专利摘要:
Method and device (1) for determining a material property, in particular the aging state or aging resistance, of a bitumen material (2), comprising the steps of: - applying a first monochromatic excitation radiation (4) of a first excitation wavelength to the bitumen material (2) λ1); - measuring the intensity (I1) of a first fluorescence radiation excited by the first excitation radiation (4) at a measuring wavelength; - Applying the bitumen material (2) having a substantially monochromatic second excitation radiation (6) of a first excitation wavelength (λ2); Measuring the intensity (I2) of a second fluorescence radiation excited by the second excitation radiation (6) at the measurement wavelength; - Determining a first characteristic number (K1) for the material property of the bitumen material (2) from the ratio between the intensity (I2) of the second fluorescence radiation to the intensity (I1) of the first fluorescence radiation.
公开号:AT517366A1
申请号:T50522/2015
申请日:2015-06-22
公开日:2017-01-15
发明作者:Dr Hofko Bernhard;Dipl Ing Hospodka Markus;Dr Füssl Josef;Dr Eberhardsteiner Lukas;Dr Grothe Hinrich;Dr Handle Florian;Dipl Ing Grossegger Daniel;Dr Blab Ronald
申请人:Technische Universität Wien;
IPC主号:
专利说明:

The invention relates to a method and a device for determining a material property of a bitumen material, which is associated in particular with the state of aging or aging resistance.
Bitumen and bituminous substances are important raw materials in construction, industry and production. Particularly in the construction industry, the requirements for material and product are constantly being increased, which necessitates improved quality control and analysis of the substances used. The increased requirements relate in particular to the aging resistance of the material, which until now could only be roughly determined in time-consuming tests. Up until now, there has been a lack of basic, rapid aging resistance testing, which makes quality testing possible at various stages of the work process. In particular, it would be desirable to record the material properties of the bitumen in the production, storage and processing process, without requiring special time expenditure.
This concerns, for example, the recycling of Straßenbaubitu-men. This is understood to mean the reuse of bituminous bonded building material, which is obtained in large quantities, especially in road construction. Most of the spent asphalt can in principle be reused for the production of new asphalt mix. However, the recycling rate of reclaimed asphalt is still low. This is due in particular to the lack of reliable quality control of the recycled material.
At present, the signs of aging of recycled asphalt are mitigated by the addition of very soft, fresh binder. However, this method is disadvantageously not efficient. Therefore, it is indispensable to include the aging mechanism of bitumen on a chemical-physical level in order to reliably predict the reusability of excavated asphalt.
Various approaches have been presented in the prior art for this purpose.
With regard to aging mechanisms in long-term aging, an advanced micelle model for bitumen is often used. The micelle model states that bitumen consists of a continuous, oily phase (malt phase) in which As-content micelles are dispersed from agglomerated asphaltene molecules (emulsion). In order for the highly polar asphaltene micelles to disperse successfully in the low-polarity phase, it requires a sheath around the micelles, which produces a polarity gradient (emulsifier). This coat is made of acrylics and resins. When attacked by oxidizing agent, they first enter the malt phase, which, however, is hardly reactive. Only at the mantle of the particles begins the intensive oxidation, which leads to an increase in polarity at the interface between the mantle and the malt phase. This reduces the quality of the dispersion, it creates as it were a predetermined breaking point at the interface, which leads to an increase in hardness and solubility of the material and thus favors the formation of brittle fractures. This can explain how brittleness increases with aging. Investigations by the applicant have shown that neither the malt phase nor the asphaltenes significantly alter their mechanical behavior as a result of aging. The increasing stiffness of bitumen with advancing aging can be explained and modeled by increasing the asphaltene concentration in relation to the concentration of smaller, less polar aromatics.
To investigate these processes, fluorescence spectroscopy and fluorescence microscopy, which are known per se in the state of the art, were used in particular (see, Handle, Florian, et al., "Understanding the microstructure of bitumen: a CLSM and fluorescence approach to model bitumen aging behavior.") Proceedings to 12th ISAP International Conference on Asphalt Pavements, Raleigh, USA 2014, Handle et al., "The bitumen microstructure: a fluorescent approach", Materials and Structures, December 2014, Bearsley et al., "Direct observation of the asphaltene structure in paving-grade bitumen using confocal laser-scanning microscopy, Journal of Microscopy, Vol. 215, 2004), and from these studies, a better understanding of the aging of bitumen was obtained.
