CN104297200A - Method for identifying asphalt brands through infrared spectrum combined with high-temperature simulation and distillation technology - Google Patents
Method for identifying asphalt brands through infrared spectrum combined with high-temperature simulation and distillation technology Download PDFInfo
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Abstract
The invention relates to a method for identifying asphalt brands through an infrared spectrum combined with a high-temperature simulation and distillation technology. The method comprises the following steps: (1) using an ATR (attenuated total reflectance) accessory for respectively obtaining infrared spectrum charts of collected asphalt of each brand sold in a market; (2) respectively performing smooth processing on the infrared spectrum charts of the collected asphalt of each brand sold in the market according to a conventional method, and determining the characteristic absorption peaks of prototype asphalt; (3) using a gas chromatograph for collecting the gas chromatogram of the asphalt of each brand sold in the market; (4) using high-temperature simulation and distillation software for processing data in the gas chromatogram of the asphalt prototype of each sale sold in the market; (5) performing an infrared spectrum test on unknown asphalt, and obtaining the characteristic absorption peak of the unknown asphalt; (6) performing a gas chromatography test on the unknown asphalt, and obtaining the gas chromatogram of the unknown asphalt; (7) processing the data in the gas chromatogram of the unknown asphalt, and obtaining the boiling range of the unknown asphalt; (8) respectively comparing the unknown asphalt with the prototype asphalt, and finally determining the brand of the unknown asphalt. The method disclosed by the invention has the advantages of short test time and accurate results.
Description
Technical field
The present invention relates to road engineering application, particularly relate to a kind of infrared spectrum differentiates pitch brand method in conjunction with High Temperature Simulation distillation technique.
Background technology
Along with the high speed development of Chinese national economy, highway construction mileage is quick ascendant trend.End 2010, China's highway breaches 7.5 ten thousand kilometers, and in country " 12 " planning, total mileage of highway will reach 550 ~ 6,000,000 kilometers.Bituminous pavement is because noise is low, flatness is good, be convenient to the widespread use that the advantages such as maintenance obtain countries in the world, wherein the highway of more than 90% all adopts bituminous pavement, pitch is the cementitious matter in pavement material, the quality of its quality has directly had influence on the quality on road surface, so, be the emphasis of for many years various countries' research to the evaluation of asphalt quality.Still there is underproof asphaltic products in investigation display China Asphalt market, 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 adjuvant such as modifier and stabilizing agent, the easy distortion of test findings.Due to the complicacy of pitch chemical property, pitch specification develops to be tested for physical characteristics, adopt the tests such as such as pen., softening point, ductility, the test of these physical characteristicss is carried 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 that highway industry detects pitch so far.But these method of testings have a lot of limitation, also there are following problems: although (1) three norms is simple to operate, pitch will dissolve in advance, from become mould, maintenance to test for up to 4 ~ 5h, consuming time longer; (2) there are many tests to be experimental, that is, before test obtains significant information, first will have on-site experience, penetration test is exactly such example, pen. embodies the denseness of pitch, but any Asphalt Penetration is with the relation between performance, must be obtained by experience; (3) pen. and the index such as viscosity, softening point can only reflect the situation under specified temp, specific load action condition, and the performance difference of pitch under other condition is difficult to embody, likely different pitch can be classified as same levels, and in fact, these pitches may under different temperature conditions, Performance Characteristics is completely different, is likely not suitable for paved roads or local climate, thus causes the generation of pavement disease.Therefore, these method of testings can not identify qualification completely, reflect performance and its performance on road surface of pitch comprehensively.
1993, Bureau of Public Road completes SHRP plan, its important research achievement is exactly Superpave, in Superpave, establish new pitch appraisement system, new index by engineering principles physical properties, and is contacted directly together with field performance, more fully can reflect the pavement performance of pitch.But SHRP Testing index is wasted time and energy, and apparatus expensive, all can not judge asphalt quality timely and effectively.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of infrared spectrum fast and accurately differentiates pitch brand method in conjunction with High Temperature Simulation distillation technique.
