CN101324531B - Nanometer gold resonance scattering spectrometry for simply and rapidly measuring trace amount Titanium - Google Patents
Nanometer gold resonance scattering spectrometry for simply and rapidly measuring trace amount Titanium Download PDFInfo
- Publication number
- CN101324531B CN101324531B CN2008100736664A CN200810073666A CN101324531B CN 101324531 B CN101324531 B CN 101324531B CN 2008100736664 A CN2008100736664 A CN 2008100736664A CN 200810073666 A CN200810073666 A CN 200810073666A CN 101324531 B CN101324531 B CN 101324531B
- Authority
- CN
- China
- Prior art keywords
- solution
- titanium
- resonance scattering
- irs
- concentration
- 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.)
- Expired - Fee Related
Links
Images
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a nano-Au resonance scattering spectrographic method for conveniently and rapidly detecting trace titanium, which is characterized in that the method comprises the following steps: (1) preparing a measuring system with the known titanium concentration, and measuring the resonance scattering intensity (IRS) thereof; (2) preparing a reagent blank system, and measuring the resonance scattering light intensity (IRS)0 without adding the Ti(SO4)2 solution as the blank,; (3) calculating based on that Delta IRS is equal to IRS minus (IRS)0; (4) plotting a work curve with the concentration of the added Ti(SO4)2 solution as the abscissa and the Delta IRS as the ordinate; (5) preparing a detecting system, measuring the titanium content in the industrial wastewater and obtaining Delta IRS of the sample to be measured; and (6) obtaining the titanium concentration of the sample to be measured according to the work curve. The method has the advantages of simple device, convenient operation, easily-accessible reagent and low cost, and can be carried out by only a fluorescence spectrophotometer.
Description
Technical field:
The present invention relates to the assay method of trace amount Ti, specifically is the nanometer gold resonance scattering spectrometry of easy fast measuring trace amount Ti.
Background technology:
Titanium is a kind of common element, extensively is present in various rocks, seawater and the biosome.Titanium has stimulating plant growth, the function of enhance immunity ability in vivo; It is called as one's own thing metal in medical treatment, can be used as the artifical bone and treats fracture; In addition, titanium still is desirable superconductor, plays crucial effect in the development of the national economy, development in Hi-Tech.At present, the method for measuring trace amount Ti both at home and abroad mainly contains: spectrophotometric method, complexometry, high performance liquid chromatography, atomic emission spectrometry, atomic absorption spectrography (AAS), plasma emission spectrometry, plasma mass spectroscopy, Flow Injection Analysis method and electrochemical method.But the complex steps that the sensitivity that costs an arm and a leg, has that these methods have accuracy not high, that have is not good enough, have is not suitable for conventional analysis.In recent years, the resonance scattering technology has been widely used in trace-metal and the biochemical analysis as high-sensitive analysis and testing technology. and gold nano particulate occupies critical role because it exists surface plasma resonance (SPR) or resonance scattering (RS) effect in surface plasma resonance sensor and Analysis on Resonance and Scattering Light Spectrum.Nm of gold is marked immune response combine, set up and have higher sensitivity and Analysis on Resonance and Scattering Light Spectrum method optionally preferably with resonance scattering spectroscopy; So far, Shang Weijian combines the report of measuring titanium with complex compound reaction and nm of gold aggreation with the resonance scattering spectroscopy technology.
Summary of the invention:
The objective of the invention is to disclose a kind of high sensitivity, measure the nanometer gold resonance scattering spectrometry of trace amount Ti simply and rapidly.
