CN110441188A - The bitumen content test method of BUTON rock asphalt - Google Patents
The bitumen content test method of BUTON rock asphalt Download PDFInfo
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- 239000010426 asphalt Substances 0.000 title claims abstract description 280
- 239000011435 rock Substances 0.000 title claims abstract description 137
- 238000010998 test method Methods 0.000 title claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 35
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 18
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 abstract description 58
- 239000007787 solid Substances 0.000 abstract description 10
- 238000005259 measurement Methods 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 5
- 231100001261 hazardous Toxicity 0.000 abstract 1
- 238000000034 method Methods 0.000 description 51
- 239000000203 mixture Substances 0.000 description 24
- 239000011295 pitch Substances 0.000 description 22
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 14
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 13
- 229960002415 trichloroethylene Drugs 0.000 description 13
- 229910052500 inorganic mineral Inorganic materials 0.000 description 11
- 239000011707 mineral Substances 0.000 description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 description 5
- 238000012937 correction Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
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- 239000000706 filtrate Substances 0.000 description 4
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- 238000000926 separation method Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052925 anhydrite Inorganic materials 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical class ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
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- 238000000605 extraction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 241001411320 Eriogonum inflatum Species 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
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- 238000011978 dissolution method Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 235000021321 essential mineral Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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Abstract
The present invention relates to a kind of bitumen content test methods of BUTON rock asphalt, high-temperature calcination is carried out to rock asphalt sample, sufficiently soluble easy decomposing carbonate solution is added to the asphaltic residue obtained after high-temperature calcination to react, obtain reaction residue, then reaction residue is dried, by the difference of the quality of the quality and rock asphalt sample of dry reaction residue, the bitumen content of BUTON rock asphalt is calculated.Compared with prior art, the present invention is based on the commonly used equipment that ordinary test room has, have the characteristics that test procedure is simple, easy to operate, test result is accurate, experimentation cost is low, and is not related to the use of harmful chemicals, it is non-hazardous to testing crew and environment；Present invention may also apply to the measurements of the bitumen content of other natural solid bitumens.
Description
Technical field
The invention belongs to Test And Check Technology fields, more particularly, to a kind of bitumen content test side of BUTON rock asphalt
Method.
Background technique
To natural rock asphalt, Department of Transportation, China formulated standard " the 5th part of asphalt modified additive:
Bitumen " (JT/T 880.5-2014), standard has also been formulated in drug in some provinces.Rock asphalt mainly has Indonesia's BUTON rock asphalt
(Buton rock asphalt, BRA), Gilsonite rock asphalt (Gilsonite, Uintaite), Iranian rock asphalt, the drip of Xinjiang rock
Blueness, Qing Chuan rock asphalt etc..Wherein, what is be most widely used in China's engineering at present is Indonesia's BUTON rock asphalt, originates in India Buddhist nun
The island Bu Dun of the West Asia southeast Sulawesi is that pitch and minerals are changed by long-term sea-bottom deposit, receiving pressure and geology
The product of formation.It is dark brown powder after processed, bitumen content 20% or so, remaining is minerals.These natural rock asphalts
It can be used as asphalt modifier, be incorporated into asphalt, the high-temperature behavior etc. of asphalt can be improved.
It is exploited and is obtained by nature due to natural rock asphalt, having a certain difference property and fluctuation on ingredient.When
Rock asphalt is incorporated into asphalt as modifying agent, should be understood first its bitumen content, bitumen content is certain
The batch rock asphalt performance and volume are determined in degree, i.e., when the bitumen content of rock asphalt is higher, volume can be reduced suitably；
When bitumen content is lower, volume then needs to properly increase.But the measurement of the bitumen content to rock asphalt, it there is no mutually take an entrance examination at present
Test method standard.In practice, the bitumen content measurement to rock asphalt is mainly referring to " highway engineering pitch and pitch mix to engineering
Expect testing regulations " several method in (JTG E20-2011) executes.Be respectively: (1) 0607 bitumen solubility of T is tested；(2)T
0722 asphalt from asphalt mixture content tests (centrifugal separation)；(3) 0735 asphalt from asphalt mixture content of T test (combustion
Burn oven process).Practice have shown that there are the following problems for meeting when referring to the bitumen content of these types of method measurement rock asphalt.
