CN104297200B - A kind of method that infrared spectrum differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique - Google Patents
A kind of method that infrared spectrum differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique Download PDFInfo
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Abstract
The present invention relates to a kind of method that infrared spectrum differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique, the method comprises the following steps: (1) adopt ATR adnexa to respectively obtain the infrared spectrogram of gathered commercially available various brands Colophonium；(2) respectively the infrared spectrogram of gathered commercially available various brands Colophonium is smoothed according to a conventional method, it is determined that the characteristic absorption peak of standard specimen Colophonium；(3) the gas chromatogram of commercially available various brands Colophonium is gathered with gas chromatograph；(4) data in the gas chromatogram of the commercially available various brands Colophonium standard specimen of software processes are distilled with High Temperature Simulation；(5) unknown Colophonium is carried out examination of infrared spectrum, obtain the characteristic absorption peak of unknown Colophonium；(6) unknown Colophonium is carried out gas chromatogram test, obtain the gas chromatogram of unknown Colophonium；(7) the data in the gas chromatogram of unknown Colophonium are processed, obtain the boiling range of unknown Colophonium；(8) respectively the unknown Colophonium and standard specimen Colophonium are contrasted, finally determine the brand of unknown Colophonium.The present invention testing time is short, and result is accurate.
Description
Technical field
The present invention relates to road engineering application, particularly relate to a kind of method that infrared spectrum differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique.
Background technology
Along with the high speed development of Chinese national economy, highway construction mileage is rapid increase trend.Ending 2010, China's highway breaches 7.5 ten thousand kilometers, and in country " 12 " planning, total mileage of highway is up to 550 ~ 6,000,000 kilometers.Bituminous paving obtains the extensive use of countries in the world owing to noise is low, flatness is good, be easy to the advantages such as maintenance, wherein the highway of more than 90% all adopts bituminous paving, Colophonium is the cementitious matter in pavement material, the quality of its quality has directly influenced the quality on road surface, so, the evaluation to asphalt quality is the emphasis that for many years various countries are studied.Investigation display China Asphalt market still suffers from underproof asphaltic products, and fake and forged phenomenon happens occasionally.
Traditional simple physical property detection method not only takes time and effort, and is subject to the impact of the additive such as modifying agent and stabilizer, the easy distortion of result of the test.Complexity due to Colophonium chemical property, Colophonium specification develops to be tested for physical characteristic, adopt the such as test such as needle penetration, softening point, ductility, the test of these physical characteristics carries out under standard test temperature, test result is used to determine whether material meets the standard of specification, three norms is the traditional detection method passing judgment on asphalt performance, and its shirtsleeve operation is that other method is not replaced, and is still the main method of highway industry detection Colophonium so far.But these method of testings have a lot of limitation, there is also following problems: although (1) three norms is simple to operate, but Colophonium to dissolve in advance, from become mould, maintenance to test for up to 4 ~ 5h, consuming time longer；(2) it is experimental for having many tests, say, that first to have field experience before test obtains significant information, penetration test is an example thus, needle penetration embodies the denseness of Colophonium, but any Asphalt Penetration is with the relation between performance, it is necessary to obtained by experience；(3) situation when needle penetration and the index such as viscosity, softening point can only reflect specified temp, specific load action, and the performance difference of Colophonium under other condition is difficult to embody, likely different Colophonium can be classified as same levels, and actually, these Colophoniumes are likely under different temperature conditions, Performance Characteristics is entirely different, it is possible to be not suitable for paved roads or local climate, thus causing the generation of pavement disease.Therefore, these method of testings can not identify qualification completely, reflects performance and its performance on road surface of Colophonium comprehensively.
1993, Bureau of Public Road completes SHRP plan, its important research achievement is exactly Superpave, in Superpave, establish new Colophonium appraisement system, new index passes through engineering principles physical properties, and directly links together with field performance, it is possible to more fully reflect the pavement performance of Colophonium.But SHRP Testing index is wasted time and energy, and apparatus expensive, asphalt quality all can not be judged timely and effectively.
