CN106124552B - A kind of foamed asphalt moisture method of testing - Google Patents
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- 239000010426 asphalt Substances 0.000 title claims abstract description 350
- 238000010998 test method Methods 0.000 title abstract description 5
- 238000005481 NMR spectroscopy Methods 0.000 claims abstract description 87
- 238000000034 method Methods 0.000 claims abstract description 34
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- 238000012360 testing method Methods 0.000 claims abstract description 18
- 238000004458 analytical method Methods 0.000 claims abstract description 9
- 239000000523 sample Substances 0.000 claims description 241
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 87
- 239000012535 impurity Substances 0.000 claims description 43
- 238000001704 evaporation Methods 0.000 claims description 37
- 230000008020 evaporation Effects 0.000 claims description 37
- 239000011521 glass Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-ZSJDYOACSA-N Heavy water Chemical compound [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 5
- 238000005187 foaming Methods 0.000 claims description 4
- 238000000685 Carr-Purcell-Meiboom-Gill pulse sequence Methods 0.000 claims description 3
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- 230000005494 condensation Effects 0.000 claims description 2
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- 239000000203 mixture Substances 0.000 description 13
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- 238000009792 diffusion process Methods 0.000 description 4
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- 238000001228 spectrum Methods 0.000 description 2
- 238000012424 Freeze-thaw process Methods 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000012369 In process control Methods 0.000 description 1
- 238000000441 X-ray spectroscopy Methods 0.000 description 1
- 238000013459 approach Methods 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
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
- G01N24/082—Measurement of solid, liquid or gas content
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
A kind of foamed asphalt moisture method of testing of the present invention, relate to the use of nuclear magnetic resonance to test or analysis of material, the moisture in foamed asphalt is determined using nuclear magnetic resonance device, step is：The preparation of the foamed asphalt sample of moisture to be tested；The constants of nuclear magnetic resonance of nuclear magnetic resonance device is set；Obtain every gram of NMR signal amount for removing deimpurity pitch；Determine the relation of moisture and NMR signal amount in standard specimen；Obtain the NMR signal total amount of the foamed asphalt sample of moisture to be tested；Obtain the quality of the foamed asphalt evaporated residue in the foamed asphalt sample of moisture to be tested；The calculating of moisture in the foamed asphalt sample of moisture to be tested.The defects of present in the asphalt moisture distribution method of testing of industry CT disclosed in moisture and the CN103558236A for not being suitable for determining in foamed asphalt the present invention overcomes above-mentioned art methods.
Description
Technical Field
The technical scheme of the invention relates to a method for testing or analyzing materials by utilizing nuclear magnetic resonance, in particular to a method for testing the moisture content of foamed asphalt.
Background
Compared with the common hot-mix asphalt mixture, the warm-mix asphalt mixture can be an asphalt mixture which is mixed, paved and rolled at a relatively low temperature. The warm mixing technology can be mainly obtained by the following four technical approaches, including: wax-based warm mix agents, foamed asphalt, emulsifiers, and surfactants. The mixing temperature of the warm-mixed asphalt mixture is 105-125 ℃, the mixing temperature of the common hot-mixed asphalt mixture is 135-165 ℃, the construction temperature is obviously reduced, and the energy can be saved by 20-30% according to calculation.
Compared with other warm mixing technologies, the foamed asphalt warm mixing technology has obvious advantages and is still in a popularization stage in the world. The technology has some technical problems until now, including whether the water introduction in the foaming process can cause water damage of the asphalt pavement and further solution is needed. After the construction is completed, the foam collapses and some water may remain in the mix, which through diffusion and freeze-thaw processes is likely to cause water damage to the asphalt pavement. In order to systematically know the moisture content and the variation law of foamed bitumen and its mixtures in advance, some prior art studied for this purpose in the field are as follows:
(1) the weight method comprises the following steps: although the method is simple to operate, because some salt which is soluble in water in the asphalt enters the water phase, the quality change of the obtained asphalt cannot directly reflect the diffusion of water in the asphalt.
(2) Infrared spectroscopy-attenuated total reflection: the method is applied to research on the diffusion problem of water in the asphalt. Because the wave number is 3000cm-1-3650cm-1Here, the intensity of the stretching vibration peak of the hydroxyl group in the water molecule is increased with the increase of the moisture entering into the asphalt, and the water molecule is at 1640cm-1The bending vibration peak does not appear when the moisture content is very low, so the strength of the hydroxyl stretching vibration peak at different time is measured, and the diffusion process of the moisture in the asphalt can be researched. The method requires that the asphalt is made into a film shape, one side of the asphalt is water, and the other side is SiO2The film is not in accordance with the use environment of the foamed asphalt, so the method is not suitable for detecting the moisture content and the change rule of the foamed asphalt.
