CN111948164A - Method for detecting construction material sulfate radical based on optical probe - Google Patents
Method for detecting construction material sulfate radical based on optical probe Download PDFInfo
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- CN111948164A CN111948164A CN202010608856.2A CN202010608856A CN111948164A CN 111948164 A CN111948164 A CN 111948164A CN 202010608856 A CN202010608856 A CN 202010608856A CN 111948164 A CN111948164 A CN 111948164A
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- 239000000523 sample Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 14
- 230000003287 optical effect Effects 0.000 title claims abstract description 14
- 239000004035 construction material Substances 0.000 title claims abstract description 11
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 7
- 238000000295 emission spectrum Methods 0.000 claims abstract description 6
- 238000002474 experimental method Methods 0.000 claims abstract description 5
- 238000004448 titration Methods 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims description 24
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 238000010276 construction Methods 0.000 abstract description 15
- 230000008901 benefit Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 238000009435 building construction Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 150000001450 anions Chemical class 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- IBGBGRVKPALMCQ-UHFFFAOYSA-N 3,4-dihydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1O IBGBGRVKPALMCQ-UHFFFAOYSA-N 0.000 description 2
- RGHHSNMVTDWUBI-UHFFFAOYSA-N 4-hydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1 RGHHSNMVTDWUBI-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- HCYIOKVZAATOEW-UHFFFAOYSA-M 1,2,3,3-tetramethylindol-1-ium;iodide Chemical compound [I-].C1=CC=C2C(C)(C)C(C)=[N+](C)C2=C1 HCYIOKVZAATOEW-UHFFFAOYSA-M 0.000 description 1
- OEVSHJVOKFWBJY-UHFFFAOYSA-M 1-ethyl-2-methylquinolin-1-ium;iodide Chemical compound [I-].C1=CC=C2[N+](CC)=C(C)C=CC2=C1 OEVSHJVOKFWBJY-UHFFFAOYSA-M 0.000 description 1
- PCYGLFXKCBFGPC-UHFFFAOYSA-N 3,4-Dihydroxy hydroxymethyl benzene Natural products OCC1=CC=C(O)C(O)=C1 PCYGLFXKCBFGPC-UHFFFAOYSA-N 0.000 description 1
- BGNGWHSBYQYVRX-UHFFFAOYSA-N 4-(dimethylamino)benzaldehyde Chemical compound CN(C)C1=CC=C(C=O)C=C1 BGNGWHSBYQYVRX-UHFFFAOYSA-N 0.000 description 1
- PRYNJOJHKYNLIS-UHFFFAOYSA-N 6-hydroxynaphthalene-2-carbaldehyde Chemical compound C1=C(C=O)C=CC2=CC(O)=CC=C21 PRYNJOJHKYNLIS-UHFFFAOYSA-N 0.000 description 1
- -1 Ac- Chemical class 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 238000001636 atomic emission spectroscopy Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000004683 dihydrates Chemical class 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000003068 molecular probe Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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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
- 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
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- 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
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Abstract
The invention discloses a method for detecting construction material sulfate radical based on an optical probe, which comprises the steps of firstly making a standard curve, taking corresponding probe solution, dissolving in water, adding HSO with different concentrations4 ‑Namely, a standard curve is obtained by a titration experiment. Adding the solution to be detected into the probe solution, and detecting the absorption spectrum and the emission spectrum of the solution. Corresponding to the standard curve to obtain the HSO contained4 ‑And (4) concentration. The optical probe is adopted 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 standardized, the construction is safe, and the construction speed is improved; before ensuring that the quality standard required by the test is metUnder the premise of obtaining better economic benefit and social benefit.
Description
Technical Field
The invention relates to a construction material detection method based on an optical probe, in particular to a construction material sulfate radical detection method based on the optical probe, and belongs to the technical field of chemical detection.
Background
With the rapid development of economic construction, the engineering test level has been continuously improved, but the detection methods of many raw material mechanical and chemical performance indexes are still not stable and mature enough, and especially the detection determination of many chemical performance indexes is realized by various traditional analysis detection methods, which not only needs expensive instruments and equipment, sufficient detection time, but also needs experienced human resources. The pressure of space, time and instrument cost, and the inaccuracy of raw and other materials chemical property index detection in time can all lead to the increase of detection expense, influence the construction progress, shorten the life of target building, reduce enterprise economic benefits. Therefore, in the construction production of bridges, underground engineering, building engineering and the like, the simple and rapid detection and control of the chemical performance indexes of the raw materials are of great importance.
Ions (HSO) harmful to concrete materials are detected by chemical indexes of current building construction raw materials4 -) Mainly comprises the following steps. Common methods for material detection are: the conventional chemical titration method, the atomic absorption spectrometry, the atomic emission spectrometry, the spectrophotometry and the like are adopted, wherein the conventional titration method is adopted as a detection means for the construction material, but all the methods have technical defects.