For solving the problem, a kind of infrared spectrum of the present invention differentiates the method for pitch brand in conjunction with High Temperature Simulation distillation technique, comprises the following steps:
(1) adopt Fourier infrared spectrograph attenuated total reflection (ATR) annex first to gather the infrared spectrum of background, and then gather commercially available various brands pitch spectrogram respectively, last background correction, namely obtain the infrared spectrogram of gathered commercially available various brands pitch respectively;
(2), respectively to the infrared spectrogram smoothing baseline correction process according to a conventional method of described gathered commercially available various brands pitch, obtain the optimization infrared spectrogram of standard specimen pitch, determine characteristic absorption peak;
(3) gather the gas chromatogram of commercially available various brands pitch with gas chromatograph, its method comprises the following steps:
1. gas chromatograph configuration detector be flame ionization ditector, chromatographic column be 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. retention time corrects boiling point: according to a conventional method Polywax 655 is dissolved in carbon disulphide, then the n-alkane of C5-C18 is added, namely Agilent SimDis corrects No. 2, potpourri, 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 by these data stored in gas chromatograph chem workstation;
4. the mensuration of reference oil: the reference oil of specifying in gas chromatograph is dissolved in solvent, then test reference oil under the service condition 2. identical with described step, obtain the gas chromatogram of reference oil, and by these data stored in gas chromatograph chem workstation; The volume ratio of described solvent and described reference oil is 45 ~ 50 mL:1 ~ 2 mL;
5. commercially available various brands pitch standard specimen is analyzed: will be dissolved in solvent by commercially available various brands pitch standard specimen respectively, then under the service condition 2. identical with described step, commercially available various brands pitch standard specimen is measured respectively, obtain the gas chromatogram of commercially available various brands pitch standard specimen, and by these data stored in gas chromatograph chem workstation; The volume ratio of described solvent and described commercially available various brands pitch standard specimen is 45 ~ 50 mL:1 ~ 2 mL;
(4), by data in the gas chromatogram of commercially available various brands pitch standard specimen described in the process of High Temperature Simulation distillation software, its method comprises the following steps:
I is clicked and is entered sample analysis hurdle, chooses gas chromatograph chem workstation, calls the calculating masterplate that software carries, after determining Report Type, clicks confirmation method;
II carries out baseline analysis, deducts the blank analysis baseline of described step 2. gained;
III sets up table of corrections: the boiling point correction data calling the 3. gained of step described in gas chromatograph chem workstation, carries out the analysis of correction sample, sets up calibration curve and table of corrections;
IV computing reference oil: call the data in the gas chromatogram of the 4. reference oil of gained of step described in gas chromatograph chem workstation, use High Temperature Simulation distillation software, calculate boiling Range Distribution Analysis result, compare with reference to the reference data in the boiling Range Distribution Analysis measurement result of oil and software for calculation, the boiling Range Distribution Analysis result of reference oil should in the repeatability interval of listed reference oil in software;
V calculates commercially available various brands pitch standard specimen: the MN.txt file calling the 5. commercially available various brands pitch standard specimen of gained of step 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 pitch standard specimen;
VI report form: the yield calculating described commercially available various brands pitch standard specimen from experiment, when yield is 0.5%, this temperature is decided to be the initial boiling point (IBP) of sample, the integral point temperature under being then spaced apart corresponding to 1% this recovery using the recovery is as the boiling range of commercially available various brands pitch standard specimen;
By described step (1) ~ method (2) carries out examination of infrared spectrum to unknown pitch, obtains unknown pitch infrared spectrogram, determine its characteristic absorption peak;
(6) by described step method (3), gas chromatography test is carried out to unknown pitch, obtain the gas chromatogram of unknown pitch;
(7) by described step method (4), the data in the gas chromatogram of unknown pitch are processed, obtain the boiling range of unknown pitch;
Respectively by described step (5) the characteristic absorption peak of the unknown pitch of gained and absorption peak area and described step (2) the characteristic absorption peak of the standard specimen pitch of gained and absorption peak area contrast, and respectively initial boiling point in the boiling Range Distribution Analysis data of the commercially available various brands pitch standard specimen of initial boiling point and described step VI gained in the boiling Range Distribution Analysis data of the described step (7) unknown pitch of gained is contrasted, the principle that the bitumen recovery rate corresponding at different or identical temperature according to temperature corresponding to the identical recovery is different, finally determines the brand of unknown pitch.
