CN111965132A - Rapid identification method for matrix asphalt brand based on ATR-FTIR and GPC - Google Patents

Rapid identification method for matrix asphalt brand based on ATR-FTIR and GPC Download PDF

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CN111965132A
CN111965132A CN202010647681.6A CN202010647681A CN111965132A CN 111965132 A CN111965132 A CN 111965132A CN 202010647681 A CN202010647681 A CN 202010647681A CN 111965132 A CN111965132 A CN 111965132A
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asphalt
sample
brand
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李晶
王珊珊
孟菲
朱昭荣
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Guangxi University
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3577Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N2021/1734Sequential different kinds of measurements; Combining two or more methods
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N2021/3595Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR

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Abstract

The invention provides a rapid identification method for a matrix asphalt brand based on ATR-FTIR and GPC, belongs to the field of asphalt test detection, and is characterized in that an infrared fingerprint interval and macromolecular LMS content errors and differences of asphalt are determined by an attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) method and a Gel Permeation Chromatography (GPC) method, an asphalt brand identification flow is established, and the type of asphalt is accurately identified. The method of the invention identifies the types of the aged asphalt by analyzing and identifying the asphalt after short-term aging.

Description

Rapid identification method for matrix asphalt brand based on ATR-FTIR and GPC
Technical Field
The invention belongs to the field of asphalt test detection, and particularly relates to a rapid identification method for a matrix asphalt brand based on ATR-FTIR and GPC.
Background
The petroleum asphalt is widely applied to highway construction, the quality of the petroleum asphalt directly affects the quality of a pavement, and the asphalt provided in the current market has the phenomenon of counterfeiting and faking. However, the quality of the asphalt is generally evaluated by adopting a macroscopic means at present, and because the composition of the asphalt is complex and the structure is complex, the use of the macroscopic means for identifying the quality of the asphalt is time-consuming and labor-consuming, and is influenced by some modifiers, and the evaluation of the asphalt property by only using the macroscopic means is not comprehensive. Therefore, some microscopic analysis means needs to be found to achieve the effect of rapidly identifying the asphalt quality.
Attenuated total reflectance fourier spectroscopy (ATR-FTIR) is commonly used for qualitative or quantitative analysis of compound structures. The functional groups contained in the compounds are detected by infrared spectroscopy to find the specific structure contained in each compound. At present, the ATR-FTIR method is widely applied to the research of the modification of asphalt and the aging of a binder thereof, and is rarely applied to the analysis of the microstructure of the asphalt. The invention discloses a Chinese patent application with publication number CN 108072626A, and discloses an asphalt brand identification method, which is based on Fourier transform attenuated total reflection infrared spectroscopy and a multi-dimensional scale analysis method, and combines various infrared spectrum data preprocessing methods such as wavelength selection, background subtraction, baseline correction, logarithmic unit variance processing, abnormal data identification and elimination, and can be used for identifying asphalt with stable quality or different types of matrix asphalt of the same brand in a classified manner.
Gel Permeation Chromatography (GPC) separates solute molecules of different sizes by their permeability differences in gels, with the Large Molecules (LMS) flowing out first, followed by medium and small molecules, depending on the size of the gel pores. GPC is currently used to evaluate the properties of asphalt, and GPC is rarely used to identify asphalt brands.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for rapidly identifying a matrix asphalt brand based on ATR-FTIR and GPC, which determines a fingerprint interval and macromolecular LMS content errors and differences of asphalt by attenuated total reflection Fourier transform infrared spectroscopy ATR-FTIR and gel permeation chromatography GPC, establishes an asphalt brand identification process and accurately identifies the type of asphalt.