The test of 0607 bitumen solubility of T is suitable for measurement bi tumenf orr oad, this kind of sticky drip of polymer modified asphalt
The solubility of residue after the evaporation of green and emulsified asphalt.It is usually dissolved with trichloroethylene solvent and impregnates pitch, then passed through again
Filter paper filtering, the trichloro ethylene solution dissolved with pitch is by filter paper filter opening, and the residue for being not dissolved in trichloro ethylene is then protected
It stays on filter paper.Pass through residue Mass Calculation bitumen solubility.For solid asphalt, solubility is traditionally considered as pitch and is contained
Amount." standard specification for construction and acceptance of highway asphalt pavement " (JTG F40-2004) is respectively as follows: various bitumen solubility technical requirements
Road asphalt is not less than 99.5%；Polymer modified asphalt is not less than 99.0%；Asphalt Emulsion Evaporation Residue is not less than
97.5%.That is the solubility of these pitches is high, and it is few not dissolve ingredient.When solubility test, the weighing quality of pitch is about
2g can relatively smoothly complete the filtering of whole filtrates after trichloro ethylene immersion dissolution is added.
But BUTON rock asphalt contains a large amount of mineralogical compositions, practice have shown that, when referring to the 0607 bitumen solubility test side T
When method, it is found that undissolved mineralogical composition can block filter paper filter opening, the rate of filtration becomes that very slowly, a large amount of three chloroethenes need to be added
Alkene cleaning and glass bar stirring can dissolve, test period greatly prolongs, reach filtrate it is colorless and transparent when, usually need for 24 hours more than
Time.In long-time filter process, trichloro ethylene volatilization pollution air.If reducing sample weighs quality, sample mass is insufficient
Or sampling will cause test error without representativeness.Zhao Shuai, Ma Linge, Han Zhihua are waited and " are improved solubility detection method to be used for
The super hard grades of bitumen (SHA) and lake asphalt (TLA) of low solubility " (" chemical management " the 28th phase in 2018) also report above-mentioned ask
Topic.
0722 asphalt from asphalt mixture content of T tests (centrifugal separation), suitable for measuring the pitch of asphalt
Content.According to extraction device is commonly centrifuged shown in specification, the test process itself is more complicated, and single test needs
1000g or more rock asphalt.Additionally, there are following problems: (1) bitumen content of rock asphalt is far longer than the pitch of asphalt
Content, therefore need to can complete to test with more trichloro ethylenes are consumed.(2) mineralogical composition of rock asphalt is 80% or so, and
Rock asphalt particle is tiny, and after extracting, a large amount of miberal powders can be leaked into extract, and the miberal powder content in extract will be far longer than
The miberal powder content that asphalt leaks after extraction test.Therefore, then after burning conversion, the miberal powder gross mass of leakage is calculated
There can be large error, the bitumen content for eventually resulting in rock asphalt, which calculates, generates large error.Institutes Of Technology Of Changsha's money shines
The above problem is also shown in its Master's thesis " research of BUTON rock asphalt material property testing ", impregnates three chloroethenes of rock asphalt
Alkene dosage is 5 times of plain asphalt mixture, and soaking time is 2 times of plain asphalt mixture.
When referring to the test of 0735 asphalt from asphalt mixture content of T (burning oven process), by specification setting ignition temperature
When (538 ± 5) DEG C, it is found that rock asphalt burning is not thorough phenomenon, and the bitumen content result obtained is obviously bigger than normal.This is mainly
Because the bitumen content of rock asphalt is far longer than the bitumen content of asphalt, and rock asphalt belongs to natural products, mineral particle
Degree is thinner, and the adsorption capacity between pitch and mineral is strong, is not easy to be completely burned completely, so method is not fully appropriate for rock
The bitumen content of pitch is tested.In addition, single test needs 1200g or more rock asphalt, and the bitumen content of rock asphalt is much
Greater than the bitumen content of asphalt, when burning, can generate a large amount of bitumen flue gas, pollute environment.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of BUTON rock asphalts
Bitumen content test method.
