CN104280378A - Method for detecting content of SBS (Styrene Butadiene Styrene) modifier in modified asphalt - Google Patents
Method for detecting content of SBS (Styrene Butadiene Styrene) modifier in modified asphalt Download PDFInfo
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- CN104280378A CN104280378A CN201410524720.8A CN201410524720A CN104280378A CN 104280378 A CN104280378 A CN 104280378A CN 201410524720 A CN201410524720 A CN 201410524720A CN 104280378 A CN104280378 A CN 104280378A
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Abstract
The invention provides a method for detecting content of an SBS (Styrene Butadiene Styrene) modifier in modified asphalt. The method mainly comprises the following steps: taking multiple modified asphalt standard samples of which the content of SBS modifiers is known, and acquiring the Raman spectrum of each modified asphalt standard sample by utilizing a Raman spectrometer; performing linear fitting on a relative ratio between a Raman characteristic peak which only belongs to SBS and a Raman characteristic peak which only belongs to matrix asphalt in each modified asphalt standard sample, thereby obtaining a standard curve; and performing a Raman spectrum test on a to-be-detected SBS modified asphalt sample, and calculating the content of the SBS modifier in the modified asphalt according to the measured relative ratio between the Raman characteristic peak which only belongs to SBS and the Raman characteristic peak which only belongs to matrix asphalt. The sample preparation process of the method is simple, and the measurement method is convenient and rapid, can be widely applied to detecting the contents of various SBS asphalt modifiers in a construction site environment and has positive significance in controlling the quality of the SBS modified asphalt and guaranteeing the road surface durability.
Description
Technical field
The present invention relates to a kind of detection method, particularly a kind of method utilizing Raman spectrum to detect SBS modifier content in modified bitumen.
Background technology
Bituminous pavement is widely adopted in countries in the world.In the high-grade highway of China, bituminous pavement proportion is more than 80%.But also clearly, such as high temperature easily trickles the shortcoming of bituminous pavement, and low temperature is easy to crack.In recent years, using SBS as the modified bitumen of modifier with its height excellent preferably, warm nature energy and outstanding elastic recovery capability, the usability on road surface can be improved comprehensively, increase substantially the serviceable life of road.SBS is the segmented copolymer of styrene and butadiene, belongs to hot attribute rubber.Add in heated bitumen by a certain amount of SBS, under uniform temperature and mechanical shear stress effect, form homogeneous mixture with pitch, this mixture is SBS modified bitumen.The petroleum chemical enterprise of current China can in a large number production SBS modifier, is just day by day widely used at present in China Higher level highway and other pavement of road engineering.
The content of SBS modifier is the important indicator affecting SBS Pavement Performance of Modified Asphalt.In common content range, the pavement performance of SBS modified bitumen improves with the increase of SBS modifier content.Although applying unit has respective requirement to the content of SBS modifier in SBS modified bitumen, because SBS is expensive, supplier, in order to reduce costs, often practises fraud in process of production, adds non-effective modifier component.At present for the content of SBS in SBS modified bitumen, can measure by having the instrument such as infrared spectrum, nuclear magnetic resonance; But these instrument and equipments are not only expensive, and be also not suitable for promoting the use of at the construction field (site).In order to carry out effective quality management and monitoring to SBS Modified Bitumen Pavement engineering, need a kind of method of inspection quick and precisely analyzing SBS modifier content in SBS modified bitumen.
The method using Raman spectrum to carry out material composition detection was found in nineteen twenty-eight, but after fairly large application occurs in the eighties in last century, popularized with the universal of laser instrument.The same with infrared absorption spectrum, Raman spectrum is also utilize vibrational spectrum technology to carry out sizing to sample to analyze, and the mechanism of quantitative test is based on Beer law.But, with infrared absorption spectrum unlike, Raman spectrum can use the better laser of beam quality to analyze, and substantially not by the impact of wavelength, requires simpler to the preparation of sample.
But the SBS content directly using Raman spectrum to detect in SBS modified bitumen is very difficult, this is because the Raman signal of SBS modifier is much smaller than background fluorescence, the Raman signal of SBS modifier is caused to be disturbed by background fluorescence and cannot Measurement accuracy.
Summary of the invention
The object of the present invention is to provide a kind of detection method that can realize raman spectral signal and amplify, utilize this Raman spectrum to measure the carrying out of SBS modifier content in modified bitumen.Wherein utilize Raman spectroscopy, measure the Raman spectrum of SBS modified bitumen, according to the area ratio of characteristic peak spectrally only belonging to SBS and matrix pitch respectively, namely wave number is at 996cm
-1and 1601cm
-1the ratio of two peak areas, measure the percentage composition of modifier in SBS modified bitumen.