Summary of the invention
The technical problem to be solved is to provide a kind of method that infrared spectrum fast and accurately differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique.
For solving the problems referred to above, the method that a kind of infrared spectrum of the present invention differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique, comprise the following steps:
(1) adopt Fourier infrared spectrograph attenuated total reflectance (ATR) adnexa first to gather the infrared spectrum of background, then gather commercially available various brands Colophonium spectrogram, last background correction more respectively, namely respectively obtain the infrared spectrogram of gathered commercially available various brands Colophonium；
(2) respectively the infrared spectrogram of described gathered commercially available various brands Colophonium is carried out smooth base correction process according to a conventional method, obtain the optimization infrared spectrogram of standard specimen Colophonium, it is determined that characteristic absorption peak；
(3) gather the gas chromatogram of commercially available various brands Colophonium with gas chromatograph, its method comprises the following steps:
1. gas chromatograph configuration detector is flame ionization ditector, chromatographic column is High Temperature Simulation distillation chromatographic column specially；
After 2. gas chromatograph service condition is set, run gas chromatograph and chem workstation thereof, detect solvent, set up blank analysis baseline；
3. boiling point is corrected by retention time: according to a conventional method Polywax655 is dissolved in Carbon bisulfide, then the n-alkane of C5-C18 is added, namely AgilentSimDis corrects mixture 2, as correction sample, then test under the service condition 2. identical with described step, the boiling point correction data of sample must be corrected, and these data are stored in gas chromatograph chem workstation；
4. the mensuration of reference oil: be dissolved in solvent by the reference oil specified in gas chromatograph, then test reference oil under the service condition 2. identical with described step, obtains the gas chromatogram of reference oil, and these data is stored in gas chromatograph chem workstation；The volume ratio of described solvent and described reference oil is 45 ~ 50mL:1 ~ 2mL；
5. commercially available various brands Colophonium standard specimen is analyzed: will be dissolved in solvent by commercially available various brands Colophonium standard specimen respectively, then under the service condition 2. identical with described step, measure commercially available various brands Colophonium standard specimen respectively, obtain the gas chromatogram of commercially available various brands Colophonium standard specimen, and these data are stored in gas chromatograph chem workstation；The volume ratio of described solvent and described commercially available various brands Colophonium standard specimen is 45 ~ 50mL:1 ~ 2mL；
(4) distilling data in the gas chromatogram of commercially available various brands Colophonium standard specimen described in software processes with High Temperature Simulation, its method comprises the following steps:
Click entrance sample analysis hurdle, choose gas chromatograph chem workstation, call the calculating masterplate that software carries, it is determined that after Report Type, click confirmation method；
Carry out baseline analysis, deduct the blank analysis baseline of described step 2. gained；
Set up checking list: call the boiling point correction data of step 3. gained described in gas chromatograph chem workstation, be corrected sample analysis, set up calibration trace and checking list；
Calculate reference oil: call step 4. gained described in gas chromatograph chem workstation reference oil gas chromatogram in data, use High Temperature Simulation distillation software, calculate boiling Range Distribution Analysis result, reference data in the boiling Range Distribution Analysis measurement result of reference oil and software for calculation being compared, the boiling Range Distribution Analysis result of reference oil should in the repeatability interval of listed reference oil in software；
Calculate commercially available various brands Colophonium standard specimen: call the MN.txt file of the commercially available various brands Colophonium standard specimen of step 5. gained described in gas chromatograph chem workstation, use High Temperature Simulation distillation software, calculate the boiling Range Distribution Analysis result measuring described commercially available various brands Colophonium standard specimen；
