CN101299016A - Method for testing concrete permeability based on multiple internal reflectance infra red spectrum - Google Patents
Method for testing concrete permeability based on multiple internal reflectance infra red spectrum Download PDFInfo
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- CN101299016A CN101299016A CN 200810071129 CN200810071129A CN101299016A CN 101299016 A CN101299016 A CN 101299016A CN 200810071129 CN200810071129 CN 200810071129 CN 200810071129 A CN200810071129 A CN 200810071129A CN 101299016 A CN101299016 A CN 101299016A
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Abstract
A method for detecting the penetrability of the concrete based on a multiple internal reflection infrared spectrum relates to a method for detecting the penetrability of the concrete, and especially relates to a method for detecting the penetrability of the concrete based on a multiple internal reflection infrared spectrum technique. The invention provides a method for detecting the penetrability of the concrete based on multiple internal reflection infrared spectrum, wherein the method has the advantages of easy operation, high operation sensibility, intuitionistic and reliable data, suitability for continuously measuring the transmission characteristic of various species in the concrete dynamically, and significant actual meaning for evaluating the penetrability of concrete material. The preparation for sample piece of concrete comprises the following steps: wet curing the sample piece of concrete under room temperature, slicing according to the required thickness, grinding and drying. An MIR-FTIR test comprises the following steps: measuring with a Fourier Transform infrared spectrometer, collecting the infrared spectrogram of dried concrete sample/total internal reflection wafer interface as a background, and when the electrolytic cell is filled with solution to be measured, collecting the infrared spectrogram at different permeation time until a time when the peak intensity of spectrogram does not increase.
Description
Technical field
The present invention relates to a kind of method for testing concrete permeability, especially relate to a kind of method for testing concrete permeability based on multiple internal reflectance infra red spectrum (MIR-FTIR) technology.
Background technology
In recent years, the permanance of reinforced concrete structure and safety issue have caused widely to be paid much attention to, and had carried out a large amount of relevant researchs.For the permanance of reinforced concrete structure and the research and the design of security, all be based upon for a long time concrete density or infiltrative evaluation certain degree.The perviousness of concrete material has become an important parameter estimating its quality.Concrete perviousness is meant gas, liquid, ion or chemical molecular under the effect of pressure, chemical potential, electric field or concentration field, the complexity of the orientation infiltration in concrete, diffusion, migration.The permanance and the concrete permeability of reinforced concrete structure are in close relations.For example: concrete carbonization is because CO
2Gas infiltrate concrete layer and with wherein Ca (OH)
2Or due to the reaction of hydrated cementitious product such as hydrated calcium silicate; Concrete chemical erosion is that concurrent biochemical reaction causes because water and aggressivity ion infiltrate concrete; The corrosion of reinforcing bar is the infiltration owing to chlorion, due to the erosion damage of passivating film; And concrete freeze-thaw damage causes owing to infiltrating the icing at low temperatures freezing up of concrete free water.Feldman points out in the meeting of the 8th international cement chemistry: " several studies to permanance shows that perviousness is a most important factor that influences concrete durability ".In general, the concrete that permeance property is low must have the ability that corrosive medium is invaded and corroded in the strong opposing environment, and therefore concrete impermeability can become important evaluation index of reinforced concrete permanance.
Concrete perviousness comprises water permeability, gas penetration potential, saturating molecule or ionic permeability etc., has developed multiple relevant concrete permeability method of testing at present.Because the destruction that the infiltration of coagulation soil water may cause the reinforced concrete structure of various ways, at present both at home and abroad to the anti-water permeability research of concrete at most.People such as Le Meilong have developed two kinds of infiltration coefficient proving installations.China's water conservancy project, harbor work adopt quick impermeability test method, adopt a pressurization as SD 105-82 " concrete for hydraulic structure testing regulations ", the test specimen of riving behind the constant voltage 24h, and the average infiltration height of test, and with this calculation permeability coefficient.People such as Khatri have contrasted the method for water infiltration capacity and two kinds of tests of permeated height concrete permeability energy, think that discharge method is more suitable for the higher concrete of perviousness, and for the higher concrete of impermeability, adopt the permeated height method more suitable.