Constituent analysis is carried out to BUTON rock asphalt using X-ray diffraction and shows that the mineralogical composition of rock asphalt is mainly
CaCO3, followed by SiO2、CaSO4, other compositions Ca (Fe, Mg) (CO3)2Content is lower.Relevant information is consulted, at 900 DEG C or so
Under calcination condition, CaSO4Equal mineral will not decompose, CaCO3It decomposes and generates CaO and CO2, CO2It escapes with the pitch in rock asphalt
Out.As it can be seen that loss of calcination quality is not to be regarded as contained asphalt quality.
If calcining and adding NH to calcining residue4HCO3Or (NH4)2CO3After solution, with (NH4)2CO3For, it may occur that such as
Lower serial reaction.
CaO+H2O=Ca (OH)2
Ca(OH)2+(NH4)2CO3=CaCO3+2NH3↑+2H2O
As it can be seen that CaCO in calcination process3Decompose the CO of loss2NH can be passed through4HCO3Or (NH4)2CO3Solution is restored.
Extra NH4HCO3Or (NH4)2CO3It resolves into gas completely under lower temperature heating condition, does not increase the matter of reaction residue
Amount.
According to the mineral characteristic of BUTON rock asphalt and above-mentioned chemical principle, the present invention is quasi- to propose one kind with ordinary test
High temperature furnace, crucible and the electronic balance that room has are capital equipment, are not related to that any harmful chemicals, step be simple, operation letter
Just, quickly, the bitumen content test method of the low BUTON rock asphalt of experimentation cost.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of bitumen content test method of BUTON rock asphalt carries out high-temperature calcination to rock asphalt sample, to high-temperature calcination
The asphaltic residue obtained afterwards adds sufficiently soluble easy decomposing carbonate solution and is reacted, and obtains reaction residue, then will
Reaction residue drying, by the difference of the quality of the quality and rock asphalt sample of dry reaction residue, is calculated Bu Dun
The bitumen content of rock asphalt.
Preferably, the temperature of high-temperature calcination is that can make the temperature of the carbonate decomposition in rock asphalt sample.And in the temperature
Under, other mineral in rock asphalt sample do not decompose.
It is further preferred that the condition of high-temperature calcination is to calcine 2h or more at (900 ± 20) DEG C.
Preferably, the solubility easily decomposing carbonate is NH4HCO3Or (NH4)2CO3。
Preferably, the condition of reaction residue drying are as follows: be first dried in reaction residue at (80 ± 10) DEG C without molten
Until liquid, then 2h or more is dried under the conditions of (115 ± 5) DEG C.
In the present invention, NH4HCO3Or (NH4)2CO3Solution can restore the carbonate in rock asphalt and decompose ease in calcination process
CO out2, extra NH4HCO3Or (NH4)2CO3Gas is resolved into completely in (80 ± 10) DEG C and (115 ± 5) DEG C drying course
Body does not increase the quality of reaction residue.
Preferably, rock asphalt sample removes moisture using drying is preceding first passed through.It is preferred that by rock asphalt sample through 50 DEG C of baking oven
Low temperature drying 8h removes moisture, and avoiding excessively high drying temperature (such as 100 DEG C) causes the lightweight organic components in rock asphalt to be waved
Send out and influence the Accurate Determining of bitumen content.
Preferably, the quality of the rock asphalt sample is (1.0~10.0) g.The dosage is far smaller than 0722 pitch of T
Mixture Asphalt Content tests (centrifugal separation) and 0735 asphalt from asphalt mixture content of T tests (burning oven process)
Sample dosage.
