CN107543811A - A kind of fluorescence analysis of boron and its application - Google Patents
A kind of fluorescence analysis of boron and its application Download PDFInfo
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- CN107543811A CN107543811A CN201710850850.4A CN201710850850A CN107543811A CN 107543811 A CN107543811 A CN 107543811A CN 201710850850 A CN201710850850 A CN 201710850850A CN 107543811 A CN107543811 A CN 107543811A
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Abstract
The present invention relates to a kind of fluorescence analysis of boron, this method reacts to form stable yellow fluorescence complex based on boron and alizarin red, beta cyclodextrin is used as sensitizer, it is highly sensitive and determine trace B with high selectivity with fluorescence method, for boron concentration in the range of 0.05 1.0mg/L, the relative intensity of fluorescence of system is directly proportional to boron concentration.
Description
Technical field
The present invention relates to a kind of fluorescence spectrometry method of boron, belong to the technical field of analysis and detection of analytical chemistry field.
Background technology
In nature, boron mainly exists in the form of boric acid, borate and its three kinds of complex compound etc. being formed with sodium, magnesium, calcium.
Contain a certain amount of boron in soil, rock, water and air, wherein Boron In Seawater content is higher, and mean concentration reaches 4.6mg/L.
The purposes of boron is quite varied, and industrial boron widely uses in industries such as metallurgy, glass, ceramics, pharmaceutically available for anti-corrosive antibacterial,
It can be additionally used in the production of cosmetics, agricultural chemicals and agricultural fertilizer, in addition, boron is also trace element necessary to animal and plant growth.Mesh
Before, the analyzing detecting method of boron can mainly be summarized as AAS, electrochemical process and atomic spectroscopy etc..
In existing analysis method, AAS is the conventional method of analysis of boron measure, typically uses curcumin and first
Imines AAS.Curcumin photometry is time-consuming more, dosage of the evaporating temperature of experiment, speed and reagent etc. all can to point
Analyse result and produce considerable influence, the precision of analysis result is poor.Azomethine photometry operation it is relatively simple, but its sensitivity and
Accuracy is below curcumin colorimetric method, it is difficult to excludes organic interference, is unsuitable for low content Boron nitrogen rings.Fluorimetry is surveyed
It is most based in concentrated acid medium or organic media to determine boron, is made troubles to measure.Atomic absorption method is typically adopted by complex reaction
It is cumbersome with indirect Determination boron, operation.The weak point of ICP-AES methods is the spectral line of emission and iron spectral line close proximity of boron,
Interference by iron is big, and the analysis for trace, ultra trace boron, its sensitivity and detection limit do not reach requirement.
The purpose of the present invention is that such as time-consuming for experiment, cumbersome, sensitive for weak point present in existing method
Degree is not high, and selectivity is undesirable etc., it is proposed that a kind of new method that detection Boron contents are analyzed using XRF.The method utilizes
Alizarin red and boron react to form stable yellow fluorescence complex, use beta-schardinger dextrin as sensitizer, with fluorescence method it is highly sensitive with
Analysis measure trace B with high selectivity.
The content of the invention
According to the first aspect of the invention, the invention provides a kind of method of alizarin red Fluorometric assay boron, including
Following steps：
(1) prepared by need testing solution：A certain amount of boron test solution is pipetted, sequentially adds Alizarin Red Aqueous Solution, Tris-HCl delays
Solution, EDTA solution and beta-schardinger dextrin solution are rushed, scale is diluted with water to, shakes up, stands, it is fully reacted, is produced for examination
Product solution；
(2) preparation of Reagent blank solutions：Take Alizarin Red Aqueous Solution, Tris-HCl cushioning liquid, EDTA solution and β-ring
Dextrin solution, scale is diluted with water to, shaken up, stood, it is fully reacted, produce Reagent blank solutions；
(3) determine：Need testing solution obtained by step (1) is taken, Reagent blank solutions obtained by step (2), is respectively placed in colorimetric
In ware, the fluorescence intensity I values of need testing solution, Reagent blank solutions are determined at excitation wavelength 450nm, launch wavelength 602nm
Fluorescence intensity I0Value；The relative intensity of fluorescence of boron measurement is defined as △ I, wherein △ I=I-I in need testing solution0。
Alizarin red concentration of the present invention is 4.0 × 10-4-6.0×10-4Mol/L, it is preferable that concentration selection for 5.0 ×
10-4mol/L.Beta-schardinger dextrin concentration is 5.0 × 10-4-2.0×10-3mol/L.Preferably, concentration selection is 1.0 × 10-3mol/
L。
EDTA plays masking action, adds 0.3-0.8mL depending on disturbed condition size in sample, it is preferable that select as 0.5mL.
