CN111948165B - Method for detecting hypochlorite ions of construction material based on optical probe - Google Patents
Method for detecting hypochlorite ions of construction material based on optical probe Download PDFInfo
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- CN111948165B CN111948165B CN202010609783.9A CN202010609783A CN111948165B CN 111948165 B CN111948165 B CN 111948165B CN 202010609783 A CN202010609783 A CN 202010609783A CN 111948165 B CN111948165 B CN 111948165B
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- 239000000523 sample Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 11
- 230000003287 optical effect Effects 0.000 title claims abstract description 9
- 239000004035 construction material Substances 0.000 title claims abstract description 8
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Inorganic materials Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 title claims abstract description 5
- -1 hypochlorite ions Chemical class 0.000 title claims abstract description 5
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000000295 emission spectrum Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000001514 detection method Methods 0.000 claims description 19
- 238000002189 fluorescence spectrum Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 230000031700 light absorption Effects 0.000 claims 2
- 239000007850 fluorescent dye Substances 0.000 claims 1
- 238000010276 construction Methods 0.000 abstract description 13
- 239000002994 raw material Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 238000004448 titration Methods 0.000 abstract description 4
- 238000009435 building construction Methods 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000006399 behavior Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910020366 ClO 4 Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Optics & Photonics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a method for detecting hypochlorite ions of construction materials based on an optical probe, which comprises the steps of firstly preparing a standard curve, dissolving corresponding probe solution in water, and adding ClO with different concentrations ‑ I.e. the titration experiment gives a standard curve. And adding the liquid to be detected into the probe solution, and measuring the absorption spectrum and the emission spectrum of the liquid to be detected. Corresponding to standard curve, knowing ClO ‑ Concentration. The optical probe is adopted to detect the building construction raw materials before construction, so that the method has the advantages of accuracy, timeliness, simplicity in operation, low material consumption and the like; the performance of raw materials can be mastered in time at a construction site, the construction is scientifically and normally performed, the construction is safe, and the construction speed is improved; and on the premise of ensuring that the quality standard required by the test is met, better economic benefit and social benefit are obtained.
Description
Technical Field
The invention relates to a detection method for detecting construction materials based on an optical probe, in particular to a method for detecting hypochlorite ions in construction materials based on an optical probe, and belongs to the technical field of chemical detection.
Background
With the rapid development of economic construction, engineering test level is improved continuously, but many detection methods of raw material mechanical and chemical performance indexes are still not stable and mature enough, and especially many detection and determination of chemical performance indexes are realized by means of various traditional analysis and detection methods, so that expensive instruments and equipment are required, sufficient detection time is required, and experienced human resources are also required. The pressure of space, time and instrument cost, the inaccuracy and timeliness of raw material chemical property index detection can all lead to the increase of detection cost, influence the construction progress, shorten the service life of target building, reduce the economic benefits of enterprises. Therefore, in construction production of bridges, underground engineering, constructional engineering and the like, simple and rapid detection and control of chemical performance indexes of raw materials are important.
At present, chemical index detection of building construction raw materials is carried out to obtain ion ClO which is harmful to concrete materials - Mainly. Common methods for material detection are: conventional chemical titration methods, atomic absorption spectrometry, atomic emission spectrometry, spectrophotometry, and the like, wherein detection means for construction materials are widely used in the conventional titration methods, but each method has technical shortcomings.
Disclosure of Invention
The invention adopts the optical probe to detect the building construction raw materials before construction, and has the advantages of accuracy, timeliness, simple operation, low material consumption and the like; the performance of raw materials can be mastered in time at a construction site, the construction is scientifically and normally performed, the construction is safe, and the construction speed is improved; and on the premise of ensuring that the quality standard required by the test is met, better economic benefit and social benefit can be obtained.
The technical scheme adopted by the invention is that the method for detecting the construction material based on the optical probe is characterized by weighing C1.9 mg and dissolving in 2mL of DMF to prepare the material with the concentration of 5.0X10 -3 The mol/L probe solution is ready for use. Firstly, making a standard curve, dissolving 6 mu L of probe solution in 3mL of water, wherein the concentration of probe molecules in the probe solution is 1.0X10 -5 mol/L, add ClO with different concentration - I.e. the titration experiment gives a standard curve. In detection, 3mL of the liquid to be detected is taken, 6 mu L of probe solution is added, and the absorption spectrum and the emission spectrum of the liquid to be detected are measured, and the liquid to be detected contains ClO with different concentrations - The absorption spectrum at 814nm is significantly reduced; the fluorescence intensity at 834nm of the emission spectrum is significantly reduced. Corresponding to standard curve, knowing ClO - Concentration.
Drawings
FIG. 1 shows the probe molecule C1 without ClO added - (≡) and ClO addition - (■) pH dependence.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples.