Assay method of the present invention comprises the steps:
1, the detection architecture of preparation known titanium concentration, and measure its resonance scattering intensity:
(1) in the 5mL color comparison tube, adds a certain amount of Ti (SO successively
4)
2Solution, 140 μ L 9.8mg/mL H
2SO
4Solution, 60 μ L 2.16 * 10
-2The H of mol/L
2O
2Solution and 0.5mL 57.96 μ g/mL nm of gold are settled to 3mL with redistilled water, shake up, and leave standstill 30min;
(2) get an amount of reacted solution in quartz cell, put on the fluorospectrophotometer, the synchronous scanning excitation wavelength lambda
ExAnd emission wavelength lambda
Em(λ
Ex=λ
Em), exciting and launch slit to be 5.0nm, mensuration voltage is 400V, obtains the resonance scattering spectroscopy of system, the scattering strength of measuring the 760nm place is I
RS
2, the method with step 1 prepares the reagent blank system; Do not add Ti (SO
4)
2Solution is done blank, surveys its resonance scattering light intensity (I
RS)
0
3, calculate Δ I
RS=I
RS-(I
RS)
0
4, the Ti (SO to add
4)
2The concentration of solution is horizontal ordinate, with Δ I
RSBe ordinate, the drawing curve;
5, the method with step 1 prepares detection architecture, and the sample of the titaniferous of the unknown concentration of adding is tried to achieve Δ I
RS
6,, try to achieve the concentration of measured object titanium according to working curve.
Do not adding Ti (SO
4)
2Before the solution, collaurum-H
2O
2The synchronous scattered signal of system is weak (Fig. 3 a), as Ti (SO
4)
2When existing, the synchronous scattering of system strengthens.Along with Ti (SO
4)
2The increase of concentration, resonance scattering intensity is linear to strengthen Ti (SO
4)
2Concentration is linear with the resonance scattering light intensity added value of 760nm wavelength in 0.067～533.6 μ g/mL scope, and its regression equation is Δ I
RS=0.16c+8.67 related coefficient 0.99, detection limit 0.04 μ g/mL.
Principle of the present invention
The principle of this reaction is: Ti
4+Because the radius of institute electrically charged height and ion is less, so has stronger polarizability, under acid condition with TiO
2+Exist, can with H
2O
2Can form yellow [TiO (H
2O
2)
2+] complex compound.Experimental result shows dilute sulfuric acid, H
2O
2Nm of gold is assembled.In the dilute sulfuric acid medium, as trace Ti O
2+Exist and and H
2O
2Can make orange-red nm of gold assemble the golden aggregation (Fig. 1) that the formation mean grain size is about 900nm after generating complex compound, cause linear the increasing of resonance scattering intensity at 760nm place.Its principle such as Fig. 2.
Advantage of the present invention:
(1) equipment is simple, easy to operate, only needs fluorospectrophotometer to finish;
(2) reagent is easy to get, and is with low cost.
Description of drawings:
Fig. 1 is Ti (SO
4)
2-H
2O
2The resonance scattering spectroscopy of-Au system;
A.0.432mmol/mL H among the figure
2O
2--457mg/L H
2SO
4-9.66 μ g/mL Au are μ g/mlTi (SO b.0.067
4)
2--457mg/L H
2SO
4-0.432mmol/L H
2O
2-9.66 μ g/mL Au are μ g/mlTi (SO c.266.8
4)
2--457mg/L H
2SO
4-0.432mmol/L H
2O
2-9.66 μ g/mL Au are μ g/mlTi (SO d.533.6
4)
2--457mg/L H
2SO
4-0.432mmol/L H
2O
2-9.66 μ g/mL Au;
Fig. 2 is reaction principle figure of the present invention.
Embodiment:
Detect the content of titanium in 3 parts of industrial waste waters with method of the present invention.
Cary eclipse type fluorospectrophotometer (U.S. VARIAN excites slit and emission slit all to select 5nm, and the PMT detector voltage is selected 400V), Nano-ZS90 type nano particle size and zeta potentiometric analyzer (Britain Malvern company).
9.8mg/mL H
2SO
4Solution; 2.16 * 10
-2Mol/L H
2O
2Solution, concentration is demarcated with permanganimetric method; 1.0%HAuCl
41.0% trisodium citrate; Agents useful for same is analyzes pure level, and experimental water is a redistilled water.