In the prior art, a variety of apparatuses for measuring fluorescence have also been proposed (cf., for example, CA 2,833,299, US 2005/0253088 A1, US 4,330,207, WO 2010/048584, US Pat. No. 7,633,071 B2)
So far, however, no satisfactory solution has been found for converting the theoretical knowledge on the aging process of bitumen obtained from fluorescence spectroscopy into a practicable method for analyzing the suitability of degrading material for reuse.
Accordingly, the object of the invention is to alleviate or eliminate the disadvantages of the prior art. The invention is therefore particularly aimed at providing a method with which the material properties of a bitumen material can be determined quickly and easily. In addition, a structurally simple device for determining the material properties of the bitumen material is to be provided.
This object is achieved by a method having the features of claim 1 and a device having the features of claim 9. Preferred embodiments are given in the dependent claims. In the method claim 14 and the Vor-direction claim 16 an alternative solution of the same task is given.
The method according to the invention therefore has at least the following steps: applying a first monochromatic excitation radiation of a first excitation wavelength to the bitumen material; Measuring the intensity of a first fluorescence radiation excited by the first excitation radiation in a measuring wavelength range; - Applying the bitumen material having a substantially monochromatic second excitation radiation of a second excitation wavelength; Measuring the intensity of a second fluorescence radiation excited by the second excitation radiation in the measurement wavelength region; - Determining a first index for the material property of the bitumen material from the ratio between the intensity of the second fluorescence radiation to the intensity of the first fluorescence radiation.
According to the invention, the bitumen material, in particular an excavation or recycling asphalt, is exposed to a first excitation radiation having a first excitation wavelength, with which in particular the fluorescent centers of the bitumen are excited to a first emission of fluorescence radiation whose intensity is detected in a predetermined measurement wavelength range becomes. Preferably, the detection of the first fluorescence radiation occurs in a substantially monochromatic wavelength range of measurement wavelength, i. a single measuring wavelength is used. Alternatively, a measurement wavelength range which is small compared with the wavelength region where the first fluorescence radiation occurs may be used. In addition, the bitumen is irradiated with a second excitation radiation of a second excitation wavelength which is different from the first excitation wavelength. The excitation of the bitumen material is preferably carried out successively at a time interval in order to ensure the resolution between the measurement signals of the first and second fluorescence radiation or fluorescence emission. The intensity of the second fluorescence radiation is detected in the same measuring wavelength range as the first fluorescence radiation. As described above, the measuring wavelength range can on the one hand be substantially monochromatic. On the other hand, the intensity of the second fluorescence radiation can be detected in a narrow range of measurement wavelengths compared to the entire wavelength range of the second fluorescence radiation. Finally, an index of the material property, in particular the aging state or aging resistance, of the bitumen is determined from the ratio between the intensity of the second fluorescence radiation and the intensity of the first fluorescence radiation. In extensive investigations, it has been found, in particular, that the aging processes in the bitumen material affect its fluorescence spectrum. The method according to the invention makes use of this finding by measuring the intensity of the fluorescence radiation at two different, discrete excitation wavelengths, wherein the ratio of the intensities of the fluorescence signals is used as an index or indication value in particular for the aging state of the bitumen material. Preferably, the second excitation wavelength is greater than the first excitation wavelength. It has been demonstrated that the uptake of a full excitation scan is not required to determine the aging of the bitumen material, but rather that the intensities of fluorescence radiation in discrete (ie The intensity of the first fluorescence radiation is used here as a reference quantity to which the intensity of the second fluorescence radiation is related The ratio between the intensity values of the fluorescence radiation at the different excitation wavelengths can be a reliable indicator of whether the aging processes In addition, the first measure of an initial test may be used to determine whether poor aging resistance of the bitumen material is due to poor R material quality, storage conditions, processing, etc. threatens to have a significantly negative impact on the material properties in the near future. Accordingly, in a preferred application, the first characteristic number can be used as a measure of the aging resistance of the bitumen material, which in particular is an expansion or recycling asphalt. In particular, experimental studies have shown that the aging of the bitumen material causes a lowering of the intensity of the second fluorescence radiation in relation to the first fluorescence radiation. Thus, the determined characteristic allows an estimation of the aging state or the aging resistance of the examined bitumen material.