It is further preferred that the quality of the rock asphalt sample is (2.0~6.0) g.On the basis of less dosage,
It ensure that test accuracy.
Preferably, specifically includes the following steps:
A) drying quality m is weighed1；
B) dry rock asphalt sample is added into crucible, weighs total quality m of crucible and rock asphalt sample2；
C) crucible equipped with rock asphalt sample is put into high temperature furnace, 2h or more is calcined under the conditions of (900 ± 20) DEG C；
D) crucible is taken out, is put into drier and is cooled to room temperature, weighs total quality m of crucible and asphaltic residue3；
E) soluble easily decomposing carbonate solution is added into the crucible equipped with asphaltic residue；
F) crucible equipped with carbonate solution is put into baking oven, is dried to reaction residue under the conditions of (80 ± 10) DEG C
Until middle no solution；
G) 2h or more is dried under the conditions of (115 ± 5) DEG C, weighs total quality m of crucible and reaction residue4；
H) the burning quality loss and bitumen content of rock asphalt sample to be measured is calculated as follows:
In formula: PL--- the burning quality of rock asphalt sample loses, %；
PB--- the bitumen content of rock asphalt sample, %；
m1--- quality, g；
m2--- total quality of crucible and rock asphalt sample, g before calcining；
m3--- total quality of crucible and asphaltic residue, g after calcining；
m4--- total quality of crucible and reaction residue, g after calcining.
Basic principle of the invention is: the essential mineral CaCO of BUTON rock asphalt3, under the conditions of 900 DEG C, decompose and generate
CaO and CO2, CO2It is escaped with the pitch in rock asphalt.As it can be seen that loss of calcination quality is greater than the asphalt quality in rock asphalt, no
Bitumen content can be calculated according to loss quality.NH is added to the calcined residue of rock asphalt4HCO3Or (NH4)2CO3Solution, it is residual
CaO in slag, which is first reacted with the water in solution, generates Ca (OH)2, Ca (OH)2Again with enough NH4HCO3Or (NH4)2CO3Reaction
Generate CaCO3, i.e., the CO that is lost in calcination process2Restored.Due to NH4HCO3Or (NH4)2CO3It easily decomposes, adds low
Under heat condition, extra NH4HCO3Or (NH4)2CO3NH can be resolved into3、CO2It is escaped with vapor.First using lower drying temperature
It spends (80 ± 10) DEG C, until being dried in reaction residue without solution, mainly common crucible limited volume prevents solution from boiling
Cause reaction residue to overflow crucible and causes mass loss.Again using 2h or more is dried under the conditions of (115 ± 5) DEG C, so that reaction
Moisture and NH in residue4HCO3Or (NH4)2CO3It is completely removed.Therefore, reaction not will increase using this kind of carbonate solution
The quality of residue.The bitumen content of rock asphalt can be calculated according to the quality of reaction residue.
The present invention is due to using above technical scheme, the high temperature for having the advantage that 1, having using ordinary test room
Furnace, crucible and electronic balance are capital equipment, do not need additionally to purchase other equipment.2, using common NH4HCO3Or
(NH4)2CO3Reagent is not related to the use of harmful chemicals trichloroethylene solvent compared with solubility method, reduce to human body and
The harm of environment.3, it is tested with asphalt from asphalt mixture content test (centrifugal separation) and asphalt from asphalt mixture content
(burning oven process) is compared, and the total dosage of sample of the present invention only needs about 25g (in the case where carrying out multiple groups parallel test), the drip of generation
Green flue gas is few, reduces the pollution to environment.4, test procedure is simple, easy to operate, is suitable for ordinary test personnel；Test
Speed is fast, and as a result accuracy is high, and repeatability error is small.
Detailed description of the invention
Fig. 1 is the flow diagram of the bitumen content test method of BUTON rock asphalt of the present invention；
Fig. 2 is BUTON rock asphalt X ray diffracting spectrum；
Fig. 3 is the test specimen after the burning oven process test of T 0735；
Fig. 4 is lake asphalt (TLA) X ray diffracting spectrum.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Referring to Fig. 1, in one embodiment, a kind of bitumen content test method measuring BUTON rock asphalt, including with
Lower step:
S1 weighs drying quality m1；
Wherein, accuracy of balance 0.1mg.