Described step (1) in the condition of work of Fourier infrared spectrograph refer to that spectral scan scope is 800 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.
Described step 2. middle gas chromatography service condition refers to stove case initial temperature 45 DEG C, stove case 0min, stove case journey speed 10 DEG C/min, stove case final temperature 430 DEG C, stove case terminal hour 10min, injection port initial temperature 80 DEG C, injection port journey speed 10 DEG C/min, injection port final temperature 430 DEG C/min, post flow 8mL/min, detector temperature 435 DEG C, hydrogen 40mL/min, air 400 mL/min, assisted gas 15 mL/min, sample size 0.4uL, sample quality concentration 2.0% at the beginning.
Described step 4. with described step 5. in solvent all refer to one in toluene, carbon disulphide, dichloroethylene.
Described step (1) in the condition of work of Fourier infrared spectrograph refer to that spectral scan scope is 800 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.
Described step 2. middle gas chromatography service condition refers to stove case initial temperature 45 DEG C, stove case 0min, stove case journey speed 10 DEG C/min, stove case final temperature 430 DEG C, stove case terminal hour 10min, injection port initial temperature 80 DEG C, injection port journey speed 10 DEG C/min, injection port final temperature 430 DEG C/min, post flow 8mL/min, detector temperature 435 DEG C, hydrogen 40mL/min, air 400 mL/min, assisted gas 15 mL/min, sample size 0.4uL, sample quality concentration 2.0% at the beginning.
Described step 4. with described step 5. in solvent all refer to one in toluene, carbon disulphide, dichloroethylene.
The present invention compared with prior art has the following advantages:
1, the present invention adopts attenuated total reflection method to gather infrared spectrum, is analyzed the molecular composition of pitch Semi-polarity component, and combines with high temperature gas chromatography simulation distil method, reach the object differentiating pitch brand by infrared spectrometer.
2, infrared spectrometer of the present invention is simple to operate, and pitch need not heat in advance or dissolve, and only need heat scraper, get pitch sample and smear evenly on crystal, and omnidistance needs 1 ~ 2min, and accuracy rate is high, and data are reliable.
3, the present invention only needs the infrared spectrogram and the boiling Range Distribution Analysis data that gather asphalt sample to be measured, and the correlativity of the infrared signature absorption peak and boiling Range Distribution Analysis data and standard specimen pitch of analyzing pitch to be measured can identify whether belong to same brand pitch with standard specimen pitch fast.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of 4 kinds of tested pitches with infrared spectrometer collection.Wherein: (a) is a gram refining-90# pitch, and (b) is SK-90# pitch, and (c) is western petrochemical industry-90# pitch, and (d) is Zhenghai-90# pitch.
Fig. 2 is the gas chromatogram of 4 kinds of tested pitches that gas chromatography gathers.Wherein: (a) is a gram refining-90# pitch, and (b) is SK-90# pitch, and (c) is western petrochemical industry-90# pitch, and (d) is Zhenghai-90# pitch.
Fig. 3 is the infrared spectrogram comparison of four kinds of pitches.
Fig. 4 is the gas chromatogram comparison of four kinds of pitches.
Fig. 5 is the component concentration comparison in four kinds of pitch different boiling intervals.
Fig. 6 is the infrared spectrum comparison that censorship gram refining-90# pitch and standard specimen gram refine-90# pitch.
Fig. 7 is the component concentration comparison chart that censorship gram refining-90# pitch and standard specimen gram refine-90# pitch different boiling interval.
Embodiment
Infrared spectrum differentiates a method for pitch brand in conjunction with High Temperature Simulation distillation technique, comprises the following steps:
(1) adopt Fourier infrared spectrograph attenuated total reflection (ATR) annex first to gather the infrared spectrum of background, and then gather commercially available various brands pitch spectrogram respectively, last background correction, namely obtain the infrared spectrogram of gathered commercially available various brands pitch respectively.
