CN108398399A - The method for identifying asphalt quality using decaying In situ ATR-FTIR standard spectrogram - Google Patents
The method for identifying asphalt quality using decaying In situ ATR-FTIR standard spectrogram Download PDFInfo
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- 239000010426 asphalt Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004483 ATR-FTIR spectroscopy Methods 0.000 title claims abstract description 17
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 17
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 102
- 239000011159 matrix material Substances 0.000 claims abstract description 69
- 238000012360 testing method Methods 0.000 claims description 78
- 238000002474 experimental method Methods 0.000 claims description 16
- 238000001228 spectrum Methods 0.000 claims description 12
- 230000035945 sensitivity Effects 0.000 claims description 11
- 238000013461 design Methods 0.000 claims description 8
- 238000010276 construction Methods 0.000 abstract description 16
- 238000011156 evaluation Methods 0.000 abstract description 11
- 238000012544 monitoring process Methods 0.000 abstract description 10
- 230000003595 spectral effect Effects 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000011295 pitch Substances 0.000 description 97
- 238000001514 detection method Methods 0.000 description 13
- 239000000203 mixture Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000011835 investigation Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 230000003252 repetitive effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZZIZZTHXZRDOFM-XFULWGLBSA-N tamsulosin hydrochloride Chemical compound [H+].[Cl-].CCOC1=CC=CC=C1OCCN[C@H](C)CC1=CC=C(OC)C(S(N)(=O)=O)=C1 ZZIZZTHXZRDOFM-XFULWGLBSA-N 0.000 description 2
- 241000208140 Acer Species 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000007824 aliphatic compounds Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000003705 background correction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
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- 229930195733 hydrocarbon Natural products 0.000 description 1
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- 150000002894 organic compounds Chemical group 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004153 renaturation Methods 0.000 description 1
- 230000033458 reproduction Effects 0.000 description 1
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- 238000011105 stabilization Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/55—Specular reflectivity
- G01N21/552—Attenuated total reflection
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Abstract
The invention discloses a kind of methods for identifying asphalt quality using decaying In situ ATR-FTIR standard spectrogram, including：Obtain 3 groups of repeatability infrared spectrums and 6 groups of reproducibility infrared spectrums, to obtain standard IR spectrogram, sample to be tested infrared spectrum is compared with standard IR spectrogram, to obtain relevance threshold, judges whether the quality of matrix pitch sample to be tested is qualified according to relevance threshold.The present invention is from the essential structure of pitch, and by carrying out full spectral region comparison to pitch, quick Identification Evaluation pitch screens the adulterated pitch of mix and convert, strong guarantee is provided for the monitoring of construction quality.In addition, the invention avoids a large amount of cumbersome road surface data and environmental factors complicated and changeable, it detects faster, experimental result can be provided within three minutes, data are accurate and reliable, it can be detected in mobile laboratory and scene, breach the limitation of traditional macro performance evaluation means, asphalt quality is timely and effectively monitored especially suitable for construction site.
Description
Technical field
The present invention relates to quality discrimination technical field more particularly to a kind of utilization decaying In situ ATR-FTIR standard spectrograms
The method for identifying asphalt quality.
Background technology
Important materials of the pitch as highway construction carry out research and development detection to it, quality monitoring is always road worker
Issues that need special attention.The detection method of the existing asphalt material in China is mainly JTG E20-2011《Highway engineering pitch and drip
Green test mixture regulation》.However, there are the following problems for the prior art：First, above-mentioned detection method can not screen existing market
On " personation " pitch.Since pitch demand increases, start modulation pitch occur in the market, it is using lightweight oil, fills out
Some underproof pitches are carried out physical modification and are made by material and other auxiliary agents, this modulation pitch can meet JTG F40-2004
《Standard specification for construction and acceptance of highway asphalt pavement》Associated specifications, but add with the volatilization of lightweight oil during military service
Acute ageing of asphalt degree so that road surface various diseases occurs ahead of time, and What is more occurs as soon as loose, passage of building stones etc. in the construction time
Phenomenon.Secondly, equipment volume is big needed for above-mentioned detection method, and test period is long, is not suitable for construction site and is carried out to asphalt material
Detection monitoring in time.Existing detection method is concentrated mainly on mechanics macro property, and required equipment full set floor space needs
30m2Left and right, and for the test of asphalt sample from sample presentation is sampled to up to laboratory's sample preparation fruit that detects to sign an undertaking at least needs
3 day time, the test period is long, therefore is not suitable for the timely detection of construction site.