(3) Diffusion-Through test method: the method is mainly used for researching the asphalt used as the nuclear waste protection asphalt. It is necessary to use a radioactive element as a tracer and study by measuring the change in the concentration of the tracer. The method is inconvenient and practical, and is not suitable for detecting the moisture content and the change rule of the foam asphalt.
(4) X-ray spectral method: the water bubbles in the foamed asphalt and the change of the water bubbles along with the time are analyzed by an X-ray spectrometry instrument adopting a synchrotron technology. However, the X-ray method does not directly answer how much moisture is introduced into the foamed bitumen because the blisters are generally hollow and the volume of the pores does not reflect the volume of water; x-rays are susceptible to interference from atomic electron clouds; the X-ray method is not very sensitive to atoms with smaller atomic weight ratio, and is not suitable for detecting the moisture content and the change rule of the foamed asphalt.
(5) Neutron small angle diffraction method: neutrons interact with atoms through short-range nuclear forces, and are therefore as effective as isotopes for atoms of smaller molecular weight; meanwhile, the neutrons without electric charges can deeply permeate the material, so that the characteristics of the material can be researched in a complex sample environment. However, the neutron source required for carrying out neutron small angle diffraction experiments is generally a neutron reactor or a transmutation neutron source, which means that nuclear fuel is required as a neutron source, so that the detection technology is very difficult to use.
(6) Electrochemical impedance method: electrochemical ac impedance is a common electrochemical testing technique, is widely used for researching the corrosion behavior of coating metal, and is a mature and simple method. However, the technology requires that one side of a sample to be detected must be metal, and the other side must be water or solution, which is not suitable for the use environment of foamed asphalt, so that the technology is not suitable for detecting the moisture content of the foamed asphalt.
(7) CN103558236A discloses "asphalt mixture moisture distribution test method based on industrial CT". The CT imaging method mainly has three defects: firstly, designing 2 times of signal conversion (signal digital-to-analog/analog-to-digital conversion) in the whole imaging process, wherein a tiny signal can be easily lost in the digital-to-analog/analog-to-digital conversion process; CT imaging has precision limitation, the existing imaging precision is generally in the range of 10 microns, and micro water drops smaller than 10 microns cannot be reflected in a CT imaging picture; and thirdly, measuring and calculating the obtained increased area of the non-void substance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method for testing the moisture content of the foamed asphalt adopts a nuclear magnetic resonance device to measure the moisture content of the foamed asphalt, and overcomes the defects that the prior art method is not suitable for measuring the moisture content of the foamed asphalt and the method for testing the moisture distribution of the asphalt mixture by the industrial CT disclosed by CN 103558236A.
The technical scheme adopted by the invention for solving the technical problem is as follows: a method for testing the moisture content of foamed asphalt adopts a nuclear magnetic resonance device to measure the moisture content of the foamed asphalt, and comprises the following steps:
step one, preparing a foamed asphalt sample to be tested for moisture content:
heating unfoamed matrix asphalt to 150 deg.C, spraying into foamed asphalt by starting indoor laboratory asphalt foaming device, collecting foamed asphalt with 1000mL glass beaker, stirring at 10 rpm for 120s, standing for 120s, injecting foamed asphalt 10 g + -1 g into glass bottle with diameter of 20mm, and accurately measuring the injected glassThe quality of the foamed asphalt sample to be tested for the water content in the glass bottle is ZFoamed asphalt sampleWhen the precision requirement reaches 0.001 g, putting the glass bottle of the foamed asphalt sample to be tested with the water content into a refrigerating chamber with the temperature of 2-6 ℃ for storage, and testing;
and step two, setting nuclear magnetic parameters of a nuclear magnetic resonance device:
setting nuclear magnetic parameters of a nuclear magnetic resonance device for measuring the moisture content of the foamed asphalt as follows: the magnetic field intensity of the permanent magnet is 0.53T, the resonance frequency is 23.347MHz, the magnet temperature is controlled at 32.00 +/-0.02 ℃, the diameter of a probe coil is 25mm, and the CPMG: SF 23MHz, O1 347913.2Hz, P1 8us, P2 15us, SW 200KHz, TW 5000ms, RFD 0.002ms, RG 120 db, DRG 13, NS 64, DR 1, PRG 3, NECH 18000, TD 1799894, TE 0.7 ms;
thirdly, acquiring the nuclear magnetic resonance signal quantity of each gram of the asphalt with impurities removed:
firstly, preparing an asphalt sample with impurities removed: melting the asphalt with impurities removed, placing the melted asphalt into a glass bottle with the diameter of 20mm, cooling, accurately weighing the mass of the asphalt sample with the impurities removed, which is placed into the glass bottle, wherein the precision is 0.001 g, setting the nuclear magnetic parameters of a nuclear magnetic resonance device for determination as shown in the second step, placing the glass bottle with the asphalt sample with the impurities removed into a coil in the nuclear magnetic resonance device to collect nuclear magnetic resonance signals, obtaining a relaxation time distribution spectrogram of the asphalt sample with the impurities removed through inversion analysis of the collected nuclear magnetic resonance signals, integrating the curve of the spectrogram to obtain the nuclear magnetic resonance signal quantity of the asphalt sample with the impurities removed, and then, removing the mass of the asphalt sample with the impurities removed, which is accurately weighed, to obtain the nuclear magnetic resonance signal quantity of the asphalt sample with the impurities removed per gram as HPergram of impurity-removed asphalt sample；
Fourthly, determining the relation between the water content in the standard sample and the nuclear magnetic resonance signal quantity:
with known massWater (H)2O) and heavy water (D) of known mass2O) preparing a mixed liquid of water and heavy water with certain mass as a standard sample, respectively putting four standard samples with known water content mass into coils in the same nuclear magnetic resonance device to collect nuclear magnetic resonance signals, and fitting a strip of asphalt sample with water content mass ZWater contentNuclear magnetic resonance signal quantity H of water content in asphalt sampleMoisture contentThe relation between the two is straight line, and the straight line equation obtained by regression is shown as formula (1):
Hmoisture content＝a×ZWater content+b (1)
In the formula, a and b are experimental regression coefficients,
the conversion is as follows:
Zwater content＝(HMoisture content-b)/a (2)
And fifthly, acquiring the total nuclear magnetic resonance signal quantity of the foamed asphalt sample to be tested with the moisture content:
taking the foamed asphalt sample to be tested prepared in the first step out of a refrigerating chamber, wiping the surface of a glass bottle with soft cloth to be condensed, placing the foamed asphalt sample to be tested in a coil in the nuclear magnetic resonance device, starting the machine to collect nuclear magnetic resonance signals of the foamed asphalt sample to be tested, obtaining a relaxation time distribution spectrogram of the foamed asphalt sample to be tested through inverse analysis of the collected nuclear magnetic resonance signals, integrating the curve of the spectrogram, and obtaining the total nuclear magnetic resonance signal amount of the foamed asphalt sample with the water content to be tested as HFoamed asphalt sample；
Sixthly, acquiring the mass of the foamed asphalt evaporation residues in the foamed asphalt sample to be tested for the water content:
putting the foamed asphalt sample which has finished the nuclear magnetic resonance signal quantity measurement in the fifth step into an oven at 80 ℃, drying to constant weight, namely the mass change is less than 0.02% within 1 hour, cooling, and measuring the moisture content of the foamed asphalt sample to be testedThe mass of the foamed asphalt evaporation residue in (1) is ZFoamed asphalt evaporation residue in the sample；
And seventhly, calculating the moisture content in the foamed asphalt sample to be tested:
the total nuclear magnetic resonance signal amount H of the foamed asphalt sample with the water content to be tested is obtained in the fifth stepFoamed asphalt sampleComposed of two parts, namely the background nuclear magnetic resonance signal H of the light oil content in the foamed asphalt sample to be tested for the water contentBackgroundAnd the nuclear magnetic resonance signal quantity H of the water in the foamed asphalt sample to be tested for the water contentMoisture content，
Comprises the following steps:
Hfoamed asphalt sample＝HBackground+HMoisture content(3)
Wherein HBackground＝HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sampleSubstituting the formula (2) to obtain:
Hfoamed asphalt sample＝HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sample+HMoisture content(4)
Further obtaining:
Hmoisture content＝HFoamed asphalt sample-HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sample(5)
Thus calculating the mass Z of the moisture content in the foamed asphalt sample to be testedMoisture content in foamed asphalt samplesComprises the following steps:
Zmoisture content in foamed asphalt samples＝((HFoamed asphalt sample-HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sample)-b)/a (6)
Wherein,Hfoamed asphalt sampleMeasured by the above fifth step, HPergram of impurity-removed asphalt sampleMeasured by the above third step, ZFoamed asphalt evaporation residue in the sampleA and b are experimental regression coefficients measured in the sixth step;
the mass percentage of the moisture content in the foamed asphalt sample to be tested is as follows:
Zmoisture content in foamed asphalt samples/ZFoamed asphalt evaporation residue in the sample×100％；
The mass unit in each step is gram.
In the foamed asphalt moisture content testing method, the number of the foamed asphalt samples to be tested for moisture content in the first step is four.
The method for testing the moisture content of the foamed asphalt comprises the steps of obtaining related equipment, instruments and raw materials by known ways.