Yet when being permeating medium with water, owing to the continuation aquation of cement, the migration of material, the change of capillary pipe structure etc. make process of osmosis be difficult to reach stable state, so the infiltration coefficient of water is difficult to accurate measurement.Kollek etc. proposed O in the concrete in 1999
2The Cembureau method of testing of infiltration coefficient obtains in the world to accept extensively, and is recommended as measurement standard by the RIEM tissue the same year.The principle of this method is: apply stable air pressure to sample, be recorded under this pressure by the gas flow of concrete sample, convert infiltration coefficient again to, estimate concrete O with this
2Permeance property.Because it is minimum to see through concrete gas flow, this method adopts soap film flowmeter.For satisfying the seal request of sample periphery, also must adopt the structure of rubber-tyred.Though this method measuring accuracy is higher, test procedure is very loaded down with trivial details, is difficult for implementing.
In addition, also having both at home and abroad many work is the quick evaluations to concrete permeability of applied electricity or electrochemical process, and wherein ASTM C 1202 methods are the most frequently used methods of chloride ion permeability in a kind of quick measurement concrete.This method is examined the concrete two ends and is applied the 60V DC voltage by giving, and measures the electric weight that 6h passes through and estimates concrete impermeability.The major defect of this method is that galvanization solution meeting temperature rise can be quickened the diffusion of chlorion, makes the actual measurement electric weight bigger than normal; In addition, serious corrosion can take place when switching on electrolysis in electrolyte solution (NaCl, NaOH) in copper mesh, thereby influences the conduction of copper mesh.In a word, all there is shortcoming in various degree in the method for present various measurement concrete permeabilities, develops new method of testing and seems very necessary.
Fourier-transform infrared (FTIR) spectrum is widely used in the mensuration of material chemistry The Nomenclature Composition and Structure of Complexes.Fourier infrared attenuated total reflection (FTIR-ATR) technology is meant that a branch of light enters the crystal with high index, in the interface incident angle of crystal and sample (low refractive index is arranged) greater than critical angle, the reflection (total reflection) on the interface almost completely thus of all light beams.The light beam end penetrates reflecting surface slightly and reflects.If the sample surfaces that contacts with crystal is to the selective absorption of light beam, the light beam that then penetrates reflecting surface weakens because of being absorbed at the energy of some wavelength, and the reflectance spectrum of gained also has the characteristics of absorption spectra.Usually the variation of primary event energy is quite little, and the absorption band of gained is very weak.If increase the number of times of total reflection, then can make absorption band strengthen multiple internal reflectance that Here it is.Fig. 1 is the principle schematic of multiple internal reflectance FFIR.
Because relevant with the frequency of exposure of sample in absorption characteristic, penetration depth and the multiple internal reflection of the degree that partly decayed of incident optical energy and sample, so spectral intensity depends on penetration depth d
p, the combine closely absorption size of situation and sample itself of order of reflection and sample and MIR crystal.According to maxwell theory, the total reflection light beam penetrates sample thickness and follows following formula:
λ in the formula: the wavelength of light beam in the internal reflection crystal;
n
1: the refractive index of internal reflection crystal;
n
2: the refractive index of sample;
d
p: light penetrates the vertical depth of sample, i.e. penetration depth;
θ: incident angle.
As can be known, the penetration depth of optical radiation and the ratio n of (1) light beam in refractive index (crystalline material) with the refractive index of sample of the intracrystalline wavelength X of reflection, (2) internal reflection crystal
1/ n
2(the MIR crystal generally adopts the high crystal of refractive index such as germanium, silicon, zinc selenide) is relevant with (3) incident angle θ.
Penetration depth is directly proportional with λ, and the light of different wave length penetrates the degree of depth difference of sample layer, and wavelength is big more, penetration depth is big more, and under the situation of incident angle greater than critical angle, incident angle is more near critical angle, penetration depth is big more, and penetration depth is generally the hundreds of nanometer extremely between several microns.
Summary of the invention
The object of the present invention is to provide a kind of easy and simple to handle, manual dexterity is high, data are intuitive and reliable, the transport property of the various species of kinetic measurement in concrete continuously, infiltrative evaluation has the method for testing concrete permeability based on multiple internal reflectance infra red spectrum of crucial practical significance for concrete material.
The present invention is from the reaction of molecular level research concrete interface, proposition is applied to concrete permeability with multiple internal reflectance FFIR (MIR-FTIR) technology and detects, designed rational experimental provision, the original position of concrete permeability, the detection of dynamic of harmless, many species have been realized, estimate concrete perviousness, from the reaction of molecular level research concrete interface.