Report form: start to calculate the yield of described commercially available various brands Colophonium standard specimen from experiment, when yield is 0.5%, this temperature is decided to be the initial boiling point (IBP) of sample, is then spaced apart the boiling range as commercially available various brands Colophonium standard specimen of the integral point temperature under this response rate corresponding to 1% using the response rate；
(5) by described step, unknown Colophonium is carried out examination of infrared spectrum by (1) ~ method (2), obtains unknown Colophonium infrared spectrogram, it is determined that its characteristic absorption peak；
(6) by described step method (3), unknown Colophonium is carried out gas chromatogram test, obtain the gas chromatogram of unknown Colophonium；
(7) process by the data in the described step method (4) gas chromatogram to unknown Colophonium, obtain the boiling range of unknown Colophonium；
(8) respectively the characteristic absorption peak of the characteristic absorption peak of the unknown Colophonium of described step (5) gained and the standard specimen Colophonium of absworption peak area and described step (2) gained and absworption peak area are contrasted, and respectively initial boiling point in the boiling Range Distribution Analysis data of initial boiling point in the boiling Range Distribution Analysis data of the unknown Colophonium of described step (7) gained and the commercially available various brands Colophonium standard specimen of described step gained is contrasted, according to the principle that bitumen recovery rate corresponding at the different or identical temperature of the temperature that the identical response rate is corresponding is different, finally determine the brand of unknown Colophonium.
The working condition of described step (1) middle Fourier infrared spectrograph refers to that spectral scan ranges for 800 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1。
Described step 2. middle gas chromatogram service condition refers to stove case initial temperature 45 DEG C, stove case 0min at the beginning, stove case 10 DEG C/min of journey speed, stove case final temperature 430 DEG C, stove case terminal hour 10min, injection port initial temperature 80 DEG C, injection port 10 DEG C/min of journey speed, 430 DEG C/min of injection port final temperature, post flow 8mL/min, detector temperature 435 DEG C, hydrogen 40mL/min, air 400mL/min, assisted gas 15mL/min, sample size 0.4uL, sample quality concentration 2.0%.
Described step 4. with described step 5. in solvent each mean the one in toluene, Carbon bisulfide, dichloroethylene.
The working condition of described step (1) middle Fourier infrared spectrograph refers to that spectral scan ranges for 800 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1。
Described step 2. middle gas chromatogram service condition refers to stove case initial temperature 45 DEG C, stove case 0min at the beginning, stove case 10 DEG C/min of journey speed, stove case final temperature 430 DEG C, stove case terminal hour 10min, injection port initial temperature 80 DEG C, injection port 10 DEG C/min of journey speed, 430 DEG C/min of injection port final temperature, post flow 8mL/min, detector temperature 435 DEG C, hydrogen 40mL/min, air 400mL/min, assisted gas 15mL/min, sample size 0.4uL, sample quality concentration 2.0%.
Described step 4. with described step 5. in solvent each mean the one in toluene, Carbon bisulfide, dichloroethylene.
The present invention compared with prior art has the advantage that
1, the present invention adopts attenuated total reflectance method to gather infrared spectrum, is analyzed the molecular composition of Colophonium Semi-polarity component by infrared spectrometer, and combines with high temperature gas chromatography simulation distillating method, reaches to differentiate the purpose of Colophonium brand.
2, infrared spectrometer of the present invention is simple to operate, and Colophonium need not heat in advance or dissolve, and only need to heat scraper, take Colophonium sample and smear uniformly on crystal, and omnidistance needs 1 ~ 2min, and accuracy rate is high, and data are reliable.
3, the present invention has only to gather the infrared spectrogram of asphalt sample to be measured and boiling Range Distribution Analysis data, and the dependency of the infrared signature absworption peak and boiling Range Distribution Analysis data and standard specimen Colophonium of analyzing Colophonium to be measured can quickly identify with whether standard specimen Colophonium belongs to same brand Colophonium.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the 4 kinds of tested Colophoniumes gathered with infrared spectrometer.Wherein: (a) is a gram refining-90# Colophonium, and (b) is SK-90# Colophonium, and (c) is western petrochemical industry-90# Colophonium, and (d) is Zhenghai-90# Colophonium.