In order to achieve the above object and other objects, the present invention adopts following technical scheme: the detection method of SBS modifier content in a kind of modified bitumen, and it comprises step:
1) substrate using artificial metal micro-nano structure as test;
2) by a certain amount of SBS modified bitumen sample dissolution to be measured in the organic solvent of predetermined volumes;
3) dissolution homogeneity being dissolved with SBS modified bitumen sample to be measured is coated on the surface of substrate;
4) Raman spectrometer is adopted to measure the Raman spectrum of SBS modified bitumen sample to be measured on substrate;
5) calculate in the Raman spectrogram of SBS modified bitumen sample to be measured, the relative ratio of the raman characteristic peak of SBS modifier and the raman characteristic peak of matrix pitch;
6) comparing, to determine the content of SBS modifier in SBS modified bitumen sample to be measured by this relative ratio and typical curve.
Wherein, the raman characteristic peak of described SBS modifier, the Raman scattering peak that the wagging vibration belonging to alkene two sections of C-H bond in SBS causes; The raman characteristic peak of described matrix pitch, belongs to the Raman scattering peak that in matrix pitch, carbon-carbon double bond vibration and phenyl ring skeletal vibration cause.
Wherein, described artificial metal micro-nano structure has Raman scattering enhancing function.
Wherein, the raman characteristic peak of described artificial metal micro-nano structure on Raman spectrogram is not overlapping with the raman characteristic peak of SBS modifier and matrix pitch.
Wherein, described artificial metal micro-nano structure comprises the micro-nano structures such as metal photonic crystal, metal nano monomer, metal nano dimer or metal nanoparticle array.
Wherein, described organic solvent can dissolve SBS modifier and pitch.
Wherein, the raman characteristic peak on the Raman spectrogram of described organic solvent is not overlapping with the raman characteristic peak of SBS and matrix pitch.
Wherein, described organic solvent is combination or wherein any one of chloroform, phenixin, methylene chloride, triclene or acetone.
The foundation of the typical curve of SBS modified bitumen standard model and SBS modifier content in the present invention
1) get have Raman scattering increase powerful artificial metal micro-nano structure as test substrate;
2) the SBS modified bitumen standard model getting known SBS modifier content is dissolved in organic solvent, is coated on the surface of substrate by the dissolution homogeneity being dissolved with SBS modified bitumen standard model;
3) use Raman spectrometer at 300-2000cm
-1the Raman spectrum of SBS modified bitumen standard model on substrate is measured in scope;
4) by the Raman spectrum of the SBS modified bitumen standard model of the multiple different SBS modifier content of above-mentioned steps replicate determination, calculate the relative ratio of the peak area of the raman characteristic peak only belonging to SBS in each standard model Raman spectrum and the raman characteristic peak only belonging to matrix pitch respectively, and using this relative ratio as ordinate, using the SBS modifier content of each standard model as horizontal ordinate record numerical value, by linear fit, obtain typical curve;
To preparation and the SBS modifier assay of SBS modified bitumen sample to be measured
1) get have Raman scattering increase powerful artificial metal micro-nano structure as test substrate;
2) by SBS modified bitumen sample dissolution to be measured in organic solvent, above-mentioned dissolution homogeneity is coated on the surface of substrate;
3) use Raman spectrometer at 300-2000cm
-1the Raman spectrum of SBS modified bitumen sample to be measured on substrate is measured in scope;
4) relative ratio of the raman characteristic peak Raman spectrogram calculating SBS modified bitumen sample to be measured being only attributed to SBS and the peak area of the raman characteristic peak only belonging to matrix pitch, then compare with typical curve, to determine the content of SBS modifier in SBS modified bitumen sample to be measured.
Described SBS modified bitumen standard model configuration, with the SBS modified bitumen standard model of known SBS modifier content, or takes SBS and matrix pitch and is jointly dissolved in organic solvent and calculates SBS modifier content as SBS modified bitumen standard model.In described SBS modified bitumen standard specimen, in SBS modified bitumen standard specimen, the percentage by weight of SBS modifier is 0.8%-8%.
Accompanying drawing explanation
Fig. 1 to be known SBS modifier content be 3.5%, 4.5%, 6.5% SBS modified bitumen Raman spectrogram.