Dry rock asphalt sample is added into crucible, weighs total quality m of crucible and rock asphalt sample by S22；
The rock asphalt quality that each crucible is added is about 5g.
Crucible equipped with sample is put into high temperature furnace by S3, and 2h or more is calcined under the conditions of (900 ± 20) DEG C；Such as calcining
Still there are dark brown coloured particles afterwards, until continuing to be fired to residue without dark brown；
S4 takes out crucible, is put into drier and is cooled to room temperature, and weighs total quality m of crucible and asphaltic residue3；
Soluble easily decomposing carbonate solution is added into the crucible equipped with asphaltic residue by S5；
Wherein, soluble easily decomposing carbonate can be NH4HCO3Or (NH4)2CO3, the additive amount of solution prepares according to solution
Concentration and asphaltic residue quality determine, to guarantee that residue can sufficiently be reacted, the corresponding NH of 1g residue4HCO3Solid masses is many
In 1.4g or (NH4)2CO3Solid masses is no less than 1.7g.
Crucible equipped with carbonate solution is put into baking oven by S6, and reaction residual is dried under the conditions of (80 ± 10) DEG C
In object without solution until；
S7 dries 2h or more under the conditions of (115 ± 5) DEG C；Weigh total quality m of crucible and reaction residue4；
The burning quality loss and bitumen content of rock asphalt sample to be measured is calculated as follows in S8
In formula: PL--- the burning quality of rock asphalt sample loses, %；
PB--- the bitumen content of rock asphalt sample, %；
m1--- quality, g；
m2--- total quality of crucible and rock asphalt sample, g before calcining；
m3--- total quality of crucible and asphaltic residue, g after calcining；
m4--- total quality of crucible and reaction residue, g after calcining.
Embodiment 1:
By taking a kind of typical representative Indonesia BUTON rock asphalt as an example, ingredient is carried out to BUTON rock asphalt using X-ray diffraction
Analysis shows the mineralogical composition of rock asphalt is mainly CaCO3, followed by SiO2、CaSO4, other compositions Ca (Fe, Mg) (CO3)2Contain
Measure lower (BUTON rock asphalt X ray diffracting spectrum is referring to fig. 2).
The bitumen content test method of BUTON rock asphalt, comprising the following steps:
(1) 4 crucibles are cleaned before sample, is wiped after doing, and through 1h drying and processing under the conditions of 900 DEG C；
(2) after quartering division, about 25g representativeness rock asphalt sample is taken, removes moisture through 50 DEG C of drying 8h of baking oven, so
After be put into it is spare in drier；
(3) 4 drying quality m are weighed respectively1；
(4) about 6g rock asphalt sample is added into every crucible, weighs total quality m of crucible and rock asphalt sample2；
(5) crucible equipped with sample is put into high temperature furnace, calcines 4h under the conditions of 900 DEG C, residue is without black after calcining
Brown particles；
(6) crucible is taken out, is put into drier and is cooled to room temperature, weighs total quality m of crucible and asphaltic residue3；
(7) 20% (NH is added into the crucible respectively equipped with asphaltic residue4)2CO3Solution about 30mL；
(8) (NH will be housed4)2CO3The crucible of solution is put into baking oven, is dried in reaction residue under the conditions of 80 DEG C
Until solution；
(9) 4h is dried under the conditions of (115 ± 5) DEG C；Weigh total quality m of crucible and reaction residue4；
The burning quality loss and bitumen content of rock asphalt sample to be measured is calculated as follows
In formula: PL--- the burning quality of rock asphalt sample loses, %；
PB--- the bitumen content of rock asphalt sample, %；
m1--- quality, g；
m2--- total quality of crucible and bitumen samples, g before calcining；
m3--- total quality of crucible and asphaltic residue, g after calcining；
m4--- total quality of crucible and reaction residue, g after calcining.
