CN106153595A - The assay method of SBS modifier content in modified pitch based on Raman spectrum - Google Patents
The assay method of SBS modifier content in modified pitch based on Raman spectrum Download PDFInfo
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- CN106153595A CN106153595A CN201510146176.2A CN201510146176A CN106153595A CN 106153595 A CN106153595 A CN 106153595A CN 201510146176 A CN201510146176 A CN 201510146176A CN 106153595 A CN106153595 A CN 106153595A
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Abstract
The invention discloses the method for quick of SBS modifier content in a kind of SBS modified pitch, comprise the steps: to prepare the modified pitch standard sample of a series of different SBS content, use portable laser Raman spectrometer detection sample at 500 3000cm‑1The Raman spectrum of scope.According to 966cm‑1The Raman spectral characteristics absworption peak area of the SBS at place accounts for matrix pitch 1600cm‑1The characteristic absorption peak area ratio at place is directly proportional to SBS content, and the SBS in SBS modified pitch is carried out detection by quantitative.The detecting instrument of the present invention is portable, simple to operate, low cost, favorable reproducibility, it is adaptable to engineering site detects, it is easy to popularizes, has a good application prospect.
Description
Technical field
The invention belongs to material analysis field, be specifically related to one and utilize spectral quality to measure drip
The method of blue or green modifier content.
Background technology
In recent years, in the high road pavement construction of China, bituminous paving proportion continues to increase,
Wherein in the high-performance road surface with express highway pavement as representative in construction, Modified Bitumen Pavement institute
Accounting heavily continues to increase, and the most universal with SBS modifier in asphalt modifier.SBS changes
Property agent basic composition is Styrene-Butadiene block polymer, present in its molecular structure
Unique soft end-hard end structure can form space net structure in Colophonium, improves the height of Colophonium
Cryogenic property, improves Colophonium rigidity, overcomes the performance deficiency of plain asphalt.Although SBS is modified
The price of agent is relatively costly, but its distinctive performance makes it still have the highest road value.
Along with recent domestic to the research of SBS modified pitch deeply, its mechanism of modification, change
Property the aspect such as technique, pavement performance achieved with lot of research, China is modified also for SBS
Colophonium proposes inspection criterion of constructing targetedly.Find under study for action, SBS modified pitch road
The pavement performance in face is directly related with SBS modifier content with service life etc..
Existing SBS modifier content detection technology has employing Fourier transform infrared spectrometer
Detection means with use conventional titration method measure degree of unsaturation detection means, the former exist makes
By apparatus expensive, affected the drawbacks such as big by temperature air etc.；The latter exists for operator's technical ability
Require too high, by the drawback such as operator's artifical influence factor is excessive, be all not easy to the actual behaviour in building site
Make.
This method introduces laser Raman spectrometer, uses precision instrument to draw data, has good
Repeatability, make personal error reduce, reduce workload simultaneously, improve detection efficiency.
Summary of the invention
It is an object of the invention to propose a kind of SBS modification drip the most accurate and with low cost
The detection scheme of SBS modifier content in green grass or young crops, it can preferably solve present modified pitch market
In be widely present market confusion, product quality is uneven, lack detection means intuitively
Problem, with standard market, improves highway construction quality monitoring dynamics, it is ensured that construction quality.
Technical scheme for achieving the above object is:
The assay method of SBS modifier content in a kind of modified pitch based on Raman spectrum,
Comprise the steps:
(1) the modified pitch standard sample of the different SBS modifier content of preparation；
(2) weigh 0.95-1.05g standard sample, and add polar solvent and be diluted to 5% change
Property cold primer-oil；
(3) the modified pitch sample solution after dilution is dripped test in laser Raman spectrometer；
(4) at 500-3000cm-1Range scans, obtains the Raman spectrogram of sample, and right
Initial data carries out pretreatment.；
(5) data process: choose 966cm-1Place's absworption peak is special as the Raman spectrum of SBS
Levy absworption peak, choose 1600cm-1The absworption peak at place as the characteristic absorption peak of matrix pitch, and
Calculate its integral area respectively, try to achieve integral area ratio；
(6) the SBS content and the two integrating peak areas ratio that utilize each standard sample carry out Linear Quasi
Close, set up SBS modifier content and the mathematical model of two peak integral area ratios.
