CN110763644A - Separation method of four components of asphalt - Google Patents
Separation method of four components of asphalt Download PDFInfo
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- CN110763644A CN110763644A CN201911066990.8A CN201911066990A CN110763644A CN 110763644 A CN110763644 A CN 110763644A CN 201911066990 A CN201911066990 A CN 201911066990A CN 110763644 A CN110763644 A CN 110763644A
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- 239000010426 asphalt Substances 0.000 title claims abstract description 102
- 238000000926 separation method Methods 0.000 title claims abstract description 15
- 238000012360 testing method Methods 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 23
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 57
- 239000002904 solvent Substances 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 9
- 239000002156 adsorbate Substances 0.000 claims description 9
- 238000010828 elution Methods 0.000 claims description 9
- 238000003795 desorption Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 8
- 239000003208 petroleum Substances 0.000 claims description 7
- 238000002211 ultraviolet spectrum Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 10
- 230000032683 aging Effects 0.000 abstract description 7
- 239000011521 glass Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 239000012156 elution solvent Substances 0.000 abstract description 4
- 230000007246 mechanism Effects 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 125000003118 aryl group Chemical group 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- 239000003480 eluent Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012492 regenerant Substances 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Immunology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Engineering & Computer Science (AREA)
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses a method for separating four components of asphalt, which adopts a solid phase extraction column method and combines an ultraviolet spectrometer to separate and measure the components of the asphalt so as to obtain the content of each component of the asphalt, the solid phase extraction column replaces a glass adsorption column, the dosage of an asphalt sample and an elution solvent is obviously reduced, the test speed is high, the solid phase extraction column is industrially and uniformly produced, is less influenced by human factors, has uniform and consistent component separation effect and has better reproducibility. According to the invention, through separation and determination of four components of the asphalt, on one hand, the research on an asphalt aging mechanism and a regeneration mechanism can be realized, and on the other hand, the improvement on a certain performance of the asphalt can be realized by adjusting the content of one or more components in the asphalt, so that the pavement performance of the asphalt mixture is improved, the operation is simple and convenient, and the asphalt mixture is suitable for wide popularization and application.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the field of analysis of chemical components of asphalt materials, and relates to a separation method of four components of asphalt.
[ background of the invention ]
Bitumen is a product obtained by the specific treatment of crude oil by distillation and other processes, and comprises various hydrocarbons and derivatives thereof, and has a relatively complex structural composition. The most common analysis method for the chemical composition of asphalt at present is the four-component analysis method. Among the four components of the asphalt, the aromatic component has the function of softening the asphalt; the colloid has good adhesiveness, can increase ductility, and enables the asphalt to have good low-temperature crack resistance; asphaltenes directly affect the rheology of asphalt, and excess asphaltenes tend to improve the high temperature stability of asphalt mix, but also adversely affect low temperature crack resistance. It can be seen that the combination of the variation of the content of the components of the asphalt and the structure has a direct influence on the performance of the asphalt and even the asphalt mixture.
The significance of researching the four components of the asphalt is that the change condition of the content of each component of the asphalt in the long-term use process can be quantitatively analyzed, so that whether the asphalt is aged or not and the aging degree of the asphalt are researched on the one hand; meanwhile, according to the change condition of asphalt components and referring to relevant specifications, a regenerant or new asphalt with a corresponding label is added into aged asphalt to adjust the components of the aged asphalt, so that the performance of the aged asphalt is improved, the performance of the aged asphalt is equivalent to that of common asphalt, and the regeneration mechanism of the asphalt is further researched. On the other hand, the improvement of a certain property of the asphalt can be realized by adjusting the content of one or more components in the asphalt, so that the pavement property of the asphalt mixture is improved, the operation is simple and convenient, and the asphalt mixture is suitable for wide popularization and application.
The traditional four-component determination method of asphalt adopts a glass adsorption column method, asphalt is sequentially washed by using elution solvents such as n-heptane, toluene, ethanol and the like, four components of the asphalt are determined by distinguishing the color of each desorption object, and the content of each component is determined after the desorption objects are dried and volatilized. In the test process, the dosage of the elution solvent such as n-heptane, toluene, ethanol and the like required by 1g of asphalt is close to 100ml, and the elution solvent needs to be heated, condensed, extracted, dried and the like when the content of each component is measured. The method has the obvious disadvantages that: firstly, the operation process of the test is complicated, the duration is too long, and the components of the asphalt have no definite color boundary; secondly, the amount of the eluent used in the test is relatively large, most of the eluent has toxicity, and the eluent is harmful to health and causes environmental pollution.