Invention content
To solve limitation and defect of the existing technology, present invention offer is a kind of to utilize decaying In situ ATR-FTIR mark
The method of quasi- spectrogram identification asphalt quality.
For this purpose, the present invention provides a kind of method using decaying In situ ATR-FTIR standard spectrogram identification asphalt quality,
Including：
Obtain matrix pitch standard sample；
Same testing crew carries out 3 infrared spectrum reperformance tests to the matrix pitch standard sample, obtains 3 groups of weights
Renaturation infrared spectrum,
Peak position is carried out out in spectrum wave-number range entirely to above-mentioned 3 groups of repeatability infrared spectrums, goes out peak intensity high sensitivity
Spectrogram compares, and determines repeatability error range；
Two different tests personnel carry out 3 infrared spectrums again respectively to the matrix pitch standard sample in different time
Existing property test, obtains 6 groups of reproducibility infrared spectrums,
Peak position is carried out out in spectrum wave-number range entirely to above-mentioned 6 groups of reproducibility infrared spectrums, goes out peak intensity high sensitivity
Spectrogram compares, and determines reproducibility error range；
The statistics that 3 groups of reperformance test infrared spectrums and 6 groups of reproducibility test infrared spectrums carry out spectrogram is calculated, is obtained
Average standard IR spectrogram of the spectrogram as matrix pitch standard sample；
To the standard IR spectrogram in 2050cm-1To 1950cm-1In the range of carry out noise testing, obtain the mark
The peak-peak noise and root mean square noise of quasi- infrared spectrum；
If the peak-peak noise is less than or equal to 0.00196 or the root mean square noise is less than or equal to
0.000559, the standard IR spectrogram is included in design asphalt spectrogram library, design asphalt spectrogram library is used for asphalitine
Discriminating is compared in amount；
Obtain the sample to be tested infrared spectrum of matrix pitch sample to be tested；
The sample to be tested infrared spectrum is carried out full spectrogram with the standard IR spectrogram to compare, test sample is waited for described in acquisition
The relevance threshold of product infrared spectrum and the standard IR spectrogram；
If the sample to be tested infrared spectrum is with the standard IR spectrogram in 4000cm-1To 650cm-1Wave-number range
Interior correlation is more than or equal to 99%, and standard deviation is less than or equal to 5%, the quality of the matrix pitch sample to be tested
It is qualified.
Optionally, the experiment parameter of test experiments is as follows：Scanning range is 4000cm-1To 650cm-1, scanning times 32
It is secondary, resolution ratio 4cm-1。
Optionally, when determining repeatability error range, arbitrary two groups of repeatability infrared spectrums are in 4000cm-1To 650cm-1Wave-number range in correlation be more than or equal to 99.63%, standard deviation be less than or equal to 0.43%.
Optionally, when determining reproducibility error range, arbitrary two groups of reproducibility infrared spectrums are in 4000cm-1To 650cm-1Wave-number range in correlation be more than or equal to 99.09%, standard deviation be less than or equal to 3.5%.
Optionally, the system that 3 groups of reperformance test infrared spectrums and 6 groups of reproducibility test infrared spectrums are carried out to spectrogram
Meter calculates, and the step of obtaining standard IR spectrogram of the average spectrogram as matrix pitch standard sample includes：
It is corresponding with 6 groups of reproducibility test each data point X values of infrared spectrum to 3 groups of reperformance test infrared spectrums
Y value is summed；
Using arithmetic mean of instantaneous value being averaged as the matrix pitch standard sample obtained by the summation of acquisition divided by spectrogram number
Spectrogram, the average spectrogram are the standard IR spectrogram of the matrix pitch standard sample.