Fig. 2 is the gas chromatogram of 4 kinds of tested Colophoniumes that gas chromatogram gathers.Wherein: (a) is a gram refining-90# Colophonium, and (b) is SK-90# Colophonium, and (c) is western petrochemical industry-90# Colophonium, and (d) is Zhenghai-90# Colophonium.
Fig. 3 is the infrared spectrogram comparison of four kinds of Colophoniumes.
Fig. 4 is the gas chromatogram comparison of four kinds of Colophoniumes.
Fig. 5 is the constituent content comparison that four kinds of Colophonium different boiling are interval.
Fig. 6 is the infrared spectrum comparison of censorship gram refining-90# Colophonium and standard specimen gram refining-90# Colophonium.
Fig. 7 is the constituent content comparison chart that censorship gram refining-90# Colophonium is interval with standard specimen gram refining-90# Colophonium different boiling.
Detailed description of the invention
A kind of method that infrared spectrum differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique, comprises the following steps:
(1) adopt Fourier infrared spectrograph attenuated total reflectance (ATR) adnexa first to gather the infrared spectrum of background, then gather commercially available various brands Colophonium spectrogram, last background correction more respectively, namely respectively obtain the infrared spectrogram of gathered commercially available various brands Colophonium.
Wherein: the working condition of Fourier infrared spectrograph refers to that spectral scan ranges for 800 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1。
(2) respectively the infrared spectrogram of gathered commercially available various brands Colophonium is carried out smooth base correction process according to a conventional method, obtain the optimization infrared spectrogram of standard specimen Colophonium, it is determined that characteristic absorption peak.
(3) gather the gas chromatogram of commercially available various brands Colophonium with gas chromatograph, its method comprises the following steps:
1. gas chromatograph configuration detector is flame ionization ditector, chromatographic column is High Temperature Simulation distillation chromatographic column specially.
After 2. gas chromatograph service condition is set, run gas chromatograph and chem workstation thereof, detect solvent, set up blank analysis baseline.
Wherein: gas chromatogram service condition refers to stove case initial temperature 45 DEG C, stove case 0min at the beginning, stove case 10 DEG C/min of journey speed, stove case final temperature 430 DEG C, stove case terminal hour 10min, injection port initial temperature 80 DEG C, injection port 10 DEG C/min of journey speed, 430 DEG C/min of injection port final temperature, post flow 8mL/min, detector temperature 435 DEG C, hydrogen 40mL/min, air 400mL/min, assisted gas 15mL/min, sample size 0.4uL, sample quality concentration 2.0%.
3. boiling point is corrected by retention time: according to a conventional method Polywax655 is dissolved in Carbon bisulfide, then the n-alkane of C5-C18 is added, namely AgilentSimDis corrects mixture 2, as correction sample, then test under the service condition 2. identical with step, the boiling point correction data of sample must be corrected, and these data are stored in gas chromatograph chem workstation.
4. the mensuration of reference oil: be dissolved in solvent by the reference oil specified in gas chromatograph, then test reference oil under the service condition 2. identical with step, obtains the gas chromatogram of reference oil, and these data is stored in gas chromatograph chem workstation.
Wherein: the volume ratio of solvent and reference oil is 45 ~ 50mL:1 ~ 2mL.
Solvent each means the one in toluene, Carbon bisulfide, dichloroethylene.
5. commercially available various brands Colophonium standard specimen is analyzed: will be dissolved in solvent by commercially available various brands Colophonium standard specimen respectively, then under the service condition 2. identical with step, measure commercially available various brands Colophonium standard specimen respectively, obtain the gas chromatogram of commercially available various brands Colophonium standard specimen, and these data are stored in gas chromatograph chem workstation.
Wherein: the volume ratio of solvent and commercially available various brands Colophonium standard specimen is 45 ~ 50mL:1 ~ 2mL.
