CN103344596A - Method for quantitatively analyzing silver or copper ions by nano porous silicon - Google Patents
Method for quantitatively analyzing silver or copper ions by nano porous silicon Download PDFInfo
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- CN103344596A CN103344596A CN2013102895577A CN201310289557A CN103344596A CN 103344596 A CN103344596 A CN 103344596A CN 2013102895577 A CN2013102895577 A CN 2013102895577A CN 201310289557 A CN201310289557 A CN 201310289557A CN 103344596 A CN103344596 A CN 103344596A
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- 229910021426 porous silicon Inorganic materials 0.000 title claims abstract description 38
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910001431 copper ion Inorganic materials 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 29
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 28
- 239000004332 silver Substances 0.000 title claims abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 22
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000012360 testing method Methods 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 238000005424 photoluminescence Methods 0.000 claims abstract description 7
- 239000002086 nanomaterial Substances 0.000 claims description 27
- 238000012113 quantitative test Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 5
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000012544 monitoring process Methods 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- 238000005286 illumination Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 10
- 238000000103 photoluminescence spectrum Methods 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 229910001385 heavy metal Inorganic materials 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- VQLYBLABXAHUDN-UHFFFAOYSA-N bis(4-fluorophenyl)-methyl-(1,2,4-triazol-1-ylmethyl)silane;methyl n-(1h-benzimidazol-2-yl)carbamate Chemical compound C1=CC=C2NC(NC(=O)OC)=NC2=C1.C=1C=C(F)C=CC=1[Si](C=1C=CC(F)=CC=1)(C)CN1C=NC=N1 VQLYBLABXAHUDN-UHFFFAOYSA-N 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- -1 silver ions Chemical class 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001142 circular dichroism spectrum Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention provides a method for quantitatively analyzing silver or copper ions by nano porous silicon. The method comprises the following steps of: illuminating the surface of nano porous silicon as a standard sample by using an ultraviolet lamp, recording a light-emitting wavelength and a light-emitting strength; respectively placing a test sample in one group of silver or copper ion-containing water solutions with concentration gradient for absorbing, washing with deionized water, then drying the test sample by using nitrogen, illuminating the surface of the test sample by using the ultraviolet lamp, recording a light-emitting wavelength and a light-emitting strength of the test sample, establishing function relationship by using the obtained light-emitting wavelengths and the obtained light-emitting strengths according to silver and copper ion concentrations and photoluminescence strength, detecting the silver or copper ion-containing water solutions to be tested by adopting the same method, comparing a strength value I with a standard curve to obtain the concentration of the silver or copper ion-containing water solutions to be tested. The method has the advantages of convenience, simplicity in operation, low cost, capability of carrying out real-time monitoring, and the like. The purpose of detecting silver and copper ions is achieved through simply comparing color change of the surface of the porous silicon before and after being in contact with the silver and copper ions under the illumination of the ultraviolet lamp.
Description
Technical field
The invention belongs to the chemical sensor technical field, relate to a kind of nano-structure porous silicon to the method for silver or copper ion quantitative test.
Background technology
At present, the method that is used for the trace heavy metal detection mainly contains spectroscopic analysis methods such as atom absorption, atomic fluorescence, inductively coupled plasma, inductively coupled plasma mass spectrometry, and ultraviolet-visible spectrophotometry etc.The required instrument of these methods itself costs expensive usually, and the operating cost height need possess skilled operating experience and enough work spaces, more time-consuming when realizing detecting on a large scale, effort; And the required complex pretreatment of method that has when measuring, need extraction, enrichment method or suppress to disturb; What have can not carry out many components or multielement analysis; The meeting that has can't be measured because of interference such as element, spectrum.The developing direction that detects at present the water environment heavy metal in the world is on-the-spot, quick, real-time, online, continuous and automatic measurement, so the microminiaturization of sensor, portability, robotization integrated and analytical instrument are the inexorable trends that develops.
