O2Concentration be 0.50mol/L.
Due to containing Hg during actually detected2+Sample to be tested source it is different, complicated component, therefore, in order to verify this hair Bright method is to containing Hg2+The universality of sample solution carries out Hg below2+Selectivity experiment and interference--free experiments.
4, selectivity experiment
The Na of 2mmol/L is prepared respectively+, K+, NH4 +, Ca2+, Cu2+, Co2+, Fe2+, Ni2+, Cd2+, Mn2+, Pb2+, Mg2+, Zn2 +, Al3+, Cr3+, Fe3+And Hg2+Solution；Citric acid and disodium hydrogen phosphate buffer solution are sequentially added in quartz colorimetric utensil (25mmol/L, 1850 μ L), Au/PEI composite material solution (100 μm of ol/L, 10 μ L), TMB (20mmol/L, 20 μ L), H2O2 (10mol/L, 100 μ L), then it is separately added into the solution (20 μ L) of above-mentioned 16 kinds of ions, solution is measured respectively after reaction 6min exists Absorbance at 652nm, as a result such as Fig. 4, figure 4, it is seen that the present invention is to Hg2+With good selectivity.
5, interference--free experiments
Identical 16 kinds of metals interfering ion solution in preparing and selectively testing respectively, successively adds in quartz colorimetric utensil Enter citrate-phosphate disodium hydrogen buffer solution (25mmol/L, 1850 μ L), then sequentially adds Au/PEI composite material solution (100 μm of ol/L, 10 μ L), one of 20 μ L interfering ions or one of 20 μ L interfering ions and Hg2+(1.0mmol/L, 20 μ L), H2O2(10mol/L, 100 μ L) and TMB (20mmol/L, 20 μ L) measures solution at 652nm after reacting 6min respectively Absorbance, as a result as shown in Figure 5.From figure 5 it can be seen that not adding Hg2+Solution have weaker absorption at 652nm, and Hg is added2+Solution has very strong absorption at 652nm afterwards, shows to detect Hg using the method for the present invention2+To other 16 kinds of metals Ion has good anti-interference.
6, Hg of the present invention2+The detailed process of sxemiquantitative or quantitative detection:
(1) Hg is established2+Macroscopic sxemiquantitative or quantitative measurement standard:
Citric acid and disodium hydrogen phosphate buffer solution (25mmol/L, 1850 μ L) are added in quartz colorimetric utensil, then according to Secondary addition Au/PEI composite material solution (100 μm of ol/L, 10 μ L), H2O2(10mol/L, 100 μ L), TMB (20mmol/L, 20 μ L) and be added Hg2+The Hg of various concentration in solution is obtained afterwards2+(0,0.5,1,2,4,6,8,10,12,14,16,18,20,22, 24,26,28 and 30nmol/L), difference recording solution color and preservation image, and absorbance of the solution at 652nm is measured, with Absorbance (y) is ordinate, Hg2+Concentration (x, nmol/L) is that abscissa obtains equation of linear regression as shown in fig. 6, linear equation Are as follows: y=0.0129x+0.0644, R2=0.9974, the range of linearity are as follows: 0.5-30nmol/L.
Under optimum experimental condition, Hg not to be added2+Reaction solution be blank solution, by above-mentioned experimental method parallel determination Absorbance value of 16 groups of blank solutions at 652nm, is calculated that (б is the standard deviation of 16 blank solutions, and k is linear by 3 б/k The slope of equation) the method for the present invention detection be limited to 0.69nmol/L.
(2) Hg in test sample solution2+:
Contain Hg to 3 according to method in (1)2+Sample solution detected, recording solution color, then with (1) in figure Picture color (namely standard color picture) compares control, determines Hg2+Concentration range, thus to contain Hg2+Sample solution progress can Depending on changing half-quantitative detection；If wanting to further realize quantitative detection, measurement 3 contain Hg2+Extinction of the sample solution at 652nm Angle value is respectively 0.153,0.303 and 0.421, is obtained in testing sample solution according to linear equation y=0.0129x+0.0644 Hg2+Concentration be respectively 6.7nmol/L, 18.5nmol/L and 27.6nmol/L.
In addition, if the concentration of sample solution exceeds the detection range of the method for the present invention certain journey can be carried out to sample solution It is detected after the dilution of degree, then releases Hg in sample solution according to extension rate is counter2+Concentration.
If not otherwise specified, the concentration of Au/PEI composite material solution of the present invention is in terms of Au.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention, Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features. All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention Within protection scope.