Concrete steps of the present invention are as follows:
1) preparation of concrete test piece
With concrete test piece wet curing at room temperature, thickness section on request, polishing, drying;
2) MIR-FTIR test
Measure with Fourier transformation infrared spectrometer, the infrared spectrum of gathering dry concrete sample/total internal reflection wafer interface after electrolytic cell is filled with solution to be measured, is gathered the infrared spectrum of different times of penetration as a setting, no longer increases up to spectral strength.
Described electrolytic cell can adopt organic glass electrolytic cell, glass electrolytic cell or various high molecular polymer electrolytic cell.The size of concrete sample can adopt the concrete sample of long 50mm * wide 10mm * thick (1～10) mm.The total internal reflection wafer adopts KRS-5, germanium or silicon.The one side that electrolytic cell opens wide is connected concrete test piece surface with cementing agent, and the electrolytic cell side is provided with circular hole, and circular hole is used for the turnover of test solution or gas.The total internal reflection wafer adopts infrared total internal reflection wafer, and the size of total internal reflection wafer can adopt 50mm * 10mm * 3mm.The light of measuring with Fourier transformation infrared spectrometer is with 20～70 ° of incidents, and the total reflection number of times is 5～30 times.Penetration depth d
pCan determine according to parameters such as different samples, angle of light, infrared total internal reflection wafer materials, be about 50～1000nm.
Because the present invention is from the reaction of molecular level research concrete interface, proposition is applied to concrete permeability with multiple internal reflectance FFIR (MIR-FTIR) technology and detects, designed rational experimental provision, the original position of concrete permeability, the detection of dynamic of harmless, many species have been realized, estimate concrete perviousness, from the reaction of molecular level research concrete interface.Therefore the invention provides a kind of easy and simple to handle, manual dexterity is high, data are intuitive and reliable, the transport property of the various species of kinetic measurement in concrete continuously, infiltrative evaluation has the method for testing concrete permeability based on multiple internal reflectance infra red spectrum of crucial practical significance for concrete material.
Description of drawings
Fig. 1 is the multiple total reflection application principle synoptic diagram of the embodiment of the invention.In Fig. 1, each code name is a total reflection wafer 1, light beam 2, and sample 3 and 4,2 θ are the reflected light angle, d
pBe thickness of sample.
Fig. 2 is that the MIR-FTIR of the embodiment of the invention measures concrete sample perviousness apparatus structure synoptic diagram.
Fig. 3 penetrates different-thickness (cement and sand ratio are 1: 2) concrete for the water of the embodiment of the invention, and the INFRARED SPECTRUM peak intensity is curve over time.In Fig. 3, horizontal ordinate is wave number Wavenumbers (cm
-1), ordinate is INFRARED SPECTRUM peak intensity Absorbance; (a) cement thickness is 2mm, and from bottom to up, the time is 2,10,20,30,40,50,60s; (b) cement thickness is 3mm, and from bottom to up, the time is 2,10,20,30,40,70s; (c) cement thickness is 5mm, and from bottom to up, the time is 2,13,24,35,46,60,105,305s.
The concrete sheet INFRARED SPECTRUM peak intensity that Fig. 4 penetrates different sand coarse aggregate ratios for the water of the embodiment of the invention is change curve in time.In Fig. 4, horizontal ordinate is wave number Wavenumbers (cm
-1), ordinate is INFRARED SPECTRUM peak intensity Absorbance; (a) C: S=1: 2, the time is from bottom to up: 2,10,20,30,50,60s; (b) C: S=1: 1, be from bottom to up: 0,35,50,65,85,145,265,145min; (c) C: S=1: 0.5, be from bottom to up: 0,20,30,75,105,165,265,570min.
Fig. 5 penetrates concrete (C: S: H for the MFP solution of the embodiment of the invention
2O=1: 1: 0.3) INFRARED SPECTRUM peak intensity change curve in time.In Fig. 5, horizontal ordinate is wave number Wavenumbers (cm
-1), ordinate is INFRARED SPECTRUM peak intensity Absorbance; Be from bottom to up: 2,15,30,55,95,120,160,200,240s.
Embodiment
Below by embodiment the present invention is elaborated.