Wherein: the condition of work of Fourier infrared spectrograph refers to that spectral scan scope is 800 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.
(2), respectively to the infrared spectrogram smoothing baseline correction process according to a conventional method of gathered commercially available various brands pitch, obtain the optimization infrared spectrogram of standard specimen pitch, determine characteristic absorption peak.
(3) gather the gas chromatogram of commercially available various brands pitch with gas chromatograph, its method comprises the following steps:
1. gas chromatograph configuration detector be flame ionization ditector, chromatographic column be 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 chromatography service condition refers to stove case initial temperature 45 DEG C, stove case 0min, stove case journey speed 10 DEG C/min, stove case final temperature 430 DEG C, stove case terminal hour 10min, injection port initial temperature 80 DEG C, injection port journey speed 10 DEG C/min, injection port final temperature 430 DEG C/min, post flow 8mL/min, detector temperature 435 DEG C, hydrogen 40mL/min, air 400 mL/min, assisted gas 15 mL/min, sample size 0.4uL, sample quality concentration 2.0% at the beginning.
3. retention time corrects boiling point: according to a conventional method Polywax 655 is dissolved in carbon disulphide, then the n-alkane of C5-C18 is added, namely Agilent SimDis corrects No. 2, potpourri, as correction sample, then test under the service condition 2. identical with step, the boiling point correction data of sample must be corrected, and by these data stored in gas chromatograph chem workstation.
4. the mensuration of reference oil: the reference oil of specifying in gas chromatograph is dissolved in solvent, then test reference oil under the service condition 2. identical with step, obtains the gas chromatogram of reference oil, and by these data stored in gas chromatograph chem workstation.
Wherein: the volume ratio of solvent and reference oil is 45 ~ 50 mL:1 ~ 2 mL.
Solvent all refers to the one in toluene, carbon disulphide, dichloroethylene.
5. commercially available various brands pitch standard specimen is analyzed: will be dissolved in solvent by commercially available various brands pitch standard specimen respectively, then under the service condition 2. identical with step, commercially available various brands pitch standard specimen is measured respectively, obtain the gas chromatogram of commercially available various brands pitch standard specimen, and by these data stored in gas chromatograph chem workstation.
Wherein: the volume ratio of solvent and commercially available various brands pitch standard specimen is 45 ~ 50 mL:1 ~ 2 mL.
Solvent all refers to the one in toluene, carbon disulphide, dichloroethylene.
(4), by data in the gas chromatogram of High Temperature Simulation distillation software process commercially available various brands pitch standard specimen, its method comprises the following steps:
I is clicked and is entered sample analysis hurdle, chooses gas chromatograph chem workstation, calls the calculating masterplate that software carries, after determining Report Type, clicks confirmation method;
II carries out baseline analysis, deducts the blank analysis baseline of described step 2. gained;
III sets up table of corrections: the boiling point correction data calling the 3. gained of step in gas chromatograph chem workstation, carries out the analysis of correction sample, sets up calibration curve and table of corrections;
IV computing reference oil: call the data in the gas chromatogram of the 4. reference oil of gained of step described in gas chromatograph chem workstation, use High Temperature Simulation distillation software, calculate boiling Range Distribution Analysis result, compare with reference to the reference data in the boiling Range Distribution Analysis measurement result of oil and software for calculation, the boiling Range Distribution Analysis result of reference oil should in the repeatability interval of listed reference oil in software;
V calculates commercially available various brands pitch standard specimen: the MN.txt file calling the 5. commercially available various brands pitch standard specimen of gained of step in gas chromatograph chem workstation, uses High Temperature Simulation distillation software, calculate the boiling Range Distribution Analysis result measuring commercially available various brands pitch standard specimen;
VI report form: the yield calculating commercially available various brands pitch standard specimen from experiment, when yield is 0.5%, this temperature is decided to be the initial boiling point (IBP) of sample, the integral point temperature under being then spaced apart corresponding to 1% this recovery using the recovery is as the boiling range of commercially available various brands pitch standard specimen.
By step (1) ~ method (2) carries out examination of infrared spectrum to unknown pitch, obtains unknown pitch infrared spectrogram, determine its characteristic absorption peak.
