CN107561047A - A kind of method that SBS contents in modified pitch are determined using fluorescence microscopy - Google Patents
A kind of method that SBS contents in modified pitch are determined using fluorescence microscopy Download PDFInfo
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- CN107561047A CN107561047A CN201710757836.XA CN201710757836A CN107561047A CN 107561047 A CN107561047 A CN 107561047A CN 201710757836 A CN201710757836 A CN 201710757836A CN 107561047 A CN107561047 A CN 107561047A
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Abstract
The invention discloses a kind of method that SBS contents in modified pitch are determined using fluorescence microscopy, comprise the following steps：1) the SBS modified pitch 2 of a variety of known SBS contents is prepared) the fluorescence microscopy test sample 3 of SBS contents known to preparation) sample is subjected to fluorescence microscopy test and carries out binary conversion treatment 4) establish calibration curve equation 5) test SBS contents.The present invention proposes a kind of direct method for visualizing of modified pitch quality evaluation, beneficial to tester in detection process according to the dense degree of fluorescence reaction spot, intuitively find out the volume situation of SBS modifier substantially, the accurate volume of SBS modifier is calculated finally by analysis.This method testing cost is relatively low, is easy to be widely applied, and avoids occurring jerry situation in engineering.Therefore, this SBS modifier method for detecting dose is significant to control modified pitch quality, saving testing cost, thus has broad application prospects.
Description
Technical field
The invention belongs to SBS assays technical field in modified pitch, is related to a kind of determined using fluorescence microscopy and changes
The method of SBS contents in property pitch.
Background technology
At present, SBS modified pitch is being produced with work progress, and the quality control of modified pitch mainly passes through existing specification
Index is tested evaluation.It however, even if meeting specification, cannot guarantee that with enough SBS dosage, also can not just ensure to change
The good pavement performance of property pitch.If controlling SBS dosage well in Practical Project, then modified pitch road can be greatly improved
The durability in face, it can effectively control modified pitch quality.At present, fractional unit detects SBS with infra-red sepectrometry under lab
Content, but infrared spectrometer is expensive, is unfavorable for being widely applied.A line of constructing is even more can only be by checking that modified pitch is given birth to
The data of control room during production, the same day actual amount of modifying agent and the actual amount of asphalt are checked to control SBS to be modified
Agent dose, some areas are even also either voluntarily controlled using the extensive mode of number sack by enterprise.These modes all can not
The main reason for realizing effective control to modified pitch SBS dosage, causing this phenomenon be just a lack of it is a kind of it is simple, effectively,
The low SBS dosage method of testings of cost.
Fluorescence microscopy is the principle according to luminescence generated by light, is excited using the light of certain wavelength glimmering in sample under microscope
Stimulative substance, it is allowed to launch fluorescence, fluoroscopic image is presented.Because the fluorescence section that different material excites is different, in blue light section, drip
The few fluorescence of green material are excited appearance, and the polymer modifiers such as SBS, PE has obvious yellow-green fluorescence to be inspired
Come.Fluorescence microscopy is exactly to observe the microstructure of SBS polymer modified pitch and analysis modified pitch using this principle
Property, and then evaluate modified pitch quality.And by the processing to modified pitch fluorescence micrograph, it can be achieved to modification
The qualitative determination of SBS contents in pitch.
The content of the invention
To solve above mentioned problem present in prior art and actual conditions, the invention provides one kind to utilize fluorescence microscopy
The method of SBS contents, comprises the following steps in method measure modified pitch：
1) the SBS modified pitch of a variety of known SBS contents is prepared
2) the fluorescence microscopy test sample of SBS contents known to preparing
3) sample is subjected to fluorescence microscopy test and carries out binary conversion treatment
4) calibration curve equation is established
5) SBS contents are tested.
Preferably, the step 1) is that the modified pitch of SBS contents known to 5 kinds is manufactured according to following technique：
A, SBS modifier is mixed after matrix pitch being heated into 140 DEG C~150 DEG C, is stirred from stirring at low speed speed
20min；
B, matrix pitch and SBS modifier mixture are selected into 4000r/min~6000r/min at 175 DEG C~185 DEG C
Rotating speed high speed shear 30min~45min；
C, 20min is gently mixed to the modified pitch incorporation stabilizer sheared from low-speed agitator；
D, modified pitch obtained above is put into 170 DEG C of baking ovens and stands swelling 60min.