Solvent each means the one in toluene, Carbon bisulfide, dichloroethylene.
(4) distill data in the gas chromatogram of the commercially available various brands Colophonium standard specimen of software processes with High Temperature Simulation, its method comprises the following steps:
Click entrance sample analysis hurdle, choose gas chromatograph chem workstation, call the calculating masterplate that software carries, it is determined that after Report Type, click confirmation method；
Carry out baseline analysis, deduct the blank analysis baseline of described step 2. gained；
Set up checking list: call the boiling point correction data of step 3. gained in gas chromatograph chem workstation, be corrected sample analysis, set up calibration trace and checking list；
Calculate reference oil: call step 4. gained described in gas chromatograph chem workstation reference oil gas chromatogram in data, use High Temperature Simulation distillation software, calculate boiling Range Distribution Analysis result, reference data in the boiling Range Distribution Analysis measurement result of reference oil and software for calculation being compared, the boiling Range Distribution Analysis result of reference oil should in the repeatability interval of listed reference oil in software；
Calculate commercially available various brands Colophonium standard specimen: call the MN.txt file of the commercially available various brands Colophonium standard specimen of step 5. gained in gas chromatograph chem workstation, use High Temperature Simulation distillation software, calculate the boiling Range Distribution Analysis result measuring commercially available various brands Colophonium standard specimen；
Report form: start to calculate the yield of commercially available various brands Colophonium standard specimen from experiment, when yield is 0.5%, this temperature is decided to be the initial boiling point (IBP) of sample, is then spaced apart the boiling range as commercially available various brands Colophonium standard specimen of the integral point temperature under this response rate corresponding to 1% using the response rate.
(5) by step, unknown Colophonium is carried out examination of infrared spectrum by (1) ~ method (2), obtains unknown Colophonium infrared spectrogram, it is determined that its characteristic absorption peak.
(6) by step method (3), unknown Colophonium is carried out gas chromatogram test, obtain the gas chromatogram of unknown Colophonium.
(7) process by the data in the step method (4) gas chromatogram to unknown Colophonium, obtain the boiling range of unknown Colophonium.
(8) respectively the characteristic absorption peak of the characteristic absorption peak of the unknown Colophonium of step (5) gained and the standard specimen Colophonium of absworption peak area and step (2) gained and absworption peak area are contrasted, and respectively initial boiling point in the boiling Range Distribution Analysis data of initial boiling point in the boiling Range Distribution Analysis data of the unknown Colophonium of step (7) gained and the commercially available various brands Colophonium standard specimen of step gained is contrasted, according to the principle that bitumen recovery rate corresponding at the different or identical temperature of the temperature that the identical response rate is corresponding is different, finally determine the brand of unknown Colophonium.
BelowEmbodimentIn, all adopt the NICOLET6700 type Fourier infrared spectrograph that Thermo Fischer Scient Inc. of the U.S. produces to gather infrared spectrum, all adopt Agilent company of U.S. 7890A gas chromatograph to gather the gas chromatogram of Colophonium.
Fourier infrared spectrograph installs attenuated total reflectance adnexa (ATR), after instrument identifies automatically, carries out the collimation of optical table, arranges collection background medium for after 1000min after having collimated, and spectral scan ranges for 650 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1.After atr crystal wiped clean, carry out background collection and preserve.Insert sampling in Colophonium by after scraper heating, while hot Colophonium is spread upon the spectrogram of atr crystal collected specimens and preserves.
7890A gas chromatograph, configuration Cool-on-column inlet, high temperature resistant stainless steel capillary column, flame ionization ditector (FID) and High Temperature Simulation distillation software.
Embodiment 1
For a gram refining-90# Colophonium, concrete testing procedure is as follows:
1, ATR adnexa installed by spectrogrph, arranges spectral scan and ranges for 650 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1.First gather background spectrogram, then gather a gram refining-90# Colophonium spectrogram, see Fig. 1 a.