Therefore, the technical scheme provided by the invention is as follows:
a method for rapidly identifying a matrix asphalt brand based on ATR-FTIR and GPC comprises the following steps:
(1) preparing asphalt samples of different brands into short-term aged asphalt standard samples;
(2) measuring an infrared spectrogram of an asphalt standard sample;
(3) measuring a gel permeation chromatogram of the asphalt standard sample;
(4) preparing a brand asphalt sample to be detected into short-term aged blind sample asphalt, and determining an infrared spectrogram and a gel permeation chromatogram of the blind sample asphalt;
(5) matching the infrared spectrogram of the blind sample asphalt with the infrared spectrogram of an asphalt standard sample; firstly, importing an asphalt standard sample infrared spectrogram into software, establishing an atlas database in which the asphalt standard sample infrared spectrogram and an asphalt standard sample brand are in one-to-one correspondence, and identifying the infrared spectrogram corresponding to the blind sample asphalt brand by using information of the atlas database;
when the similarity between the searched blind sample asphalt infrared spectrogram and the infrared spectrogram in the spectrogram library is 99-100%, namely the matching is successful, and the brand of the blind sample asphalt is the brand corresponding to the successfully matched infrared spectrogram;
when the similarity between the searched blind sample asphalt infrared spectrogram and the infrared spectrogram in the spectrogram library is lower than 99 percent, the matching is unsuccessful;
(6) verifying the successfully matched blind sample asphalt by using a gel permeation chromatogram, and further identifying the unsuccessfully matched blind sample asphalt by using the gel permeation chromatogram; specifically, the macromolecular content of the asphalt standard sample is calculated by a gel permeation chromatogram of the asphalt standard sample, then the macromolecular content of the blind sample asphalt is calculated by the same method, the comparison is carried out as follows,
for the blind sample asphalt successfully matched in the step (5): when the calculated macromolecule content of the blind sample asphalt falls into the macromolecule content range of the asphalt standard sample, the identification result in the step (5) is correct; when the calculated macromolecule content of the blind sample asphalt does not fall into the range of the macromolecule content of the asphalt standard sample, indicating that the identification result in the step (5) is incorrect, and performing the step (5) again for matching;
for blind pitch that did not match successfully in step (5): when the calculated macromolecular content of the blind sample asphalt falls into the macromolecular content range of the corresponding brand asphalt standard sample, indicating that the blind sample asphalt brand is the brand corresponding to the falling asphalt standard sample; and (5) when the calculated macromolecule content of the blind sample asphalt does not fall into the macromolecule content range of the asphalt standard sample, confirming that the matching is unsuccessful again, and performing the methods in the steps (5) and (6) again for matching again.
Further, the establishment of the map library in the step (5) is to utilize OMNIC 9.2 software to add the infrared spectrogram of the asphalt standard sample into the newly-established asphalt map library and correspond to the brand of the asphalt standard sample one by one; the establishment of the map library is as follows: firstly, establishing a corresponding retrieval spectrogram library by using a 'spectrogram library management' option in OMNIC software; and then, importing the infrared spectrogram of asphalt standard samples of IS, SK, DH and other brands into OMNIC software, and sequentially adding the infrared spectrogram into a newly-built infrared spectrogram library by utilizing a spectrogram adding and storing option of the software.
Further, the short term aging is: and respectively putting the asphalt standard sample or the blind sample asphalt into an oven with the temperature of 163 +/-0.5 ℃ to be heated for 75-85 min.
Further, the method for measuring the infrared spectrogram comprises the following steps: respectively heating standard pitch or blind pitch to 70-75 deg.C, uniformly coating the heated pitch on ATR wafer, performing infrared spectrum test, and selecting pitch with resolution of 4cm-1The number of scans was 32.
Further, in the step (6), the key peak selected from the infrared spectrogram in matching is 876cm-1、810cm-1And 744cm-1,722cm-1. Wherein the key peak is 876cm-1、810cm-1And 744cm-1Is a characteristic absorption peak of disubstituted benzene ring, 722cm-1Is (-CH)2-)n(n.gtoreq.4) characteristic absorption peak of substituent.
Further, the determination method of the gel permeation chromatogram comprises the following steps: tetrahydrofuran was used to dissolve pitch standards or blind pitch, respectively, and after dissolution the solution was injected into a chromatographic column and tested through a 0.2mm filter, set to a sample size of 20 μ L.
Further, in the step (7), the calculation method of the macromolecular content is as follows: the gel permeation chromatogram was divided into 13 parts on average, the starting end and knotThe beam ends are respectively counted by 5 percent of the highest signal intensity, the first 5 parts are taken as the areas where the macromolecules are located, and the areas are calculated according to a formula
Figure BDA0002573734000000031
Calculating the macromolecular content of the asphalt.
The invention has the following beneficial effects:
(1) the invention determines the fingerprint interval and macromolecular LMS content error and difference of the asphalt by an attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR) method and a Gel Permeation Chromatography (GPC) method, establishes a standard asphalt brand identification process and an operation method, and accurately identifies the type of the asphalt by analyzing and identifying the asphalt aged for a short time.