The higher the first ratio, the greater the aging resistance of the bitumen material. On the basis of the first ratio can thus be decided whether the bitumen material for initial, reuse or re-use should be provided. By using individual, substantially monochromatic excitation signals, the constructional outlay for the implementation of the method can be kept low. Advantageously, the recording of an excitation spectrum over a wide interval of excitation wavelengths can be dispensed with. The aging state of the bitumen material can be analyzed according to the invention with a minimum number of fluorescence measurements. As a result, the time required for the method can also be substantially reduced, which in particular enables real-time application of the method, for example on a hand-held device. In order to apply the substantially monochromatic excitation radiation to the bitumen sample, on the one hand radiation sources can be used, which are essentially monochromatic radiation, i. Radiation with a very low bandwidth, send out. In particular, light-emitting diodes or lasers are suitable for this purpose. On the other hand, radiation sources such as gas lamps can be used, which emit broadband excitation radiation, from which the desired substantially monochromatic excitation radiation is obtained with the aid of a filter or a monochromator.
The method according to the invention is particularly suitable for implementation on a portable handset, in which only those wavelengths are excited, which are also essential for the assessment of the state of aging. Thus, for the first time, a method can be created with which flexibility in the laboratory, on the
Construction site and even when installed, the aging resistance of the bitumen used can be evaluated easily, quickly and favorably.
If the first characteristic number is compared with a first reference value for the material property of the bitumen material, the decision can be made in a particularly simple manner as to whether the investigated bitumen material can be supplied for first or reuse or if the aging resistance of the bitumen material is already so impaired that a first or re-use of the bitumen material would not be expedient, since in the near future severe damage caused by material aging can be expected. Accordingly, a poor quality of the bitumen material with regard to the aging state and / or the aging resistance can be determined if the first code falls below the first reference value. The reference value can be obtained on the one hand from theoretical considerations or from empirical data from previous investigations on bitumen materials with different degrees of aging. Preferably, the reference value is stored in a database. In carrying out the method, the reference value is retrieved from the database in order to enable a comparison with the first code number, which was determined from the measured values of the fluorescence radiation at different excitation wavelengths.
The investigations have shown that aging based on the first measure alone could not be reliably detected in all Bitu samples. It has been found that the first index is unremarkable in some bitumen samples, although the material properties are already compromised by complex processes, such as aging in pre-use or thermal damage during storage, etc. In order to make this class of bituminous materials available to the method for determining the aging, in a preferred embodiment of the method the further steps are - applying to the bitumen material having a substantially monochromatic third excitation radiation of a third wavelength; Measuring the intensity of a third fluorescence radiation excited by the third excitation radiation in the measurement wavelength region; Determining a second characteristic for the material property of the bitumen from the ratio between the intensity of the third fluorescence radiation to the intensity of the first fluorescence radiation.
In this embodiment, the fluorescence emission of the bitumen material is detected due to the excitation with the third excitation radiation of the third excitation wavelength, wherein the third excitation wavelength is different from both the first and the second excitation wavelength. The intensity of the third fluorescence radiation, which can be measured at a time interval to the first and second fluorescence radiation, is then set in relation to the intensity of the first fluorescence radiation in order to obtain a second characteristic number, in particular for the aging state of the bitumen material. As a result, age-resistant bitumen samples can be reliably distinguished from those bitumen samples whose first ratio is above the first reference value but have nevertheless undergone radical aging processes. The causes of the aging processes are insignificant, which may be due to long-term changes during the service life of a recycling material or to material damage due to poor storage or processing.
In order to be able to determine the quality of the bitumen material examined in a simple manner, it is advantageous if the second code is compared with a second reference value. In this embodiment, therefore, the initial or reuse of the bitumen material can be made dependent on the first
Measure exceeds the first reference value and the second measure exceeds the second reference value.
In extensive experiments on the fluorescence of bitumen, it has been found that certain excitation wavelengths are particularly advantageous in order to determine the material property to be investigated, in particular the aging state, of the bitumen material. The first excitation wavelength of the first excitation radiation is preferably selected from a wavelength range between 260 and 280 nanometers. Upon excitation of the bitumen in said wavelength range, the global maximum of the fluorescence of the bitumen is obtained, the intensity of which can provide complementary information about the state of aging. However, the intensity of the observed emission can be greatly influenced by the measurement or sample structure, in particular with regard to photoscopes and distances. These influences can be problematic, especially with rough sample surfaces. The ratio of the intensities, however, is essentially independent of the measurement and sample geometry, provided the residual intensity is sufficient. In particular, it has been shown in studies that the ratio of the intensities of the different fluorescence maxima allows a reliable statement about the sought material property. Accordingly, the first excitation wavelength from the region of the global maximum of the fluorescence is particularly suitable for use as a reference for the age-related intensity decrease of the fluorescence, which is detectable at larger wavelengths of the excitation radiation.