The synthesis of probe molecule C1 is as follows:
the ultraviolet-visible spectrum is adopted to study the absorption spectrum behaviors of the probe molecule C1 and various common ion identification. At a concentration of 2.0X10 -5 In the mol/L solution system, the absorption spectrum of the probe molecule C1 shows a characteristic absorption peak at 814nm, when 5 times of other ions (Ac) - ,BF 4 - ,Br - ,ClO - ,Cl - ,ClO 4 - ,CO 3 2- ,F - ,HCO 3 - ,H 2 PO 4 - ,HPO 4 2- ,P 2 O 7 2- ,OH - ,PO 4 - ,HSO 4 - ,NO 2 - ,NO 3 - ,S 2- ,SO 4 2- TBHP), the absorbance spectrum of probe molecule C1 at 814nm does not change significantly, indicating that there is no strong interaction between probe molecule C1 and these ions, and thus no strong effect on the uv absorption of the probe at 814 nm; in contrast, at 5 times ClO addition - Thereafter, the absorption spectrum of probe molecule C1 at 814nm was significantly reduced, indicating that probe molecules C1 and ClO - A stronger effect occurs between them.
To further determine the probe molecule C1 versus ClO - In the solvent system, the behavior of the probe molecule C1 in identifying the fluorescence spectrum of different ions was examined. The probe molecule C1 has a strong fluorescence emission peak, and the position of the emission peak is 834nm. When 5 times of other ions are added (5.0X10) -5 mol/L), while some ions also cause a weak decrease in fluorescence spectrum intensity, only ClO - The quenching effect of (2) is most pronounced. The above phenomenon indicates that in an aqueous system, the probe molecule C1 can act as ClO - Selection ofA sex recognition probe.
In aqueous solution, probe molecule C1 pair ClO - Has good selectivity to ClO - Can reach a detection limit of 10 - 7 mol/L. And ClO can still be detected over a broad pH range - This is of great importance for the application of the probe molecule C1 in the practical rapid detection of chloride ions.
As can be seen from FIG. 1, the pH value is in the range of 5.5 to 10.0, and the fluorescence intensity is insensitive to the pH value change. This suggests that probe molecule C1 can react with ClO over a wide acid-base variation range - Interaction, which is the actual detection of ClO for probe molecule C1 - Has important significance in application.
Claims (1)
1. A method for detecting hypochlorite ions of construction materials based on optical probes is characterized by comprising the following steps: the method comprises ClO - Concentration detection, clO - The concentration detection process is as follows, the probe molecule C1.9. 6.9mg is weighed and dissolved in 2mL DMF to prepare the probe molecule with the concentration of 5.0X10 -3 The mol/L probe solution is reserved; firstly, making a standard curve, dissolving 6 mu L of probe solution in 3mL water, wherein the concentration of probe molecules in the probe solution is 1.0X10 -5 mol/L, add ClO with different concentration - Measuring the ultraviolet visible light absorption spectrum and the fluorescence emission spectrum of the fluorescent probe; containing ClO in different concentrations - The absorption spectrum at 814nm is significantly reduced; the fluorescence intensity at the position of the emission spectrum 834nm is obviously reduced, and a standard curve is obtained; in detection, 3mL of the liquid to be detected is taken, 6 mu L of probe solution is added, the ultraviolet-visible light absorption spectrum and the fluorescence emission spectrum of the liquid to be detected are detected, and the ClO contained in the liquid to be detected is obtained corresponding to a standard curve - Concentration;
the synthesis of probe molecule C1 is as follows:
。
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CN202010609783.9A CN111948165B (en) | 2020-06-29 | 2020-06-29 | Method for detecting hypochlorite ions of construction material based on optical probe |
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CN202010609783.9A CN111948165B (en) | 2020-06-29 | 2020-06-29 | Method for detecting hypochlorite ions of construction material based on optical probe |
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CN111948165B true CN111948165B (en) | 2023-09-19 |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106841148A (en) * | 2017-03-15 | 2017-06-13 | 湖北文理学院 | The fluorescence probe and method of quick detection hypochlorite and its application in originally water sample detection |
CN110174397A (en) * | 2019-06-15 | 2019-08-27 | 贵州医科大学 | A kind of application of colorimetric probe |
CN110372632A (en) * | 2019-07-26 | 2019-10-25 | 广东轻工职业技术学院 | A kind of fluorescent probe molecule and its preparation method and application of quick identification hypochlorite ion |
-
2020
- 2020-06-29 CN CN202010609783.9A patent/CN111948165B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106841148A (en) * | 2017-03-15 | 2017-06-13 | 湖北文理学院 | The fluorescence probe and method of quick detection hypochlorite and its application in originally water sample detection |
CN110174397A (en) * | 2019-06-15 | 2019-08-27 | 贵州医科大学 | A kind of application of colorimetric probe |
CN110372632A (en) * | 2019-07-26 | 2019-10-25 | 广东轻工职业技术学院 | A kind of fluorescent probe molecule and its preparation method and application of quick identification hypochlorite ion |
Non-Patent Citations (2)
Title |
---|
"A mitochondria-targeted fluorescence probe for ratiometric detection of endogenous hypochlorite in the living cells";Wen-Li Wu et al.;《Analytica Chimica Acta》;20170115;第950卷;第1-6页 * |
次氯酸比色荧光探针的研究进展;余青 等;《有机化学》;20200115;第40卷;第1206~1231页 * |
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