(1) thickness of test piece is to the influence of concrete permeability
Fig. 3 detects at different-thickness 2mm (a) for multiple internal reflectance infra red spectrum, 3mm (b), the dynamic process of water infiltration in 5mm (c) (cement and sand ratio are 1: 2) the concrete test piece.Table 1 has been listed the maximum absorbance of water and has been reached the required time of maximum absorbance.Wide range peak 3100～3650cm among the figure
-1Be the H-O-H stretching vibration peak, and 1625～1645cm
-1It then is the flexural vibrations peak of H-O key.As can be seen, the transmission course of water in the concrete test piece is very fast, can detect tangible water peak-to-peak signal for the test piece of thickness 2mm concrete at the interface in 2 seconds, and the water peak-to-peak signal constantly strengthens in time subsequently, promptly is tending towards saturated after 60 seconds.And, arrive the time phenomenal growth at interface by the concrete layer transmission by water when the concrete thickness increase.Test finds, when concrete thickness when 2mm increases to 3mm, the amount of water transmission has reduced about 10 times in the same time.Experiment shows that the thickness of concrete layer is a topmost factor of retained water transmission.Can also investigate concrete density, cement in the concrete/sand ratio, humidity, factors such as temperature are to the influence of water transport behavior and speed.Also explanation simultaneously, utilize the original position multiple internal reflectance infra red spectrum to detect that the water transmission has high sensitivity in the concrete layer, can detect the monomolecular water layer in interface in principle, and can further carry out quantitative test, this be at present other measuring technology can not compare.
(2) test piece packing is to the influence of concrete permeability
Fig. 4 is respectively (water cement ratio is 30%) C: S=1: 2 (a) for multiple internal reflectance infra red spectrum detects at cement and sand ratio, C: S=1: 1 (b), C: S=1: the dynamic process of water infiltration in the concrete test piece of 0.5 (c).Table 1 has been listed maximum absorbance and has been reached the maximum absorbance required time.
Table 1 water sees through maximum absorbance value and the required time that the concrete of different sand factors reaches
| Aggregate-to-cement ratio | Time of penetration t (s) | Maximum absorbance A (%) |
| 2∶1 | 1 | 63 |
| 1∶1 | 415 | 50 |
| 1∶2 | 570 | 18 |
Can find out obviously that from chart along with the reduction of sand cut, reach the maximum absorbance required time and extend gradually, the maximum absorbance value reduces gradually.Experiment shows, the transmission speed of water and transmission quantity all significantly reduce with the increase of concrete cement/sand ratio, when concrete aggregate-to-cement ratio when bring up to 1: 2 at 2: 1, can reduce about 3500 times to the perviousness of water.Concrete cement/sand is higher than more, in the concrete layer infiltration of water difficult more, just concrete anti-permeability performance is strong more.But this variation tendency is not linear with the numerical value of aggregate-to-cement ratio.
(3) sodium monofluorophosphate osmosis in concrete
(Na2PO3F is a kind of nontoxic inorganic migration-type corrosion inhibiter MFP) to sodium monofluorophosphate, is a kind of important reinforced concrete system corrosion inhibiter.The effect of MFP is mainly based on two aspects: 1, penetrate into concrete pore, generate insoluble compound with the reaction of hole liquid, make concrete finer and close; 2, by realizing protection to reinforcing bar with the rebar surface effect.This shows that the corrosion inhibition of MFP mainly depends on transport behavior and the transmission speed in concrete.Yet, also be difficult at present transport behavior and the transmission speed of MFP in concrete carried out original position, dynamically and the research of molecular level.Fig. 5 is for using the detected MFP of multiple internal reflectance infra red spectrum method at concrete test piece (C: S: H
2O=1: 1: 0.3, thickness of test piece: process of osmosis 0.3mm), spectral strength changed in time.
Two characteristic spectrum peaks appear among the figure, wherein, and strong wide range peak 1125cm
-1Be the stretching vibration peak of P-O singly-bound, narrower spectrum peak 1039cm
-1It is the stretching vibration peak of the two keys of P=O.So spectral strength growth has in time reflected the dynamic behaviour of the process of osmosis of sodium monofluorophosphate in the concrete test piece.The result shows that the speed of the transmission course of sodium monofluorophosphate in the concrete test piece is very fast, and along with the growth of time, sodium monofluorophosphate concentration constantly increases, and accumulates at the interface, thereby brings into play significant corrosion inhibition.But with same thickness, the infiltration of water is compared in the concrete test piece of proportioning of the same race, and it is longer that MFP reaches the used time of the strongest spectrum peak, this explanation, and the seepage velocity of MFP in concrete layer is slower in the seepage velocity under the similarity condition than water.
To sum up show, detect new method, can realize the original position to concrete permeability, the detection of dynamic of harmless, many species, estimate concrete perviousness, from the reaction of molecular level research concrete interface based on the concrete permeability of multiple internal reflectance infra red spectrum.This method sensitivity is high, data science, intuitive and reliable, easy and simple to handle, the transport property of the various species of kinetic measurement in concrete continuously, and infiltrative evaluation has unique advantages and important Practical significance for concrete material.