Claims (10)

  1. Purposes of the 1.Au nano particle/polyethyleneimine composite material in detection mercury ion.
  2. 2. purposes according to claim 1, it is characterised in that: the Au nano particle/polyethyleneimine composite material is logical It crosses and includes the following steps to be made: after mixing by the ethanol solution of the ethanol solution of polyethyleneimine and sodium chloraurate, being added Sodium borohydride, reduction generate Au nano particle/polyethyleneimine composite material.
  3. 3. purposes according to claim 2, it is characterised in that: the mass ratio of sodium chloraurate and polyethyleneimine be 1:1~ 10, preferably mass ratio is 1:5.
  4. 4. purposes according to claim 2, it is characterised in that: the weight average molecular weight of the polyethyleneimine be 20000~ 30000.Preferably weight average molecular weight is 25000.
  5. 5. purposes according to claim 1, it is characterised in that: with Au nano particle/polyethyleneimine composite material detection The step of mercury ion includes:
    To Au nano particle/polyethyleneimine composite material, to be detected is added in the buffer solution of citric acid and disodium hydrogen phosphate Sample solution, H2O2With 3,3', 5,5'- tetramethyl benzidine of color developing agent, then the color of solution or measurement are mixed after record mixing The absorbance of solution after conjunction, obtains Hg in sample solution2+Concentration.
  6. 6. purposes according to claim 5, it is characterised in that: the pH of the buffer solution of the citric acid and disodium hydrogen phosphate It is 3.5~4.5, preferably pH is 4.
  7. 7. purposes according to claim 5, it is characterised in that: by addition H2O2Afterwards, H in solution2O2Concentration be 0.05~ 0.55mol/L, preferably concentration are 0.50mol/L.
  8. 8. purposes according to claim 5, it is characterised in that: by addition 3,3', 5,5'- tetramethyl benzidine of color developing agent Afterwards, the concentration of 3,3', 5,5'- tetramethyl benzidines is 0.05~0.25mmol/L in solution, and preferably concentration is 0.20mmol/ L。
  9. 9. purposes according to claim 5, it is characterised in that: by addition Au nano particle/polyethyleneimine composite material Afterwards, Au nano particle/concentration of the polyethyleneimine composite material in terms of Au is 0.1~1 μm of ol/L in solution, and preferably concentration is 0.5μmol/L。
  10. 10. purposes according to claim 5, it is characterised in that: absorbance of the measurement mixed solution at 652nm, detection Temperature is 35 DEG C.
CN201810501307.8A 2018-05-23 2018-05-23 Purposes of the Au nano particle/polyethyleneimine composite material in detection mercury ion Pending CN108956590A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111337485A (en) * 2020-03-19 2020-06-26 江苏科技大学 Hexavalent chromium colorimetric detection method based on silver nanocluster nanoenzyme
CN112697781A (en) * 2020-11-26 2021-04-23 南京师范大学 Visual Hg2+Preparation method of detection material, detection material prepared by preparation method and application of detection material
CN113848190A (en) * 2021-09-26 2021-12-28 北京建工环境修复股份有限公司 Rapid detection method and detection device for medium-long chain perfluorocarboxylic acid in water sample
CN114486781A (en) * 2022-02-10 2022-05-13 青海大学 Method for high-sensitivity detection of mercury ions by novel Au/C nano composite sensor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111337485A (en) * 2020-03-19 2020-06-26 江苏科技大学 Hexavalent chromium colorimetric detection method based on silver nanocluster nanoenzyme
CN112697781A (en) * 2020-11-26 2021-04-23 南京师范大学 Visual Hg2+Preparation method of detection material, detection material prepared by preparation method and application of detection material
CN112697781B (en) * 2020-11-26 2023-01-31 南京师范大学 Visual Hg 2+ Preparation method of detection material, detection material prepared by preparation method and application of detection material
CN113848190A (en) * 2021-09-26 2021-12-28 北京建工环境修复股份有限公司 Rapid detection method and detection device for medium-long chain perfluorocarboxylic acid in water sample
CN114486781A (en) * 2022-02-10 2022-05-13 青海大学 Method for high-sensitivity detection of mercury ions by novel Au/C nano composite sensor

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Application publication date: 20181207