Disclosure of Invention
The invention aims to detect the building construction raw materials before construction by adopting an optical probe, 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 standardized, 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 invention adopts the technical scheme that the construction material detection is based on an optical probeSide measurement, HSO4 -The concentration detection process is as follows, L13.81 mg is weighed and dissolved in 2mL DMF to prepare the solution with the concentration of 5.0X 10-3The probe solution in mol/L is ready for use. First, a standard curve is prepared, 6. mu.L of probe solution is dissolved in 3mL of ethanol-water (1:1) solution, and the concentration of probe molecules in the solution is 1.0X 10- 5mol/L, adding HSO with different concentrations4 -Namely, a standard curve is obtained by a titration experiment. In actual detection, 3mL of the solution to be detected is added with 6 μ L of L1 probe solution, and absorption spectrum and emission spectrum are detected, wherein the solution contains HSO with different concentrations4 -The absorption spectrum of the liquid to be detected at 556nm is obviously reduced, and a new absorption peak is generated gradually at 454 nm; the emission spectrum is remarkably enhanced in fluorescence at 546nm and is blue-shifted in peak value. Corresponding to the curve, the HSO contained in the curve is obtained4 -The concentration and the color of the solution can be changed to know the HSO contained in the solution4 -And (4) concentration.
Said HSO4 -L1 in the concentration detection process can be replaced with L2.
Drawings
FIG. 1 shows the color change of the solution of L1 and L2 in a solvent system of ethanol-water (volume ratio 1:1) after the addition of 10 equivalents of the anion to be tested. (a) And (c) are photographs under natural light, and (b) and (d) are photographs under irradiation of an ultraviolet lamp having a wavelength of 365 nm. L1 or L2 and F are sequentially arranged from left to right in the photo-,Cl-,Br-,I-,HSO4 -,Ac-,H2PO4 -,NO2 -,NO3 -And SO4 2-。
FIG. 2 shows the addition of HSO at 572nm to L1(10 μ M) at 546nm and L2(10 μ M) at 10 times the presence of the other anions tested in an ethanol-water 1:1 solvent system4 -The fluorescence intensity change rate (excitation wavelength of 454nm,476 nm; slit width of 10.0nm,10.0nm) was then determined. Wherein 1 to 10 each represent Ac-,Br-,Cl-,F-,H2PO4 -,HSO4 -,I-,NO2 -,NO3 -,SO4 2-。
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
The synthesis of the probe molecule L series is as follows:
the corrosive action of the soluble sulfate can greatly shorten the service life of the construction building. The erosion effect of the soluble sulfate is mainly reflected in the following two aspects: on one hand, the concrete reacts with soluble sulfate to generate volume-expanded dihydrate gypsum, and also reacts with hydrated calcium aluminate to generate crystal water-containing calcium sulphoaluminate with a larger expansion coefficient, so that the concrete structure is cracked; on the other hand, the sulfate ions can corrode the steel bars, cause brittle fracture of the prestressed steel bars in severe cases, and cause serious cracking of concrete due to large-scale expansion of the corroded body, thereby causing serious potential safety hazards. Therefore, it is important to control the sulfate content in the concrete material to prevent the corrosion of the concrete by soluble sulfate. However, the detection of sulfur trioxide such as cement and admixture in the currently adopted national standard (GB/T176-2008) needs to be placed still for more than 12 hours, the operation is time-consuming, the required reagents are various, and the trouble is caused to the field material detection.
Water is used after secondary distillation; medicines such as N-methyl-2, 3, 3-trimethylindolium iodide, N-ethyl-2, 3, 3-trimethylbenzindolinum iodide, N-ethyl-2-methylquinolinium iodide, 3, 4-dihydroxybenzaldehyde, 6-hydroxy-2-naphthaldehyde, 4-hydroxybenzaldehyde, 4-dimethylaminobenzaldehyde, absolute ethyl alcohol and the like are laboratory existing reagents, and anions used in a probe molecule identification performance characterization experiment are analytically pure salts; except for special mention, the reagent is commercial and is used directly without treatment.
The aggregation properties of the dye molecules are closely related to the concentration. The effect of concentration on the optical properties of the probe molecules L1, L2 was therefore investigated using absorption and emission spectroscopy. The specific experimental steps are as follows: getDifferent volumes 5.0X 10-3Dissolving mol/L probe molecule in 3mL solvent system (volume ratio is 1:1) of ethanol and water to prepare solutions (5.0 × 10) with different concentrations-6M～8.0×10-5M). After shaking uniformly, standing, and measuring the ultraviolet-visible absorption spectrum and the fluorescence emission spectrum at room temperature.
The characteristic absorption peaks (556nm and 576nm) of the L1 and L2 monomers increase linearly with the increase of the concentration of the probe molecules, but no new absorption peak appears in the short wavelength direction, which indicates that the H-aggregate cannot be formed by increasing the concentration of the probe molecules. L1 and L2 have two emission peaks at the position with the wavelength more than 500nm, which indicates that the probe molecule has an equilibrium state of two structures, namely a benzene ring structure (A) and a quinoid structure (B). In addition, when the concentration of the probe is more than 10 mu M, the obvious red shift 'internal filtering effect' is shown at the long-wavelength part of the emission spectrum. By combining the above results with the addition of HSO4 -Comparing the later ultraviolet absorption spectrum to draw a conclusion that the spectrum is HSO4 -Plays a crucial role in the formation of H-aggregates by probe molecules. Meanwhile, the probe can be used for actual construction detection.