Under such overall background, simple to operate for having, volume is little, cost is low, do not need the research of the chemical sensor of advantages such as pre-service more and more to be paid close attention to.On detection method, chemical sensor mainly is to utilize instruments such as galvanochemistry, ultraviolet, fluorescence, infrared, circular dichroism spectra and nuclear-magnetism to realize.According to applied detection method, chemical sensor can be divided into electrochemical sensor, fluorescent optical sensor and add lustre to (ultraviolet) sensor etc.The sensor that adds lustre to wherein refers to the sensor of change color as the segment signal output of chemical sensor, with respect to electrochemical sensor and fluorescent optical sensor, the sensor application of adding lustre to more extensive, because it is without any need for the instrument of costliness, directly the observation by naked eyes just can reach identifying purpose.Except detecting by an unaided eye, the sensor that adds lustre to often carries out quantitative examination with the variation of ultraviolet spectrum.These advantages make the sensor that adds lustre to become one of sensor that most possible large tracts of land popularizes and promote.
As a kind of novel nano-material, about the existing a lot of reports of porous silicon ultra-violet light-emitting The Characteristic Study, but the core of paying close attention to is by improving its luminescent properties at hole silicon face modified metal species (comprising noble metal, transition metal or metal oxide) at present.The interaction of research different metal species and porous silicon surface and to the influence of its characteristics of luminescence, purpose is to seek a kind of method that improves porous silicon luminescence intensity or prolongation luminescent lifetime.Even in some documents, also reported when porous silicon and the phenomenon that has fluorescent weakening or cancellation after silver or copper ion contact, but be a phenomenon even be considered to improving porous silicon luminescence disadvantageous " bad thing ", do not seeing that so far this phenomenon of utilization realizes the report to silver, copper or other metallic ions.
Summary of the invention
The present invention exactly utilizes the phenomenon of porous silicon fluorescent quenching, to realize the fast qualitative of silver, copper ion or the purpose that quantitatively detects, this method has conveniently, simple to operate, cost is low and monitoring and other advantages in real time, this is to popularizing of detecting of heavy metal ion (copper, silver) and promote significant.
The present invention realizes by following technical proposal: a kind of nano-structure porous silicon passes through following each step to the method for silver or copper ion quantitative test:
(1) nano-structure porous silicon is placed the darkroom as standard sample, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 200～400nm, record its emission wavelength and intensity;
(2) adopt the nano-structure porous silicon identical with standard sample as the test sample, place one group of argentiferous or copper ion aqueous solution with concentration gradient to adsorb 1～600min respectively it, use deionized water rinsing again, dry up the test sample with nitrogen then, to test sample and place the darkroom respectively, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 200～400nm, record its emission wavelength and intensity;
(3) with step (1) and (2) gained emission wavelength and intensity, set up funtcional relationship by silver, copper ion concentration (C) with photoluminescence intensity (I), obtain the typical curve of comparing in the quantitative test process (C-I);
(4) adopt the nano-structure porous silicon identical with standard sample as detecting sample, be placed in the argentiferous of concentration to be measured or the copper ion aqueous solution and adsorb 1～600min, use deionized water rinsing again, dry up the detection sample with nitrogen then, to detect sample and place the darkroom, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 200～400nm, record its emission wavelength and intensity, with intensity level I comparison step (3) gained typical curve (C-I), namely obtain the concentration C of argentiferous to be measured or copper ion aqueous solution then.
The scope of the concentration gradient of described step (2) is 0.001 μ mol/L～10mol/L.
The nano-structure porous silicon that the present invention uses is to prepare by application number 201110389121.6 disclosed methods.
Advantage of the present invention and effect: nano-structure porous silicon shows certain selectivity as Ultraviolet sensor to silver, copper ion, and it is to Zn
2+, Fe
2+, Na
+, K
+, Mg
2+, Ca
2+, Pb
2+, Al
3+Plasma is insensitive.The phenomenon of Ultraluminescence cancellation takes place in the present invention behind absorption silver, copper metal ion according to the porous silicon with ultraviolet photoluminescence, it is applied to detection silver-colored, the copper heavy metal ion, this method has conveniently, simple to operate, cost is low and monitoring and other advantages in real time, this is to popularizing of detecting of heavy metal ion (copper, silver) and promote significant.This method is contacting front and back by simple contrast porous silicon surface with silver, copper ion, change color under ultra violet lamp reaches the purpose that silver, copper ion are detected, compare with traditional metal ion inspection (atom absorption, atomic fluorescence, inductively coupled plasma), this method has conveniently, simple to operate, cost is low and monitoring and other advantages in real time, this is to popularizing of detecting of heavy metal ion (copper, silver) and promote significant.