[ summary of the invention ]
The invention aims to solve the problems of complex operation, fuzzy boundary among components and environmental pollution in the traditional asphalt four-component determination method in the prior art, and provides an asphalt four-component separation method with simple operation and high reproducibility.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a method for separating four components of asphalt comprises the following steps:
step 1: respectively adding asphalt and an n-heptane solvent into a test tube, and mixing and dissolving by ultrasonic oscillation;
step 2: placing the test tube in the step 1 into a high-speed centrifuge for centrifugation for 10 minutes;
and step 3: taking out the supernatant in the test tube in the step 2, and obtaining insoluble substances which are the asphaltene after the solvent in the test tube is naturally volatilized;
and 4, step 4: adding an n-heptane solvent into the solid-phase extraction column, and activating the solid-phase extraction column;
and 5: putting the supernatant obtained in the step 3 into the solid phase extraction column in the step 4, adding an ethanol solvent for carrying out first elution, and putting the desorbed substance solution into a test tube No. 1;
step 6: adding a benzene solvent into the solid phase extraction column to carry out secondary elution on the adsorbate, and placing the desorbed solution into a No. 2 test tube;
and 7: adding an n-heptane solvent into the solid phase extraction column to carry out third elution on the adsorbate, and placing the adsorbate solution into a No. 3 test tube;
and 8: drying test tubes No. 1, 2 and 3 in an oven, and cooling at room temperature to obtain three substances;
and step 9: and (4) carrying out ultraviolet spectrum measurement on the three substances obtained in the step 8, and verifying the test result in the step 8.
The invention further improves the following steps:
the specific steps of ultraviolet spectroscopy determination in step 9 are as follows:
and (3) respectively adding the same amount of petroleum ether into the test tubes No. 1, No. 2 and No. 3 dried in the step 8, respectively putting the three obtained mixed solutions into an ultraviolet spectrometer after the three desorption matters are fully dissolved by the petroleum ether, and judging the components of the desorption matters by comparing the absorption peaks of the ultraviolet spectrograms of the three mixed solutions.
In the step 1, the mass ratio of the asphalt to the n-heptane is 1: 40, the mass of the asphalt is 0.095-0.105 g.
The rotating speed of the high-speed centrifuge in the step 2 is 12000 r/min.
The amount of n-heptane solvent used in step 4 was 10 mL.
In the step 5, the dosage of the supernatant is 2mL, and the dosage of the ethanol solvent is 3 mL.
The amount of benzene solvent used in step 6 was 3 mL.
The amount of n-heptane solvent used in step 7 was 3 mL.
In the step 8, the drying temperature is 55-65 ℃, and the drying time is 8-10 h.
Compared with the prior art, the invention has the following beneficial effects:
the method for separating the four components of the asphalt provided by the invention adopts the solid-phase extraction column for separation, simplifies the steps compared with the traditional glass adsorption column method, shortens the separation time, accurately determines the components of the desorbed substances which are preliminarily identified as colloid, aromatic components and saturated components through ultraviolet spectrum, simultaneously verifies the feasibility of separating the four components of the asphalt by the solid-phase extraction column, and avoids the defect of poor separation effect caused by the fact that no clear color limit exists among the components of the asphalt in the traditional method. In addition, the dosage of the eluent adopted in the test process is reduced from hundreds of milliliters to milliliters, so that the harm to human bodies and the pollution to the environment are reduced. The asphalt four-component separation method adopted by the invention has the advantages that the test process is simple and convenient to operate, the solid phase extraction column is industrially and uniformly produced, is less influenced by human factors, has uniform and consistent component separation effect, has better reproducibility, has better separation effect on the asphalt four-component, and is suitable for wide popularization.
[ description of the drawings ]
FIG. 1 is a schematic diagram of a solid phase extraction column apparatus of the present invention, wherein ① - ④ represent four components of pitch, ⑤ - ⑦ represent adsorbates, and ⑧ represents desorbents;
FIG. 2 is a flow chart of a four-component test for separating asphalt by a solid phase extraction column method according to the present invention;
FIG. 3 is a UV spectrum of the components of the asphalt of the present invention.