1. nm of gold adopts the preparation of sodium citrate reducing process: inferior boiling water 100.0mL is placed in the clean conical flask boil, under agitation add 1.00% gold chloride 1mL, add 1.00% sodium citrate aqueous solution 4.0mL rapidly, continuing to boil 15min takes off, under no heating condition, stir 15min, cooling is settled to 100.0mL, and sterile sealing is preserved.This collaurum concentration is 57.96 μ g/mL (calculating with Au), and its particle diameter is about 10nm;
2. in the 5mL color comparison tube, add 40.0 μ L industrial waste waters successively, 140 μ L 9.8mg/mL H
2SO
4Solution, 60 μ L2.16 * 10
-2The H of mol/L
2O
2Solution and 0.5mL 57.96 μ g/mL collaurums. be settled to 3mL with redistilled water, shake up, leave standstill 30min;
3. get an amount of reacted solution in quartz cell, put on the fluorospectrophotometer, the synchronous scanning excitation wavelength lambda
ExAnd emission wavelength lambda
Em(λ
Ex=λ
Em), exciting and launch slit to be 5.0nm, mensuration voltage is 400V, obtains the resonance scattering spectroscopy of system, the scattering strength of measuring the 760nm place is I
RS
4. processing industry waste water is not made blank, surveys its resonance scattering light intensity (I
RS)
0
5. calculate Δ I
RS=I
RS-(I
RS)
0
6. the content of titanium in the calculating industrial waste water.
By the content of titanium elements in the above determination of experimental method water, and use the titanium spectrphotometric method for measuring simultaneously, compare result such as table 1.Two methods are unanimity as a result, and relative standard deviation is between 0.10-0.44%.
Table 1 sample analysis result
Table1?Results?for?the?Determination?of?H
2O
2?in?Serum?Samples
Claims (2)
1. nanometer gold resonance scattering spectrometry of measuring trace amount Ti, it is characterized in that: assay method comprises the steps:
1) detection architecture of preparation known titanium concentration, and measure its resonance scattering intensity:
(1) in the 5mL color comparison tube, adds a certain amount of Ti (SO successively
4)
2Solution, 140 μ L 9.8mg/mL H
2SO
4Solution, 60 μ L 2.16 * 10
-2The H of mol/L
2O
2Solution and 0.5mL 57.96 μ g/mL nm of gold are settled to 3mL with redistilled water, shake up, and leave standstill 30min;
(2) get an amount of reacted solution in quartz cell, put on the fluorospectrophotometer, synchronous scanning excitation wavelength lambda ex and emission wavelength lambda em, and make λ ex=λ em, excite and launch slit and be 5.0nm, mensuration voltage is 400V, obtains the resonance scattering spectroscopy of system, and the scattering strength of measuring the 760nm place is I
RS
2) method with step 1) prepares the reagent blank system: do not add Ti (SO
4)
2Solution is done blank, surveys its resonance scattering light intensity (I
RS)
0
3) calculate Δ I
RS=I
RS-(I
RS)
0
4) Ti (SO to add
4)
2The concentration of solution is horizontal ordinate, with Δ I
RSBe ordinate, the drawing curve;
5) method with step 1) prepares detection architecture, measures the content of titanium in the industrial waste water, tries to achieve the Δ I of sample
RS
6), try to achieve the concentration of titanium in the sample according to working curve.
