2.2.1. Adhesion Evaluation for Asphalt and Crumb Rubber Coarse Aggregate
The net adsorption test developed by the Strategic Highway Research Program in the USA is based on the bitumen–water–mineral system [
44]. This test was developed to evaluate the affinity of bitumen for aggregate and to determine the water sensitivity of a given bitumen–aggregate pair. Briefly, the aggregate is placed in a flowing bitumen–toluene solution, and the absorbance of the solution is measured using a photometer to calculate the amount of bitumen being stripped off. The static immersion test (AASHTO T 182) uses water osmosis to simulate the water-related damage after an actual road surface comes in contact with water [
45]. Nonetheless, the above-mentioned mainstream foreign methods include subjective analyses and have long test durations and insufficient reliability. China’s “Testing Procedures for the Mixing of Asphalt and Asphalt Mixtures for Highway Engineering” (JTG E 20-2011) adopts a water-boiling method in which the adhesion grade is determined according to the degree of peeling of bitumen membrane from the surface of a coarse aggregate particle in boiling water (grades range from 1 to 5) [
46]. After a comprehensive analysis, this study proposed an improved evaluation method based on the existing standard boiling method.
The improved method is based on the method of “Adhesion test of asphalt and coarse aggregate (T 0616)” [
46] and “Standard Practice for Effect of Water on Bituminous-Coated Aggregate Using Boiling Water” (ASTM D 3625) [
47]. It can be used for both crumb rubber–aggregate and rock aggregate by making the following specific modifications:
(a) The rubber crumbs have low density. To prevent the bitumen-covered crumbs from failing to be immersed in water, which would otherwise affect the test results, stone and rubber crumb are tied together with a cotton thread before testing so that the rubber crumbs will be weighed down by the mineral materials. However, in the boiling water, they are separated by 5 cm, with the mineral material beneath the rubber crumb (
Figure 2a), and both become completely immersed in boiling water.
(b) In the actual production of the crumb rubber–asphalt mixture, the rubber crumbs are directly dispersed in the mixing tank without heating. Therefore, the rubber crumbs are required to be immersed in hot asphalt at a normal temperature, and the mineral aggregate is required to be immersed in hot asphalt at a higher temperature (175 °C).
(c) In the suspension cooling process, it is preferable to suspend the mineral material parallel to the rubber crumbs to prevent the asphalt on the surface of the asphalt-coated rubber crumbs from dripping onto the surface of the mineral material (
Figure 2c).
(d) Considering that the crumb rubber–asphalt mixture is more deformable than an ordinary mixture, the working environment places higher adhesion requirements upon it, thus the boiling time of 3 min (or 10 min by ASTM D 3625) in the original specification is adjusted to 20 min, while the evaluation standard remains unchanged.
The coarse aggregate in the crumb rubber–asphalt mixture is divided into stone material and rubber crumbs. Their sizes are different; therefore, to avoid incomparability in test results caused by different aggregate specifications, a consistent aggregate size of 9.5–13.2 mm was used in this study. The method easily detected the differences in the adhesion of bitumen to stone minerals and rubber crumbs under the same test conditions.
2.2.2. Adhesion Evaluation Method for Bitumen and Crumb Rubber Fine Aggregate
At present, the test methods for evaluation of adhesion pertain to coarse aggregates. In contrast, fewer adhesion test methods have been developed for fine aggregates [
34]. However, damage to the mixture and peeling off are more likely to arise from finer aggregates than from coarser aggregates because their adhesion with bitumen is poorer. Therefore, the influence of the adhesion of fine rubber-particle aggregate with bitumen on the moisture stability of the mixture should not be ignored, and it is necessary to propose an evaluation method for the adhesion of bitumen to fine aggregate. This study proposed that the adhesion of asphalt and fine aggregate can be evaluated by a combined boiling–sieving method, as follows:
(1). Three 500-g samples of crumb rubber–asphalt mixture were prepared according to the design grade and the corresponding asphalt–aggregate ratio and were each placed on a flat bottom plate. The three samples were subjected to the following tests, and the average value was considered as the test result.
(2). The hot asphalt mixture on the flat bottom plate was cooled to room temperature. While cooling, the crumb rubber asphalt mixture was gently turned with a shovel so as not to damage the agglomerate; it should not be separated by hand or broken with a hammer.