(7) to measuring sample, carry out to (5) according to step (1), utilize mathematics
Model is calculated SBS content in testing sample.
Wherein, described polar reagent is: trichloro ethylene, oxolane, the one of toluene or
Person is several.
Wherein, described Raman microprobe is Surface Enhanced probe based on photonic crystal fiber.
Wherein, Raman spectrogram initial data preprocess method is Wavelet Transform.
The beneficial effects of the present invention is:
(1) Surface Enhanced Raman probe is used can substantially to make the Raman signal of SBS obtain
Enhancing with a number of level；And reduce the glimmering of benzene ring structure in SBS to a certain extent
Light background.
(2) use wavelet modulus maxima method that the Raman spectrum initial data obtained is carried out
Process, effectively inhibit the interference of background fluorescence and noise to increase substantially ratio.
(3) method that the present invention proposes, sample preparation and test process are simple, can be single
Operation；On the premise of ensureing precision, test speed is fast；Whole process about needs 5-10min；
Low to test experiments site requirements, can in the wild, job site fast and accurate measurement.Protecting
Card accuracy of detection on the premise of, it is achieved that the miniaturization of equipment, decrease simultaneously sample use with
Loss amount, significantly reduces testing cost.And with infrared spectrometry, gel permeation chromatography phase
Ratio, this method instrument cost, cost of labor are respectively provided with clear superiority.
Accompanying drawing explanation
Fig. 1 SBS content is the SBS modified pitch laser Raman spectroscopy figure of 2%.
Fig. 2 is SBS modifier content and the Model fitting curve of two integrating peak areas ratio
Detailed description of the invention
Following example are used for illustrating the present invention, but are not limited to the scope of the present invention.
In embodiment, the domestic laser Raman spectrometer of LR-3 type.Surface Enhanced Raman probe.
Embodiment 1
Highway construction scene, Guangxi District is carried out SBS modifier assay.
Take SK70# matrix pitch and the modifying agent SBS (model: 791H) of engineering site respectively,
Preparing SBS content according to the SBS modified pitch collocation method of this highway is 2%, 4%,
6%, 4 kinds of standard sample of the SBS modified pitch of 8%.
As steps described below 4 above-mentioned standard sample are carried out redox potentiometry.
(1) weighing the sample of 1 ± 0.05g respectively, weighing error controls at ± 0.05g, and adds
Polar solvent trichloro ethylene, is diluted to the modified asphalt solutions of 5% (mass ratio).
(3) the modified pitch sample solution after dilution is dripped test in laser Raman spectrometer.
(4) at 500-3000cm-1Range scans, obtains the Raman spectrogram of sample, Fig. 1
For the Raman collection of illustrative plates after wavelet transform process that SBS content is 2%.And initial data is entered
Row pretreatment.
(5) data process: choose 966cm-1Place's absworption peak is special as the Raman spectrum of SBS
Levying absworption peak, peak area is labeled as An', choose 1600cm-1The absworption peak at place drips as substrate
Blue or green characteristic absorption peak, and calculate its area respectively, peak area is labeled as A0' try to achieve area ratio
ValueSee table 1.
(6) the SBS content and the two integrating peak areas ratio that utilize each standard sample carry out Linear Quasi
Close, set up SBS modifier content and the mathematical model of two integrating peak areas ratio.See Fig. 2.
(7) to measuring the sample sample of 2% (the known SBS with the addition of) sampling, according to upper
State step (1) to carry out to (5), calculate A968=0.306, A1600=3.194, then
A968/A1600=0.0958, utilize mathematical model to be calculated SBS content in testing sample to be
1.83%, and originally SBS with the addition of 2% difference is-0.17%, in range of error.
Table 1A 'n/A′0～SBS content
| SBS content (x-axis)/% | 2 | 4 | 6 | 8 |
| A′n/A′0(y-axis) | 0.09728 | 0.15384 | 0.20106 | 0.248297 |
Embodiment 2
The asphalt sample of unknown SBS modifier content is measured.