Using the average value of 4 results as final result.
Test initial data and calculated result are shown in Table 1.
Bitumen content test result (the method for the present invention (NH of 1 BUTON rock asphalt of table4)2CO3)
It to above-mentioned same BUTON rock asphalt sample, is tested using the method for the present invention, test method step and above-mentioned reality
The method and step for applying example is identical, and it is 15%NH that the main distinction, which is to being respectively equipped in the crucible of asphaltic residue be added,4HCO3Solution
25mL.Test initial data and calculated result are shown in Table 2.
Bitumen content test result (the method for the present invention NH of 2 BUTON rock asphalt of table4HCO3)
By Tables 1 and 2 it is found that using the method for the present invention, the test result of acquisition repeatability is preferably, it was demonstrated that side of the present invention
The accuracy of method test result.
For the accuracy for proving the method for the present invention test result, reference " highway engineering pitch and Asphalt Mixture Experiment rule
Journey " in (JTG E20-2011) test of 0607 bitumen solubility of T same BUTON rock asphalt sample is tested, with the present invention
Methods and results are compared therewith, analyze the accuracy of the method for the present invention test result.For the sake of simplicity, to the dissolution in specification
Degree method test procedure is slightly modified, mainly comprises the steps that
(1) the BUTON rock asphalt about 2g for weighing drying, is poured into conical flask, sample mass is denoted as m5。
(2) about 250mL trichloro ethylene reagent is added into conical flask, covers bottle stopper, impregnates 6h, in the process, repeatedly
Conical flask is shaken, the dissolution of rock asphalt is accelerated.
(3) filter paper of drying is weighed, quality is denoted as m6。
(4) folded filter paper is mounted on funnel, pitch soaking solution is poured into filter paper, until filtrate is all filtered
It is complete, and conical flask is cleaned multiple times with trichloro ethylene, and pour into filter paper filter again, until filtrate is colorless and transparent.
(5) filter paper containing insoluble matter is put into baking oven, (105 ± 5) DEG C drying 2h.
(6) filter paper is taken out, is put into after being cooled to room temperature in drier, is weighed total quality of filter paper and insoluble matter, be denoted as
m7。
(7) solubility (bitumen content) of rock asphalt to be measured is calculated as follows
In formula: SB--- the solubility (bitumen content) of rock asphalt, %；
m5--- filter paper quality, g；
m6--- total quality of filter paper and rock asphalt sample, g；
m7--- total quality of filter paper and rock asphalt insoluble matter, g.
Parallel test 4 times, using average value as final result.
Bitumen content (solubility method) the test initial data and calculated result of BUTON rock asphalt are shown in Table 3.
The bitumen content (solubility method) of 3 BUTON rock asphalt of table
Comparison sheet 1, table 2 and 3 result of table are it is found that the method for the present invention differs very little with the result that solubility method obtains, it was demonstrated that
The accuracy of the method for the present invention test result, the method for the present invention are feasible to the bitumen content measurement of BUTON rock asphalt.
Sample is dried to above-mentioned same BUTON rock asphalt, using the test (burning of 0735 asphalt from asphalt mixture content of T
Oven process) it is tested, in order to avoid generating excessive bitumen flue gas, when test, the bitumen samples quality of single test is about 200g,
Ignition temperature is set as 540 DEG C, burning time 6h.Test initial data and calculated result are shown in Table 4.
The bitumen content (combustion method) of 4 BUTON rock asphalt of table
In table: P --- the bitumen content of rock asphalt, %；
m8--- the quality of rock asphalt, g before burning；
m9--- the quality of rock asphalt, g after burning.
As shown in Table 4, the test result that combustion method obtains is noticeably greater than the test result of dissolution method.Even if in addition, burning
Time has been up to 6h, still there is dark brown coloured particles after test (referring to Fig. 3).As it can be seen that 0735 asphalt from asphalt mixture content of T is tried
Test the bitumen content measurement that (burning oven process) is not directly adaptable to use rock asphalt.