Preferably, the step 2) comprises the following steps：
A, the 5 kinds of SBS mixed up modified pitch are placed in heater box and heated, heating-up temperature is set as 180 DEG C, adds
Substantially oneself hot about 15h post-modifications pitch, through reaching molten condition, then stir the pitch dissolved with clean glass bar；
B, 5 slides are taken, are dried up after being cleaned up with alcoholic solution with hair-dryer；Then slide is marked with label
To distinguish the modified pitch sample of different SBS contents；5 glass bars are taken, are wrapped up glass bar with clean masking foil, it is same to use
Label indicates the content for sampling, and is polluted as former state with avoiding glass bar mixed；
C, corresponding modified pitch fused solution is dipped with 5 glass bars respectively, dropped on corresponding 5 slides；
D, the slide for having modified pitch is placed in heater box, depending on the size of modified pitch amount, heats 2~5min, treat
Its uniform fold formed on slide thickness uniformly, after the film of surfacing, in the molten state with tweezers gently by lid glass
Piece, which is covered on modified pitch film, makes its smooth and complete close contact, and slide is taken out, is cooled to solidification；
E, the sample centralized collection that will be made, prevent from being contaminated.
Preferably, the step 3) comprises the following steps：
SBS modified pitch sample is observed using 2,000,000 times of multiplication factor, each sample takes an observation position
Clapped, the fluorescence microscopy for obtaining sample shines；According to the property and feature of image of asphalt material, the picture that experiment is obtained is whole
Using the global binaryzation in binarization method；Binary-state threshold is chosen, the pixel that gray scale is more than or equal to threshold value is determined
For SBS polymer, its gray value is 255, it is determined as white, other pixels are identified as matrix pitch mixture, and gray value is
0, it is determined as black；
By the fluorescence micrograph of various different SBS contents modified pitch in viewing test, by binary conversion treatment it
Fluorescence micrograph afterwards can clearly find the distribution of SBS polymer in modified pitch and be crosslinked situation, white in photo
Part is judged as SBS polymer, and black background part is judged as matrix pitch.
Preferably, the threshold value of binaryzation is chosen using alternative manner, the result obtained by iteration is 170, therefore sets threshold
It is worth for 170.
Preferably, the method that the step 4) establishes calibration curve equation is：
MATLAB software programming corresponding programs are borrowed, are calculated by program juice, the fluorescence after analytic statistics binary conversion treatment shows
The area of the white portion of SBS fluorescence on micro- photo, calculate the ratio that SBS fluorescence areas account for the observation gross area：SBS faces
Product/observation the gross area, that is, the content of SBS in modified pitch is reacted；
The statistical result of the modified pitch of different SBS contents is carried out curve fitting, establishes SBS volumes and SBS faces
Product/observation the gross area than calibration curve equation.
Preferably, the step 5) is：
The modified pitch of unknown SBS contents is tested using fluorescence microscopy, SBS fluorescence area/sight is calculated by step 3
Gross area ratio is surveyed, the calibration curve equation that step 4 is drawn is substituted into, draws SBS contents in SBS modified pitch to be checked.
A kind of method that SBS contents in modified pitch are determined using fluorescence microscopy proposed by the present invention is modified pitch matter
Amount, which is assessed, provides direct method for visualizing, beneficial to tester in detection process according to the dense degree of fluorescence reaction spot,
Intuitively find out the volume situation of SBS modifier substantially, the accurate volume of SBS modifier is calculated finally by analysis.Cause
This, the fluorescence microscopy drawn by this patent analysis is to observe the microstructure of modified pitch, SBS in modified pitch
A kind of effective ways of SBS contents in distribution and fast qualitative analysis utilizing modified pitch, and testing cost is relatively low,
It is easy to be widely applied, avoids occurring jerry situation in engineering.Therefore, this SBS modifier method for detecting dose is to control
Modified pitch quality processed, to save testing cost significant, thus has broad application prospects.