The present invention has following advantageous effects：
It is provided by the invention to include using the method that In situ ATR-FTIR standard spectrogram identifies asphalt quality that decays：It obtains
Matrix pitch standard sample, same testing crew carry out 3 infrared spectrum reperformance tests to the matrix pitch standard sample,
Obtain 3 groups of repeatability infrared spectrums, two different tests personnel to the matrix pitch standard sample different time respectively into
3 infrared spectrum reproducibility tests of row, obtain 6 groups of reproducibility infrared spectrums, according to 3 groups of reperformance test infrared spectrums and 6 groups
Reproducibility tests the standard IR spectrogram that infrared spectrum obtains matrix pitch standard sample, obtains waiting for for matrix pitch sample to be tested
The sample to be tested infrared spectrum is compared sample infrared spectrum with the standard IR spectrogram, described in obtaining
The relevance threshold of sample to be tested infrared spectrum and the standard IR spectrogram judges the matrix according to the relevance threshold
Whether the quality of pitch sample to be tested is qualified.Technical solution provided by the invention is from the essential structure of pitch, by drip
Blueness carries out full spectral region comparison, and quick Identification Evaluation pitch screens the adulterated pitch of mix and convert, provided for the monitoring of construction quality
Strong guarantee.In addition, technical solution provided by the invention avoids a large amount of cumbersome road surface data and ring complicated and changeable
Border factor, detection is faster, can provide experimental result within three minutes, and data are accurate and reliable, in mobile laboratory and can show
Field is detected, and breaches the limitation of traditional macro performance evaluation means, in time, is effectively monitored especially suitable for construction site
Asphalt quality has great promotional value and market prospects.
Description of the drawings
Fig. 1 is the infrared comparison spectrogram of reperformance test for the matrix pitch standard sample that the embodiment of the present invention one provides；
Fig. 2 is the reperformance test standard deviation INFRARED SPECTRUM for the matrix pitch standard sample that the embodiment of the present invention one provides
Figure；
Fig. 3 is that the reproducibility for the matrix pitch standard sample that the embodiment of the present invention one provides tests infrared comparison spectrogram；
Fig. 4 is the reproducibility testing standard deviation INFRARED SPECTRUM for the matrix pitch standard sample that the embodiment of the present invention one provides
Figure；
Fig. 5 is the standard IR spectrogram for the matrix pitch standard sample that the embodiment of the present invention one provides；
Fig. 6 is the comparison chart of sample to be tested infrared spectrum and standard IR spectrogram that the embodiment of the present invention one provides.
Specific implementation mode
To make those skilled in the art more fully understand technical scheme of the present invention, the present invention is carried below in conjunction with the accompanying drawings
The method using decaying In situ ATR-FTIR standard spectrogram identification asphalt quality of confession is described in detail.
Embodiment one
Infrared spectrum is the infrared ray of the certain wavelength of molecule energy selective absorbing, and causes vibration level and rotation in molecule
The transition of energy level, the detection absorbed situation of infrared ray can be obtained the infrared absorption spectrum of substance, also known as molecular vibration spectrum or
Vibration rotation spectrum.Infrared spectrum technology is as one of the important means of organic compound structure identification, the structural information that can be provided
It is abundant, applied widely, instrument is easy to use.Therefore, among pitch chemical composition, structural analysis infrared spectrum technology by
A degree of concern.
Fig. 1 is the infrared comparison spectrogram of reperformance test for the matrix pitch standard sample that the embodiment of the present invention one provides, Fig. 2
For the reperformance test standard deviation infrared spectrum for the matrix pitch standard sample that the embodiment of the present invention one provides.Such as Fig. 1 and Fig. 2
Shown, the present embodiment provides a kind of methods for identifying asphalt quality using decaying In situ ATR-FTIR standard spectrogram to include：It obtains
Take matrix pitch standard sample；Same testing crew carries out 3 infrared spectrum repeatability to the matrix pitch standard sample and surveys
Examination obtains 3 groups of repeatability infrared spectrums；To above-mentioned 3 groups of repeatability infrared spectrums full spectrum wave-number range in carry out out peak position,
Go out the comparison of peak intensity high sensitivity spectrogram, determines repeatability error range.Sheet of the technical solution provided in this embodiment from pitch
Matter structure is set out, and by carrying out full spectral region comparison to pitch, quick Identification Evaluation pitch screens the adulterated pitch of mix and convert, is
The monitoring of construction quality provides strong guarantee.