(2) The invention respectively determines the fingerprint intervals, LMS content errors and differences of different brands of asphalt by using ATR-FTIR and GPC, and ensures high-quality inspection results and accuracy.
(3) The invention utilizes GPC to assist ATR-FTIR to identify the types of the matrix asphalt and identifies different types of asphalt from molecular level, and has the advantages of rapidness and accuracy.
Drawings
FIG. 1 is a chart of macromolecular content of seven brands of asphalt standards according to the example of the present invention.
FIG. 2 IS a gel permeation chromatogram of IS brand blinded asphalt of example 1 of the present invention.
FIG. 3 IS a gel permeation chromatogram of IS brand blinded asphalt of example 2 of the present invention.
FIG. 4 is a chart of the infrared spectra of asphalt standards of brands FL and SL according to the invention.
FIG. 5 is a gel permeation chromatogram of a blind sample pitch of example 3 of the present invention.
FIG. 6 is a gel permeation chromatogram of a blind sample pitch of example 4 of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
Example 1
A method for rapidly identifying a matrix asphalt brand based on ATR-FTIR and GPC comprises the following steps:
1. preparing asphalt standard sample data
(1) Respectively sampling 35 +/-0.5 g of asphalt samples of the brands SK, IS, Shell, SL, DH, FL and GS, putting the samples into an oven at the temperature of 163 +/-0.5 ℃ for heating for 75min, and respectively preparing short-term aged asphalt standard samples;
(2) measuring an infrared spectrogram of an asphalt standard sample: heating the asphalt standard sample to 70 ℃, then uniformly coating the heated asphalt standard sample on an ATR wafer, performing infrared spectrum test, and selecting the sample with the resolution of 4cm-1The number of scanning times is 32;
(3) determining a gel permeation chromatogram of the asphalt standard sample: dissolving 30g of asphalt standard sample by using tetrahydrofuran, injecting the solution into a chromatographic column after dissolution, and testing through a 0.2mm filter, wherein the sample injection amount is set to be 20 mu L;
dividing the gel permeation chromatogram into 13 parts, respectively counting the initial end and the ending end by 5% of the highest signal intensity, taking the first 5 parts as the region where the macromolecule is located, and calculating the average value according to a formula
Figure BDA0002573734000000041
Calculating the macromolecular content of the asphalt standard sample to obtain the macromolecular content of the asphalt standard sample as shown in figure 1;
FIG. 1 is a graph of macromolecular content of seven branded asphalt standards; as can be seen from FIG. 1, the difference between the LMS content of each brand of asphalt after short-term aging is about 1.0%, that is, the LMS content is about 1.0%
Figure BDA0002573734000000042
As can be seen from FIG. 1, the LMS range after short-term aging of SK-brand asphalt IS 5.9-7.9%, the LMS range after short-term aging of IS-brand asphalt IS 7.0-9.0%, the LMS range after short-term aging of Shell-brand asphalt IS 8.0-10.0%, the LMS range after short-term aging of SL-brand asphalt IS 8.3-10.3%, the LMS range after short-term aging of DH-brand asphalt IS 9.5-11.5%, the LMS range after short-term aging of FL-brand asphalt IS 9.7-11.7%, and the LMS range after short-term aging of GS-brand asphalt IS 9.7-11.7The LMS range after aging is 9.5-11.5%;
2. preparation of blind sample asphalt data
(4) Sampling 35 +/-0.5 g of brand asphalt sample to be tested, and putting the sample into a drying oven with the temperature of 163 +/-0.5 ℃ for heating for 75min to prepare short-term aging blind sample asphalt; determining an infrared spectrogram and a gel permeation chromatogram of the blind sample asphalt;
infrared spectrum of blind sample pitch: respectively heating asphalt standard sample or blind sample asphalt to 70 deg.C, uniformly coating the heated asphalt on ATR wafer, performing infrared spectrum test, and selecting asphalt with resolution of 4cm-1The number of scanning times is 32;
gel permeation chromatogram of blind bitumen: dissolving 30g of blind sample asphalt by using tetrahydrofuran, injecting the solution into a chromatographic column after dissolution, and testing through a 0.2mm filter, wherein the sample injection amount is set to be 20 mu L; the obtained gel permeation chromatogram is shown in FIG. 2;
3. matching and verification