Embodiment
A kind of method that SBS contents in modified pitch are determined using fluorescence microscopy, is comprised the following steps：
1. prepare the SBS modified pitch of a variety of known SBS contents
The modified pitch of SBS contents known to 5 kinds is manufactured according to following technique：
(1) SBS modifier is mixed after matrix pitch being heated into 140 DEG C~150 DEG C, is stirred from stirring at low speed speed
20min；
(2) matrix pitch and SBS modifier mixture are selected into 4000r/min~6000r/ at 175 DEG C~185 DEG C
Min rotating speed high speed shears 30min~45min；But electric current is excessive during to prevent from starting starting burns motor, preferably first selects low speed
After gradually step up shear rate.
(3) due to that can be mixed into large quantity of air in the preparation process of modified pitch, SBS modified pitch is longer in standing time
When segregation phenomenon can occur, this can influence the performance test follow-up to pitch, need to select modification of the low-speed agitator to shearing
Pitch incorporation stabilizer is gently mixed 20min.
(4) modified pitch obtained above is put into 170 DEG C of baking ovens and stands swelling 60min.
2. the fluorescence microscopy test sample of SBS contents known to preparing
Band disposable glove is needed in the manufacturing process of sample, ensures the specification of sample making course, sample is paid attention to after making
Protection, prevents the pollution of dust, sweat stain etc..Its sample preparation step is as follows：
(1) the 5 kinds of SBS mixed up modified pitch are placed in heater box first and heated, heating-up temperature is set as 180
DEG C, oneself, through reaching molten condition, then stirs the pitch dissolved with clean glass bar heating about 15h post-modifications pitch substantially
Uniformly；
(2) 5 slides are taken, are dried up after being cleaned up with alcoholic solution with hair-dryer；Then by slide label mark
Remember to distinguish the modified pitch sample of different SBS contents；5 glass bars are taken, are wrapped up glass bar with clean masking foil, equally
The content for sampling is indicated with label, is polluted as former state with avoiding glass bar mixed；
(3) corresponding modified pitch fused solution is dipped with 5 glass bars respectively, dropped on corresponding 5 slides；
(4) slide for having modified pitch is placed in heater box, depending on the size of modified pitch amount, heats 2~5min, treat
Its uniform fold formed on slide thickness uniformly, after the film of surfacing, in the molten state with tweezers gently by lid glass
Piece, which is covered on modified pitch film, makes its smooth and complete close contact, and slide is taken out, is cooled to solidification；
(5) the sample centralized collection that will be made, prevents from being contaminated.
3. sample is subjected to fluorescence microscopy test and carries out binary conversion treatment
SBS modified pitch sample is observed using 2,000,000 times of multiplication factor, each sample takes an observation position
Clapped, the fluorescence microscopy for obtaining sample shines.According to the property and feature of image of asphalt material, the picture that experiment is obtained is whole
Using the global binaryzation in binarization method.The selection of binary-state threshold has a variety of methods, and we apply alternative manner herein
The threshold value of binaryzation is chosen, the result obtained by iteration is 170, therefore given threshold is 170, and gray scale is more than or equal to threshold value
Pixel is judged as SBS polymer, and its gray value is 255, it is determined as white, other pixels are identified as matrix pitch mixing
Thing, gray value 0, it is determined as black.
By the fluorescence micrograph of various different SBS contents modified pitch in viewing test, by binary conversion treatment it
Fluorescence micrograph afterwards can clearly find the distribution of SBS polymer in modified pitch and be crosslinked situation, white in photo
Part is judged as SBS polymer, and black background part is judged as matrix pitch.
4. establish calibration curve equation
MATLAB software programming corresponding programs are borrowed, are calculated by program juice, the fluorescence after analytic statistics binary conversion treatment shows
The area of the white portion (i.e. pixel of the gray value more than or equal to 170) of SBS fluorescence, calculates SBS faces on micro- photo
Product accounts for the ratio of the observation gross area：The SBS fluorescence area/observation gross area, that is, reacted the content of SBS in modified pitch.