The experiment parameter of test experiments provided in this embodiment is as follows：Scanning range is 4000cm-1To 650cm-1, scanning
Number is 32 times, resolution ratio 4cm-1.Infrared spectrogram provided in this embodiment can be considered as " fingerprint " or " DNA " of pitch,
On the basis of obtaining standard substrates pitch used in the project of highway building site, by the experiment for studying matrix pitch standard sample
It is feasible to judge that detection method controls asphalt quality for method, reperformance test error, reproducibility test error, noise level
Property.Moreover, technical solution provided in this embodiment is established brand, oil sources etc. and is significantly marked by matrix pitch standard IR spectrogram
Relationship between knowledge and characteristic peak, is compared in full spectral region with asphalt sample to be measured, to true in error range
Determine asphalt quality used in traffic engineering and whether there is the case where not being consistent with description.
Fig. 3 is that the reproducibility for the matrix pitch standard sample that the embodiment of the present invention one provides tests infrared comparison spectrogram, Fig. 4
For the reproducibility testing standard deviation infrared spectrum for the matrix pitch standard sample that the embodiment of the present invention one provides.Such as Fig. 3 and Fig. 4
Shown, the present embodiment provides a kind of methods for identifying asphalt quality using decaying In situ ATR-FTIR standard spectrogram to further include：
Two different tests personnel carry out 3 infrared spectrum reproducibilities in different time to the matrix pitch standard sample and survey respectively
Examination obtains 6 groups of reproducibility infrared spectrums；To above-mentioned 6 groups of reproducibility infrared spectrums full spectrum wave-number range in carry out out peak position,
Go out the comparison of peak intensity high sensitivity spectrogram, determines reproducibility error range；By 3 groups of reperformance test infrared spectrums and 6 groups of reproductions
Property test infrared spectrum carry out the statistics of spectrogram and calculate, obtain standard IR spectrum of the average spectrogram as matrix pitch standard sample
Figure.Technical solution provided in this embodiment avoids a large amount of cumbersome road surface data and environmental factor complicated and changeable, and detection is fast
It is fast quick, experimental result can be provided within three minutes, data are accurate and reliable, can be detected in mobile laboratory and scene, dash forward
The limitation for having broken traditional macro performance evaluation means, especially suitable for construction site in time, effectively monitor asphalt quality, have
Great promotional value and market prospects.
Oil plant contact method is provided according to project management department, the present embodiment carries out practical investigation to matrix pitch producer, to
Obtain matrix pitch standard sample.The present embodiment adjusts Nicolet iS5 infrared spectrometers states to stabilization, is all-trans using decaying
(ATR) attachment is penetrated, matrix pitch standard sample is uniformly smeared to the ZnSn crystal wafers of covering attachment, so that it is determined that experiment parameter.
The present embodiment obtains infrared spectrogram using infrared spectrometer multiple reflections test asphalt film sample, then asphalt sample is infrared
Spectrogram carries out serial analysis after using OMNIC processing software background corrections.
The present embodiment carries out repetitive test to matrix pitch standard sample and reproducibility is tested, and acquires INFRARED SPECTRUM respectively
Figure, analyzes infrared spectrum using OMNIC processing softwares, and high sensitivity is carried out in spectrum wave-number range entirely after background correction
Spectrogram goes out peak position and goes out peak intensity comparison, so that it is determined that related coefficient and test error range.When determining repeatability error model
When enclosing, arbitrary two groups of repeatability infrared spectrums are in 4000cm-1To 650cm-1Wave-number range in correlation be more than or equal to
99.63%, standard deviation is less than or equal to 0.43%.When determining reproducibility error range, arbitrary two groups of reproducibilities are infrared
Spectrogram is in 4000cm-1To 650cm-1Wave-number range in correlation be more than or equal to 99.09%, standard deviation be less than or
Person is equal to 3.5%.The present embodiment determines the infrared spectrum characteristic peak of matrix pitch, by matrix pitch reperformance test infrared spectrum
The statistics that spectrogram is carried out with reproducibility test infrared spectrum calculates, its average spectrogram is taken to be composed as the standard IR of the matrix pitch
Figure.
