CN101694486A - Method for detecting dose of polymers in modified asphalt based on gel chromatography technology - Google Patents
Method for detecting dose of polymers in modified asphalt based on gel chromatography technology Download PDFInfo
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- CN101694486A CN101694486A CN200910024352A CN200910024352A CN101694486A CN 101694486 A CN101694486 A CN 101694486A CN 200910024352 A CN200910024352 A CN 200910024352A CN 200910024352 A CN200910024352 A CN 200910024352A CN 101694486 A CN101694486 A CN 101694486A
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Abstract
The invention relates to a technology for detecting the dose of polymers in modified asphalt and discloses a method for detecting the dose of polymers in modified asphalt based on a gel chromatography technology, which is applied to the detection of the dose of the polymers in finished modified asphalt. The method comprises the following steps: (1) drawing a gel chromatography curve of a sample to be measured: firstly, preparing a sample to be measured of modified asphalt, respectively measuring and drawing the gel chromatography curve of the sample to be measured under the condition that the separation time is 45min and the temperature is 30 DEG C by a gel chromatographic instrument, wherein the horizontal coordinate represents time and the vertical coordinate represents peak height response; and (2) determining the dose of the polymers in the modified asphalt to be measured: wherein the drawn gel chromatography curve has adjacent small feature peak and large feature peak, respectively marking the area of the small feature peak and the area of the large feature peak with A and B, then respectively measuring the values of the area A and the area B by utilizing mesh coordinate paper to obtain a ratio of the area A/(the area A and the area B), which is the mass percentage content of the polymers in the modified asphalt.
Description
Technical field
The present invention relates to the detection technique of dose of polymer in the modified bitumen, particularly a kind of detection method of the dose of polymers in modified asphalt based on gel chromatography technology is applied to the detection to dose of polymer in the finished product asphaltum.
Background technology
Fast development along with the road pavement technology, modified bitumen has obtained application more and more widely, modified bitumen can significantly improve pavement behavior, is widely used in the mating formation of antiskid top layer, the deck paving of highway, city expressway, major trunk roads, particularly steel bridge face.Dose of polymer in the modified bitumen (the quality percentage composition of polymkeric substance in the modified bitumen) has very important influence to the various engineering indexs of pitch, therefore, important effect is being brought into play in the detection of dose of polymer in the work progress of road and bridge, particularly the modifier addition has considerable influence to the short-term and the long-term behaviour of modified bitumen, but less for the detection method research of modifier dosage both at home and abroad.
Summary of the invention
The object of the present invention is to provide a kind of detection method of the dose of polymers in modified asphalt based on gel chromatography technology, this detection method detects quick, and workable, the result accurately and reliably.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A kind of detection method based on dose of polymer in the modified bitumen of gel chromatography technology is characterized in that, may further comprise the steps:
(1) the gel chromatography curve of drafting sample to be tested
At first, the sample to be tested of preparation modified bitumen utilizes gel permeation chrommatograph to measure and draw sample to be tested respectively and is 45min at disengaging time, and temperature is the gel chromatography curve under 30 ℃ the condition, and wherein horizontal ordinate is the time, and ordinate is the peak response value;
(2) determine the dose of polymer of modified bitumen to be measured
The gel chromatography curve of drawing has adjacent little characteristic peak and big characteristic peak, and the area of little characteristic peak and big characteristic peak is designated as A and B respectively, utilize the numerical value of mesh coordinate paper difference survey area A and area B then, then the ratio of area A/(area A+area B) is the shared quality percentage composition of polymkeric substance in the modified bitumen.
Further characteristics of the present invention are that the test basic parameter of described gel permeation chrommatograph is as follows:
A, tetrahydrofuran be as moving phase, speed 1.0ml/min;
B, polyvinyl alcohol (PVA) standard specimen, mass concentration are 2.5～8g/L;
C, sample solution mass concentration 10～12g/L, sample size are 100 μ L.