According to a particularly preferred embodiment, it is provided that the second excitation wavelength of the second excitation radiation is selected from a wavelength range between 350 and 380 nanometers. Fluorescence analyzes have shown that the intensity of the fluorescence radiation has a local maximum or a spectral shoulder between 350 and 380 nanometers. Accordingly, the second excitation wavelength is selected from a local extremity of fluorescence at which the derivative function of the fluorescence signal is substantially zero. On the one hand, this embodiment has the advantage that the age-related deviation of the intensity of the fluorescence radiation in the region of the local maximum is particularly great. On the other hand, the measurement accuracy can be increased since the change of the fluorescence signal in the region of the local maximum is small.
Moreover, it is favorable if the third excitation wavelength of the third excitation radiation is selected from a wavelength range between 470 and 500 nanometers. The fluorescence spectrum of the bitumen material has a further local maximum in the stated wavelength range, so that it is particularly advantageous for the abovementioned reasons to determine the fluorescence upon excitation in this wavelength range.
In some cases it may be favorable if the intensity of a fourth fluorescence radiation is detected, which is excited with a substantially monochromatic fourth excitation radiation of a fourth excitation wavelength between 440 and 460 nm. In this area there is another spectral field of the fluorescence spectrum, which can be used for the evaluation of the material property. However, this local maximum is comparatively weak and therefore more susceptible to errors than the previously described local maxima of the fluorescence radiation.
Extensive investigations have shown that these ranges for the first and second excitation wavelengths are characteristic of certain fractions of the bitumen, so-called aromatics and resins, which have a significant influence on the structural and mechanical properties of bitumen. By examining the fluorescence upon excitation of the bitumen material with the preferred values of the first and second excitation wavelength, respectively, the frequency, resistance and chemical resistance to oxidation of the aromatics and resins can be determined. For this purpose, it is preferable to calculate the first and second indices from which the aging resistance of the investigated bitumen material can be estimated.
According to a preferred embodiment, the measuring wavelength range is substantially monochromatic with a measuring wavelength of between 390 and 650 nanometers, in particular substantially 525 nanometers. In this embodiment, advantageously, a maximum signal can be obtained.
The device according to the invention for determining a material property, in particular the aging state and / or aging resistance, of a bitumen material has at least the following components: a first radiation device for impinging the bitumen material with an essentially monochromatic first excitation radiation of a first excitation wavelength; a second radiation device for acting on the bitumen material with a substantially monochromatic second excitation radiation of a second excitation wavelength; a measuring device for measuring the intensity of a first fluorescence radiation excited by the first excitation radiation in a predetermined measuring wavelength range and for measuring the intensity of a second fluorescence radiation excited by the second excitation radiation in the predetermined measuring wavelength range; - A computing device with a first ratio images for determining a first index for the material property of the bitumen material from the ratio between the intensity of the second fluorescence radiation to the intensity of the first fluorescence radiation.
The device has the same advantages as the previously explained method, so that reference may be made to the above statements. It is essential for the invention that particularly simple radiation devices can be used, since the first characteristic for the material property, in particular the aging of the bitumen material, is determined from only two fluorescence signals, which are recorded at two discrete excitation wavelengths. In particular, it is not necessary for Demgegentiber to design the radiation, measuring or computing device such that an excitation spectrum is evaluated over a broad wavelength range of the excitation wavelength.
In order to identify the inappropriate for a first or reuse Bitu-menproben, the device for determining the material property of the bitumen material preferably also has the following components: - a third radiation means for applying the bitumen material having a substantially monochromatic third excitation radiation a third excitation wavelength, wherein the measuring device for measuring the intensity of a third fluorescence radiation excited by the third excitation radiation is set up in the predetermined measuring wavelength range; a second ratio pattern for determining a second characteristic for the material property of the bitumen material from the ratio between the intensity of the third fluorescence radiation to the intensity of the first fluorescence radiation.
In order to determine the usability of the bitumen material in a simple manner, it is advantageous if the computing device has a first database with a first reference value for the material property of the bitumen material and a first comparison module for comparing the first code with the first reference value, wherein the computing device Preferably, a second database having a second reference value for the material property of the bitumen material and a second comparison module for comparing the second ratio with the second reference value. If the first figure below the first reference value, the bitumen material according to a preferred
Application of the method of a first or re-use or recycling can be excluded. In addition, a use of the bitumen material is then not carried out without further measures, although the first ratio is above the first reference value, but the second ratio falls below the second reference value. Only when the first ratio exceeds the first reference value and the second ratio exceeds the second reference value does the used bitumen material have the material properties desired for use, so that the selection process can be substantially improved.
According to a particularly preferred embodiment, the first and second radiation means are different from each other, wherein the first radiation means is arranged to emit the substantially monochromatic first excitation radiation of the first excitation wavelength and the second radiation means is arranged to emit the substantially monochromatic excitation radiation of the second excitation wavelength.