Furthermore, as can be seen from FIG. 1, HSO is being added4 -The solution color of the latter two probe molecules changed significantly: l1 and L2 respectively change from red to purple to yellow. Furthermore, under 365nm ultraviolet lamp irradiation, HSO is added4 -The color of the solution was also significantly different from that of the solution to which other ions were added, and the above results indicate that both L1 and L2 have the ability to detect HSO as a visual selectivity4 -The potential of the fluorescent molecular probe of (1).
For further study of L1, L2 as selectively detectable HSO4 -The practical application possibility of the fluorescent probe is that an ion interference experiment is carried out. The operation steps are as follows: at a concentration of 1.0X 10 in 3mL-5Adding 1.0X 10 mol/L probe molecule solution-230 μ L (10 times) of other anions in mol/L, and HSO of the same concentration4 -30 μ L (10 times), and the fluorescence emission spectrum was measured after shaking (excitation wavelengths of 454nm and 476nm, respectively, as shown in FIG. 2). As can be seen from the figures, it is,various anions such as Ac-,Br-,Cl-,F-,H2PO4 -,I-,NO2 -,NO3 -And SO4 2-Presence of (2) to L1+ HSO4 -,L2+HSO4 -The fluorescence emission intensity of (a) was not much affected, but a significant fluorescence enhancement was still observed.
A novel optical probe molecule L series is synthesized, and the spectrum recognition behavior of the optical probe molecule L series on common ions is realized. Wherein the probe molecule L2 is opposite to HSO in ethanol water solution4 -Has excellent selectivity to HSO4 -Can reach 10-7And M. And can still detect HSO in a wide pH range4 -Therefore, a good technical detection means is provided for the rapid detection of sulfate ions in the field environment of actual construction materials in the future.
Claims (3)
1. A method for detecting construction material sulfate radical based on an optical probe is characterized in that: HSO4 -The concentration detection process is as follows, L13.81mg is weighed and dissolved in 2mLDMF to prepare the solution with the concentration of 5.0 multiplied by 10-3A mol/L probe solution is reserved; first, a standard curve is prepared, 6. mu.L of probe solution is dissolved in 3mL of ethanol-water (1:1) solution, and the concentration of probe molecules in the solution is 1.0X 10-5mol/L, adding HSO with different concentrations4 -Namely, obtaining a standard curve by a titration experiment; in actual detection, 3mL of the solution to be detected is added with 6 μ L of L1 probe solution, and absorption spectrum and emission spectrum are detected, wherein the solution contains HSO with different concentrations4 -The absorption spectrum of the liquid to be detected at 556nm is obviously reduced, and a new absorption peak is generated gradually at 454 nm; the emission spectrum is 546nm, and the fluorescence is obviously enhanced and the peak value is blue-shifted; corresponding to the curve, the HSO contained in the curve is obtained4 -The concentration and the color of the solution can be changed to know the HSO contained in the solution4 -And (4) concentration.
2. The method for detecting the sulfate radical of the construction material based on the optical probe as claimed in claim 1, wherein the method comprises the following steps: said HSO4 -L1 in the concentration detection process can be replaced with L2.
3. The method for detecting the sulfate radical of the construction material based on the optical probe as claimed in claim 1, wherein the method comprises the following steps: the synthesis of probe molecules L1 and L2 was as follows:
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140010763A1 (en) * | 2011-03-15 | 2014-01-09 | Ramot At Tel-Aviv University Ltd. | Activatable fluorogenic compounds and uses thereof as near infrared probes |
| CN104418874A (en) * | 2013-08-28 | 2015-03-18 | 苏州罗兰生物科技有限公司 | Fluorescent molecular probe for detecting fluoride ions in aqueous solutions as well as synthesis method and application thereof |
| CN105424661A (en) * | 2015-11-13 | 2016-03-23 | 贵州大学 | Probe method for detecting a trace amount of F- through ratio fluorescence and ratio absorption or visual observation |
-
2020
- 2020-06-29 CN CN202010608856.2A patent/CN111948164A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140010763A1 (en) * | 2011-03-15 | 2014-01-09 | Ramot At Tel-Aviv University Ltd. | Activatable fluorogenic compounds and uses thereof as near infrared probes |
| CN104418874A (en) * | 2013-08-28 | 2015-03-18 | 苏州罗兰生物科技有限公司 | Fluorescent molecular probe for detecting fluoride ions in aqueous solutions as well as synthesis method and application thereof |
| CN105424661A (en) * | 2015-11-13 | 2016-03-23 | 贵州大学 | Probe method for detecting a trace amount of F- through ratio fluorescence and ratio absorption or visual observation |
Non-Patent Citations (1)
| Title |
|---|
| TING YU ET AL.: ""A novel colorimetric and fluorescent probe for simultaneous detection of SO32-/HSO3- and HSO4- by different emission channels and its bioimaging in living cells"", 《TALANTA》 * |
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