Fig. 2 is the typical curve drawn according to SBS modified bitumen standard model test result.
Fig. 3 is the Raman spectrogram of SBS modified bitumen sample to be measured.
Embodiment
For the ease of understanding the present invention, below in conjunction with accompanying drawing, embodiments of the invention being described, it will be appreciated by those skilled in the art that following explanation is just for the ease of making an explanation to invention, and not as the concrete restriction to its scope.
Adopt the content of Raman spectrometer to SBS modifier to detect in the present invention, described Raman spectrometer is can carry out the normal instrument measured to asphalt sample, preferably adopts Horiba JY HR800 Raman spectrometer in the present invention.Because Raman signal is much smaller than background fluorescence, realize the amplification to Raman signal, eliminate the impact of background fluorescence, in the present invention, test sample is placed in artificial metal micro-nano structure, this artificial metal micro-nano structure can realize the enhancing to Raman signal, in this artificial metal micro-nano structure, the Raman signal recorded can strengthen 5 to 6 orders of magnitude, and the Raman signal recorded can meet the demand of measurement completely.
First, the standard criterion of SBS modified bitumen standard model and SBS modifier content is set up.Obtain the design asphalt sample of different SBS modifier content, in order to ensure the accuracy measured, choose some design asphalt samples, the sample of preferred employing more than 5 or more than 10, further, in the SBS modified bitumen standard model of known SBS modifier content, the sample that the percentage by weight choosing SBS modifier and matrix pitch is respectively 1%, 2%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6.5%, 7%, 8% is tested.Choose have Raman scattering increase powerful artificial metal micro-nano structure as test substrate, preferably this artificial metal micro-nano structure is metal photonic crystal, metal nano monomer, metal nano dimer or metal nanoparticle array etc.; Get a certain amount of SBS modified bitumen standard model, preferably this SBS modified bitumen standard model is 0.5 gram or other arbitrary selected amount, SBS modifier content in this SBS modified bitumen standard model is known, this SBS modified bitumen standard model of 0.5 gram is dissolved in the solvent of predetermined volumes, preferably this solvent be organic solvent further this organic solvent be combination or wherein any one of chloroform, phenixin, methylene chloride, triclene or acetone; Then, the dissolution homogeneity being dissolved with SBS modified bitumen standard model is coated on the surface of above-mentioned substrate; Adopt Raman spectrometer at 300-2000cm
-1the Raman spectrum of SBS modified bitumen standard model on substrate surface is measured in scope; By the Raman spectrum of the modified bitumen standard model of the multiple different SBS modifier content of above-mentioned steps replicate determination.
SBS modifier content is as shown in Figure 1 the Raman spectrum of the SBS modified bitumen standard model of 3.5%, 4.5%, 6.5%, and in the Raman spectrum described in Fig. 1, the peak position of the raman characteristic peak of SBS modifier is 996cm
-1, the Raman scattering peak that its wagging vibration belonging to alkene two sections of C-H bond in SBS causes; The peak position only belonging to the raman characteristic peak of matrix pitch is 1601cm
-1, it belongs to the Raman scattering peak that in matrix pitch, carbon-carbon double bond vibration and phenyl ring skeletal vibration cause; In the Raman spectrogram of any one SBS modified bitumen standard model, above-mentioned two peak areas are directly proportional to the constituent concentration belonged to separately; Get the ratio between above-mentioned two peak areas, and do 5 parallel testings and get mathematical mean, namely obtain typical ratio.Content as selected in Fig. 1 is the SBS modified bitumen standard model of 3.5%, 4.5%, 6.5%, by the ratio between the area that calculates two characteristic peaks, thus to obtain SBS modifier content be in the Raman spectrum of SBS modified bitumen standard model of 3.5%, 4.5%, 6.5%, the raman characteristic peak only belonging to SBS is respectively 0.011,0.014,0.020 with the typical ratio of the peak area of the raman characteristic peak only belonging to matrix pitch.
In addition, SBS modified bitumen standard model is in the above-described embodiment the standard model of known SBS modifier content, as further embodiment, by accurately taking the proportions standard model of SBS and matrix pitch, repeat by measuring some standard models configuring ratio detection and the calculating that above-mentioned step carries out Raman spectrum.
As shown in Figure 2, according to SBS modified bitumen standard model test result, with SBS modifier content for horizontal ordinate, with 996cm
-1peak area and 1601cm
-1ratio between peak area is ordinate, by linear fit, obtains typical curve, by at least two samples, be preferably 3, or 5 or 10 or the test result of more Multi-example, obtain the corresponding relation figure of ratio between SBS modifier content and the characteristic peak area of Raman spectrum.