When solid asphalt is mainly by being dissolvable in water the pitch class material of trichloro ethylene and being not dissolved in the mineral of trichloro ethylene
Composition, and when the content of organics that is not dissolved in trichloro ethylene is few, it is suitable for the pitch of this kind of solid asphalt contains
The measurement of amount.
Embodiment 2:
Lake asphalt refers to Trinidad Lake Asphalt (Trinidad Lake Asphalt, TLA), and the spy for originating in South America is vertical
The domestic pitch lake of trinidad and tobago is the hard blocks of solid of black, and needle penetration is almost 0, in airport roadway, Steel Bridge Deck
There is good application effect.
Using the method for the present invention, lake asphalt (TLA) is tested, the method and step of test method step and embodiment 1
Identical, it is 15% (NH that the main distinction, which is to being respectively equipped in the crucible of asphaltic residue be added,4)2CO3Solution 20mL.Lake asphalt
(TLA) initial data and calculated result are shown in Table 5.
The bitumen content test result (the method for the present invention) of 5 lake asphalt of table (TLA)
As shown in Table 5, lake asphalt sample is smaller through 900 DEG C of burning quality losses and bitumen content test result difference.This
It is primarily due to, X-ray diffraction test result shows (lake asphalt X ray diffracting spectrum is referring to fig. 4), the mineralogical composition of lake asphalt
Mainly SiO2, mica, Fe2O3, carbonate content is very low, because of the mass loss very little of carbonate decomposition contribution, quality in calcining
Loss is mainly contributed by asphalt component and other organic matters.
Using solubility method method, test method step is identical as the method and step of embodiment 1.Lake asphalt (TLA) test
Initial data and calculated result are shown in Table 6.
The bitumen content (solubility method) of 6 lake asphalt of table (TLA)
Comparison sheet 5 and table 6 are it is found that the result of the method for the present invention acquisition is bigger than the result that solubility method obtains by 8.49%.This
It is primarily due to, about 3% other organic matters contained in the non-mineral ingredient of lake asphalt other than pitch class material and about 4%
Mineral combination water be not dissolved in trichloro ethylene, and under 900 DEG C of calcination conditions, this kind of composition material calcining and decomposing, therefore this
The result that inventive method obtains is larger.If on the basis of solubility method, test result and its difference that the method for the present invention is obtained
Value can be used as bitumen content correction factor, and such as in the present embodiment, bitumen content correction factor is 8.49%.Using present invention side
Method is measured the bitumen content of same batch lake asphalt, and applies correction factor, then can get the pitch with batch lake asphalt
The accurate result of content.
There are difference, some, which contains, to be not dissolved in for the bitumen content of different sources source natural solid bitumen and mineral composition
The organic constituents of trichloro ethylene.Therefore, when the present invention for other solid asphalts bitumen content test when, while with dissolve
Degree method is tested, and the result obtained to two kinds of methods is compared, and obtains bitumen content correction factor, the correction factor
The measurement of bitumen content applied to subsequent same batch solid asphalt.
Embodiment 3
The bitumen content test method of the present embodiment and BUTON rock asphalt of the invention in embodiment 1 is essentially identical, different
Place is, in the present embodiment, the quality that rock asphalt sample is added in every crucible is about 1.0g.
Embodiment 4
The bitumen content test method of the present embodiment and BUTON rock asphalt of the invention in embodiment 1 is essentially identical, different
Place is, in the present embodiment, the quality that rock asphalt sample is added in every crucible is about 10.0g.
Embodiment 5
The bitumen content test method of the present embodiment and BUTON rock asphalt of the invention in embodiment 1 is essentially identical, different
Place is, in the present embodiment, the quality that rock asphalt sample is added in every crucible is about 2.0g.
The above-mentioned description to embodiment is for ease of ordinary skill in the art to understand and use the invention.It is ripe
The personnel for knowing art technology obviously easily can make various modifications to these embodiments, and general original described herein
It ought to use in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, this field
Technical staff's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be in guarantors of the invention
Within the scope of shield.