The present embodiment carries out noise testing to matrix pitch standard IR spectrogram, judges spectrometer, inspection according to measurement result
Survey device, experiment parameter are arranged and the stability of system physical performance, and the standard IR spectrogram of the matrix pitch is included in pitch mark
Quasi- spectrogram library to asphalt quality in engineer application to be compared discriminating.Specifically, the present embodiment is to the standard IR
Spectrogram is in 2050cm-1To 1950cm-1In the range of carry out noise testing, obtain the standard IR spectrogram peak-peak noise and
Root mean square noise, if the peak-peak noise is less than or equal to 0.00196 or the root mean square noise is less than or equal to
0.000559, the standard IR spectrogram is included in design asphalt spectrogram library, design asphalt spectrogram library is used for asphalitine
Discriminating is compared in amount.
Fig. 5 is the standard IR spectrogram for the matrix pitch standard sample that the embodiment of the present invention one provides, and Fig. 6 is that the present invention is real
The comparison chart of the sample to be tested infrared spectrum and standard IR spectrogram of the offer of example one is provided.As shown in Figure 5 and Figure 6, the present embodiment obtains
Obtain the sample to be tested infrared spectrum of matrix pitch sample to be tested；By the sample to be tested infrared spectrum and the standard IR spectrogram
Full spectrogram comparison is carried out, the relevance threshold of the sample to be tested infrared spectrum and the standard IR spectrogram is obtained；If described
Sample to be tested infrared spectrum is with the standard IR spectrogram in 4000cm-1To 650cm-1Wave-number range in correlation be more than
Or be equal to 99%, standard deviation be less than or equal to 5%, the matrix pitch sample to be tested it is up-to-standard.
Repetitive test provided in this embodiment refers to preparing sample 3 times to the same testing crew of same matrix pitch, is pressed
Examination of infrared spectrum is carried out according to the experimental method, 3 spectrograms of acquisition carry out out peak position in spectrum wave-number range entirely, go out peak intensity
The highly sensitive spectrogram of degree compares.Reproducibility experiment provided in this embodiment refers to using two differences to same matrix pitch sample
Testing crew carries out sample preparation in different time, and examination of infrared spectrum is carried out according to the experimental method, and it is total to acquire 3 spectrograms respectively
6 groups of infrared spectrums full spectrum wave-number range carry out out peak position, go out peak intensity high sensitivity spectrogram compare.It is composed described in the present embodiment
It refers to right to each data point (X values) among 9 spectrograms obtained by reperformance test and reproducibility test that the statistics of figure, which calculates,
The Y value answered is added, and summation is again divided by spectrogram number obtains arithmetic mean of instantaneous value, and the present embodiment is using above-mentioned arithmetic mean of instantaneous value as the matrix
The average spectrogram of pitch takes its average standard IR spectrogram of the spectrogram as the matrix pitch.
The present embodiment carries out noise testing to matrix pitch standard IR spectrogram and refers in 2050cm-1To 1950cm-1Model
Noise testing is carried out within enclosing, and is as a result indicated with peak-peak noise and root mean square (RMS) noise.Sample to be tested infrared spectrum
Refer to that sample to be tested infrared spectrum carries out height with standard spectrogram within the scope of full infrared spectrum with standard spectrogram relevance threshold
Sensitivity spectrogram compares, if the two related coefficient is more than or equal to 99%, standard deviation is less than or equal to 5%, you can
Think that sample to be tested is consistent with standard sample, otherwise sample to be tested is not consistent with standard sample.Technical side provided in this embodiment
Case is from the essential structure of pitch, and by carrying out full spectral region comparison to pitch, quick Identification Evaluation pitch screens mix and convert
Adulterated pitch provides strong guarantee for the monitoring of construction quality.
The present embodiment uses the Nicolet iS5 infrared spectrometers and Sinopec of Thermo Fischer Scient Inc. of the U.S.