2, weigh a gram refining-90# Colophonium 0.0396g, add 2.0002gCS2Dissolve.Operation method, tests Colophonium.Obtain the gas chromatogram 2a of Colophonium.
3, call High Temperature Simulation distillation software, deduct baseline, set up the retention time checking list to boiling point；Call reference oil test data, it is determined that the response factor of instrument；Analyze a gram form and aspect chromatographic data for refining-90# Colophonium, obtain initial boiling point and the boiling point distribution curve of this Colophonium, in Table 1.
1 gram of table refining-90# Colophonium boiling range cutting compartmental results
Embodiment 2
For SK-90# Colophonium, step is as follows:
1, ATR adnexa installed by spectrogrph, arranges spectral scan and ranges for 650 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1.First gather background spectrogram, then gather SK-90# Colophonium spectrogram, see Fig. 1 b.
2, weigh SK-90# Colophonium 0.040g and add 2.0125gCS2Dissolve.Operation method, tests Colophonium.Obtain the gas chromatogram 2b of Colophonium.
3, call High Temperature Simulation distillation software, deduct baseline, set up the retention time checking list to boiling point；Call reference oil test data, it is determined that the response factor of instrument；Analyze the form and aspect chromatographic data of SK-90# Colophonium, obtain initial boiling point and the boiling point distribution curve of this Colophonium, in Table 2.
Table 2SK90-# Colophonium boiling range cutting compartmental results
Embodiment 3
To the west of petrochemical industry-90# Colophonium be example, concrete testing procedure is as follows:
1, ATR adnexa installed by spectrogrph, arranges spectral scan and ranges for 650 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1.First gather background spectrogram, then gather gram western petrochemical industry-90# Colophonium spectrogram, see Fig. 1 c.
2, weigh western petrochemical industry-90# Colophonium 0.0403, add 2.012gCS2Dissolve.Operation method, tests Colophonium.Obtain the gas chromatogram of Colophonium, see Fig. 2 c.
3, call High Temperature Simulation distillation software, deduct baseline, set up the retention time checking list to boiling point；Call reference oil test data, it is determined that the response factor of instrument；Analyze the form and aspect chromatographic data of western petrochemical industry-90# Colophonium, obtain initial boiling point and the boiling point distribution curve of this Colophonium, in Table 3.
Table 3 western petrochemical industry-90# Colophonium boiling range cutting compartmental results
Embodiment 4
For Zhenghai-90# Colophonium, concrete testing procedure is as follows:
1, ATR adnexa installed by spectrogrph, arranges spectral scan and ranges for 650 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1.First gather background spectrogram, then gather Colophonium spectrogram, see Fig. 1 d.
2, weigh Zhenghai-90# Colophonium 0.0389g, add 1.9876CS2Dissolve.Operation method, tests Colophonium.Obtain the gas chromatogram 2d of Colophonium.
3, call High Temperature Simulation distillation software, deduct baseline, set up the retention time checking list to boiling point；Call reference oil test data, it is determined that the response factor of instrument；Analyze the form and aspect chromatographic data of Zhenghai-90# Colophonium, obtain initial boiling point and the boiling point distribution curve of this Colophonium, in Table 4.
Table 4 Zhenghai-90# boiling range cutting compartmental results
As shown in Fig. 3, Fig. 4, Fig. 5, the Colophonium infrared spectrum of the 4 kinds of brands characteristic absorption peak in finger print region has obvious difference, the component that simultaneously gas chromatogram of 4 kinds of brand Colophoniumes and different temperatures interval are contained is also entirely different, can be distinguished by the Colophonium of various brands accordingly.
Embodiment 5
Certain second grade highway censorship gram refining-90# Colophonium, step is as follows:
1, ATR adnexa installed by spectrogrph, arranges spectral scan and ranges for 650 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1.First gather background spectrogram, then gather censorship Colophonium spectrogram, refine-90# Colophonium spectrogram comparison with standard specimen gram, see Fig. 6.