(5) Matching the infrared spectrogram of the blind sample asphalt with the infrared spectrogram of an asphalt standard sample; firstly, importing an asphalt standard sample infrared spectrogram into software, establishing an atlas database in which the asphalt standard sample infrared spectrogram and an asphalt standard sample brand are in one-to-one correspondence, identifying the infrared spectrogram corresponding to the blind sample asphalt brand by utilizing information of the atlas database, and selecting a key peak of 876cm-1、810cm-1And 744cm-1,722cm-1When the similarity between the searched blind sample asphalt infrared spectrogram and the infrared spectrogram in the spectrogram library is 99-100%, the matching is successful; matching the blind sample asphalt in the embodiment with an asphalt standard sample infrared spectrogram through an infrared spectrogram to obtain the asphalt standard sample with the best matching brand of IS;
(6) verifying the successfully matched blind sample asphalt by using a gel permeation chromatogram;
calculating the macromolecular content of the blind sample asphalt by using the same method of asphalt standard samples, wherein FIG. 2 is a gel permeation chromatogram of the blind sample asphalt in the embodiment, and the LMS content of the blind sample asphalt is calculated to be 8.7% through the gel permeation chromatogram;
LMS of blind bitumen was compared to LMS of bitumen standards:
in the embodiment, the blind sample asphalt IS matched through the infrared spectrogram in the step (5) to obtain the best match of the blind sample asphalt as the IS brand, the LMS of the blind sample asphalt IS calculated to be 8.7%, the LMS of the blind sample asphalt just falls within the LMS range of 7.0-9.0% of the IS brand asphalt standard sample, the brand IS the same as the matching result of the infrared spectrogram, the brand IS also the same as the actual brand, the identification IS correct, and the identification result in the step (5) IS correct.
Example 2
A method for rapidly identifying a matrix asphalt brand based on ATR-FTIR and GPC comprises the following steps:
1. preparation of asphalt Standard sample data in accordance with example 1
2. Preparation of blind sample asphalt data
(4) Sampling 35 +/-0.5 g of brand asphalt sample to be tested, putting the sample into a drying oven with the temperature of 163 +/-0.5 ℃ and heating for 85min to prepare short-term aging blind sample asphalt; the infrared spectrum and gel permeation chromatogram of the blind sample asphalt were determined according to the method of example 1, wherein the obtained gel permeation chromatogram is shown in FIG. 3:
3. matching and verification
(5) Matching the infrared spectrogram of the blind sample asphalt with the infrared spectrogram of an asphalt standard sample; firstly, importing an asphalt standard sample infrared spectrogram into software, establishing an atlas database in which the asphalt standard sample infrared spectrogram and an asphalt standard sample brand are in one-to-one correspondence, identifying the infrared spectrogram corresponding to the blind sample asphalt brand by utilizing information of the atlas database, and selecting a key peak of 876cm-1、810cm-1And 744cm-1,722cm-1When the similarity between the searched blind sample asphalt infrared spectrogram and the infrared spectrogram in the spectrogram library is 99-100%, the matching is successful;
the blind sample asphalt in the embodiment is matched with the asphalt standard sample infrared spectrogram through the infrared spectrogram, so that brands FL and SL with the matching similarity of 99-100% are obtained; the infrared spectrogram of the asphalt standard sample of the brands FL and SL is shown in FIG. 4; two brands of asphalt standard samples are at 920-690cm-1The peak area and the peak height of the characteristic absorption peak in the fingerprint interval are similar because FL and SL brand asphaltThe preparation process, the temperature and other conditions are almost the same, so that the two kinds of asphalt are mixed at 920-690cm-1The infrared spectrograms in the interval are similar and need to be further determined by adopting gel permeation chromatography;
(6) the blind sample asphalt which is not successfully matched is further identified by using a gel permeation chromatogram;
the macromolecular content of the blind sample asphalt was calculated in the same manner as in example 1, and the LMS content was calculated to be 11.2% by the gel permeation chromatogram of the blind sample asphalt shown in fig. 4;
LMS of blind bitumen was compared to LMS of bitumen standards:
in the embodiment, the LMS of the blind sample asphalt is calculated to be 11.2 percent, and the blind sample asphalt falls within the LMS range of 9.7-11.7 percent of FL brand asphalt standard sample, and is identical with the actual brand thereof, and the identification is correct.