For this purpose, it is favorable if the first radiation device is a first light-emitting diode for emitting the first excitation radiation at the first excitation wavelength and / or the second radiation device is a second light-emitting diode for emitting the second excitation radiation having the second excitation wavelength and / or the third radiation device is a second third light emitting diode for emitting the third excitation radiation having the third excitation wavelength. As an alternative to the light-emitting diodes, diode lasers can be used.
According to a further preferred embodiment, the first and second radiation device, if appropriate also the third radiation device, are formed by a common radiation device, which has a radiation source for emitting a broadband excitation radiation. In this embodiment, a device for selecting the first, second or third excitation wavelength is provided between the radiation source for the broadband excitation radiation and the bitumen material, which device is formed, for example, by a filter or a monomer.
In order to inform the user of the device about the material property, in particular the aging state, of the bitumen material, it is favorable if the device also has a display unit for displaying the first and / or the second characteristic number and / or the first reference value and / or the second reference value for the material property of the bitumen material. In the prior art, such display units, such as displays, are well known, so that further explanations on this can be dispensed with.
On the other hand, the object on which the invention is based is achieved by a method for determining a material property, in particular the aging state and / or the aging resistance of a bitumen material, with the following steps: applying a substantially monochromatic excitation light to the bitumen material; Measuring the intensity of a first fluorescence signal excited by the excitation light at a first emission wavelength; Measuring the intensity of a second fluorescence signal excited by the excitation light at a second emission wavelength; Determining a first characteristic for the material property of the bitumen material from the ratio between the intensity of the second fluorescence signal at the second emission wavelength to the intensity of the first fluorescence signal at the first emission wavelength.
In contrast to the embodiment of the invention described above, in this embodiment, individual or discrete intensity values of the emission spectrum (at a first and a different second emission wavelength) due to the excitation with a substantially monochromatic excitation light are used, the first characteristic number especially for the aging state of the bitumen material. Both embodiments of the invention have the advantage that the recording of a complete spectrum, namely the excitation spectrum in the first embodiment variant or the emission spectrum in the second embodiment variant of the invention, can be omitted since the material property , in particular the aging state or the resistance to aging, of the bitumen material can be reliably determined already from the individual measurement values of the fluorescence.
In order to reliably detect the aging-related deterioration of the material properties of the bitumen, the method described above can be performed by the further steps of measuring the intensity of a third fluorescence signal excited by the excitation light at a third emission wavelength; Determining a second characteristic for the material property of the bitumen from the ratio between the intensity of the third fluorescence signal at the third emission wavelength to the intensity of the first fluorescence signal at the first emission wavelength can be advantageously extended.
The device for determining a material property, in particular the aging state or aging resistance, of a bitumen material has, according to the alternative solution described above, at least the following components: a radiation unit for applying the bitumen material to a substantially monochromatic one excitation light; a measuring unit for measuring the intensity of a first fluorescence signal excited by the excitation light at a first emission wavelength and for measuring the intensity of a second fluorescence signal excited by the excitation light at a second emission wavelength; a calculation unit for determining a first characteristic for the material property of the bitumen material from the ratio between the intensity of the second fluorescence signal at the second emission wavelength to the intensity of the first fluorescence signal at the first emission wavelength.
The invention will be further explained below by means of a preferred embodiment, to which, however, it should not be restricted. In the drawing show:
Fig. 1 shows schematically an apparatus for determining the aging state of a bitumen material;
FIG. 2 shows a flowchart for illustrating an embodiment variant of the method according to the invention for determining the aging state of the bitumen material; FIG. and
3 shows the excitation spectra of each of an age-resistant and a non-aging-resistant bitumen sample.
In Fig. 1, a device 1 for determining the aging state of a bitumen material 2, i. a material containing the binder of bitumen. The bitumen material 2 is present in particular as an expansion asphalt whose aging resistance is to be investigated with regard to recycling.