The concentration of Alizarin Red Aqueous Solution used in the step of fluorescence analysis of boron of the present invention (1) and (2)
For 5.0 × 10-4Mol/L, dosage are 1mL, and the concentration of beta-schardinger dextrin is 1.0 × 10-3Mol/L dosages are 0.5mL, Tris-
HCl cushioning liquid dosages are that the concentration of 2mL, EDTA solution is that 0.1mol/L dosages are 0.5mL.
The pH of Tris-HCl cushioning liquid used in the step of fluorescence analysis of boron of the present invention (1) and (2)
It is worth for 6.8-8.0, preferably 7.5.
The concentration of boron test solution described in the step of fluorescence analysis of boron of the present invention (1) is 0.05-1.0mg/
L。
The reaction time fully reacted in the step of fluorescence analysis of boron of the present invention (1) is 10min.
A kind of Boron nitrogen rings method in soil, the assay method are carried out using the fluorescence analysis of boron of the present invention
Measure.
A kind of Boron nitrogen rings method in water, the assay method are surveyed using the fluorescence analysis of boron of the present invention
It is fixed.
A kind of Boron nitrogen rings method in fertilizer, the assay method are carried out using the fluorescence analysis of boron of the present invention
Measure.
Agents useful for same of the present invention is that analysis is pure, and water is redistilled water.
Boron concentration of the present invention is in the range of 0.05-1.0mg/L, and the relative intensity of fluorescence △ I of system and the concentration of boron are into just
Than.Equation of linear regression is △ I=127.1C+236.6, and C is the concentration (mg/L) of boron (III) in formula, according to linear regression side
Journey can calculate the concentration of the boron corresponding to any fluorescence intensity.
According to another aspect of the present invention, the method for alizarin red Fluorometric assay boron of the present invention can be used for detection boron to contain
Amount.
The specific detection method of Boron contents comprises the following steps：
1) drawing curve
If taking Heavenly Stems and Earthly Branches 10mL colorimetric cylinders, it is according to what the method for above-mentioned alizarin red Fluorometric assay boron prepared various concentrations
Row boron standard liquid, the relative intensity of fluorescence △ I of system are determined, mapped with concentration with corresponding relative intensity of fluorescence △ I, drawn
Working curve obtains equation of linear regression；The boron concentration of standard solution scope is 0.05-1.0mg/L；
2) in determination sample boron concentration
Boron sample solution is added into colorimetric cylinder, its relative intensity of fluorescence is determined, boron in sample is determined according to working curve
Content；Or the content of boron in sample is calculated according to equation of linear regression.
The detection method can exclude the interference of Common Cations and anion, and detection limit can reach 10.2 μ g/L；Institute
Stating Common Cations and anion includes Na+(1000),K+(1000),Ca2+(500),Mg2+(500),Mn2+(500),Zn2+
(500),Co2+(500),Pb2+(500),Cu2+(300),Fe3+(50),Al3+(50),NO3 -(1000),PO4 3-(1000),SO4 2-
(1000),SiO3 2-(1000),C2O4 2-(1000),Cl-(1000),Br-(1000),F-(1000),CH3COO-(1000),I-
(500),CO3 2-(500).Data in bracket are the ratio between the mass concentration of interfering ion and boron (CB=0.2mg/L)；Disturbing
In the presence of material, compared with being not added with interfering material, it is that standard determines whether to do to be no more than ± 5% with system fluorescence intensity change
Disturb.
The beneficial effects of the invention are as follows：
(1) the fluorescence method high sensitivity that this method uses, alizarin red form stable complex compound with boron, pass through sensitizer pair
The sensitization of complex compound fluorescence, realize the fluoroscopic examination to boron.
(2) weak point of current photometric method measurement boron is overcome, such as operation requires strict, and required time is longer, sensitive
Degree is not high.
(3) this law agents useful for same is cheap and easy to get, and easy, quick and sensitive detection can be achieved, and analysis detection range is wide.
Brief description of the drawings
Fig. 1：For fluorescence excitation spectrum, in figure：A is boron standard liquid；B is boron standard liquid+alizarin red aqueous solution；C is boron
Standard liquid+alizarin red aqueous solution+beta-schardinger dextrin.
Fig. 2：For fluorescence emission spectrum, in figure：A is boron standard liquid；B is boron standard liquid+alizarin red aqueous solution；C is boron
Standard liquid+alizarin red aqueous solution+beta-schardinger dextrin.
Embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, with reference to embodiment, to this
Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
The measure of the Effective Boron of Soil of embodiment 1
The air-dried soil sample 15.0g of 20 mesh sieves was weighed in 250mL quartz triangular flasks, 30mL water is added, installs returned cold
Condenser, it is boiled by slow fire and keeps micro-boiling 5min (accurate timing), remove thermal source, continues reflux condensation mode 5 minutes (accurate timing), take
Lower triangular flask, 4 drop 0.5mol/L CaCl is added after cooling2Solution, 50mL plastics are filled into quantitative filter paper after solution clarification
Standby in bottle, this liquid is used to determine effective boron.
