CN106083677A - A kind of chloride test reagent and detect the application of chloride ion in cement - Google Patents
A kind of chloride test reagent and detect the application of chloride ion in cement Download PDFInfo
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- CN106083677A CN106083677A CN201610496937.1A CN201610496937A CN106083677A CN 106083677 A CN106083677 A CN 106083677A CN 201610496937 A CN201610496937 A CN 201610496937A CN 106083677 A CN106083677 A CN 106083677A
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- Prior art keywords
- chloride
- test reagent
- cement
- chloride test
- fluorescent chemicals
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C323/00—Thiols, sulfides, hydropolysulfides or polysulfides substituted by halogen, oxygen or nitrogen atoms, or by sulfur atoms not being part of thio groups
- C07C323/50—Thiols, sulfides, hydropolysulfides or polysulfides substituted by halogen, oxygen or nitrogen atoms, or by sulfur atoms not being part of thio groups containing thio groups and carboxyl groups bound to the same carbon skeleton
- C07C323/62—Thiols, sulfides, hydropolysulfides or polysulfides substituted by halogen, oxygen or nitrogen atoms, or by sulfur atoms not being part of thio groups containing thio groups and carboxyl groups bound to the same carbon skeleton having the sulfur atom of at least one of the thio groups bound to a carbon atom of a six-membered aromatic ring of the carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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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
- G01N21/62—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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1003—Carbocyclic compounds
- C09K2211/1007—Non-condensed systems
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- Molecular Biology (AREA)
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- Engineering & Computer Science (AREA)
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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Abstract
The present invention relates to cement detection field, particularly to a kind of chloride test reagent and the application that detects chloride ion in cement thereof.A kind of chloride test reagent, containing the component of following parts by weight: solvent 95 ~ 100 parts, dispersant 1 ~ 3 part, fluorescent chemicals 0.5 ~ 1.3 part.The chloride test reagent of present invention synthesis is easily prepared, and after test result indicate that this detectable adsorbing chloride ions, there is Fluorescence-quenching, and fluorescence property will not be disturbed by other aniones, therefore it can be used to qualitative and detection by quantitative chloride ion, and the sensitivity of detectable is high, detected value is accurate so that this detectable has extraordinary potential application prospect as when detecting chloride ion in cement field.
Description
Technical field
The present invention relates to cement detection field, particularly to a kind of chloride test reagent and detect in cement chlorine from
The application of son.
Background technology
Chloride ion is a kind of harmful components in cement and cement raw material, directly in advance in New Type Dry-process Cement Production
Hot device and kiln calcining produce impact, cause the accident such as ring formation and putty, affect operation rate and cement clinker quality；At cement
In exceed certain content and reinforced steel bar strength can be made also to produce expansion and make while reducing the reinforcing bars rusting in concrete
Become the destruction of concrete, cause concrete to burst apart time serious, hide some dangers for construction quality, so must strictly control.Therefore,
The national standard of some advanced technology all defines limitation and the detection method of the chloride ion in cement in the world,
Can ensure that quality and the long-time stability of engineering.Have in the GB/T 176-2008 of domestic current national standard and detect chlorine accordingly
The method of ion；Wherein the ammonium thiocyanate volumetric method operating time is long, for quickly detecting inconvenience；Although and mercury salt titrimetry
Fast and convenient, but it to use the Mercury pernitrate. reagent of severe toxicity, easily to environment.Therefore, need badly now and develop
A kind of novel method quickly detecting chloride ion.
Summary of the invention
The technical problem to be solved is to provide a kind of chloride test reagent.
Further object is that the application that chloride ion is provided in the cement of offer above-claimed cpd.
A kind of chloride test reagent, containing the component of following parts by weight: solvent 95 ~ 100 parts, dispersant 0.1 ~ 0.3
Part, fluorescent chemicals 0.5 ~ 1.3 part.
Further, the chemical formula of described fluorescent chemicals is C16H6O8S2Mn, wherein, C16H6O8S2For 3-((3,5-bis-
Carboxyl phenyl) disulphanes base) phthalandione root, described fluorescent chemicals is anorthic system,P -1Space group, cell parameter isa =
12.126 (3),b=9.635 (2),c=13.332 (1),α =79.311 (1),β =81.173 (2),γ =
75.328 (7), V=1557.63 (1)3。
Further, described dispersant is anion surfactant.