2. the method for claim 1, it is characterized in that: titanium is linear with the resonance scattering light intensity added value of 760nm wavelength in 0.067-533.6 μ g/mL scope, and its regression equation is Δ I
RS=0.16c+8.67, related coefficient 0.99, detection limit 0.04 μ g/mL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100736664A CN101324531B (en) | 2008-07-03 | 2008-07-03 | Nanometer gold resonance scattering spectrometry for simply and rapidly measuring trace amount Titanium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100736664A CN101324531B (en) | 2008-07-03 | 2008-07-03 | Nanometer gold resonance scattering spectrometry for simply and rapidly measuring trace amount Titanium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101324531A CN101324531A (en) | 2008-12-17 |
| CN101324531B true CN101324531B (en) | 2010-09-15 |
Family
ID=40188156
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100736664A Expired - Fee Related CN101324531B (en) | 2008-07-03 | 2008-07-03 | Nanometer gold resonance scattering spectrometry for simply and rapidly measuring trace amount Titanium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101324531B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101532957B (en) * | 2009-04-17 | 2011-04-13 | 广西师范大学 | Catalyst resonance scattering spectrophotometric method capable of measuring ultra-trace rhenium |
| CN105891073A (en) * | 2016-04-05 | 2016-08-24 | 西安西热电站化学科技有限公司 | Online detection device and method for iron content in thermodynamic system start washing water |
| CN109884010A (en) * | 2019-02-27 | 2019-06-14 | 黑龙江大学 | A kind of preparation method of high specific surface area porous carbonitride and method using its fluorescence detection TNP |
-
2008
- 2008-07-03 CN CN2008100736664A patent/CN101324531B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101324531A (en) | 2008-12-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104458704B (en) | The method that SERS substrates based on DNA modification detect Low Concentration Mercury ion | |
| Erbao et al. | Flow injection determination of adenine at trace level based on luminol–K2Cr2O7 chemiluminescence in a micellar medium | |
| CN109696430B (en) | Method for measuring concentration of microcystin | |
| Chen et al. | A dual-mode fluorometric/colorimetric sensor for Cu 2+ detection based on hybridized carbon dots and gold–silver core–shell nanoparticles | |
| Gao et al. | Selective “turn-on” fluorescent sensing for biothiols based on fluorescence resonance energy transfer between acridine orange and gold nanoparticles | |
| Chen et al. | Quantitative evaluation of proteins with bicinchoninic acid (BCA): Resonance Raman and surface-enhanced resonance Raman scattering-based methods | |
| Gore et al. | A novel FRET probe for selective and sensitive determination of vitamin B 12 by functionalized CdS QDs in aqueous media: applications to pharmaceutical and biomedical analysis | |
| CN104345053B (en) | Gold nanoparticle biological sensor for detecting serum creatinine and preparation method of gold nanoparticles biological sensor | |
| CN105842225A (en) | Silicon-based SERS chip for quantitatively detecting lead ion concentration in actual water sample and preparation method thereof | |
| CN103604792A (en) | Resonance Rayleigh scattering (RRS) method for measuring bromide ion | |
| CN110987843A (en) | Phosphate radical colorimetric detection method based on bimetallic MOF nano-oxidase | |
| CN105319192A (en) | Method for detecting hypochlorite anions through water-soluble fluorescent silica nanoparticle | |
| CN101324531B (en) | Nanometer gold resonance scattering spectrometry for simply and rapidly measuring trace amount Titanium | |
| Gao et al. | Reliable SERS detection of nitrite based on pH and laser irradiance-dependent diazotization through a convenient sampling micro-chamber | |
| CN102661943B (en) | Method for measuring cystine through surface-enhanced raman spectroscopy | |
| Xiao et al. | Highly sensitive determination of trace potassium ion in serum using the resonance light scattering technique with sodium tetraphenylboron | |
| CN112499614A (en) | Malic acid-arginine functionalized carbon quantum dot and preparation method and application thereof | |
| CN102879350B (en) | Quick measuring method for copper ions by heat-treated bare nano-gold as developing probe | |
| CN109632736B (en) | Preparation method of fluorescence sensor for detecting aristolochic acid A | |
| CN103901033A (en) | Method for detecting lead ion concentration in sample | |
| CN115074123B (en) | Boron-nitrogen-sulfur doped carbon quantum dot, preparation method thereof, method for detecting minimum concentration detectable by Ag+ and method for detecting pH | |
| CN108827921B (en) | Room-temperature phosphorescence detection method for lysozyme and application | |
| CN104165852A (en) | Resonance Rayleigh scattering energy transfer spectroscopy method for determining fluorinion simply and rapidly | |
| Lei et al. | Nano-fluorescent probes based on DNA-templated copper nanoclusters for fast sensing of thiocyanate | |
| Amjadi et al. | Gold nanoparticles-based resonance light scattering method for the determination of phenothiazine drugs |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100915 Termination date: 20110703 |