The apparatus 1 has a first radiation device 3 for emitting a substantially monochromatic first excitation radiation 4 of a first excitation wavelength λΐ. In addition, the device 1 has a second radiation device 5 for emitting a substantially monochromatic second excitation radiation 6 of a second excitation wavelength λ2. Finally, the device 1 has a third radiation device 7 for emitting a substantially monochromatic third excitation radiation 8 of a third excitation wavelength λ3. The device 1 further comprises a conventional Lich known in the art per se measuring device 9, which is adapted to the intensity II of an excited by the first excitation radiation 4 in the bitumen material 2 first fluorescence radiation, the intensity 12 of a through the second excitation radiation 6 excited second fluorescence radiation and the intensity 13 of an excited by the third excitation radiation 8 second fluorescence radiation to measure. The fluorescence is in each case at the same, predetermined measuring or. Emission wavelength of, for example, 515 nanometers measured. For this purpose, the first radiation device 3, the second radiation device 5 and the third radiation device 7 are activated one after the other in the embodiment shown, wherein the measuring device 9 respectively detects the first fluorescence radiation 4, second fluorescence radiation 8 and third fluorescence radiation 8 emanating from the bitumen material , Alternatively to the activation of the first 3, second 5 and third radiation device 7 at a time interval from one another, changing filter sets or diaphragms can be used. In the illustrated embodiment, the first radiation device 3 is a first light-emitting diode 3 ', the second radiation device 5 is a second light-emitting diode 5' and the third radiation device 7 is a third light-emitting diode 7 '.
The individual components of the device 1 are known in the prior art (cf., for example, CA 2,833,299, US 2005/0253088 A1, US 4,330,207, WO 2010/048584, US Pat. No. 7,633,071 B2) in various designs, so that further explanations are unnecessary can.
As is also apparent from FIG. 1, the device 1 also has a computing device 10 with a first ratio image 11 for determining a first characteristic K1 for the aging state of the bitumen material from the ratio between the intensity 12 of the second fluorescence radiation to the intensity II of the first fluorescence radiation , In addition, the computing device 10 has a second ratio image 12 for determining a second characteristic number K2 for the aging state of the bi-tuminal material 2 from the ratio between the intensity 13 of the third fluorescence radiation to the intensity II of the first fluorescence radiation.
In order to prepare the decision on the reuse of the investigated bitumen material 2, the computing device 10 has a first database 13 with a first reference value R1 for the aging state of the bitumen material 2 and a first comparison module 14 for comparing the first code K1 with the first reference value R1 , In addition, the computing device 10 has a second database 15 with a second reference value R2 for the aging state of the bitumen material and a second comparison module 16 for comparing the second code with the second reference value. The first reference value R1 and the second reference value R2 are characteristic of age-resistant bitumen materials 2.
As can also be seen from FIG. 1, the device 1 additionally has a display unit 17 for displaying the first K1 and / or the second characteristic K2 and / or the first reference value R1 and / or the second reference value R1 for the aging state of the bitumen material 2.
The inventive method is apparent from the flowchart of FIG. After the start 18 of the method, the intensity II of the first fluorescence radiation, the intensity 12 of the second fluorescence radiation and the intensity 13 of the third fluorescence radiation are detected one after the other (panel 19). Thereafter, it is measured whether the intensity II of the first fluorescence radiation, the intensity 12 of the second fluorescence radiation and the intensity 13 of the third fluorescence radiation exceeds a threshold value Imin (field 20). If this is not the case, the fluorescence measurement is repeated (arrow 21). Otherwise, the first characteristic K1 is determined as the ratio between the intensity 12 of the second fluorescence radiation and the intensity II of the first fluorescence radiation (field 22). Thereafter, the first characteristic K1 is compared with the first reference value R1 (box 23). If the first characteristic K1 is smaller than the first reference value R1, the bitumen material 2 can be detected as unsuitable for recycling (box 24). If the first characteristic K1 is greater than the first reference value R1, a comparison is made between the second characteristic K2 and the second reference value R2 (field 25). If the second characteristic K2 falls below the second reference value R2, the bitumen material 2 is considered to be non-aging-resistant (box 26). Only if the second characteristic K2 is above the second reference value R2, the aging resistance of the investigated bitumen material 2 is assumed (box 27). Such samples are suitable for reuse. Field 28 indicates the end of the proceedings.
FIG. 3 shows a diagram with the excitation spectra 29, 30 of two bitumen samples 2, wherein the excitation spectrum 29 relates to an age-resistant bitumen sample and the excitation spectrum 30 to a non-age-resistant bitumen sample. The wavelength λ of the excitation radiation is plotted on the x axis, and the intensity I of the fluorescence is plotted on the y axis at a measurement wavelength of 515 nanometers (nm). It can be seen that the fluorescence of the aged bitumen sample is reduced at excitation wavelengths λ above the maximum at about 270 nm compared to the age resistant bitumen sample. In addition, the spectra have characteristic local maxima at about 370 nm and 480 nm.