(6) by step method (3), gas chromatography test is carried out to unknown pitch, obtain the gas chromatogram of unknown pitch.
(7) by step method (4), the data in the gas chromatogram of unknown pitch are processed, obtain the boiling range of unknown pitch.
Respectively by step (5) the characteristic absorption peak of the unknown pitch of gained and absorption peak area and step (2) the characteristic absorption peak of the standard specimen pitch of gained and absorption peak area contrast, and respectively initial boiling point in the boiling Range Distribution Analysis data of the commercially available various brands pitch standard specimen of initial boiling point and step VI gained in the boiling Range Distribution Analysis data of the step (7) unknown pitch of gained is contrasted, the principle that the bitumen recovery rate corresponding at different or identical temperature according to temperature corresponding to the identical recovery is different, finally determines the brand of unknown pitch.
Below
embodimentin, the NICOLET 6700 type Fourier infrared spectrograph all adopting Thermo Fischer Scient Inc. of the U.S. to produce gathers infrared spectrum, all adopts U.S. Agilent company 7890A gas chromatograph to gather the gas chromatogram of pitch.
Fourier infrared spectrograph installs attenuated total reflection annex (ATR), after instrument identifies automatically, carries out the collimation of optical table, and arrange after having collimated and gather background medium for after 1000min, spectral scan scope is 650 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.After atr crystal wiped clean, carry out background collection and preserve.Sampling inserting in pitch after scraper heating, while hot pitch being spread upon the spectrogram of atr crystal collected specimens and preserving.
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# pitch, concrete testing procedure is as follows:
1, ATR annex installed by spectrometer, and arranging spectral scan scope is 650 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.First gather background spectrogram, then gather a gram refining-90# pitch spectrogram, see Fig. 1 a.
2, take a gram refining-90# pitch 0.0396g, add 2.0002 g CS
2dissolve.Operation method, test pitch.Obtain the gas chromatogram 2a of pitch.
3, call High Temperature Simulation distillation software, deduction baseline, sets up the table of corrections of retention time to boiling point; Call reference oil test data, determine the response factor of instrument; Analyze a gram form and aspect chromatographic data for refining-90# pitch, obtain initial boiling point and the boiling point distribution curve of this pitch, in table 1.
Table 1 gram refining-90# pitch boiling range cutting compartmental results
embodiment 2
For SK-90# pitch, step is as follows:
1, ATR annex installed by spectrometer, and arranging spectral scan scope is 650 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.First gather background spectrogram, then gather SK-90# pitch spectrogram, see Fig. 1 b.
2, take SK-90# pitch 0.040g and add 2.0125 g CS
2dissolve.Operation method, test pitch.Obtain the gas chromatogram 2b of pitch.
3, call High Temperature Simulation distillation software, deduction baseline, sets up the table of corrections of retention time to boiling point; Call reference oil test data, determine the response factor of instrument; Analyze the form and aspect chromatographic data of SK-90# pitch, obtain initial boiling point and the boiling point distribution curve of this pitch, in table 2.
Table 2 SK90-# pitch boiling range cutting compartmental results
embodiment 3
To the west of petrochemical industry-90# pitch be example, concrete testing procedure is as follows:
1, ATR annex installed by spectrometer, and arranging spectral scan scope is 650 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.First gather background spectrogram, then gather gram western petrochemical industry-90# pitch spectrogram, see Fig. 1 c.
2, take western petrochemical industry-90# pitch 0.0403, add 2.012 g CS
2dissolve.Operation method, test pitch.Obtain the gas chromatogram of pitch, see Fig. 2 c.
3, call High Temperature Simulation distillation software, deduction baseline, sets up the table of corrections of retention time to boiling point; Call reference oil test data, determine the response factor of instrument; Analyze the form and aspect chromatographic data of western petrochemical industry-90# pitch, obtain initial boiling point and the boiling point distribution curve of this pitch, in table 3.
The western petrochemical industry of table 3-90# pitch boiling range cutting compartmental results
embodiment 4
For Zhenghai-90# pitch, concrete testing procedure is as follows:
1, ATR annex installed by spectrometer, and arranging spectral scan scope is 650 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.First gather background spectrogram, then gather pitch spectrogram, see Fig. 1 d.