The invention has the beneficial effects that: compared with the prior art, the method has the prominent substantive characteristics and remarkable progresses that: the method is characterized in that a nuclear magnetic resonance device is adopted to determine the moisture content in the foamed asphalt, the change of a magnetic field signal of a foamed asphalt sample to be determined is directly determined, the magnetic field signal is directly converted into an electric signal, a mathematical tool is adopted to directly calculate the electric signal, a relaxation time distribution spectrogram can be obtained, the moisture content in the foamed asphalt sample can be obtained through formula calculation, the whole process only has 1 time of magnetic signal conversion into the electric signal, the analog signal conversion is realized, and the conversion of the signal can be considered to be lossless. The relaxation time distribution spectrogram and the moisture content have direct, clear and definite functional relation, multiple signal conversion and processing are not needed, and the testing precision is high, so that the defects that the prior art method is not suitable for measuring the moisture content in the foamed asphalt and the asphalt mixture moisture distribution testing method of the industrial CT disclosed by the CN103558236A are overcome.
The method for analyzing the water content of the foamed asphalt based on the nuclear magnetic resonance testing method has the advantages of simple operation, high precision, high detection speed, small human error, good repeatability, simple analysis method, convenience in process control and capability of realizing nondestructive detection. The analysis method provides a reliable, accurate and simple analysis method for researching water migration in the warm-mixing technology of the foamed asphalt, and has important practical value for detecting and controlling the quality of the foamed asphalt on the engineering site.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a graph showing the relaxation time distribution of four decontaminated asphalt samples.
FIG. 2 is a straight line graph showing the relationship between the mass of the water content in the four standard samples and the nuclear magnetic resonance signal amount of water in the standard samples.
FIG. 3 is a relaxation time distribution spectrum of four foamed asphalt samples to be tested for moisture content.
Detailed Description
Examples
The method for testing the moisture content of the foamed asphalt comprises the following steps:
step one, preparing a foamed asphalt sample to be tested for moisture content:
heating unfoamed matrix asphalt to 150 deg.C, spraying into foamed asphalt by using laboratory asphalt foaming device, collecting foamed asphalt with 1000mL glass beaker, stirring at 10 rpm for 120s, standing for 120s, and injecting 10 g + -1 g foamed asphalt into 20mm glass bottleThen accurately determining the mass Z of the foamed asphalt sample injected into the glass bottleFoamed asphalt sampleAnd the precision requirement reaches 0.001 g, the glass bottle of the foamed asphalt sample with the water content to be tested is placed into a refrigerating chamber with the temperature of 2-6 ℃ for storage, and four foamed asphalt samples with the water content to be tested are prepared, namely 5# foamed asphalt sample with the water content to be tested, and the mass of the sample is ZNo. 5 foamed asphalt sample10.112 g, 6# foamed asphalt sample to be tested for moisture content, having a mass ZNo. 6 foamed asphalt sample10.247 g of No. 7 foamed bitumen sample to be tested for moisture content, mass ZNo. 7 foamed asphalt sample10.560 g, 8# foamed asphalt sample to be tested for moisture content, with mass ZNo. 8 foamed asphalt sample9.789 g, to be measured;
and step two, setting nuclear magnetic parameters of a nuclear magnetic resonance device:
setting nuclear magnetic parameters of a nuclear magnetic resonance device for measuring the moisture content of the foamed asphalt as follows: the magnetic field intensity of the permanent magnet is 0.53T, the resonance frequency is 23.347MHz, the magnet temperature is controlled at 32.00 +/-0.02 ℃, the diameter of a probe coil is 25mm, and the CPMG: SF 23MHz, O1 347913.2Hz, P1 8us, P2 15us, SW 200KHz, TW 5000ms, RFD 0.002ms, RG 120 db, DRG 13, NS 64, DR 1, PRG 3, NECH 18000, TD 1799894, TE 0.7 ms;
thirdly, acquiring the nuclear magnetic resonance signal quantity of each gram of the asphalt with impurities removed:
firstly, four asphalt samples with impurities removed are prepared, namely a 1# asphalt sample with impurities removed, a 2# asphalt sample with impurities removed, a 3# asphalt sample with impurities removed and a 4# asphalt sample with impurities removed, pure asphalt with impurities removed by melting is put into a glass bottle with the diameter of 20mm, after cooling, the mass of the pure asphalt sample is accurately weighed, the precision is 0.001 g, wherein, the sample number 1# of the asphalt sample without impurities is 9.227 g, the sample number 2# of the asphalt sample without impurities is 10.629 g, the sample number 3# of the asphalt sample without impurities is 10.258 g, and the sample number 4# of the asphalt sample without impurities is 10.844 g, the nuclear magnetic parameters of the nuclear magnetic resonance device for measurement are set as the second step, the four glass bottles containing the asphalt sample without impurities are respectively put into the coil of the nuclear magnetic resonance device to collect nuclear magnetic resonance signals, and fig. 1 is a relaxation time distribution spectrum of the four asphalt samples without impurities.