Secondly, testing sample is detected.
Choose have Raman scattering increase powerful artificial metal micro-nano structure as test substrate; A certain amount of SBS modified bitumen sample to be measured is dissolved in organic solvent completely, preferred SBS modified bitumen sample to be measured is 0.1 gram or 0.5 gram or other arbitrary selected amount, be preferably the combination for chloroform, phenixin, methylene chloride, triclene or acetone or wherein any one, the dissolution homogeneity being dissolved with SBS modified bitumen sample to be measured is coated on the surface of substrate; Test the Raman spectrum of SBS modified bitumen sample to be measured over the substrate surface with Raman spectrometer, Fig. 3 illustrates at 300-2000cm
-1raman spectrum through on average obtaining after 5 tests in scope; 996cm in calculated Raman spectrum
-1place and 1601cm
-1the relative ratio of place's peak area is 0.017; The typical curve drawn with Fig. 2 is compared, then in testing sample, SB5 modifier content is 5.6%, thus realizes by the quantitative detection of Raman spectrum to SBS modifier in SBS modified bitumen.
Be understandable that, although the present invention with preferred embodiment disclose as above, but above-described embodiment and be not used to limit the present invention.For any those of ordinary skill in the art, do not departing under technical solution of the present invention ambit, the technology contents of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or be revised as the Equivalent embodiments of equivalent variations.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent variations and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (8)
1. the detection method of SBS modifier content in modified bitumen, it comprises step:
1) substrate using artificial metal micro-nano structure as test;
2) by a certain amount of SBS modified bitumen sample dissolution to be measured in the organic solvent of predetermined volumes;
3) dissolution homogeneity being dissolved with SBS modified bitumen sample to be measured is coated on the surface of substrate;
4) Raman spectrometer is adopted to measure the Raman spectrum of SBS modified bitumen sample to be measured on substrate;
5) calculate in the Raman spectrogram of SBS modified bitumen sample to be measured, the relative ratio of the raman characteristic peak of SBS modifier and the raman characteristic peak of matrix pitch;
6) comparing, to determine the content of SBS modifier in SBS modified bitumen sample to be measured by this relative ratio and typical curve.
2. the detection method of SBS modifier content in a kind of modified bitumen as claimed in claim 1, is characterized in that: the raman characteristic peak of described SBS modifier, the Raman scattering peak that the wagging vibration belonging to alkene two sections of C-H bond in SBS causes; The raman characteristic peak of described matrix pitch, belongs to the Raman scattering peak that in matrix pitch, carbon-carbon double bond vibration and phenyl ring skeletal vibration cause.
3. the detection method of SBS modifier content in a kind of modified bitumen as claimed in claim 1, is characterized in that: described artificial metal micro-nano structure has Raman scattering and strengthens function.
4. the detection method of SBS modifier content in a kind of modified bitumen as claimed in claim 1, is characterized in that: the raman characteristic peak of described artificial metal micro-nano structure on Raman spectrogram is not overlapping with the raman characteristic peak of SBS modifier and matrix pitch.
5. the detection method of SBS modifier content in a kind of modified bitumen as claimed in claim 1, is characterized in that: described artificial metal micro-nano structure comprises the micro-nano structures such as metal photonic crystal, metal nano monomer, metal nano dimer or metal nanoparticle array.
6. the detection method of SBS modifier content in a kind of modified bitumen as claimed in claim 1, is characterized in that: described organic solvent can dissolve SBS modifier and pitch.
7. the detection method of SBS modifier content in a kind of modified bitumen as claimed in claim 1, is characterized in that: the raman characteristic peak on the Raman spectrogram of described organic solvent is not overlapping with the raman characteristic peak of SBS and matrix pitch.
8. the detection method of SBS modifier content in a kind of modified bitumen as claimed in claim 1, is characterized in that: described organic solvent is combination or wherein any one of chloroform, phenixin, methylene chloride, triclene or acetone.
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| CN110779906A (en) * | 2019-11-26 | 2020-02-11 | 清华大学 | Quantitative analysis method for trace substance based on enhanced Raman scattering relative intensity external standard method |
| CN114280027A (en) * | 2021-12-28 | 2022-04-05 | 招商局重庆交通科研设计院有限公司 | Evaluation method for aging state of recycled asphalt |
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Application publication date: 20150114 |