2, take Zhenghai-90# pitch 0.0389g, add 1.9876CS
2dissolve.Operation method, test pitch.Obtain the gas chromatogram 2d of pitch.
3, call High Temperature Simulation distillation software, deduction baseline, sets up the table of corrections of retention time to boiling point; Call reference oil test data, determine the response factor of instrument; Analyze the form and aspect chromatographic data of Zhenghai-90# pitch, obtain initial boiling point and the boiling point distribution curve of this pitch, in table 4.
Table 4 Zhenghai-90# boiling range cutting compartmental results
As shown in Fig. 3, Fig. 4, Fig. 5, the pitch infrared spectrum of 4 kinds of brands has obvious difference at the characteristic absorption peak of fingerprint region, the gas chromatogram of 4 kinds of brand pitches is also completely different with the interval component contained of different temperatures simultaneously, the pitch of various brand can be distinguished accordingly.
embodiment 5
Certain second grade highway censorship gram refining-90# pitch, step is as follows:
1, ATR annex installed by spectrometer, and arranging spectral scan scope is 650 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.First gather background spectrogram, then gather censorship pitch spectrogram, refine the comparison of-90# pitch spectrogram with standard specimen gram, see Fig. 6.
2, take a gram refining-90# pitch 0.0421g, add 2.0019 g CS
2dissolve.Operation method, test pitch.Obtain the gas chromatogram of pitch, contrast with standard specimen pitch, see Fig. 7.
3, the infrared spectrogram of pitch to be measured is completely different from standard specimen pitch with meteorological chromatogram, infers that pitch is converted through overmulling and is in harmonious proportion, and is not a gram refining 90# pitch.
Above-mentioned
embodimentbe to further description of the present invention, but do not mean that any limitation of the invention.When not departing from the above-mentioned thought of the present invention, the various substitute mode made according to ordinary skill knowledge and conventional means or change, be all included within the present invention.
Claims (4)
1. infrared spectrum differentiates a method for pitch brand in conjunction with High Temperature Simulation distillation technique, comprises the following steps:
(1) adopt Fourier infrared spectrograph attenuated total reflection annex first to gather the infrared spectrum of background, and then gather commercially available various brands pitch spectrogram respectively, last background correction, namely obtain the infrared spectrogram of gathered commercially available various brands pitch respectively;
(2), respectively to the infrared spectrogram smoothing baseline correction process according to a conventional method of described gathered commercially available various brands pitch, obtain the optimization infrared spectrogram of standard specimen pitch, determine characteristic absorption peak;
(3) gather the gas chromatogram of commercially available various brands pitch with gas chromatograph, its method comprises the following steps:
1. gas chromatograph configuration detector be flame ionization ditector, chromatographic column be 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. retention time corrects boiling point: according to a conventional method Polywax 655 is dissolved in carbon disulphide, then the n-alkane of C5-C18 is added, namely Agilent SimDis corrects No. 2, potpourri, 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 by these data stored in gas chromatograph chem workstation;
4. the mensuration of reference oil: the reference oil of specifying in gas chromatograph is dissolved in solvent, then test reference oil under the service condition 2. identical with described step, obtain the gas chromatogram of reference oil, and by these data stored in gas chromatograph chem workstation; The volume ratio of described solvent and described reference oil is 45 ~ 50 mL:1 ~ 2 mL;
5. commercially available various brands pitch standard specimen is analyzed: will be dissolved in solvent by commercially available various brands pitch standard specimen respectively, then under the service condition 2. identical with described step, commercially available various brands pitch standard specimen is measured respectively, obtain the gas chromatogram of commercially available various brands pitch standard specimen, and by these data stored in gas chromatograph chem workstation; The volume ratio of described solvent and described commercially available various brands pitch standard specimen is 45 ~ 50 mL:1 ~ 2 mL;
(4), by data in the gas chromatogram of commercially available various brands pitch standard specimen described in the process of High Temperature Simulation distillation software, its method comprises the following steps:
I is clicked and is entered sample analysis hurdle, chooses gas chromatograph chem workstation, calls the calculating masterplate that software carries, after determining Report Type, clicks confirmation method;