The curves in fig. 1 are respectively, from bottom to top, a curve of a relaxation time distribution spectrogram of a 1# impurity-removed asphalt sample, a curve of a relaxation time distribution spectrogram of a 2# impurity-removed asphalt sample, a curve of a relaxation time distribution spectrogram of a 3# impurity-removed asphalt sample, and a curve of a relaxation time distribution spectrogram of a 4# impurity-removed asphalt sample, the curves of the spectrograms are integrated to obtain nuclear magnetic resonance signal quantities of the impurity-removed asphalt samples, and then the nuclear magnetic resonance signal quantities per gram of the impurity-removed asphalt sample are obtained by dividing the mass of the impurity-removed asphalt sample accurately weighed by the mass of the impurity-removed asphalt samplePergram of impurity-removed asphalt sample(ii) a Table 1 shows the NMR signal values H per gram for four samples of impurity-removed asphaltPergram of impurity-removed asphalt sample。
TABLE 1 NMR Signal values per gram H for four samples of decontaminated asphaltPergram of impurity-removed asphalt sample
Fourthly, determining the relation between the water content in the standard sample and the nuclear magnetic resonance signal quantity:
with water (H) of known mass2O) and heavy water (D) of known mass2O) preparing a mixed liquid of water and heavy water of a certain mass as a standard sample, putting four standard samples with known water content masses of 9# -0.05 g, 10# -0.3 g, 11# -0.6 g and 12# -1.0 g into a coil in the same nuclear magnetic resonance device respectively, collecting nuclear magnetic resonance signals, and fitting a water content mass Z in one standard sampleWater contentNuclear magnetic resonance with water in standard sampleVibration signal quantity HMoisture contentThe relation between the two is straight line, and the straight line equation obtained by regression is shown as formula (1):
Hmoisture content＝a×ZWater content+b (1)
In the formula, a and b are experimental regression coefficients,
the conversion is as follows:
Zwater content＝(HMoisture content-b)/a (2)
FIG. 2 is a line graph showing the relationship between the mass of the water content in the four standard samples and the NMR signal amount of water in the standard sample, and the regression result is HMoisture content＝57387×ZWater content+754.63，R20.9998, wherein the experimental regression coefficient a is 57387, the experimental regression coefficient b is 754.63, and R2The closer this value is to 1, the better the regression fit,
equation (2) can be written as:
Zwater content＝(HMoisture content-754.63)/57387 (2’)
And fifthly, acquiring the total nuclear magnetic resonance signal quantity of the foamed asphalt sample to be tested with the moisture content:
taking the foamed asphalt sample to be tested prepared in the first step out of a refrigerating chamber, wiping the surface of a glass bottle with a soft cloth for condensation, respectively placing the 5# foamed asphalt sample to be tested with water content, the 6# foamed asphalt sample with water content, the 7# foamed asphalt sample with water content and the 8# foamed asphalt sample with water content to be tested in coils of the nuclear magnetic resonance device, starting the nuclear magnetic resonance device to collect nuclear magnetic resonance signals of the foamed asphalt sample to be tested, and performing inversion analysis on the collected nuclear magnetic resonance signals to obtain relaxation time distribution spectrograms of the foamed asphalt samples to be tested, wherein fig. 3 is the relaxation time distribution spectrograms of the four foamed asphalt samples, and curves in the chart are respectively 5# foamed asphalt sample to be tested from bottom to topIntegrating the curve of the relaxation time distribution spectrogram of the foamed asphalt sample with the tested moisture content, the curve of the relaxation time distribution spectrogram of the foamed asphalt sample with the tested moisture content No. 6, the curve of the relaxation time distribution spectrogram of the foamed asphalt sample with the tested moisture content No. 7 and the curve of the relaxation time distribution spectrogram of the foamed asphalt sample with the tested moisture content No. 8 to obtain the total nuclear magnetic resonance signals of the foamed asphalt sample with the tested moisture content, wherein the total nuclear magnetic resonance signals of the foamed asphalt sample with the tested moisture content are respectively HNo. 5 foamed asphalt sample＝10423.512、HNo. 6 foamed asphalt sample＝10213.490、HNo. 7 foamed asphalt sample＝9645.871、HNo. 8 foamed asphalt sample＝8994.754；