Further, described anion surfactant is dodecylbenzene sodium sulfonate.
Further, described solvent is distilled water.
Above-mentioned chloride test reagent is applied in cement detects.
Dispersant and fluorescent chemicals only need to be dispersed in solvent by the preparation method of the detectable of the present invention.
There is advantages that
The chloride test reagent of present invention synthesis is easily prepared, and after test result indicate that this detectable adsorbing chloride ions
Fluorescence-quenching occurring, and fluorescence property will not be disturbed by other aniones, therefore it can be used to qualitative and fixed
Amount detection chloride ion, and the sensitivity of detectable is high, detected value is accurate so that and this detectable is examined as in cement field
Extraordinary potential application prospect is had when surveying chloride ion.
Accompanying drawing explanation
Fig. 1 is the coordination schematic diagram of the fluorescent chemicals used by the present invention.
Fig. 2 be after the detectable adsorbing chloride ions of the present invention fluorescence spectrum figure.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It it not limitation of the invention.
Wherein, the fluorescent chemicals used by the present invention synthesizes the most using the following method:
0.3mmol3-((3,5-dicarboxyphenyi) disulphanes base) phthalandione and 0.3mmol manganese nitrate are dissolved in 6mL acetonitrile and 12mL
In the middle of the mixed solvent of dimethyl acetylamide, form mixed liquor A after being stirred at room temperature dissolving, then described mixed liquor A is existed
Stand at 40 DEG C and obtain mixed liquid B in 72 hours, transfer to mixed liquid B subsequently, in politef autoclave, be put
155 DEG C of baking ovens react 24 hours, is down to room temperature with 5 DEG C/h afterwards and is filtrated to get described fluorescent chemicals.
Wherein, the English name of described 3-((3,5-dicarboxyphenyi) disulphanes base) phthalandione is 3-((3,5-
Dicarboxyphenyl) disulfanyl) phthalic acid, chemical constitution is as follows:
The preparation method of fluorescent chemicals used by the present invention uses the method for solvent thermal after first standing, and first passes through at 40 DEG C
Within 72 hours, stand and form small crystal nucleus so that solvent thermal process afterwards can obtain our desired fluorescent chemicals.If it is straight
Connect and use the method for solvent thermal to will be unable to, so that this fluorescent chemicals crystallizes, the fluorescent chemicals of the present invention to be can not get, and obtain
Be a kind of unformed compound.
Then the fluorescent chemicals of gained is carried out monocrystalline sign.
The X ray diffracting data of this fluorescent chemicals is to visit on diffractometer in Bruker Smart Apex CCD face, uses
MoKαRadiation (λ=0.71073), collects and carries out Lp factor correction with ω scan mode, and absorption correction uses SADABS journey
Sequence.Use direct method solution structure, then obtain whole non-hydrogen atom coordinate by difference Fourier method, and obtain hydrogen with theoretical hydrogenation method
Atom site (C H 1.083), is modified structure with method of least square.Evaluation work uses SHELXTL journey on PC
Sequence bag completes.
Resolving after tested and understand, the chemical formula of this fluorescent chemicals is C16H6O8S2Mn, wherein, C16H6O8S2For 3-((3,
5-dicarboxyphenyi) disulphanes base) phthalandione root, described fluorescent chemicals is anorthic system,P -1Space group, cell parameter isa
=12.126 (3),b=9.635 (2),c=13.332 (1),α =79.311 (1),β =81.173 (2),γ =75.328 (7), V=1557.63 (1)3, Z=2.
Its coordination schematic diagram as it is shown in figure 1, Mn atom takes the pattern of 6 coordinations, the most each Mn atom respectively with 3 3-
6 O atom coordinations on ((3,5-dicarboxyphenyi) disulphanes base) phthalandione molecule, wherein, two 3-((3,5-dicarboxyl benzene
Base) disulphanes base) two carboxyls of phthalandione are respectively adopted bidentate chelating pattern and are connected with Mn atom, and another 3-((3,5-bis-
Carboxyl phenyl) disulphanes base) on two carboxyls be then connected with Mn atom with monodentate pattern.
Embodiment 1
A kind of chloride test reagent, containing the component of following parts by weight: distilled water 98 parts, dodecylbenzene sodium sulfonate 0.2
Part, fluorescent chemicals 1 part.