On the basis of these findings, it is preferably provided that the first excitation wavelength λΐ of the first excitation radiation 4 from a wavelength range between 260 and 280 nm, in particular essentially 270 nm, the second excitation wavelength λ2 of the second excitation radiation 6 from a wavelength range between 350 and 380 nm, in particular substantially 370 nm, and the third excitation wavelength λ3 of the third excitation radiation 8 is selected from a wavelength range between 470 and 500 nm, in particular substantially 480 nm. As a result, the first excitation wavelength λΐ can be used as a reference for the intensity drop at larger excitation wavelengths 1.
The excitation in the region of the local maxima of the excitation spectrum is particularly advantageous for metrological reasons.
The inventive principle can also be realized in a (not shown) device having a radiation unit for applying the bitumen material having a substantially monochromatic excitation light of an excitation wavelength of, for example, 280 nm. This stimulates the bitumen material to fluoresce. This embodiment of the device 1 further comprises a measuring unit which is adapted to measure the intensity of the first fluorescence signal excited by the excitation light at a first emission wavelength and the intensity of a second fluorescence signal excited by the excitation light at a second emission wavelength. The apparatus further includes a calculating unit for determining a first ratio of the aged state of the bitumen material from the ratio between the intensity of the second fluorescence signal at the second emission wavelength to the intensity of the first fluorescence signal at the first emission wavelength. Accordingly, the second measure of the aging state of the bitumen may be formed from the ratio between the intensity of the third fluorescence signal at the third emission wavelength to the intensity of the first fluorescence signal at the first emission wavelength.
权利要求:
Claims (16)
[1]
claims:
1. A method for determining a material property, in particular the aging state or the aging resistance, of a bitumen material (2), comprising the steps of: - applying to the bitumen material (2) a substantially monochromatic first excitation radiation (4) of a first th excitation wavelength (λΐ); Measuring the intensity (II) of a first fluorescence radiation excited by the first excitation radiation (4) in a measuring wavelength range; - Applying the bitumen material (2) having a substantially monochromatic second excitation radiation (6) of a first excitation wavelength (λ2); - measuring the intensity (12) of a second fluorescence radiation excited by the second excitation radiation (6) in the measurement wavelength range; Determining a first characteristic number (K1) for the material property of the bitumen material (2) from the ratio between the intensity (12) of the second fluorescence radiation and the intensity (II) of the first fluorescence radiation.
[2]
2. The method according to claim 1, characterized in that the first characteristic number (K1) is compared with a first reference value (R1) for the material property of the bitumen material (2).
[3]
3. The method according to claim 1 or 2, characterized by the further steps - applying the bitumen material (2) with a substantially monochromatic third excitation radiation (8) of a third excitation wavelength (λ3); Measuring the intensity (13) of a third fluorescence radiation excited by the third excitation radiation (8) in the measurement wavelength range; - Determining a second index (K2) for the material property of the bitumen material (2) from the ratio between the intensity (13) of the third fluorescence radiation to the intensity (II) of the first fluorescence radiation.
[4]
4. The method according to any one of claims 1 to 3, characterized in that the second characteristic number (K2) is compared with a second reference value (R2).
[5]
5. The method according to any one of claims 1 to 4, characterized marked, characterized in that the first excitation wavelength (λΐ) of the first excitation radiation (4) is selected from a wavelength range between 260 and 280 nanometers.
[6]
6. The method according to any one of claims 1 to 5, characterized marked, characterized in that the second excitation wavelength (λ2) of the second excitation radiation (6) is selected from a wavelength range between 350 and 380 nanometers.
[7]
7. The method according to any one of claims 1 to 6, characterized marked, characterized in that the third excitation wavelength (λ3) of the third excitation radiation (8) is selected from a wavelength range between 470 and 500 nanometers.
[8]
8. The method according to any one of claims 1 to 6, characterized in that the measuring wavelength range is substantially monochromatic with a measuring wavelength between 390 and 650 nanometers, in particular substantially 525 nanometers.
[9]
9. Device (1) for determining a material property, in particular of the aging state or aging resistance, of a bitumen material (2), comprising: - a first radiation device (3) for acting on the bi-tumen material (2) with a substantially monochromatic first excitation radiation (4) a first excitation wavelength (λΐ); - A second radiation means (5) for acting on the bitumen material (2) having a substantially monochromatic second excitation radiation of a second excitation wavelength (λ2); a measuring device (9) for measuring the intensity (II) of a first fluorescence radiation excited by the first excitation radiation (4) in a predetermined measuring wavelength range and for measuring the intensity (12) of a second fluorescence radiation excited by the second excitation radiation (6) the predetermined measuring wavelength range; - A computing device (10) having a first ratio images (10) for determining a first characteristic number (Kl) for the Materi-aleigenschaft the bitumen material (2) from the ratio between the intensity (12) of the second fluorescence radiation to the intensity (II ) of the first fluorescence radiation.