The inventor finds through great deal of experimental, the dose of polymer of modified bitumen has typical one-to-one relationship with the quality percentage composition that two characteristic peak areas that utilize its gel chromatography curve calculate, the gel chromatography curve presents orderly arrangement, increase along with polymkeric substance SBS dosage, the gel chromatography peak of curve of respective samples is gradually to high molecular direction skew and highly slightly increase, it is more little that the rule of molecular weight increases progressively the big more pen. of lucky checking mean molecular weight, softening point is high more, viscosity is big more, is the almost relation.Intermediate molecular weight and part high molecular part also is goodish linear relationship to the adhesiveness of pitch and mineral in the pitch.The present invention utilizes the These characteristics of modified bitumen to detect, and with respect to traditional detection method, has and detects fast, and workable, the result is characteristics accurately and reliably.
Description of drawings
Below in conjunction with description of drawings and specific embodiment the present invention is described in further details
Fig. 1 is the gel chromatography curve map of the modified bitumen to be measured of test example 1;
Fig. 2 is the gel chromatography curve map of the modified bitumen to be measured of test example 2;
Fig. 3 is the gel chromatography curve map of the modified bitumen to be measured of test example 3;
Embodiment
One, draw the gel chromatography curve of modified bitumen, present embodiment adopts DGU-20A3 gel permeation chrommatograph (gel permeation chrommatograph of other models and kind also can) certainly to detect, and is specific as follows.
This experimental test basic parameter is as follows:
A, tetrahydrofuran be as moving phase, speed 1.0ml/min;
B, polyvinyl alcohol (PVA) standard specimen, mass concentration are 2.5～8g/L;
C, sample solution mass concentration 10～12g/L, sample size are 100 μ L;
D, disengaging time 45min, 30 ℃ of temperature.
1, start
(1), pump: moving phase will be outgased with ultrasonic cleaner before the turn on pump.Open the power switch of pump, preset flow.Press the EDIT/ENTER key on the control panel, use key adjusting flow up and down, press the RUN/STOP key then and make the pump entry into service.Thereby press the EDIT/ENTER key and up and down key regulate flow and press the flow that the MENU key determines to change pump.Speed is too not fast when changing flow, wait to carry out next step behaviour again after the pressure stability of pump and do.If have bubble to exist in the feed tube of discovery pump, should in time remove bubble.Method is: earlier the flushing valve on the pump head is unscrewed, press MENU key on the control panel of pump then and make and show one of purge on the display screen, promptly begin to wash pump head after determining by the EDIT/ENTER key again.Behind Preset Time (being generally 5 minutes), flushing process can stop automatically.Menu recalled to show flow velocity one hurdle, readjust the flow velocity pump that brings into operation.
(2), detecting device: the power switch of opening detecting device.Press 2nd func key then by the Int ℃ of temperature that will show detecting device.When changing detector temperature, press 2nd func key and press Set ℃ of key then and import the temperature value that to set again, press the ENTER key at last and get final product.Behind each replacing solvent, need the flushing reference cell about 30 minutes.Pressing 2nd func key and Purge key can begin to clean.After cleaning finishes, press 2nd func key again and the Purge key can recover detected state.
3, Data Receiving
Open the data-interface power switch and open gel permeation chrommatograph (GPC) software, behind the Data Receiving key on the click software, can begin to carry out Data Receiving work.
2, test
(1), the preparation of sample: the sample for preparing need be placed 24 hours so that sample fully dissolves.Solvent sample also will be used membrane filtration, removes insoluble matter (this is for preventing to damage gel column).
(2), sample introduction: microsyringe cleans 4 to 5 times with moving phase earlier, and then sample wash 4 to 5 times.During sample introduction, must make does not have bubble to exist in the syringe.During sample introduction, elder generation pulls the injector sample introduction after detecting device is returned zero again, and approximately sample introduction turned back original position with the injector handle after 5 minutes.
3, shutdown
After test finishes, reduce the flow velocity of pump gradually until arriving zero after should under test traffic, continuing again to move 30 minutes; At last, close successively pump power supply,, the power supply of detecting device, interface power supply, withdraw from software.
Two, the detection method of dose of polymers in modified asphalt of the present invention specifically may further comprise the steps.