Sixthly, acquiring the mass of the foamed asphalt evaporation residues in the foamed asphalt sample to be tested for the water content:
putting the four foamed asphalt samples with the moisture contents to be tested and subjected to the nuclear magnetic resonance signal quantity measurement in the fifth step into an oven with the temperature of 80 ℃, drying to constant weight, namely the mass change in 1 hour is less than 0.02%, and after cooling, determining the mass of the foamed asphalt evaporation residues in the foamed asphalt samples with the moisture contents to be tested to be ZFoamed asphalt evaporation residue in the sampleRespectively, the following steps: zFoamed asphalt evaporation residue in sample No. 510.015 g, ZFoamed asphalt evaporation residue in sample No. 610.164 g, ZFoamed asphalt evaporation residue in sample No. 710.476 g, ZFoamed asphalt evaporation residue in sample No. 89.712 g;
and seventhly, calculating the moisture content in the foamed asphalt sample to be tested:
the total nuclear magnetic resonance signal amount H of each foamed asphalt sample to be tested for the moisture content obtained in the fifth stepFoamed asphalt sampleComposed of two parts, i.e. background nuclear magnetic resonance signal H of light oil in asphaltBackgroundAnd moisture NMR signal quantity HMoisture content，
Comprises the following steps:
Hfoamed asphalt sample＝HBackground+HMoisture content(3)
Wherein HBackground＝HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sampleSubstituting the formula (2) to obtain:
Hfoamed asphalt sample＝HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sample+HMoisture content(4)
Further obtaining:
Hmoisture content＝HFoamed asphalt sample-HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sample(5)
Thus calculating the mass Z of the moisture content in the foamed asphalt sample to be testedMoisture content in foamed asphalt samplesComprises the following steps:
Zmoisture content in foamed asphalt samples＝((HFoamed asphalt sample-HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sample)-b)/a (6)
Wherein HFoamed asphalt sampleMeasured by the above fifth step, HPergram of impurity-removed asphalt sampleMeasured by the above third step, ZFoamed asphalt evaporation residue in the sampleA and b are experimental regression coefficients measured in the sixth step;
obtaining: zMoisture content in No. 5 foamed asphalt sample＝0.0973，ZMoisture content in No. 6 foamed asphalt sample＝0.0963，ZMoisture content in No. 7 foamed asphalt sample＝0.1019，ZMoisture content in No. 8 foamed asphalt sample＝0.07903。
The mass percentage of the moisture content in the foamed asphalt sample to be tested is as follows:
Zmoisture content in foamed asphalt samples/ZFoamed asphalt evaporation residue in the sample×100％；
The mass unit in each step is gram.
TABLE 2 test results of moisture content in four foamed asphalt samples to be tested for moisture content
Table 2 lists the results of testing the moisture content of four foamed asphalt samples to be tested for moisture content, in which:
Hfoamed asphalt sampleThe total nuclear magnetic resonance signal quantity Z of the foamed asphalt sample to be tested with the moisture content obtained in the fifth stepFoamed asphalt evaporation residue in the sampleThe mass H of the foamed asphalt evaporation residue in the foamed asphalt sample to be tested for the moisture content measured in the sixth stepPergram of impurity-removed asphalt sampleThe arithmetic mean is H as listed in Table 1Pergram of impurity-removed asphalt sampleArithmetic mean, ZMoisture content in foamed asphalt samplesAnd the water content quality of the foamed asphalt sample with the water content to be tested, which is obtained by the seventh step, is calculated.
The equipment, instruments and raw materials involved in the above examples are all available in known ways.