During measure, the above-mentioned testing sample solutions of 4mL are taken to sequentially add 1mL Alizarin Red Aqueous Solutions in 10mL colorimetric cylinder
(5.0×10-3Mol/L), 2mL Tris-HCl cushioning liquid, 0.5mL EDTA solution (0.1mol/L) and 0.5mL beta-schardinger dextrins
Solution (2.0 × 10-2Mol/L), scale is diluted with water to, is shaken up, 1cm cuvettes are used after standing 10min, in excitation wavelength
The relative intensity of fluorescence △ I of measure system at 450nm, launch wavelength 602nm, containing for boron in sample is determined according to working curve
Amount.
This law is used with step as stated above to Soil Boron standard substance GBW07412 (0.52 ± 0.14mg/ of standard value
Kg) it is measured with GBW07414 (0.34 ± 0.17mg/kg of standard value), the average value Boron contents of 3 measurement results are respectively
0.53mg/kg and 0.33mg/kg, show that the analysis result of this law is more accurate.
Embodiment 2：Boron nitrogen rings in water
Boron nitrogen rings are carried out to the actual water sample of two kinds of different matrix of river and lake water using standard addition method respectively.Measure
When, water sample 5.0mL is drawn in 10mL colorimetric cylinders, is separately added into different amounts of boron standard liquid, the quality of added boron is respectively
1.0 μ g, 3.0 μ g, 5.0 μ g, the concentration of boron in water after mark-on is set to be located at the basic, normal, high concentration range of standard curve respectively.Mark-on
Afterwards, 1mL Alizarin Red Aqueous Solutions (5.0 × 10 are sequentially added-3Mol/L), 2mL Tris-HCl cushioning liquid, 0.5mL EDTA are molten
Liquid (0.1mol/L) and 0.5mL beta-schardinger dextrins solution (2.0 × 10-2Mol/L), scale is diluted with water to, is shaken up, stands 10min
1cm cuvettes are used afterwards, the relative intensity of fluorescence △ I of measure system at excitation wavelength 450nm, launch wavelength 602nm, according to work
The content of boron in sample is determined as curve.The recovery of standard addition of measurement result river is 98.2-102.5%, and the mark-on of lake water returns
Yield is 97.8-102.8%, is as a result satisfied with.
Embodiment 3：Boron nitrogen rings in complex fertilizer
Using the content of boron in Standard Addition Method for Determination fertilizer.During measure, weigh fertilizer sample (according to Boron contents height)
5-10g, 0.0001g is accurate to, be placed in 250mL polytetrafluoroethylene beakers, added deionized water 150mL, cap upper surface ware, boil
15min, remove, be cooled to room temperature, be transferred in 250mL volumetric flasks, scale is diluted to deionized water, mix, do filtering.Abandon
Retain residual filtrate after going primary filtrate, the sample solution as measure boron.
Mark-on sample is prepared by above-mentioned identical method and steps, is separately added into different amounts of boron standard (5.0 μ during preparation
G/g, 10.0 μ g/g, 20.0 μ g/g), make mark-on handle after in test solution boron concentration respectively positioned at the basic, normal, high dense of standard curve
Spend scope.
During measure, test solution 4.0mL is pipetted in 10mL colorimetric cylinders, sequentially adds 1mL Alizarin Red Aqueous Solutions (5.0 × 10- 3Mol/L), 2mL Tris-HCl cushioning liquid, 0.5mL EDTA solution (0.1mol/L) and 0.5mL beta-schardinger dextrins solution (2.0
×10-2Mol/L), scale is diluted with water to, is shaken up, 1cm cuvettes are used after standing 10min, in excitation wavelength 450nm, transmitted wave
The relative intensity of fluorescence △ I of measure system at long 602nm, determine that the content of boron in sample is 4.67 μ g/g according to working curve,
Recovery of standard addition is 98.2-102.5%.