Claims (9)
1. a kind of bitumen content test method of BUTON rock asphalt, which is characterized in that high-temperature calcination is carried out to rock asphalt sample, it is right
The asphaltic residue obtained after high-temperature calcination adds sufficiently soluble easy decomposing carbonate solution and is reacted, and obtains reaction residual
Then object dries reaction residue, by the difference of the quality of the quality and rock asphalt sample of dry reaction residue, calculate
Obtain the bitumen content of BUTON rock asphalt.
2. a kind of bitumen content test method of BUTON rock asphalt according to claim 1, which is characterized in that high-temperature calcination
Temperature be that can make the temperature of the carbonate decomposition in rock asphalt sample.
3. a kind of bitumen content test method of BUTON rock asphalt according to claim 2, which is characterized in that high-temperature calcination
Condition be that 2h or more is calcined at (900 ± 20) DEG C.
4. a kind of bitumen content test method of BUTON rock asphalt according to claim 1, which is characterized in that described can
The easy decomposing carbonate of dissolubility is NH4HCO3Or (NH4)2CO3。
5. a kind of bitumen content test method of BUTON rock asphalt according to claim 1, which is characterized in that reaction residual
The condition of object drying are as follows: until being first dried in reaction residue at (80 ± 10) DEG C without solution, then in (115 ± 5) DEG C item
2h or more is dried under part.
6. a kind of bitumen content test method of BUTON rock asphalt according to claim 1, which is characterized in that rock asphalt examination
Sample first removes moisture through low temperature drying using preceding.
7. a kind of bitumen content test method of BUTON rock asphalt according to claim 1, which is characterized in that the rock
The quality of bitumen samples is (1.0~10.0) g.
8. a kind of bitumen content test method of BUTON rock asphalt according to claim 7, which is characterized in that the rock
The quality of bitumen samples is (2.0~6.0) g.
9. the bitumen content test method of any a kind of BUTON rock asphalt according to claim 1~8, which is characterized in that
Specifically includes the following steps:
A) drying quality m is weighed1；
B) dry rock asphalt sample is added into crucible, weighs total quality m of crucible and rock asphalt sample2；
C) crucible equipped with rock asphalt sample is put into high temperature furnace, 2h or more is calcined under the conditions of (900 ± 20) DEG C；
D) crucible is taken out, is put into drier and is cooled to room temperature, weighs total quality m of crucible and asphaltic residue3；
E) soluble easily decomposing carbonate solution is added into the crucible equipped with asphaltic residue；
F) crucible equipped with carbonate solution is put into baking oven, is dried to nothing in reaction residue under the conditions of (80 ± 10) DEG C
Until solution；
G) 2h or more is dried under the conditions of (115 ± 5) DEG C, weighs total quality m of crucible and reaction residue4；
H) the burning quality loss and bitumen content of rock asphalt sample to be measured is calculated as follows:
In formula: PL--- the burning quality of rock asphalt sample loses, %；
PB--- the bitumen content of rock asphalt sample, %；
m1--- quality, g；
m2--- total quality of crucible and rock asphalt sample, g before calcining；
m3--- total quality of crucible and asphaltic residue, g after calcining；
m4--- total quality of crucible and reaction residue, g after calcining.
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| CN106018762A (en) * | 2016-05-12 | 2016-10-12 | 华南理工大学 | Gradational segregation situation considered method for detecting asphalt content through laboratory test |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106018762A (en) * | 2016-05-12 | 2016-10-12 | 华南理工大学 | Gradational segregation situation considered method for detecting asphalt content through laboratory test |
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| Title |
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| 李福普等: "《公路工程沥青及沥青混合料试验规程(JTG E20-2011)》", 31 December 2011 * |
| 沈金安: "《公路工程沥青及沥青混合料试验规程》(JTJ 052-2000)》", 1 October 2000 * |
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