Claims (1)
1. A method for testing the moisture content of foamed asphalt is characterized by comprising the following steps: the method for measuring the moisture content in the foamed asphalt by adopting the nuclear magnetic resonance device comprises the following steps:
step one, preparing a foamed asphalt sample to be tested for moisture content:
heating unfoamed matrix asphalt to 150 deg.C, spraying into foamed asphalt by starting indoor laboratory asphalt foaming device, collecting foamed asphalt with 1000mL glass beaker, stirring at 10 rpm for 120s, standing for 120s, and transferring into 20mm glass bottle10 g +/-1 g of foamed asphalt is injected into the glass bottle, and then the mass of the foamed asphalt sample injected into the glass bottle is accurately determined to be ZFoamed asphalt sampleAnd the precision requirement reaches 0.001 g, the glass bottle of the foamed asphalt sample with the water content to be tested is placed into a refrigerating chamber with the temperature of 2-6 ℃ for storage, and four foamed asphalt samples with the water content to be tested are prepared, namely 5# foamed asphalt sample with the water content to be tested, and the mass of the sample is ZNo. 5 foamed asphalt sampleSample of foamed bitumen having a moisture content to be tested of # 6, =10.112 g, mass ZNo. 6 foamed asphalt sampleSample No. 7 foamed asphalt to be tested for moisture content, with mass Z, of 10.247 gNo. 7 foamed asphalt sampleSample No. 8 foamed asphalt to be tested for moisture content, with mass Z, of 10.560 gNo. 8 foamed asphalt sample=9.789 g, to be tested;
and step two, setting nuclear magnetic parameters of a nuclear magnetic resonance device:
setting nuclear magnetic parameters of a nuclear magnetic resonance device for measuring the moisture content of the foamed asphalt as follows: the magnetic field intensity of the permanent magnet is 0.53T, the resonance frequency is 23.347MHz, the magnet temperature is controlled at 32.00 +/-0.02 ℃, the diameter of a probe coil is 25mm, and the CPMG: SF =23MHz, O1=347913.2Hz, P1=8us, P2=15us, SW =200KHz, TW = 5000ms, RFD =0.002ms, RG1=20db, DRG1=3, NS =64, DR =1, PRG =3, NECH =18000, TD = 1799894, TE = 0.7 ms;
thirdly, acquiring the nuclear magnetic resonance signal quantity of each gram of the asphalt with impurities removed:
firstly, four samples of the asphalt with impurities removed are prepared, namely a 1# sample of the asphalt with impurities removed, a 2# sample of the asphalt with impurities removed, a 3# sample of the asphalt with impurities removed and a 4# sample of the asphalt with impurities removed, the melted pure asphalt with impurities removed is put into a glass bottle with the diameter of 20mm, after cooling, the mass of the taken pure asphalt sample is accurately weighed, the precision is 0.001 g, wherein the 1# sample of the asphalt with impurities removed =9.227 g, the 2# sample of the asphalt with impurities removed =10.629 g, the 3# sample of the asphalt with impurities removed =10.258 g and the 4# sample of the asphalt with impurities removed =10.844 g, the nuclear magnetic parameters of a nuclear magnetic resonance device for measurement are set as shown in the second step, and the four samples of the asphalt with impurities removed are put into the glassRespectively placing glass bottles into a coil in the nuclear magnetic resonance device to collect nuclear magnetic resonance signals, and performing inversion analysis on the collected nuclear magnetic resonance signals to obtain a relaxation time distribution spectrogram of the asphalt sample without impurities, which comprises a curve of the relaxation time distribution spectrogram of the asphalt sample without impurities 1#, a curve of the relaxation time distribution spectrogram of the asphalt sample without impurities 2#, a curve of the relaxation time distribution spectrogram of the asphalt sample without impurities 3#, and a curve of the relaxation time distribution spectrogram of the asphalt sample without impurities 4#, integrating the curves of the spectrograms to obtain nuclear magnetic resonance signal quantity of each asphalt sample without impurities, and then dividing the nuclear magnetic resonance signal quantity of each gram of the asphalt sample without impurities accurately weighed into HPergram of impurity-removed asphalt sample(ii) a Wherein, H of 1# decontaminated asphalt samplePergram of impurity-removed asphalt sampleH of No =394.444, 2# decontaminated asphalt samplePergram of impurity-removed asphalt sampleH of asphalt sample with impurity removed =365.354, 3#Pergram of impurity-removed asphalt sampleH of asphalt sample with impurity removed =390.389, 4#Pergram of impurity-removed asphalt sample=376.233；
Fourthly, determining the relation between the water content in the standard sample and the nuclear magnetic resonance signal quantity:
with water (H) of known mass2O) and heavy water (D) of known mass2O) preparing a mixed liquid of water and heavy water with certain mass as a standard sample, respectively putting four standard samples with known water content masses of 9# =0.05g, 10# =0.3g, 11# =0.6g and 12# =1.0g into a coil in the same nuclear magnetic resonance device for collecting nuclear magnetic resonance signals, and fitting the mass Z of the water content in one standard sampleWater contentNuclear magnetic resonance signal quantity H from water in standard sampleMoisture contentThe relation between the two is straight line, and the straight line equation obtained by regression is shown as formula (1):
Hmoisture content=a×ZWater content+b （1）
In the formula, a and b are experimental regression coefficients,
the conversion is as follows:
Zwater content= （HMoisture content- b）/ a （2）