Detectable in embodiment 1 is carried out fluorescence spectrum test, excitation wavelength by adding the chloride ion of variable concentrations
For 314nm.Fluorescence spectrum figure is as it is shown in figure 1, it will be seen that along with the concentration of chloride ion increases to from 0 from figure
0.006mol/L, fluorescence intensity is gradually lowered, and, if add is nitrate anion, sulfate radical or acetate not shadow
Ringing sensor of the invention fluorescence intensity (not shown in the diagram), its fluorescence intensity is similar when being 0mM with concentration substantially, therefore may be used
To utilize the change of fluorescence intensity that chloride ion is carried out qualitative and detection by quantitative.
The acid of the common portland cement of 0.3g is dissolved, is settled to 50mL；Then the 50mL embodiment of the present invention 1 is added
Chloride test reagent to 100mL, carry out fluorescence spectrum test after stirring.Measured fluorescence intensity and Fig. 1 gained
Intensity contrast, if intensity is less than the fluorescence intensity of 0.005mol/L, then can know this common portland cement by calculating
The 0.06% of the substandard requirement of chlorine ion concentration.Therefore, the detectable of the present invention is as detecting chloride ion in cement field
Time have extraordinary potential application prospect.
Embodiment 2
A kind of chloride test reagent, containing the component of following parts by weight: distilled water 95 parts, dodecylbenzene sodium sulfonate 0.1
Part, fluorescent chemicals 1.2 parts.
Embodiment 3
A kind of chloride test reagent, containing the component of following parts by weight: distilled water 100 parts, dodecylbenzene sodium sulfonate 0.3
Part, fluorescent chemicals 0.6 part.
Embodiment described above only have expressed embodiments of the present invention, therefore it describes more concrete and detailed, but can not be
And it is interpreted as the restriction to the scope of the claims of the present invention, as long as using the technical side that the form of equivalent or equivalent transformation is obtained
Case, all should fall within the scope and spirit of the invention.
Claims (6)
1. a chloride test reagent, it is characterised in that containing the component of following parts by weight: solvent 95 ~ 100 parts, dispersant
0.1 ~ 0.3 part, fluorescent chemicals 0.5 ~ 1.3 part.
A kind of chloride test reagent the most according to claim 1, it is characterised in that the chemical formula of described fluorescent chemicals
For C16H6O8S2Mn, wherein, C16H6O8S2For 3-((3,5-dicarboxyphenyi) disulphanes base) phthalandione root, described fluorescent chemicals
For anorthic system,P -1Space group, cell parameter isa=12.126 (3),b=9.635 (2),c=13.332 (1),α =79.311 (1),β =81.173 (2),γ =75.328 (7), V=1557.63 (1)3。
A kind of chloride test reagent the most according to claim 2, it is characterised in that described dispersant is anionic surface
Activating agent.
A kind of chloride test reagent the most according to claim 3, it is characterised in that described anion surfactant is
Dodecylbenzene sodium sulfonate.
A kind of chloride test reagent the most according to claim 4, it is characterised in that described solvent is distilled water.
6. the application of the chloride test reagent described in a claim 1, it is characterised in that: described chloride test reagent should
It is used in cement detection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610496937.1A CN106083677A (en) | 2016-07-18 | 2016-07-18 | A kind of chloride test reagent and detect the application of chloride ion in cement |
Applications Claiming Priority (1)
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| CN201610496937.1A CN106083677A (en) | 2016-07-18 | 2016-07-18 | A kind of chloride test reagent and detect the application of chloride ion in cement |
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| CN201610496937.1A Pending CN106083677A (en) | 2016-07-18 | 2016-07-18 | A kind of chloride test reagent and detect the application of chloride ion in cement |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102495032A (en) * | 2011-11-15 | 2012-06-13 | 深圳大学 | Chloride ion fluorescence detection method, device thereof and application thereof |
-
2016
- 2016-07-18 CN CN201610496937.1A patent/CN106083677A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102495032A (en) * | 2011-11-15 | 2012-06-13 | 深圳大学 | Chloride ion fluorescence detection method, device thereof and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| LING ZHANG: "2,20-Dithioditerephthalic acid", 《ACTA CRYST.》 * |
| MANISHKUMAR R. SHIMPI ET AL.: "Synthesis and structural evaluation of five coordination complexes of benzenepentacarboxylic acid with aza-donor ligands", 《JOURNAL OF MOLECULAR STRUCTURE》 * |
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Application publication date: 20161109 |