(3). The mixture was collected, weighed to determine the mass
, and then passed through a sieve with 4.75-mm-wide holes (as shown in
Figure 3). A small shovel was used to guide the mixture gently so that it passed through the sieve holes freely without damaging its bonding state. The use of a shaker was strictly forbidden. The mixture on the 4.75 mm-square mesh was collected and weighed to determine the mass
.
(4). The collected mixture was immersed in a large beaker containing boiling water, and the degree of heating was adjusted to keep the water in a boiling state. The mixture was gently stirred with a glass rod during the boiling process, and a piece of paper was used to remove asphalt floating on the water surface.
(5). After boiling for 20 min, the mixture was taken out, placed in a flat pan, and cooled to room temperature. While cooling, the mixture was gently tumbled with a shovel, as in step 2.
(6). After the cooling of the mixture and the occurrence of complete evaporation of water, the mixture was again passed through the 4.75-mm-square mesh, using a shovel to help any free mixture to pass through the sieve, with the same requirements as in step 3. The part of the mixture that did not pass through the 4.75-mm sieve holes was weighed and its mass was recorded as .
The design concepts and calculation methods of the boiling–sieving method are as follows:
The mixture was in a freely bonded state after mixing and cooling. The crumb rubber asphalt mixture generally adopted intermittent gradation (2.36–4.75 mm). For convenience, this study used 4.75 mm as the boundary point between coarse and fine aggregates.
It was assumed that the mass of asphalt mastic (bitumen and mineral powder) coating the surface of the aggregate was directly proportional to the mass of the coarse and fine aggregate. In the mixture design, the mass ratio of the coarse aggregate was recorded as
, and the mass ratio of fine aggregate was recorded as
.
In Equations (1) and (2):
—The mass of coarse aggregate covered with asphalt and mineral powder (g);
—The mass of fine aggregates coated with asphalt and mineral powder (g);
—Total mass of the mixture (g);
—The mass ratio of coarse aggregate in the mix design (%);
—The mass ratio of fine aggregate in the mix design (%);
Boiling led to peeling off of some fine aggregates from the surface of the coarse aggregates, and the peeling rate of the fine aggregate was the ratio of the mass of the exfoliated fine aggregate to the mass of the fine aggregate on the surface of the coarse aggregate before boiling:
In Equation (3):
△L—Fine aggregate peeling off rate after boiling (%);
—The mass of the mixture with particles above 4.75 mm in diameter after mixing and cooling, including coarse aggregates coated with asphalt, adhering fine aggregates, and fine aggregates coated with asphalt forming agglomerates (g);
—The mass of the mixture with particles above 4.75 mm in diameter after boiling and secondary screening (g);
The boiling–sieving method has some deficiencies for evaluating the adhesion of asphalt to fine aggregates. This method can only be used to evaluate the overall adhesion of asphalt to all fine aggregates, including stone aggregates and rubber particles. This is the first method developed that can be used to evaluate the adhesion properties of fine aggregates in the asphalt mixture.
2.2.3. Moisture Stability Evaluation Method of Crumb Rubber–asphalt Mixture
Owing to the mechanical and deformational properties of the crumb rubber–asphalt mixture, the harsh environmental conditions, and repeated traffic load to which it is exposed, the study of the moisture stability of the crumb rubber–asphalt pavement is significantly important [
48]. Conventional evaluation methods for asphalt mixture moisture stability, such as the Marshall water immersion test and the indirect tensile strength test under freeze–thaw cycle, are not sufficient to evaluate the long-term moisture stability of crumb rubber–asphalt pavement under special environmental conditions and repeated traffic load [
49,
50]. Based on the characteristics of rubber crumbs, the actual environmental conditions of the pavement and load effects to which it was exposed [
38], this study proposed the indirect tensile strength test under a freeze–thaw–boil cycle as the main evaluation method for the moisture stability of the crumb rubber–asphalt mixture. Furthermore, considering the deformation performance of the crumb rubber–asphalt mixture, the Cántabro abrasion test [
46] under water immersion was used as an auxiliary evaluation method. This test method can be used to comprehensively evaluate the long-term water stability of the crumb rubber–asphalt mixture.