Obtaining a regression result H from a linear graph of the relationship between the mass of the water content in the four standard samples and the nuclear magnetic resonance signal quantity of the water in the standard samplesMoisture content=57387×ZWater content+754.63，R2=0.9998, wherein the experimental regression coefficient a =57387, the experimental regression coefficient b =754.63, R is the ratio of the sum of squares of regression and the sum of squares of total deviations, the closer this value is to 1, the better the regression fit is,
equation (2) can be written as:
Zwater content=（HMoisture content-754.63）/57387 （2’）
And fifthly, acquiring the total nuclear magnetic resonance signal quantity of the foamed asphalt sample to be tested with the moisture content:
taking the foamed asphalt sample to be tested prepared in the first step out of a refrigerating chamber, wiping the surface of a glass bottle with a soft cloth for condensation, respectively placing the 5# foamed asphalt sample to be tested with water content, the 6# foamed asphalt sample with water content, the 7# foamed asphalt sample with water content and the 8# foamed asphalt sample with water content to be tested in coils of the nuclear magnetic resonance device, starting to collect nuclear magnetic resonance signals of the foamed asphalt sample to be tested, and performing inverse analysis on the collected nuclear magnetic resonance signals to obtain relaxation time distribution spectrograms of the four foamed asphalt samples to be tested, wherein the relaxation time distribution spectrograms comprise a relaxation time distribution spectrogram curve of the 5# foamed asphalt sample with water content to be tested, a relaxation time distribution spectrogram curve of the 6# foamed asphalt sample with water content to be tested, a relaxation time distribution spectrogram curve of the 7# foamed asphalt sample with water content to be tested and an 8# water sample with water content to be tested Integrating the curve of the relaxation time distribution spectrogram of the foamed asphalt sample with the content, and acquiring the total nuclear magnetic resonance signals of the foamed asphalt samples with the water content to be tested, wherein the total nuclear magnetic resonance signals of the foamed asphalt samples with the water content to be tested are respectively HNo. 5 foamed asphalt sample=10423.512、HNo. 6 foamed asphalt sample=10213.490、HNo. 7 foamed asphalt sample=9645.871、HNo. 8 foamed asphalt sample=8994.754；
Sixthly, acquiring the mass of the foamed asphalt evaporation residues in the foamed asphalt sample to be tested for the water content:
putting the four foamed asphalt samples with the moisture contents to be tested and subjected to the nuclear magnetic resonance signal quantity measurement in the fifth step into an oven with the temperature of 80 ℃, drying to constant weight, namely the mass change in 1 hour is less than 0.02%, and after cooling, determining the mass of the foamed asphalt evaporation residues in the foamed asphalt samples with the moisture contents to be tested to be ZFoamed asphalt evaporation residue in the sampleRespectively, the following steps: zFoamed asphalt evaporation residue in sample No. 5=10.015 g, ZFoamed asphalt evaporation residue in sample No. 6=10.164 g, ZFoamed asphalt evaporation residue in sample No. 7=10.476 g, ZFoamed asphalt evaporation residue in sample No. 8=9.712 grams;
and seventhly, calculating the moisture content in the foamed asphalt sample to be tested:
the total nuclear magnetic resonance signal amount H of each foamed asphalt sample to be tested for the moisture content obtained in the fifth stepFoamed asphalt sampleComposed of two parts, i.e. background nuclear magnetic resonance signal H of light oil in asphaltBackgroundAnd moisture NMR signal quantity HMoisture content，
Comprises the following steps:
Hfoamed asphalt sample=HBackground+HMoisture content（3）
Wherein HBackground=HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sampleSubstituting the formula (2) to obtain:
Hfoamed asphalt sample=HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sample+HMoisture content（4）
Further obtaining:
Hmoisture content= HFoamed asphalt sample- HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sample（5）
Thus calculating the mass Z of the moisture content in the foamed asphalt sample to be testedMoisture content in foamed asphalt samplesComprises the following steps:
Zmoisture content in foamed asphalt samples= （（HFoamed asphalt sample- HPergram of impurity-removed asphalt sample×ZFoamed asphalt evaporation residue in the sample）- b）/ a （6）
Wherein HFoamed asphalt sampleMeasured by the above fifth step, HPergram of impurity-removed asphalt sampleMeasured by the above third step, ZFoamed asphalt evaporation residue in the sampleA and b are experimental regression coefficients measured in the sixth step;
obtaining: zMoisture content in No. 5 foamed asphalt sample=0.0973 g, ZMoisture content in No. 6 foamed asphalt sample=0.0963 g, ZMoisture content in No. 7 foamed asphalt sample=0.1019 g, ZMoisture content in No. 8 foamed asphalt sample=0.07903 grams;
the mass percentage of the moisture content in the foamed asphalt sample to be tested is as follows:
Zmoisture content in foamed asphalt samples/ZFoamed asphalt evaporation residue in the sample×100%；
The results were: the mass percentage of the moisture content in the 5# foamed asphalt sample to be tested with the moisture content is 1.017%, the mass percentage of the moisture content in the 6# foamed asphalt sample to be tested with the moisture content is 0.957%, the mass percentage of the moisture content in the 7# foamed asphalt sample to be tested with the moisture content is 0.819%, and the mass percentage of the moisture content in the 8# foamed asphalt sample to be tested with the moisture content is 0.814%;
the mass unit in each step is gram.
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