The 70#A grades East Sea pitch of Qilu Petrochemical Company is tested.The present embodiment is included in matrix pitch standard IR spectrogram：In determination
After the information such as brand, the trade mark, the oil sources of matrix pitch used in project, oil plant contact method is provided according to project management department, to base
Matter pitch producer carries out practical investigation and obtains matrix pitch standard sample.Prepared by sample to the same testing crew of same matrix pitch
Product 3 times carry out examination of infrared spectrum according to above-mentioned experimental method, and 3 spectrograms of acquisition carry out out peak position in spectrum wave-number range entirely
It sets, go out the comparison of peak intensity high sensitivity spectrogram, determine repeatability error range.Through comparing, arbitrary two groups of repeatability is infrared
Spectrogram is in 4000cm-1To 650cm-1Wave-number range in correlation be more than or equal to 99.63%, standard deviation be less than or
Person is equal to 0.43%.
The present embodiment carries out sample preparation using two different tests personnel to same matrix pitch sample in different time, according to
Above-mentioned experimental method carries out examination of infrared spectrum, acquires 3 spectrograms totally 6 groups of infrared spectrums respectively, in spectrum wave-number range entirely into
Row goes out peak position, goes out the comparison of peak intensity high sensitivity spectrogram, determines reproducibility error range.Through comparing, arbitrary two groups again
Existing property infrared spectrum is in 4000cm-1To 650cm-1Wave-number range in correlation be more than or equal to 99.09%, standard deviation
Difference is less than or equal to 3.5%.
The present embodiment carries out spectrum analysis, the characteristic peak of 70#A grades of East Sea pitch according to the infrared spectrum of gained matrix pitch
For：Phenyl ring-C-H- antisymmetric stretching vibrations the peak of aromatic compound is in 3030cm-1Place, in-plane bending vibration peak exists
1300cm-1To 1000cm-1In range, wagging vibration peak is in 900cm-1To 650cm-1In range；The vibration peak of phenyl ring skeleton
In 1600cm-1Place.The antisymmetric stretching vibration peak, symmetrical stretching vibration peak of alkane-C-H- is located in aliphatic compound
2923cm-1、2852cm-1Locate, stretching vibration peak is in 1460cm in face-1Place, symmetric deformation vibration peak is in 1380cm-1Place；Chain hydrocarbon
Skeleton-C-C- vibration peaks are in 1250cm-1To 1150cm-1In range ,-C=C- vibration peaks also are located at 1600cm-1Place.1030cm-1
The spectral peak at place is the vibration peak of sub- maple base, illustrates to contain S atom among pitch.
The reperformance test infrared spectrum (3 groups) of 70#A grades of East Sea pitch and reproducibility are tested infrared spectrum by the present embodiment
The statistics of (6 groups) totally 9 groups of carry out spectrograms calculates, and takes its average standard IR spectrogram of the spectrogram as 70#A grades of East Sea pitch.This
The technical solution that embodiment provides avoids a large amount of cumbersome road surface data and environmental factor complicated and changeable, and detection is rapid fast
Victory can provide experimental result in three minutes, and data are accurate and reliable, can be detected, breach in mobile laboratory and scene
The limitation of traditional macro performance evaluation means, especially suitable for construction site in time, effectively monitor asphalt quality, have very big
Promotional value and market prospects.
The present embodiment compare the East Sea 70# design asphalt sample the infrared comparison spectrogram of reperformance test and reproducibility test it is red
Outer comparison spectrogram, in 4000cm-1To 650cm-1Wave-number range in correlation be all higher than 99%, standard deviation is less than or waits
In 3.5%, illustrate that the monitoring method using decaying In situ ATR-FTIR standard spectrogram method Rapid identification asphalt quality accurately may be used
It leans on.
The present embodiment selects the design asphalt infrared spectrum in 2050cm-1To 1950cm-1Range carry out noise testing,
Measurement result is as follows：Peak-peak noise is 0.00196, and root mean square (RMS) noise is 0.000559.Illustrate in above-mentioned experimentation
Among, spectrometer, detector, experiment parameter are arranged and the physical property of system is good, and signal-to-noise ratio is big, and gained spectrogram information is steady
It is fixed, therefore the standard IR spectrogram of 70#A grades of East Sea pitches can be included in matrix pitch standard spectrogram database, with to engineering
Discriminating is compared in pitch in.Technical solution provided in this embodiment is from the essential structure of pitch, by drip
Blueness carries out full spectral region comparison, and quick Identification Evaluation pitch screens the adulterated pitch of mix and convert, provided for the monitoring of construction quality
Strong guarantee.