[ detailed description ] embodiments
The invention is described in further detail below with reference to the accompanying drawings:
further details are given by taking A-90 asphalt provided by Niegy to Tengke first-level highway project, asphalt aged by 85min rotary film oven (abbreviated as 85min aged asphalt) and asphalt recycled from original asphalt pavement (abbreviated as RAP aged asphalt) as examples:
the technical performances of the used A-90 asphalt, 85min aged asphalt and aged asphalt in RAP were tested according to JTG E40-2011, and the test results are shown in Table 1. Wherein the method for extracting the aged asphalt in the RAP is a centrifuge extraction-microporous membrane vacuum reduced pressure filtration-rotary evaporator distillation combination method.
TABLE 1 summary of test results for asphalt A-90, aged asphalt in RAP, and aged asphalt 85min
The detection result shows that the performances of the A-90 asphalt before and after aging can meet the national requirements, the A-90 asphalt can be used for tests, the aging asphalt in 85min and the RAP can be seriously aged, and the penetration degree and the ductility can not meet the related requirements.
Example 1
Step 1: dissolving 0.1gA-90 asphalt in a test tube, adding 5.85ml of n-heptane solvent, and ultrasonically oscillating for 10min to mix uniformly;
step 2: placing the test tube in the step 1 into a high-speed centrifuge with the rotating speed of 12000r/min for centrifuging for 10 minutes to effectively separate;
and step 3: taking out the supernatant in the test tube, and obtaining insoluble substances which are asphaltene after the solvent in the test tube is naturally volatilized;
and 4, step 4: adding 10ml of n-heptane into the solid phase extraction column for activation;
and 5: placing 2ml of the supernatant obtained in the step 3 into the solid phase extraction column obtained in the step 4, adding 3ml of ethanol for first elution, and placing the desorbed solution into a No. 1 glass test tube;
step 6: adding 3ml of benzene into the solid phase extraction column, carrying out secondary elution on the adsorbate, and placing the desorbed solution into a No. 2 glass test tube;
and 7: adding 3ml of n-heptane into the solid phase extraction column, carrying out third elution on the residual adsorbate, and placing the obtained desorbent solution into a No. 3 glass test tube;
and 8: placing test tubes No. 1, 2 and 3 in an oven at 60 deg.C for 8h to fully dry and volatilize the eluting solvent in the test tubes, cooling at room temperature to obtain three substances which are primarily considered as colloid, aromatic component and saturated component, and measuring the mass of the three substances;
and step 9: and (3) carrying out ultraviolet spectrum determination on the three substances obtained in the step (8): adding equal amount of petroleum ether into 3 test tubes respectively, and placing the three mixed solutions into an ultraviolet spectrometer respectively after the petroleum ether fully dissolves the three kinds of desorption matters. The ultraviolet spectrograms of three kinds of desorption substances, namely colloid, aromatic components and saturated components are determined by comparing the change conditions of the absorption peaks of the ultraviolet spectrograms of different solutions and are shown in figure 3. The added petroleum ether is a saturated solvent and has no absorption peak in the ultraviolet spectrum region.
In order to more intuitively show the principle and the process of separating four components of asphalt by a solid phase extraction column method, a test flow chart shown in figure 2 is designed.
Example 2
This example differs from example 1 in that 0.095g of aged bitumen in RAP was used, the amount of n-heptane solvent used was 5.55mL, the drying temperature in step 8 was 65 ℃ and the drying time was 8.5 h.
Example 3
This example differs from example 1 in that 0.103g of pitch was aged in an 85min rotary film oven using 6mL of n-heptane solvent at a temperature of 55 ℃ for 10h in step 8.
In summary, the results of the compositional testing of A-90 bitumen, aged bitumen in RAP, and bitumen aged by an 85min rotary film oven can be obtained, as shown in Table 2.