(1) the gel chromatography curve of drawing standard sample
At first, the sample to be tested of preparation modified bitumen, utilizing gel permeation chrommatograph (GPC) to measure and draw each sample to be tested respectively is 45min at disengaging time, temperature is the gel chromatography curve under 30 ℃ the condition, wherein horizontal ordinate is the time, and ordinate is the peak response value;
(2) determine the dose of polymer of modified bitumen to be measured
The gel chromatography curve of drawing has adjacent little characteristic peak and big characteristic peak, little characteristic peak and big characteristic peak are approximate triangle, and the subtriangular area of little characteristic peak and big characteristic peak is designated as A and B respectively, utilize the numerical value of mesh coordinate paper difference survey area A and area B then, then the ratio of area A/(area A+area B) is the shared quality percentage composition of polymkeric substance in the modified bitumen.Under the situation of known polymers in modified asphalt type, detection method of the present invention is more quick.
Three, below in conjunction with the detection method of dose of polymers in modified asphalt of the present invention the detection validation of known dose of polymers in modified asphalt being tested example is described in further detail.
Test example 1:
(dosage of this test is 3.8% to the known modified bitumen that contains certain dose of polymer, polymer type is SBS), with detection method shown in the present this modified bitumen is carried out detection validation, under following basic test parameters, utilize gel permeation chrommatograph to draw the gel chromatography curve of sample to be tested:
A, tetrahydrofuran be as moving phase, speed 1.0ml/min;
B, polyvinyl alcohol (PVA) standard specimen, mass concentration are 2.5～8g/L;
C, sample solution mass concentration 10～12g/L, sample size are 100 μ L;
D, disengaging time 45min, 30 ℃ of temperature.
Area under two characteristic peaks among this gel chromatography figure is labeled as area A and area B respectively, wherein area A representative is area under the less characteristic peak, promptly be to represent dose of polymer in the modified bitumen, area B representative be area under the bigger characteristic peak, promptly be the dosage of representing the modified bitumen medium pitch, utilize mesh coordinate pile area A and area B to measure then, the value that draws area A is 11.5mm
2, the numerical value of area B is 291.0mm
2, then utilize formula area A/(area A+area B) to calculate that polymer content is 3.8% in the modified bitumen, the content that can judge this polymers in modified asphalt thus is 3.8%, and is consistent with actual dose.
Test example 2:
(dosage of this test is 5.0% to the known modified bitumen that contains certain dose of polymer, polymer type is SBS), with detection method shown in the present this modified bitumen is carried out detection validation, under following basic test parameters, utilize gel permeation chrommatograph to draw the gel chromatography curve of sample to be tested:
A, tetrahydrofuran be as moving phase, speed 1.0ml/min;
B, polyvinyl alcohol (PVA) standard specimen, mass concentration are 2.5～8g/L;
C, sample solution mass concentration 10～12g/L, sample size are 100 μ L;
D, disengaging time 45min, 30 ℃ of temperature.
Area under two characteristic peaks among this gel chromatography figure is labeled as area A and area B respectively, wherein area A representative is area under the less characteristic peak, promptly be to represent dose of polymer in the modified bitumen, area B representative be area under the bigger characteristic peak, promptly be the dosage of representing the modified bitumen medium pitch, we utilize mesh coordinate pile area A and area B to measure then, and the value that draws area A is 12.5mm
2, the numerical value of area B is 237.5mm
2, then utilize formula area A/(area A+area B) to calculate that polymer content is 5.0% in the modified bitumen, the content that can judge this polymers in modified asphalt thus is 5.0%, and is consistent with actual dose.
Test example 3:
(dosage of this test is 5.5% to the known modified bitumen that contains certain dose of polymer, polymer type is SBS), with detection method shown in the present this modified bitumen is carried out detection validation, under following basic test parameters, utilize gel permeation chrommatograph to draw the gel chromatography curve of sample to be tested:
A, tetrahydrofuran be as moving phase, speed 1.0ml/min;
B, polyvinyl alcohol (PVA) standard specimen, mass concentration are 2.5～8g/L;
C, sample solution mass concentration 10～12g/L, sample size are 100 μ L;
D, disengaging time 45min, 30 ℃ of temperature.