Description of drawings
Fig. 1 is the ultraviolet photoluminescence spectrum before and after nano-structure porous silicon absorption silver or the copper ion.
Embodiment
The present invention will be further described below in conjunction with drawings and Examples.
(1) prepares nano-structure porous silicon by application number 201110389121.6 disclosed methods, nano-structure porous silicon is placed the darkroom as standard sample, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 200nm, adopt its photoluminescence spectrum of fluorescence spectrophotometer measurement, record its emission wavelength and intensity;
(2) adopt the nano-structure porous silicon identical with standard sample as the test sample, it is placed one group of argentiferous deionized water solution (0.001 μ mol/L with concentration gradient respectively, 0.005 μ mol/L, 0.01 μ mol/L, 0.02 μ mol/L, 0.03 μ mol/L, 0.04 μ mol/L ... 7mol/L, 8mol/L, 9mol/L, 10mol/L) adsorb 300min, use deionized water rinsing again, dry up the test sample with nitrogen then, to test sample and place the darkroom respectively, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 200nm, adopt its photoluminescence spectrum of fluorescence spectrophotometer measurement, record its emission wavelength and intensity;
(3) with step (1) and (2) gained emission wavelength and intensity, set up funtcional relationship by concentration of silver ions (C) and photoluminescence intensity (I), obtain the typical curve of comparing in the quantitative test process (C-I);
(4) adopt the nano-structure porous silicon identical with standard sample as detecting sample, be placed in the argentiferous deionized water solution of concentration to be measured and adsorb 300min, use deionized water rinsing again, dry up the detection sample with nitrogen then, to detect sample and place the darkroom, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 200nm, adopt its photoluminescence spectrum of fluorescence spectrophotometer measurement, record its emission wavelength and intensity, with intensity level I comparison step (3) gained typical curve (C-I), namely obtain the concentration C of argentiferous deionized water solution to be measured then.
Embodiment 2
(1) prepares nano-structure porous silicon by application number 201110389121.6 disclosed methods, nano-structure porous silicon is placed the darkroom as standard sample, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 300nm, adopt its photoluminescence spectrum of fluorescence spectrophotometer measurement, record its emission wavelength and intensity;
(2) adopt the nano-structure porous silicon identical with standard sample as the test sample, it is placed one group of copper ions aqueous solution (0.001 μ mol/L with concentration gradient respectively, 0.005 μ mol/L, 0.01 μ mol/L, 0.02 μ mol/L, 0.03 μ mol/L, 0.04 μ mol/L ... 7mol/L, 8mol/L, 9mol/L, 10mol/L) adsorb 600min, use deionized water rinsing again, dry up the test sample with nitrogen then, to test sample and place the darkroom respectively, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 300nm, adopt its photoluminescence spectrum of fluorescence spectrophotometer measurement, record its emission wavelength and intensity;
(3) with step (1) and (2) gained emission wavelength and intensity, set up funtcional relationship by copper ion concentration (C) and photoluminescence intensity (I), obtain the typical curve of comparing in the quantitative test process (C-I);
(4) adopt the nano-structure porous silicon identical with standard sample as detecting sample, be placed in the copper ions aqueous solution of concentration to be measured and adsorb 600min, use deionized water rinsing again, dry up the detection sample with nitrogen then, to detect sample and place the darkroom, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 300nm, adopt its photoluminescence spectrum of fluorescence spectrophotometer measurement, record its emission wavelength and intensity, with intensity level I comparison step (3) gained typical curve (C-I), namely obtain the concentration C of copper ions aqueous solution to be measured then.