Example 3
A method for rapidly identifying a matrix asphalt brand based on ATR-FTIR and GPC comprises the following steps:
1. preparation of asphalt Standard sample data in accordance with example 1
2. Preparation of blind sample asphalt data
(4) Sampling 35 +/-0.5 g of brand asphalt sample to be tested, and putting the sample into a drying oven with the temperature of 163 +/-0.5 ℃ for heating for 80min to prepare short-term aging blind sample asphalt; the infrared spectrogram and the gel permeation chromatogram of the blind sample asphalt are determined according to the method of example 1; the obtained gel permeation chromatogram is shown in FIG. 5;
3. matching and verification
(5) Matching the infrared spectrogram of the blind sample asphalt with the infrared spectrogram of an asphalt standard sample; firstly, importing an asphalt standard sample infrared spectrogram into software, establishing an atlas database in which the asphalt standard sample infrared spectrogram and an asphalt standard sample brand are in one-to-one correspondence, identifying the infrared spectrogram corresponding to the blind sample asphalt brand by utilizing information of the atlas database, and selecting a key peak of 876cm-1、810cm-1And 744cm-1,722cm-1When the similarity between the searched blind sample asphalt infrared spectrogram and the infrared spectrogram in the spectrogram library is 99-100%, the matching is successful;
the blind sample asphalt in the embodiment is matched with the asphalt standard sample infrared spectrogram through the infrared spectrogram, so that brands FL and SL with the matching similarity of 99-100% are obtained; the infrared spectrogram of the asphalt standard sample of the brands FL and SL is shown in FIG. 4;
(6) the blind sample asphalt which is not matched successfully is further identified by using a gel permeation chromatogram;
calculating the macromolecular content of the blind sample asphalt by the same method in the example 1, wherein FIG. 5 is a gel permeation chromatogram of the blind sample asphalt in the example, and the LMS content calculated by the gel permeation chromatogram is 9.3%;
LMS of blind bitumen was compared to LMS of bitumen standards:
in the embodiment, the LMS of the blind sample asphalt is calculated to be 9.3 percent, and the blind sample asphalt falls within the LMS range of 8.3-10.3 percent of the SL brand asphalt standard sample, and is the same as the actual brand and is identified correctly.
Example 4
A method for rapidly identifying a matrix asphalt brand based on ATR-FTIR and GPC comprises the following steps:
1. preparation of asphalt Standard sample data in accordance with example 1
2. Preparation of blind sample asphalt data
(4) Sampling 35 +/-0.5 g of brand asphalt sample to be tested, and putting the sample into a drying oven with the temperature of 163 +/-0.5 ℃ for heating for 75min to prepare short-term aging blind sample asphalt; the infrared spectrogram and the gel permeation chromatogram of the blind sample asphalt are determined according to the method of example 1; the obtained gel permeation chromatogram is shown in FIG. 6;
3. matching and verification
(5) Matching the infrared spectrogram of the blind sample asphalt with the infrared spectrogram of an asphalt standard sample; firstly, importing an asphalt standard sample infrared spectrogram into software, establishing an atlas database in which the asphalt standard sample infrared spectrogram and an asphalt standard sample brand are in one-to-one correspondence, identifying the infrared spectrogram corresponding to the blind sample asphalt brand by utilizing information of the atlas database, and selecting a key peak of 876cm-1、810cm-1And 744cm-1,722cm-1When the blind sample pitch infrared spectrogram is searched out and the infrared in the atlas databaseWhen the similarity of the spectrogram is 99-100%, the matching is successful;
the blind sample asphalt in the embodiment is matched with the infrared spectrogram of an asphalt standard sample through the infrared spectrogram, so that a brand with the matching similarity reaching 99-100% cannot be obtained;
(6) the blind sample asphalt which is not matched successfully is further identified by using a gel permeation chromatogram;
calculating the macromolecular content of the blind sample asphalt by the same method in the example 1, wherein FIG. 6 is a gel permeation chromatogram of the blind sample asphalt in the example, and the LMS content calculated by the gel permeation chromatogram is 6.7%;
LMS of blind bitumen was compared to LMS of bitumen standards:
in the embodiment, the LMS of the blind sample asphalt is calculated to be 6.7%, the blind sample asphalt falls within the LMS range of 5.9-7.9% of the SK brand asphalt standard sample, and the blind sample asphalt is identical to the real brand thereof and is identified correctly.