2, weigh a gram refining-90# Colophonium 0.0421g, add 2.0019gCS2Dissolve.Operation method, tests Colophonium.Obtain the gas chromatogram of Colophonium, contrast with standard specimen Colophonium, see Fig. 7.
3, the infrared spectrogram of Colophonium to be measured and meteorological chromatogram are entirely different with standard specimen Colophonium, infer that Colophonium is converted through overmulling and is in harmonious proportion, are not a gram refining 90# Colophonium.
Above-mentionedEmbodimentIt is the further description to the present invention, but does not mean that any limitation of the invention.When thought above-mentioned without departing from the present invention, the various substitute modes made according to ordinary skill knowledge and conventional means or change, it is all contained within the present invention.
Claims (4)
1. the method that infrared spectrum differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique, comprises the following steps:
(1) adopt Fourier infrared spectrograph attenuated total reflectance adnexa first to gather the infrared spectrum of background, then gather commercially available various brands Colophonium spectrogram, last background correction more respectively, namely respectively obtain the infrared spectrogram of gathered commercially available various brands Colophonium；
(2) respectively the infrared spectrogram of described gathered commercially available various brands Colophonium is carried out smooth base correction process according to a conventional method, obtain the optimization infrared spectrogram of standard specimen Colophonium, it is determined that characteristic absorption peak；
(3) gather the gas chromatogram of commercially available various brands Colophonium with gas chromatograph, its method comprises the following steps:
1. gas chromatograph configuration detector is flame ionization ditector, chromatographic column is High Temperature Simulation distillation chromatographic column specially；
After 2. gas chromatograph service condition is set, run gas chromatograph and chem workstation thereof, detect solvent, set up blank analysis baseline；
3. boiling point is corrected by retention time: according to a conventional method Polywax655 is dissolved in Carbon bisulfide, then the n-alkane of C5-C18 is added, namely obtain AgilentSimDis and correct mixture 2, as correction sample, then test under the service condition 2. identical with described step, the boiling point correction data of sample must be corrected, and these data are stored in gas chromatograph chem workstation；
4. the mensuration of reference oil: be dissolved in solvent by the reference oil specified in gas chromatograph, then test reference oil under the service condition 2. identical with described step, obtains the gas chromatogram of reference oil, and these data is stored in gas chromatograph chem workstation；The volume ratio of described solvent and described reference oil is 45 ~ 50mL:1 ~ 2mL；
5. commercially available various brands Colophonium standard specimen is analyzed: be dissolved in solvent by commercially available various brands Colophonium standard specimen respectively, then under the service condition 2. identical with described step, measure commercially available various brands Colophonium standard specimen respectively, obtain the gas chromatogram of commercially available various brands Colophonium standard specimen, and these data are stored in gas chromatograph chem workstation；The volume ratio of described solvent and described commercially available various brands Colophonium standard specimen is 45 ~ 50mL:1 ~ 2mL；
(4) distilling the data in the gas chromatogram of commercially available various brands Colophonium standard specimen described in software processes with High Temperature Simulation, its method comprises the following steps:
Click entrance sample analysis hurdle, choose gas chromatograph chem workstation, call the calculating masterplate that software carries, it is determined that after Report Type, click confirmation method；
Carry out baseline analysis, deduct the blank analysis baseline of described step 2. gained；
Set up checking list: call the boiling point correction data of step 3. gained described in gas chromatograph chem workstation, be corrected sample analysis, set up calibration trace and checking list；
Calculate reference oil: call step 4. gained described in gas chromatograph chem workstation reference oil gas chromatogram in data, use High Temperature Simulation distillation software, calculate boiling Range Distribution Analysis result, reference data in the boiling Range Distribution Analysis measurement result of reference oil and software for calculation being compared, the boiling Range Distribution Analysis result of reference oil should in the repeatability interval of listed reference oil in software；