[10]
10. Device (1) according to claim 9, characterized by - a third radiation means (7) for applying the bitumen material (2) with a substantially monochromatic third excitation radiation (8) a third excitation wavelength (λ3), wherein the measuring device (9 ) is arranged for measuring the intensity (13) of a third fluorescence radiation excited by the third excitation radiation (8) in the predetermined measuring wavelength range; - A second ratio images for determining a second characteristic (K2) for the material property of the bitumen material (2) from the ratio between the intensity (13) of the third fluorescence radiation to the intensity (II) of the first fluorescence radiation.
[11]
11. Device (1) according to claim 9 or 10, characterized marked, characterized in that the computing device (10) has a first database (13) with a first reference value (Rl) for the material property of the bitumen material (2) and a first comparison module (14) for comparing the first characteristic number (K1) with the first reference value (R1), wherein the computing device (10) preferably has a second database (15) with a second reference value (R2) for the material property of the bitumen material (2). and a second comparison module (16) for comparing the second characteristic number (K2) with the second reference value (R2).
[12]
12. Device (1) according to one of claims 9 to 11, characterized in that the first radiation device (3) has a first light-emitting diode (3 ') for emitting the first excitation radiation (4) with the first excitation wavelength (λΐ) and / or the second radiation device (5) has a second light-emitting diode (5 ') for emitting the second excitation radiation (6) with the second excitation wavelength (λ2) and / or the third radiation device (7) a third light-emitting diode (7') for emitting the third excitation radiation (8) with the third excitation wavelength (λ3).
[13]
13. Device (1) according to one of claims 9 to 12, characterized by a display unit (17) for displaying the first (Kl) and / or the second characteristic number (K2) and / or the first reference value (Rl) and / or the second reference value (K2) for the material property of the bitumen material (2).
[14]
14. A method for determining a material property, in particular the aging state or the aging resistance of a bitumen material (2), comprising the steps of: - subjecting the bitumen material (2) with a substantially monochromatic excitation light; Measuring the intensity of a first fluorescence signal excited by the excitation light at a first emission wavelength; Measuring the intensity of a second fluorescence signal excited by the excitation light at a second emission wavelength; - Determining a first index (Kl) for the material property of the bitumen material (2) from the ratio between the intensity of the second fluorescence signal at the second emis sion wavelength to the intensity of the first fluorescence signal at the first emission wavelength.
[15]
15. Method according to claim 14, characterized by the further steps - measuring the intensity of a third fluorescence signal excited by the excitation light at a third emission wavelength; - Determining a second characteristic (K2) for the material property of the bitumen from the ratio between the intensity of the third fluorescence signal at the third emission wavelength to the intensity of the first fluorescence signal at the first emission wavelength.
[16]
16. A device (1) for determining a material property, in particular the aging state or the aging resistance, of a bitumen material, comprising: - a radiation unit for acting on the bitumen material with a substantially monochromatic excitation light; a measuring unit for measuring the intensity of a first fluorescence signal excited by the excitation light at a first emission wavelength and for measuring the intensity of a second fluorescence signal excited by the excitation light at a second emission wavelength; a computation unit for determining a first characteristic for the material property of the bitumen material from the ratio between the intensity of the second fluorescence signal at the second emission wavelength to the intensity of the first fluorescence signal at the first emission wavelength.
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同族专利:
公开号 | 公开日
AT517366B1|2017-07-15|
WO2016205847A1|2016-12-29|
US10527547B2|2020-01-07|
EP3311141A1|2018-04-25|
CA2990022A1|2016-12-29|
US20180188174A1|2018-07-05|
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法律状态:
优先权:
申请号 | 申请日 | 专利标题
ATA50522/2015A|AT517366B1|2015-06-22|2015-06-22|Method and device for determining a material property of a bitumen material|ATA50522/2015A| AT517366B1|2015-06-22|2015-06-22|Method and device for determining a material property of a bitumen material|
US15/739,123| US10527547B2|2015-06-22|2016-06-22|Method and device for determining a material property of a bitumen material|
EP16740932.5A| EP3311141A1|2015-06-22|2016-06-22|Method and device for determining a material property of a bitumen material|
CA2990022A| CA2990022A1|2015-06-22|2016-06-22|Method and device for determining a material property of a bitumen material|
PCT/AT2016/050219| WO2016205847A1|2015-06-22|2016-06-22|Method and device for determining a material property of a bitumen material|
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