Testing sample is sampled 1.0106g, carries out to (5) according to above-mentioned steps (1), meter
Calculate to obtain A968=0.552, A1600=3.532, then A968/A1600=0.1562, utilize mathematics
It is 4.21% that model is calculated SBS content in testing sample.
Those skilled in the art in the art are it should be appreciated that above-described embodiment is intended merely to
The present invention is described, and is not used as limitation of the invention, as long as at the connotation of the present invention
In the range of, to the conversion of above-described embodiment, modification all by the scope in the claims in the present invention that falls
In.
Claims (4)
1. an assay method for SBS modifier content in modified pitch based on Raman spectrum,
It is characterized in that, comprise the steps:
(1) the modified pitch standard sample of the different SBS modifier content of preparation；
(2) weigh 0.95-1.05g standard sample, and add polar solvent and be diluted to 5% change
Property cold primer-oil；
(3) the modified pitch sample solution after dilution is dripped test in laser Raman spectrometer；
(4) at 500-3000cm-1Range scans, obtains the Raman spectrogram of sample, and right
Initial data carries out pretreatment；
(5) data process: choose 966cm-1Place's absworption peak is special as the Raman spectrum of SBS
Levy absworption peak, choose 1600cm-1The absworption peak at place as the characteristic absorption peak of matrix pitch, and
Calculate its integral area respectively, area ratio of quadraturing；
(6) the SBS content and the two integrating peak areas ratio that utilize each standard sample carry out Linear Quasi
Close, set up SBS modifier content and the mathematical model of two peak integral area ratios；
(7) to measuring sample, it is measured to (5) according to step (1), utilizes
Mathematical model is calculated SBS content in testing sample.
Assay method the most according to claim 1, it is characterised in that described polarity
Reagent is: trichloro ethylene, oxolane, one or several in toluene.
Assay method the most according to claim 1, it is characterised in that described laser
The Raman microprobe of Raman spectrum is Surface Enhanced probe based on photonic crystal fiber.
Assay method the most according to claim 1, it is characterised in that Raman spectrogram
Initial data preprocess method is Wavelet Transform.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107831158A (en) * | 2017-11-10 | 2018-03-23 | 厦门斯贝克科技有限责任公司 | The method of organic solvent content in portable Raman quick detection organic wastewater |
| CN108426992A (en) * | 2018-04-23 | 2018-08-21 | 中石化石油工程技术服务有限公司 | A kind of method of insoluble high molecular polymerization species solid content in measurement modified pitch |
| CN110208243A (en) * | 2019-06-12 | 2019-09-06 | 中国原子能科学研究院 | Method that is a kind of while measuring uranyl nitrate and concentration of nitric acid in water phase |
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| CN104237200A (en) * | 2014-09-12 | 2014-12-24 | 浙江大学 | Glyphosate concentration detection method based on Raman signals of chlorella pyrenoidosa |
| CN104280378A (en) * | 2014-09-28 | 2015-01-14 | 李伟 | Method for detecting content of SBS (Styrene Butadiene Styrene) modifier in modified asphalt |
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| CN1815197A (en) * | 2006-02-24 | 2006-08-09 | 清华大学 | Photon crystal optical-fiber probe sensor based on nano grain surface increasing Raman spectrum |
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| CN102721679A (en) * | 2012-05-03 | 2012-10-10 | 清华大学 | SERS (Surface Enhanced Raman Scattering)-based and CARS (Coherent Anti-stokes Raman Scattering)-based detection system and method |
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| CN107831158A (en) * | 2017-11-10 | 2018-03-23 | 厦门斯贝克科技有限责任公司 | The method of organic solvent content in portable Raman quick detection organic wastewater |
| CN108426992A (en) * | 2018-04-23 | 2018-08-21 | 中石化石油工程技术服务有限公司 | A kind of method of insoluble high molecular polymerization species solid content in measurement modified pitch |
| CN110208243A (en) * | 2019-06-12 | 2019-09-06 | 中国原子能科学研究院 | Method that is a kind of while measuring uranyl nitrate and concentration of nitric acid in water phase |
| CN110208243B (en) * | 2019-06-12 | 2020-10-09 | 中国原子能科学研究院 | Method for simultaneously determining concentrations of uranyl nitrate and nitric acid in aqueous phase |
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Application publication date: 20161123 |