II carries out baseline analysis, deducts the blank analysis baseline of described step 2. gained;
III sets up table of corrections: the boiling point correction data calling the 3. gained of step described in gas chromatograph chem workstation, carries out the analysis of correction sample, sets up calibration curve and table of corrections;
IV computing reference oil: call the data in the gas chromatogram of the 4. reference oil of gained of step described in gas chromatograph chem workstation, use High Temperature Simulation distillation software, calculate boiling Range Distribution Analysis result, compare with reference to the reference data in the boiling Range Distribution Analysis measurement result of oil and software for calculation, the boiling Range Distribution Analysis result of reference oil should in the repeatability interval of listed reference oil in software;
V calculates commercially available various brands pitch standard specimen: the MN.txt file calling the 5. commercially available various brands pitch standard specimen of gained of step 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 pitch standard specimen;
VI report form: the yield calculating described commercially available various brands pitch standard specimen from experiment, when yield is 0.5%, this temperature is decided to be the initial boiling point of sample, the integral point temperature under being then spaced apart corresponding to 1% this recovery using the recovery is as the boiling range of commercially available various brands pitch standard specimen;
By described step (1) ~ method (2) carries out examination of infrared spectrum to unknown pitch, obtains unknown pitch infrared spectrogram, determine its characteristic absorption peak;
(6) by described step method (3), gas chromatography test is carried out to unknown pitch, obtain the gas chromatogram of unknown pitch;
(7) by described step method (4), the data in the gas chromatogram of unknown pitch are processed, obtain the boiling range of unknown pitch;
Respectively by described step (5) the characteristic absorption peak of the unknown pitch of gained and absorption peak area and described step (2) the characteristic absorption peak of the standard specimen pitch of gained and absorption peak area contrast, and respectively initial boiling point in the boiling Range Distribution Analysis data of the commercially available various brands pitch standard specimen of initial boiling point and described step VI gained in the boiling Range Distribution Analysis data of the described step (7) unknown pitch of gained is contrasted, the principle that the bitumen recovery rate corresponding at different or identical temperature according to temperature corresponding to the identical recovery is different, finally determines the brand of unknown pitch.
2. a kind of infrared spectrum as claimed in claim 1 differentiates the method for pitch brand in conjunction with High Temperature Simulation distillation technique, it is characterized in that: described step (1) in the condition of work of Fourier infrared spectrograph refer to that spectral scan scope is 800 ~ 4000cm
-1, scanning times 32 times, sweep spacing 2cm
-1.
3. a kind of infrared spectrum as claimed in claim 1 differentiates the method for pitch brand in conjunction with High Temperature Simulation distillation technique, it is characterized in that: described step 2. middle gas chromatography service condition refers to stove case initial temperature 45 DEG C, stove case 0min at the beginning, stove case journey speed 10 DEG C/min, stove case final temperature 430 DEG C, stove case terminal hour 10min, injection port initial temperature 80 DEG C, injection port journey speed 10 DEG C/min, injection port final temperature 430 DEG C/min, post flow 8mL/min, detector temperature 435 DEG C, hydrogen 40mL/min, air 400 mL/min, assisted gas 15 mL/min, sample size 0.4uL, sample quality concentration 2.0%.
4. a kind of infrared spectrum as claimed in claim 1 differentiates the method for pitch brand in conjunction with High Temperature Simulation distillation technique, it is characterized in that: described step 4. with described step 5. in solvent all refer to one in toluene, carbon disulphide, dichloroethylene.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106969967A (en) * | 2017-05-07 | 2017-07-21 | 兰州理工大学 | Damage FTIR asphalt test pieces draft machine and complex shear modulus Forecasting Methodology can be applied |
| 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 |
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| 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 |
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| CN106969967A (en) * | 2017-05-07 | 2017-07-21 | 兰州理工大学 | Damage FTIR asphalt test pieces draft machine and complex shear modulus Forecasting Methodology can be applied |
| 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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