Claims (10)
1. a kind of fluorescence analysis of boron, it is characterised in that this method comprises the following steps：
(1) prepared by need testing solution：A certain amount of boron test solution is pipetted, it is molten to sequentially add Alizarin Red Aqueous Solution, Tris-HCl bufferings
Liquid, EDTA solution and beta-schardinger dextrin solution, are diluted with water to scale, shake up, and stand, it is fully reacted, it is molten to produce test sample
Liquid；
(2) preparation of Reagent blank solutions：Take Alizarin Red Aqueous Solution, Tris-HCl cushioning liquid, EDTA solution and beta-schardinger dextrin
Solution, scale is diluted with water to, shaken up, stood, it is fully reacted, produce Reagent blank solutions；
(3) determine：Need testing solution obtained by step (1) is taken, Reagent blank solutions obtained by step (2), is respectively placed in cuvette,
The fluorescence intensity I values of need testing solution, the fluorescence of Reagent blank solutions are determined at excitation wavelength 450nm, launch wavelength 602nm
Intensity I0Value；The relative intensity of fluorescence of boron measurement is defined as △ I, wherein △ I=I-I in need testing solution0。
2. the fluorescence analysis of boron according to claim 1, it is characterised in that in the step (1) and (2) described in this method
The concentration of Alizarin Red Aqueous Solution used is 4.0 × 10-4-6.0×10-4Mol/L, dosage are 1mL, the concentration of beta-schardinger dextrin
For 5.0 × 10-4-2.0×10-3Mol/L dosages are 0.5mL, and Tris-HCl cushioning liquid dosage is 2mL, the concentration of EDTA solution
It is 0.3-0.8mL for 0.1mol/L dosages.
3. the fluorescence analysis of boron according to claim 2, it is characterised in that in the step (1) and (2) described in this method
The concentration of Alizarin Red Aqueous Solution used is 5.0 × 10-4Mol/L, dosage are 1mL, and the concentration of beta-schardinger dextrin is 1.0 × 10- 3Mol/L dosages are 0.5mL, and Tris-HCl cushioning liquid dosages are that the concentration of 2mL, EDTA solution is that 0.1mol/L dosages are
0.5mL。
4. the fluorescence analysis of boron according to claim 3, it is characterised in that the pH value of the Tris-HCl cushioning liquid
For 6.8-8.0.
5. the fluorescence analysis of boron according to claim 4, it is characterised in that the pH value of the Tris-HCl cushioning liquid
For 7.5.
6. the fluorescence analysis of boron according to claim 5, it is characterised in that boron test solution described in the step (1)
Concentration is 0.05-1.0mg/L.
7. according to the fluorescence analysis of any one of the claim 1-6 boron, it is characterised in that in the step (1) fully
The reaction time of reaction is 10min.
8. a kind of Boron nitrogen rings method in soil, it is characterised in that the assay method is using described in claim any one of 1-7
The fluorescence analysis of boron is measured.
9. a kind of Boron nitrogen rings method in water, it is characterised in that the assay method is used as described in claim any one of 1-7
The fluorescence analysis of boron is measured.
10. a kind of Boron nitrogen rings method in fertilizer, it is characterised in that the assay method is using described in claim any one of 1-7
The fluorescence analysis of boron be measured.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104007111A (en) * | 2014-06-18 | 2014-08-27 | 南京麦思德餐饮管理有限公司 | Kit for detecting sodium borate in food |
| CN104020166A (en) * | 2014-06-18 | 2014-09-03 | 南京麦思德餐饮管理有限公司 | Simple qualitative detection method of borax in food |
| CN105675571A (en) * | 2016-03-07 | 2016-06-15 | 北京化工大学 | Tiopronin concentration determination fluorescence sensor and preparation method thereof |
| CN107084950A (en) * | 2017-04-05 | 2017-08-22 | 河南师范大学 | The method of beta cyclodextrin enhanced sensitivity methylene blue fluorescence spectrometry antibiotics content |
-
2017
- 2017-09-20 CN CN201710850850.4A patent/CN107543811A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104007111A (en) * | 2014-06-18 | 2014-08-27 | 南京麦思德餐饮管理有限公司 | Kit for detecting sodium borate in food |
| CN104020166A (en) * | 2014-06-18 | 2014-09-03 | 南京麦思德餐饮管理有限公司 | Simple qualitative detection method of borax in food |
| CN105675571A (en) * | 2016-03-07 | 2016-06-15 | 北京化工大学 | Tiopronin concentration determination fluorescence sensor and preparation method thereof |
| CN107084950A (en) * | 2017-04-05 | 2017-08-22 | 河南师范大学 | The method of beta cyclodextrin enhanced sensitivity methylene blue fluorescence spectrometry antibiotics content |
Non-Patent Citations (3)
| Title |
|---|
| ANA M. GARCIA CAMPANA ET AL.: "Spectrofluorimetric Determination of Boron in Soils, Plants and Natural Waters With Alizarin Red S", 《ANALYST》 * |
| 张敏 等: "β-环糊精及其衍生物的荧光增敏作用研究进展", 《食品科学》 * |
| 张晓林: "茜素红S荧光光度法测定土壤、植物和天然水中的硼", 《国外医学（卫生学分册）》 * |
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Application publication date: 20180105 |