(1) prepares nano-structure porous silicon by application number 201110389121.6 disclosed methods, nano-structure porous silicon is placed the darkroom as standard sample, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 400nm, adopt its photoluminescence spectrum of fluorescence spectrophotometer measurement, record its emission wavelength and intensity;
(2) adopt the nano-structure porous silicon identical with standard sample as the test sample, it is placed one group of argentiferous deionized water solution (0.001 μ mol/L with concentration gradient respectively, 0.005 μ mol/L, 0.01 μ mol/L, 0.02 μ mol/L, 0.03 μ mol/L, 0.04 μ mol/L ... 7mol/L, 8mol/L, 9mol/L, 10mol/L) adsorb 1min, use deionized water rinsing again, dry up the test sample with nitrogen then, to test sample and place the darkroom respectively, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 400nm, adopt its photoluminescence spectrum of fluorescence spectrophotometer measurement, record its emission wavelength and intensity;
(3) with step (1) and (2) gained emission wavelength and intensity, set up funtcional relationship by concentration of silver ions (C) and photoluminescence intensity (I), obtain the typical curve of comparing in the quantitative test process (C-I);
(4) adopt the nano-structure porous silicon identical with standard sample as detecting sample, be placed in the argentiferous deionized water solution of concentration to be measured and adsorb 1min, use deionized water rinsing again, dry up the detection sample with nitrogen then, to detect sample and place the darkroom, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 400nm, adopt its photoluminescence spectrum of fluorescence spectrophotometer measurement, record its emission wavelength and intensity, with intensity level I comparison step (3) gained typical curve (C-I), namely obtain the concentration C of argentiferous deionized water solution to be measured then.
Claims (2)
1. a nano-structure porous silicon is characterized in that through following each step the method for silver or copper ion quantitative test:
(1) nano-structure porous silicon is placed the darkroom as standard sample, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 200～400nm, record its emission wavelength and intensity;
(2) adopt the nano-structure porous silicon identical with standard sample as the test sample, place one group of argentiferous or copper ion aqueous solution with concentration gradient to adsorb 1～600min respectively it, use deionized water rinsing again, dry up the test sample with nitrogen then, to test sample and place the darkroom respectively, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 200～400nm, record its emission wavelength and intensity;
(3) with step (1) and (2) gained emission wavelength and intensity, set up funtcional relationship by silver, copper ion concentration (C) with photoluminescence intensity (I), obtain the typical curve of comparing in the quantitative test process (C-I);
(4) adopt the nano-structure porous silicon identical with standard sample as detecting sample, be placed in the argentiferous of concentration to be measured or the copper ion aqueous solution and adsorb 1～600min, use deionized water rinsing again, dry up the detection sample with nitrogen then, to detect sample and place the darkroom, at room temperature adopt emission wavelength on its surface of ultra violet lamp of 200～400nm, record its emission wavelength and intensity, with intensity level I comparison step (3) gained typical curve (C-I), namely obtain the concentration C of argentiferous to be measured or copper ion aqueous solution then.
2. nano-structure porous silicon according to claim 1 is characterized in that the method for silver or copper ion quantitative test: the scope of the concentration gradient of described step (2) is 0.001 μ mol/L～10mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947290A (en) * | 2017-03-31 | 2017-07-14 | 合肥悦兰信息技术有限公司 | The preparation method of colored silicon-dioxide powdery material |
Citations (2)
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|---|---|---|---|---|
| US20070153266A1 (en) * | 2005-12-30 | 2007-07-05 | Tae-Woong Koo | Porous silicon on-chip spectroscopy system |
| CN102520041A (en) * | 2011-11-30 | 2012-06-27 | 昆明理工大学 | Method for preparing amino functional multiporous silica-based composite material for ion detection |
-
2013
- 2013-07-11 CN CN2013102895577A patent/CN103344596A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070153266A1 (en) * | 2005-12-30 | 2007-07-05 | Tae-Woong Koo | Porous silicon on-chip spectroscopy system |
| CN102520041A (en) * | 2011-11-30 | 2012-06-27 | 昆明理工大学 | Method for preparing amino functional multiporous silica-based composite material for ion detection |
Non-Patent Citations (3)
| Title |
|---|
| BING XIA 等: "Fluorescence quenching in luminescent porous silicon nanoparticles for the detection of intracellular Cu2+", 《ANALYST》, vol. 138, 17 April 2013 (2013-04-17) * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947290A (en) * | 2017-03-31 | 2017-07-14 | 合肥悦兰信息技术有限公司 | The preparation method of colored silicon-dioxide powdery material |
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