Area under two characteristic peaks among this gel chromatography figure is labeled as area A and area B respectively, wherein area A representative is area under the less characteristic peak, promptly be to represent dose of polymer in the modified bitumen, area B representative be area under the bigger characteristic peak, promptly be the dosage of representing the modified bitumen medium pitch, we utilize mesh coordinate pile area A and area B to measure then, and the value that draws area A is 10mm
2, the numerical value of area B is 172mm
2, then utilize formula area A/(area A+area B) to calculate that polymer content is 5.5% in the modified bitumen, the content that can judge this polymers in modified asphalt thus is 5.5%, and is consistent with actual dose.
Test explanation: the sample production of the modified bitumen of this checking with to the check of modified bitumen sample by different personnel's separate operation, the possibility of having avoided data to disturb, be not difficult to draw detection method result of the present invention accurately and reliably by above experiment, simple and efficient, requirement to equipment is lower, being easy to promote, is the means for dose of polymer in a kind of effective detection modified bitumen.
Claims (2)
1. the detection method based on the dose of polymers in modified asphalt of gel chromatography technology is characterized in that, may further comprise the steps:
(1) the gel chromatography curve of drafting sample to be tested
At first, the sample to be tested of preparation modified bitumen utilizes gel permeation chrommatograph to measure and draw sample to be tested respectively and is 45min at disengaging time, and temperature is the gel chromatography curve under 30 ℃ the condition, and wherein horizontal ordinate is the time, and ordinate is the peak response value;
(2) determine the dose of polymer of modified bitumen to be measured
The gel chromatography curve of drawing has adjacent little characteristic peak and big characteristic peak, and the area of little characteristic peak and big characteristic peak is designated as A and B respectively, utilize the numerical value of mesh coordinate paper difference survey area A and area B then, then the ratio of area A/(area A+area B) is the shared quality percentage composition of polymkeric substance in the modified bitumen.
2. the detection method of a kind of dose of polymers in modified asphalt based on gel chromatography technology according to claim 1 is characterized in that the test basic parameter of described gel permeation chrommatograph is as follows:
A, tetrahydrofuran be as moving phase, speed 1.0ml/min;
B, polyvinyl alcohol (PVA) standard specimen, mass concentration are 2.5～8g/L;
C, sample solution mass concentration 10～12g/L, sample size are 100 μ L.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198429A (en) * | 2014-09-12 | 2014-12-10 | 广西大学 | Method for analysis and differentiation of asphalt by combining infrared chromatography with gel permeation chromatography |
| CN104267115A (en) * | 2014-09-12 | 2015-01-07 | 中国建材检验认证集团股份有限公司 | Method for measuring content of chemical root-retardant agent in root-puncture-resistant material |
| CN106526027A (en) * | 2016-11-10 | 2017-03-22 | 山西省交通科学研究院 | Liquid chromatography-based SBS modified asphalt dosage test method |
| CN109540740A (en) * | 2018-12-04 | 2019-03-29 | 江西蓝星星火有机硅有限公司 | A kind of needle penetration fitting detection method of Molecular Weight of Silicone Rubber |
| CN109668993A (en) * | 2017-10-16 | 2019-04-23 | 宝武炭材料科技有限公司 | A kind of method of gel permeation chromatography measurement coal tar asphalt |
-
2009
- 2009-10-16 CN CN200910024352A patent/CN101694486A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104198429A (en) * | 2014-09-12 | 2014-12-10 | 广西大学 | Method for analysis and differentiation of asphalt by combining infrared chromatography with gel permeation chromatography |
| CN104267115A (en) * | 2014-09-12 | 2015-01-07 | 中国建材检验认证集团股份有限公司 | Method for measuring content of chemical root-retardant agent in root-puncture-resistant material |
| CN106526027A (en) * | 2016-11-10 | 2017-03-22 | 山西省交通科学研究院 | Liquid chromatography-based SBS modified asphalt dosage test method |
| CN109668993A (en) * | 2017-10-16 | 2019-04-23 | 宝武炭材料科技有限公司 | A kind of method of gel permeation chromatography measurement coal tar asphalt |
| CN109540740A (en) * | 2018-12-04 | 2019-03-29 | 江西蓝星星火有机硅有限公司 | A kind of needle penetration fitting detection method of Molecular Weight of Silicone Rubber |
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Open date: 20100414 |