Calculate commercially available various brands Colophonium standard specimen: call the MN.txt file of the commercially available various brands Colophonium standard specimen of step 5. gained described in gas chromatograph chem workstation, use High Temperature Simulation distillation software, calculate the boiling Range Distribution Analysis result measuring described commercially available various brands Colophonium standard specimen；
Report form: start to calculate the response rate of described commercially available various brands Colophonium standard specimen from experiment, when the response rate is 0.5%, this temperature is decided to be the initial boiling point of sample, is then spaced apart the boiling range as commercially available various brands Colophonium standard specimen of the integral point temperature under this response rate corresponding to 1% using the response rate；
(5) by described step, unknown Colophonium is carried out examination of infrared spectrum by (1) ~ method (2), obtains unknown Colophonium infrared spectrogram, it is determined that its characteristic absorption peak；
(6) by described step method (3), unknown Colophonium is carried out gas chromatogram test, obtain the gas chromatogram of unknown Colophonium；
(7) process by the data in the described step method (4) gas chromatogram to unknown Colophonium, obtain the boiling range of unknown Colophonium；
(8) respectively the characteristic absorption peak of the characteristic absorption peak of the unknown Colophonium of described step (5) gained and the standard specimen Colophonium of absworption peak area and described step (2) gained and absworption peak area are contrasted, and respectively initial boiling point in the boiling Range Distribution Analysis data of initial boiling point in the boiling Range Distribution Analysis data of the unknown Colophonium of described step (7) gained and the commercially available various brands Colophonium standard specimen of described step gained is contrasted, according to the principle that bitumen recovery rate corresponding at the different or identical temperature of the temperature that the identical response rate is corresponding is different, finally determine the brand of unknown Colophonium.
2. the method that a kind of infrared spectrum as claimed in claim 1 differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique, it is characterised in that: the working condition of described step (1) middle Fourier infrared spectrograph refers to that spectral scan ranges for 800 ~ 4000cm-1, scanning times 32 times, sweep spacing 2cm-1。
3. the method that a kind of infrared spectrum as claimed in claim 1 differentiates Colophonium brand in conjunction with High Temperature Simulation distillation technique, it is characterized in that: described step 2. middle gas chromatogram service condition refers to stove case initial temperature 45 DEG C, stove case 0min at the beginning, stove case 10 DEG C/min of journey speed, stove case final temperature 430 DEG C, stove case terminal hour 10min, injection port initial temperature 80 DEG C, injection port 10 DEG C/min of journey speed, 430 DEG C/min of injection port final temperature, post flow 8mL/min, detector temperature 435 DEG C, hydrogen 40mL/min, air 400mL/min, assisted gas 15mL/min, sample size 0.4uL, sample quality concentration 2.0%.
4. a kind of infrared spectrum as claimed in claim 1 in conjunction with High Temperature Simulation distillation technique differentiate Colophonium brand method, it is characterised in that: described step 4. with described step 5. in solvent each mean the one in toluene, Carbon bisulfide, dichloroethylene.
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| CN108169164A (en) * | 2017-12-22 | 2018-06-15 | 江苏中路工程技术研究院有限公司 | It is a kind of that the method that trichloro ethylene is remained in recycling pitch is detected using FTIR |
| CN108398398A (en) * | 2018-02-12 | 2018-08-14 | 山西省交通科学研究院 | The method for identifying asphalt quality using decaying In situ ATR-FTIR standard spectrogram |
| 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 |
| CN110108865A (en) * | 2019-04-28 | 2019-08-09 | 河海大学 | A kind of mechanism of modification research method of used oil to asphalt material |
| CN110609008A (en) * | 2019-08-28 | 2019-12-24 | 甘肃省交通规划勘察设计院股份有限公司 | Rapid assessment method for RAP (rapid asphalt ratio) mixing amount in recycled asphalt mixture based on infrared spectrum |
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