Because specimen surface cannot be guaranteed to reach absolute smooth with smooth in sample making course, so should during analysis
Choose SBS in fluorescence micrograph and be distributed the statistics meter that the scope relatively good than more uniform, observation effect carries out SBS fluorescence areas
Calculate, and the statistical result of the modified pitch of different SBS contents carried out curve fitting, establish SBS volumes and SBS fluorescence area/
Observe the gross area than calibration curve equation.
5. test SBS contents
The modified pitch of unknown SBS contents is tested using fluorescence microscopy, SBS fluorescence area/sight is calculated by step 3
Gross area ratio is surveyed, the calibration curve equation that step 4 is drawn is substituted into, draws SBS contents in SBS modified pitch to be checked.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in the present invention's
Within protection domain.
Claims (7)
- A kind of 1. method that SBS contents in modified pitch are determined using fluorescence microscopy, it is characterised in that comprise the following steps：1) the SBS modified pitch of a variety of known SBS contents is prepared；2) the fluorescence microscopy test sample of SBS contents known to preparing；3) sample is subjected to fluorescence microscopy test and carries out binary conversion treatment；4) calibration curve equation is established；5) SBS contents are tested.
- 2. the method according to claim 1 that SBS contents in modified pitch are determined using fluorescence microscopy, its feature are existed In：The step 1) is that the modified pitch of SBS contents known to 5 kinds is manufactured according to following technique：A, SBS modifier is mixed after matrix pitch being heated into 140 DEG C~150 DEG C, 20min is stirred from stirring at low speed speed；B, matrix pitch and SBS modifier mixture are selected into 4000r/min~6000r/min rotating speeds at 175 DEG C~185 DEG C High speed shear 30min~45min；C, 20min is gently mixed to the modified pitch incorporation stabilizer sheared from low-speed agitator；D, modified pitch obtained above is put into 170 DEG C of baking ovens and stands swelling 60min.
- 3. the method according to claim 1 that SBS contents in modified pitch are determined using fluorescence microscopy, its feature are existed In：The step 2) comprises the following steps：A, the 5 kinds of SBS mixed up modified pitch are placed in heater box and heated, heating-up temperature is set as 180 DEG C, and heating is about Substantially oneself 15h post-modifications pitch, through reaching molten condition, then stir the pitch dissolved with clean glass bar；B, 5 slides are taken, are dried up after being cleaned up with alcoholic solution with hair-dryer；Then slide is marked with area with label Divide the modified pitch sample of different SBS contents；5 glass bars are taken, glass bar is wrapped up with clean masking foil, equally uses label The content for sampling is indicated, is polluted as former state with avoiding glass bar mixed；C, corresponding modified pitch fused solution is dipped with 5 glass bars respectively, dropped on corresponding 5 slides；D, the slide for having modified pitch is placed in heater box, depending on the size of modified pitch amount, heats 2~5min, treat that its is equal Even be covered on slide forms thickness uniformly, after the film of surfacing, in the molten state gently covered cover glass with tweezers Cover makes its smooth and complete close contact on modified pitch film, and slide is taken out, is cooled to solidification；E, the sample centralized collection that will be made, prevent from being contaminated.
- 4. the method according to claim 1 that SBS contents in modified pitch are determined using fluorescence microscopy, its feature are existed In：The step 3) comprises the following steps：SBS modified pitch sample is observed using 2,000,000 times of multiplication factor, each sample takes an observation position to carry out Clap, the fluorescence microscopy for obtaining sample shines；According to the property and feature of image of asphalt material, the picture that experiment is obtained all uses Global binaryzation in binarization method；Binary-state threshold is chosen, the pixel that gray scale is more than or equal to threshold value is judged as SBS Polymer, its gray value are 255, it is determined as white, other pixels are identified as matrix pitch mixture, gray value 0, it is determined as Black；By the fluorescence micrograph of various different SBS contents modified pitch in viewing test, after binary conversion treatment Fluorescence micrograph can clearly find distribution and the crosslinking situation of SBS polymer in modified pitch, white portion in photo SBS polymer is judged as, black background part is judged as matrix pitch.