(1) Indirect Tensile Strength Test under Freeze–Thaw–Boil cycle
The proposed indirect tensile strength test differs from the conventional indirect tensile strength test under freeze–thaw (as ASTM D 4867) [
51] in that a set of test specimens are subjected to freeze–thaw and boiling treatment, and the water stability performance of these specimens is analyzed compared to untreated test specimens and test specimens under special treatment. The test method is based on the following principles: the water that enters the interior of the mixture in the ice and snow season is simulated by exposing a vacuum-saturated test specimen to a freeze–thaw cycle; and, the repeated scouring action of the dynamic water pressure generated by dynamic wheel load is simulated by continuous boiling in water at 100 °C. By incorporating these two aspects, the improved method test can better evaluate the water stability of crumb rubber–asphalt mixture than the conventional freeze–thaw split test. Further, as described above, in order to more objectively evaluate the long-term water stability performance of the crumb rubber–asphalt mixture, a test specimen that has been aged for a long term (refer to “Practice for Shortened Long Term Aging of Hot Mix Asphalt ” T 0734) [
46] is also subjected to the indirect tensile strength test under a freeze–thaw–boil cycle, and the durability of this mixture specimen against water damage is obtained by comparative analysis. The test implementation process is shown in
Figure 4.
The specific steps in the indirect tensile strength test under a freeze–thaw–boil operation are as follows:
- (a)
The test specimens, which correspond to the samples of the mixture that have been subjected to standard Marshall compaction molding, are randomly divided into three groups, each group comprising no less than four specimens.
- (b)
The average value of the splitting strength of the first group of specimens at 25 °C, recorded as , is obtained directly. The second and third sets of specimens are vacuum-saturated for 15 min at 97.3–98.7 kPa and then returned to normal pressure for 0.5 h in water. The test specimens are taken out of the water and placed at a temperature of −18 °C for 16 h.
- (c)
The second set of test specimens are thawed to 25 °C, and the average value of the splitting strength of the set is determined and recorded as . After the freeze–thaw cycle, the third set of test specimens are immediately placed in boiling water for 2 h and then cooled to 25 °C before measuring the splitting strength, which is recorded as.
- (d)
The tensile strength ratios
of the crumb rubber–asphalt mixture,
, and
are respectively calculated according to Equations (4) and (5) as follows:
In the formulas:
—The indirect tensile strength ratio under freeze–thaw cycle (%);
—The indirect tensile strength ratio under freeze–thaw–boil cycle (%);
—Average value indirect tensile strength of the first set of effective specimens under normal conditions (MPa);
—Average value of indirect tensile strength of the second set of effective specimens after a freezing and thawing cycle (MPa);
—Average value of indirect tensile strength of the third set of effective specimens under long-term aged after a freeze-thaw-boil cycle (MPa).
Long-term aging treatment of the third set of specimens is required to assess the long-term water stability of the mixture (refer to test method T 0734-2000 in “Testing Procedures for Asphalt and Asphalt Mixtures for Highway Engineering”; loose mix 135 °C/4 h, compacted test specimen 85 °C/5 d) [
46]. After aging, the freeze–thaw–boiling–splitting test for the third set of test specimens as described above was carried out on this specimen to obtain the splitting strength ratio, which was recorded as
. At present, the Chinese standard generally uses an unaged asphalt mixture for freeze–thaw split testing to evaluate water stability, while AASHTO tests the long-term aged mixture in America. For an ordinary asphalt mixture, the impact of the implementation of the Chinese standard is not significant, but considering the special mechanical characteristics and the complex working environment experienced by the crumb rubber–asphalt mixture, this study proposes that it is necessary to carry out the above-mentioned freeze–thaw boiling procedure on a long-term aged test specimen.
(2) Cántabro Abrasion Test under water-immersion
The Cántabro test is usually used for assessing the water damage resistance of the porous mixtures, of which the main distress is aggregate stripping. Thus, because the main distress of crumb rubber–asphalt pavement is also aggregate stripping, we here introduce it as an auxiliary evaluation method. A water immersion test was carried out by immersing the specimens in the water at 60 °C for 48 h. The main objective of the Cántabro abrasion test [
46] under water immersion was to investigate the expansion of rubber crumbs in hot water. The pressure of the Marshall specimen in the test machine was used to simulate its stability after instantaneous extrusion and elastic recovery of the mixture under dynamic traffic load.