Although the present invention has been described in detail in this specification with reference to specific embodiments and illustrative embodiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto based on the present invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (6)

1. A method for rapidly identifying a matrix asphalt brand based on ATR-FTIR and GPC is characterized by comprising the following steps:
(1) preparing asphalt samples of different brands into short-term aged asphalt standard samples;
(2) measuring an infrared spectrogram of an asphalt standard sample;
(3) measuring a gel permeation chromatogram of the asphalt standard sample;
(4) preparing a brand asphalt sample to be detected into short-term aged blind sample asphalt, and determining an infrared spectrogram and a gel permeation chromatogram of the blind sample asphalt;
(5) matching the infrared spectrogram of the blind sample asphalt with the infrared spectrogram of an asphalt standard sample; firstly, importing an asphalt standard sample infrared spectrogram into software, establishing an atlas database in which the asphalt standard sample infrared spectrogram and an asphalt standard sample brand are in one-to-one correspondence, and identifying the infrared spectrogram corresponding to the blind sample asphalt brand by using information of the atlas database;
when the similarity between the searched blind sample asphalt infrared spectrogram and the infrared spectrogram in the spectrogram library is 99-100%, namely the matching is successful, and the brand of the blind sample asphalt is the brand corresponding to the successfully matched infrared spectrogram;
when the similarity between the searched blind sample asphalt infrared spectrogram and the infrared spectrogram in the spectrogram library is lower than 99 percent, the matching is unsuccessful;
(6) verifying the successfully matched blind sample asphalt by using a gel permeation chromatogram, and further identifying the unsuccessfully matched blind sample asphalt by using the gel permeation chromatogram; specifically, the macromolecular content of the asphalt standard sample is calculated by a gel permeation chromatogram of the asphalt standard sample, then the macromolecular content of the blind sample asphalt is calculated by the same method, the comparison is carried out as follows,
for the blind sample asphalt successfully matched in the step (5): when the calculated macromolecule content of the blind sample asphalt falls into the macromolecule content range of the asphalt standard sample, the identification result in the step (5) is correct; when the calculated macromolecule content of the blind sample asphalt does not fall into the range of the macromolecule content of the asphalt standard sample, indicating that the identification result in the step (5) is incorrect, and performing the step (5) again for matching;
for blind pitch that did not match successfully in step (5): when the calculated macromolecular content of the blind sample asphalt falls into the macromolecular content range of the corresponding brand asphalt standard sample, indicating that the blind sample asphalt brand is the brand corresponding to the falling asphalt standard sample; and (5) when the calculated macromolecule content of the blind sample asphalt does not fall into the macromolecule content range of the asphalt standard sample, confirming that the matching is unsuccessful again, and performing the methods in the steps (5) and (6) again for matching again.
2. The method for rapid identification of a brand of matrix asphalt based on ATR-FTIR and GPC according to claim 1, characterized in that the short term aging is: and respectively putting the asphalt standard sample or the blind sample asphalt into an oven with the temperature of 163 +/-0.5 ℃ to be heated for 75-85 min.
3. The method for rapid identification of a brand of matrix asphalt based on ATR-FTIR and GPC according to claim 1, wherein the method for determination of the infrared spectrogram is: respectively heating standard pitch or blind pitch to 70-75 deg.C, uniformly coating the heated pitch on ATR wafer, performing infrared spectrum test, and selecting pitch with resolution of 4cm-1The number of scans was 32.
4. The method for rapidly identifying the brand of matrix asphalt based on ATR-FTIR and GPC as claimed in claim 3, wherein in the step (5), the key peak selected from the infrared spectrogram in matching is 876cm-1、810cm-1And 744cm-1,722cm-1
5. The method for rapid identification of a matrix asphalt brand based on ATR-FTIR and GPC according to claim 1, wherein the gel permeation chromatogram is determined by: tetrahydrofuran was used to dissolve pitch standards or blind pitch, respectively, and after dissolution the solution was injected into a chromatographic column and tested through a 0.2mm filter, set to a sample size of 20 μ L.
6. The method for rapid identification of a brand of matrix asphalt based on ATR-FTIR and GPC according to claim 1, wherein in step (6), the calculation method of the macromolecular content is: dividing the gel permeation chromatogram into 13 parts, respectively counting the initial end and the ending end by 5% of the highest signal intensity, taking the first 5 parts as the region where the macromolecule is located, and calculating the average value according to a formula
Figure FDA0002573733990000021
Calculating the macromolecular content of the asphalt.
CN202010647681.6A 2020-07-07 2020-07-07 Rapid identification method for matrix asphalt brand based on ATR-FTIR and GPC Pending CN111965132A (en)

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