TABLE 2 asphalt composition Change test results
By adopting the method, the content change conditions of various components of the asphalt with different aging degrees can be quantitatively analyzed. As can be seen from Table 2, compared with the aged asphalt in RAP and the aged asphalt A-90, the aged asphalt in RAP has a larger content of large molecules such as asphaltene and a smaller content of light components such as aromatic compounds, which indicates that the aged asphalt in RAP is more severely aged. Further, by adopting the method, the aging degree of the asphalt in the asphalt mixture material of the pavement can be accurately judged by measuring the content of the internal components of the aged asphalt of the pavement, so that the aging degree of the asphalt pavement can be judged.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. The method for separating the four components of the asphalt is characterized by comprising the following steps of:
step 1: respectively adding asphalt and an n-heptane solvent into a test tube, and mixing and dissolving by ultrasonic oscillation;
step 2: placing the test tube in the step 1 into a high-speed centrifuge for centrifugation for 10 minutes;
and step 3: taking out the supernatant in the test tube in the step 2, and obtaining insoluble substances which are the asphaltene after the solvent in the test tube is naturally volatilized;
and 4, step 4: adding an n-heptane solvent into the solid-phase extraction column, and activating the solid-phase extraction column;
and 5: putting the supernatant obtained in the step 3 into the solid phase extraction column in the step 4, adding an ethanol solvent for carrying out first elution, and putting the desorbed substance solution into a test tube No. 1;
step 6: adding a benzene solvent into the solid phase extraction column to carry out secondary elution on the adsorbate, and placing the desorbed solution into a No. 2 test tube;
and 7: adding an n-heptane solvent into the solid phase extraction column to carry out third elution on the adsorbate, and placing the adsorbate solution into a No. 3 test tube;
and 8: drying test tubes No. 1, 2 and 3 in an oven, and cooling at room temperature to obtain three substances;
and step 9: and (4) carrying out ultraviolet spectrum measurement on the three substances obtained in the step 8, and verifying the test result in the step 8.
2. The method for separating four components of asphalt according to claim 1, wherein the ultraviolet spectroscopy measurement in step 9 comprises the following steps:
and (3) respectively adding the same amount of petroleum ether into the test tubes No. 1, No. 2 and No. 3 dried in the step 8, respectively putting the three obtained mixed solutions into an ultraviolet spectrometer after the three desorption matters are fully dissolved by the petroleum ether, and judging the components of the desorption matters by comparing the absorption peaks of the ultraviolet spectrograms of the three mixed solutions.
3. The method for separating the four components of the asphalt according to claim 1, wherein the mass ratio of the asphalt to the n-heptane in the step 1 is 1: 40, the mass of the asphalt is 0.095-0.105 g.
4. The method for separating the four components of asphalt according to claim 1, wherein the rotation speed of the high-speed centrifuge in the step 2 is 12000 r/min.
5. The process for the separation of four components of asphalt according to claim 1, wherein the amount of n-heptane solvent used in step 4 is 10 mL.
6. The method for separating the four components of asphalt according to claim 1, wherein the amount of the supernatant in step 5 is 2mL and the amount of the ethanol solvent is 3 mL.
7. The process for the separation of four components of asphalt according to claim 1, wherein the amount of benzene solvent used in step 6 is 3 mL.
8. The process for the separation of four components of bitumen according to claim 1, wherein the amount of n-heptane solvent used in step 7 is 3 mL.
9. The method for separating the four components of the asphalt according to claim 1, wherein the drying temperature in the step 8 is 55-65 ℃ and the drying time is 8-10 h.
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| CN112755578A (en) * | 2020-12-22 | 2021-05-07 | 同济大学 | Asphalt cement separation method based on supercritical fluid extraction |
| CN113466081A (en) * | 2021-08-09 | 2021-10-01 | 西北大学 | Method for efficiently determining four components of coal tar |
| CN115184520A (en) * | 2022-07-11 | 2022-10-14 | 西南交通大学 | Asphalt component rapid separation method based on solubility parameter |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112755578A (en) * | 2020-12-22 | 2021-05-07 | 同济大学 | Asphalt cement separation method based on supercritical fluid extraction |
| CN113466081A (en) * | 2021-08-09 | 2021-10-01 | 西北大学 | Method for efficiently determining four components of coal tar |
| CN115184520A (en) * | 2022-07-11 | 2022-10-14 | 西南交通大学 | Asphalt component rapid separation method based on solubility parameter |
| CN115184520B (en) * | 2022-07-11 | 2023-08-01 | 西南交通大学 | Asphalt component rapid separation method based on solubility parameter |
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