The present embodiment samples asphalt field, infrared spectrogram acquisition is carried out according to experimental method, according to matrix pitch mark
The reperformance test of quasi- sample and reproducibility test result error range consider testing inspection environment, operating personnel's difference
Etc. factors, determine that sample to be tested infrared spectrum and standard spectrogram correlation up to 99% or more are qualified, think product less than 99%
Board or oil sources are not consistent with standard sample, refuse into tank, check on to carry out source quality to asphalt applications.Referring to Fig. 6, this reality
Example is applied according to the sample to be tested infrared spectrum and the standard IR spectrogram in 4000cm-1To 650cm-1Wave-number range in
Correlation values judge whether the quality of sample to be tested meets situation.As can be seen that the sample to be tested infrared spectrum with it is described
The correlation of standard IR spectrogram is 96.95%, in fingerprint region 1350cm-1To 650cm-1It is only 93.23% in range, and
In fingerprint region 1379cm-1To 919cm-1In range, sample to be tested no matter peak shape or peak area size with standard spectrogram not
Together, therefore it can be assumed that sample to be tested is not consistent with pitch used in engineering.
It is provided in this embodiment to include using the method that In situ ATR-FTIR standard spectrogram identifies asphalt quality that decays：It obtains
Matrix pitch standard sample, same testing crew is taken to carry out 3 infrared spectrum repeatability to the matrix pitch standard sample and survey
Examination, obtains 3 groups of repeatability infrared spectrums, and two different tests personnel distinguish the matrix pitch standard sample in different time
3 infrared spectrum reproducibility tests are carried out, 6 groups of reproducibility infrared spectrums are obtained, according to 3 groups of reperformance test infrared spectrums and 6
Group reproducibility test infrared spectrum obtains the standard IR spectrogram of matrix pitch standard sample, obtains the to be measured of asphalt sample to be measured
The sample to be tested infrared spectrum is compared sample infrared spectrum with the standard IR spectrogram, to be waited for described in acquisition
The relevance threshold of sample infrared spectrum and the standard IR spectrogram judges the drip to be measured according to the relevance threshold
Whether the quality of green sample is qualified.Technical solution provided in this embodiment from the essential structure of pitch, by pitch into
The full spectral region of row compares, and quick Identification Evaluation pitch screens the adulterated pitch of mix and convert, provides and has by force for the monitoring of construction quality
The guarantee of power.In addition, technical solution provided in this embodiment avoids a large amount of cumbersome road surface data and environment complicated and changeable
Factor, detection is faster, can provide experimental result within three minutes, data are accurate and reliable, can be in mobile laboratory and scene
It is detected, breaches the limitation of traditional macro performance evaluation means, timely especially suitable for construction site, effective monitoring drip
Green quality has great promotional value and market prospects.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, in the essence for not departing from the present invention
In the case of refreshing and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (5)
1. a kind of method using decaying In situ ATR-FTIR standard spectrogram identification asphalt quality, which is characterized in that including：
Obtain matrix pitch standard sample；
Same testing crew carries out 3 infrared spectrum reperformance tests to the matrix pitch standard sample, obtains 3 groups of repeatability
Infrared spectrum；
Peak position is carried out out in spectrum wave-number range entirely to above-mentioned 3 groups of repeatability infrared spectrums, goes out peak intensity high sensitivity spectrogram
It compares, determines repeatability error range；
Two different tests personnel carry out 3 infrared spectrum reproducibilities respectively to the matrix pitch standard sample in different time
Test obtains 6 groups of reproducibility infrared spectrums；
Peak position is carried out out in spectrum wave-number range entirely to above-mentioned 6 groups of reproducibility infrared spectrums, goes out peak intensity high sensitivity spectrogram
It compares, determines reproducibility error range；
The statistics that 3 groups of reperformance test infrared spectrums and 6 groups of reproducibility test infrared spectrums carry out spectrogram is calculated, is averaged
Standard IR spectrogram of the spectrogram as matrix pitch standard sample；
To the standard IR spectrogram in 2050cm-1To 1950cm-1In the range of carry out noise testing, obtain the standard IR
The peak-peak noise and root mean square noise of spectrogram；
If the peak-peak noise is less than or equal to 0.00196 or the root mean square noise is less than or equal to
0.000559, the standard IR spectrogram is included in design asphalt spectrogram library, design asphalt spectrogram library is used for asphalitine
Discriminating is compared in amount；
Obtain the sample to be tested infrared spectrum of matrix pitch sample to be tested；
The sample to be tested infrared spectrum is carried out full spectrogram with the standard IR spectrogram to compare, it is red to obtain the sample to be tested
The relevance threshold of outer spectrogram and the standard IR spectrogram；
If the sample to be tested infrared spectrum is with the standard IR spectrogram in 4000cm-1To 650cm-1Wave-number range in phase
Close property be more than or equal to 99%, standard deviation be less than or equal to 5%, the matrix pitch sample to be tested it is up-to-standard.