1.MIR-FTIR detect the measuring device for permeability of concrete design
Fig. 2 detects the infiltrative device synoptic diagram of concrete sample for MIR-FTIR.This device is provided with infrared light supply 22, organic glass (glass or various high molecular polymer) electrolytic cell 23, total internal reflection wafer (KRS-5, germanium or silicon) 24 and detecting device 25, and concrete sample 21 is of a size of 50mm * 10mm * different thickness; Wherein, electrolytic cell 23 is of a size of long 50mm, wide 10mm, and thick 1～10mm, unlimited one side is connected concrete test piece surface with cementing agent, and the circular hole of 2 diameter 0.3-3.0mm is left in the electrolytic cell side, is used for the turnover of test solution or gas.The infrared total reflection crystalline size 50mm * 10mm * 3mm that adopts.Light is with 20～70 ° of incidents, and the total reflection number of times is 5～30 times.Penetration depth d
pCan be about 50～1000nm according to parameters such as different samples, angle of light, infrared total reflection crystalline materials.
2. the preparation of concrete test piece
The concrete test piece can be made by concrete requirement of experiment, and adopt 3 kinds of different qualities than making, i.e. cement: water: sand is 1: 0.3: 2; 1: 0.3: 1 and 1: 0.3: 0.5; The concrete thickness of test piece is respectively 2mm, 3mm, and 5mm makes 9 kinds of test pieces.Take off mould behind the test piece 1～6d that makes, at room temperature wet curing 10～20d with the thickness section on request of diamond saw blade, with the fine sandpaper polishing, should be placed in the exsiccator fully dry, standby before the test.
3.MIR-FTIR test
Available extensive stock Fourier transformation infrared spectrometer is measured.Use FTIR 380 intelligent Fourier transformation infrared spectrometers (U.S. Nicolet company) logotype Model 300 continuously variable ATR (U.S. Spectra-Tech company) original position research H
2The infiltration capacity of O and MFP (sodium monofluorophosphate) solution in concrete over time.During test, before electrolytic cell injects solution, the infrared spectrum at collection dry concrete sample/germanium wafer interface as a setting earlier.After electrolytic cell was filled with solution to be measured, the infrared spectrum when gathering different time of penetration no longer increased up to spectral strength, and sample keeps motionless at the sample indoor location around here, and measurement parameter and light path are also constant fully.
Claims (7)
1. method for testing concrete permeability based on multiple internal reflectance infra red spectrum is characterized in that concrete steps are as follows:
1) preparation of concrete test piece
With concrete test piece wet curing at room temperature, thickness section on request, polishing, drying;
2) MIR-FTIR test
Measure with Fourier transformation infrared spectrometer, the infrared spectrum of gathering dry concrete sample/total internal reflection wafer interface after electrolytic cell is filled with solution to be measured, is gathered the infrared spectrum of different times of penetration as a setting, no longer increases up to spectral strength.
2. a kind of method for testing concrete permeability based on multiple internal reflectance infra red spectrum as claimed in claim 1 is characterized in that described electrolytic cell is organic glass electrolytic cell, glass electrolytic cell or high molecular polymer electrolytic cell.
3. a kind of method for testing concrete permeability based on multiple internal reflectance infra red spectrum as claimed in claim 1 is characterized in that concrete sample is of a size of the concrete sample of long 50mm * wide 10mm * thick (1～10) mm.
4. a kind of method for testing concrete permeability based on multiple internal reflectance infra red spectrum as claimed in claim 1 is characterized in that the total internal reflection wafer is KRS-5 wafer, germanium wafer or silicon wafer.
5. a kind of method for testing concrete permeability as claimed in claim 1 based on multiple internal reflectance infra red spectrum, the unlimited one side that it is characterized in that described electrolytic cell is connected concrete test piece surface with cementing agent, and the electrolytic cell side is provided with the turnover circular hole that is used for test solution or gas.
6. as claim 1 or 4 described a kind of method for testing concrete permeability, it is characterized in that the total internal reflection wafer is of a size of 50mm * 10mm * 3mm based on multiple internal reflectance infra red spectrum.
7. a kind of method for testing concrete permeability as claimed in claim 1 based on multiple internal reflectance infra red spectrum, the light that it is characterized in that measuring with Fourier transformation infrared spectrometer is with 20～70 ° of incidents, and the total reflection number of times is 5～30 times.
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