- 5. the method according to claim 4 that SBS contents in modified pitch are determined using fluorescence microscopy, its feature are existed In：The threshold value of binaryzation is chosen using alternative manner, the result obtained by iteration is 170, therefore given threshold is 170.
- 6. the method according to claim 1 that SBS contents in modified pitch are determined using fluorescence microscopy, its feature are existed In：The method that the step 4) establishes calibration curve equation is：MATLAB software programming corresponding programs are borrowed, are calculated by program juice, the fluorescence microscopy after analytic statistics binary conversion treatment shines The area of the white portion of SBS fluorescence on piece, calculate the ratio that SBS fluorescence areas account for the observation gross area：SBS fluorescence area/sight The gross area is surveyed, that is, has reacted the content of SBS in modified pitch；The statistical result of the modified pitch of different SBS contents is carried out curve fitting, establishes SBS volumes and SBS fluorescence area/sight Survey the gross area than calibration curve equation.
- 7. the method according to claim 1 that SBS contents in modified pitch are determined using fluorescence microscopy, its feature are existed In：The step 5) is：The modified pitch of unknown SBS contents is tested using fluorescence microscopy, calculates SBS fluorescence area/observation gross area ratio, generation Enter the calibration curve equation that step 4 is drawn, draw SBS contents in SBS modified pitch to be checked.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108106977A (en) * | 2018-01-12 | 2018-06-01 | 河南工业大学 | A kind of SBS modifier and matrix pitch compatibility and optimal content of modifier preferred method |
| CN108426992A (en) * | 2018-04-23 | 2018-08-21 | 中石化石油工程技术服务有限公司 | A kind of method of insoluble high molecular polymerization species solid content in measurement modified pitch |
| CN112507287A (en) * | 2020-11-10 | 2021-03-16 | 山东省交通科学研究院 | Polymer modified asphalt compatibility design method |
| CN112986295A (en) * | 2021-02-04 | 2021-06-18 | 中国铝业股份有限公司 | X-ray fluorescence spectrum determination tabletting sample of asphalt and sample preparation method thereof |
| CN114594240A (en) * | 2022-03-17 | 2022-06-07 | 贵州理工学院 | Method for detecting mixing amount of SBS (styrene butadiene styrene) modifier in modified asphalt based on surface morphology parameters |
| CN115165834A (en) * | 2022-08-04 | 2022-10-11 | 山东海韵沥青有限公司 | Method for detecting storage stability of SBS modified asphalt |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108106977A (en) * | 2018-01-12 | 2018-06-01 | 河南工业大学 | A kind of SBS modifier and matrix pitch compatibility and optimal content of modifier preferred method |
| CN108426992A (en) * | 2018-04-23 | 2018-08-21 | 中石化石油工程技术服务有限公司 | A kind of method of insoluble high molecular polymerization species solid content in measurement modified pitch |
| CN112507287A (en) * | 2020-11-10 | 2021-03-16 | 山东省交通科学研究院 | Polymer modified asphalt compatibility design method |
| CN112507287B (en) * | 2020-11-10 | 2022-11-29 | 山东省交通科学研究院 | Polymer modified asphalt compatibility design method |
| CN112986295A (en) * | 2021-02-04 | 2021-06-18 | 中国铝业股份有限公司 | X-ray fluorescence spectrum determination tabletting sample of asphalt and sample preparation method thereof |
| CN112986295B (en) * | 2021-02-04 | 2023-10-20 | 中国铝业股份有限公司 | X-ray fluorescence spectrometry pressed sample for asphalt and sample preparation method thereof |
| CN114594240A (en) * | 2022-03-17 | 2022-06-07 | 贵州理工学院 | Method for detecting mixing amount of SBS (styrene butadiene styrene) modifier in modified asphalt based on surface morphology parameters |
| CN115165834A (en) * | 2022-08-04 | 2022-10-11 | 山东海韵沥青有限公司 | Method for detecting storage stability of SBS modified asphalt |
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Application publication date: 20180109 |