2. the method according to claim 1 using decaying In situ ATR-FTIR standard spectrogram identification asphalt quality,
It is characterized in that, the experiment parameter of test experiments is as follows：Scanning range is 4000cm-1To 650cm-1, scanning times are 32 times, point
Resolution is 4cm-1。
3. the method according to claim 1 using decaying In situ ATR-FTIR standard spectrogram identification asphalt quality,
It is characterized in that, when determining repeatability error range, arbitrary two groups of repeatability infrared spectrums are in 4000cm-1To 650cm-1Wave
Correlation in number range is more than or equal to 99.63%, and standard deviation is less than or equal to 0.43%.
4. the method according to claim 1 using decaying In situ ATR-FTIR standard spectrogram identification asphalt quality,
It is characterized in that, when determining reproducibility error range, arbitrary two groups of reproducibility infrared spectrums are in 4000cm-1To 650cm-1Wave
Correlation in number range is more than or equal to 99.09%, and standard deviation is less than or equal to 3.5%.
5. the method according to claim 1 using decaying In situ ATR-FTIR standard spectrogram identification asphalt quality,
It is characterized in that, the statistics meter that 3 groups of reperformance test infrared spectrums and 6 groups of reproducibility test infrared spectrums are carried out to spectrogram
The step of calculating, obtaining standard IR spectrogram of the average spectrogram as matrix pitch standard sample include：
Y value corresponding with 6 groups of reproducibility test each data point X values of infrared spectrum to 3 groups of reperformance test infrared spectrums
It sums；
Using the arithmetic mean of instantaneous value obtained by the summation of acquisition divided by spectrogram number as the average spectrogram of the matrix pitch standard sample,
The average spectrogram is the standard IR spectrogram of the matrix pitch standard sample.
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| CN201810172290.6A CN108398399A (en) | 2018-03-01 | 2018-03-01 | The method for identifying asphalt quality using decaying In situ ATR-FTIR standard spectrogram |
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| CN201810172290.6A CN108398399A (en) | 2018-03-01 | 2018-03-01 | The method for identifying asphalt quality using decaying In situ ATR-FTIR standard spectrogram |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109406436A (en) * | 2018-10-30 | 2019-03-01 | 甘肃省交通规划勘察设计院股份有限公司 | Road asphalt based on infrared spectroscopy big data quickly detects method for early warning |
| CN111337448A (en) * | 2020-03-26 | 2020-06-26 | 杭州老爸标准技术集团有限公司 | Method for identifying cosmetics based on infrared spectrum technology |
| CN113340930A (en) * | 2021-05-17 | 2021-09-03 | 鞍山钢铁冶金炉材科技有限公司 | Method for identifying whether asphalt for converter large-surface feed supplement is adulterated or not by one-step method |
-
2018
- 2018-03-01 CN CN201810172290.6A patent/CN108398399A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109406436A (en) * | 2018-10-30 | 2019-03-01 | 甘肃省交通规划勘察设计院股份有限公司 | Road asphalt based on infrared spectroscopy big data quickly detects method for early warning |
| CN111337448A (en) * | 2020-03-26 | 2020-06-26 | 杭州老爸标准技术集团有限公司 | Method for identifying cosmetics based on infrared spectrum technology |
| CN113340930A (en) * | 2021-05-17 | 2021-09-03 | 鞍山钢铁冶金炉材科技有限公司 | Method for identifying whether asphalt for converter large-surface feed supplement is adulterated or not by one-step method |
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