Tests on Bitumen

Experience in using bitumen in engineering projects has led to the adoption of certain test procedures that are indicative of the characteristics that identify adequate performance levels. Some of the tests have evolved with the development of the industry and are empirical methods. Consequently it is essential that they are carried out in strict compliance with the recommended procedures if they are to be accurate measurements of the bitumen's properties. 1. Penetration Test 2. Flash Point Test 3. Solubility Test 4. Ductility Test 5. Viscosity Test 6. TFOT test

Test 1. Penetration Test on Bitumen
The penetration test is one of the oldest and most commonly used tests on asphalt cements or residues from distillation of asphalt cutbacks or emulsions. The standardized procedure for this test can be found in ASTM D5 [ASTM, 2001]. It is an empirical test that measures the consistency (hardness) of an asphalt at a specified test condition. Procedure of Penetration Test on Bitumen: In the standard test condition, a standard needle of a total load of 100 g is applied to the surface of an asphalt or Liquid bitumen sample at a temperature of 25 °C for 5 seconds. The amount of penetration of the needle at the end of 5 seconds is measured in units of 0.1 mm (or penetration unit). A softer asphalt will have a higher penetration, while a harder asphalt will have a lower penetration. Other test conditions that have been used include 1. 0 °C, 200 g, 60 sec., and 2.46 °C, 50 g, 5 sec. The penetration test can be used to designate grades of asphalt cement, and to measure changes in hardness due to age hardening or changes in temperature. Read a detailed procedure of Bitumen Penetration Test with Sample Data

Test 2. Flash Point Test on asphalt:
The flash point test determines the temperature to which an asphalt can be safely heated in the presence of an open flame. The test is performed by heating an asphalt sample in an open cup at a

Results of several . The solubility test is used to detect contamination in asphalt cement. Unfortunately. Specifications for asphalt cements normally require a minimum solubility in trichloroethylene of 99. The bitumen content of a bituminous material is measured by means of its solubility in carbon disulfide. The commonly used flash point test methods include 1. The material retained on the filter is then dried and weighed. When the flash point test is used to detect contaminating materials. The use of trichloroethylene will most likely be banned in the near future.specified rate and determining the temperature at which a small flame passing over the surface of the cup will cause the vapors from the asphalt sample temporarily to ignite or flash. the Pensky-Martens Closed Tester method (ASTM D93). Read a detailed procedure of Bitumen Penetration Test with Sample Data Test 3. rather than solubility in carbon disulfide. is normally used. Minimum flash point requirements are included in the specifications for asphalt cements for safety reasons. while the Tag Open-Cup method is used on cutback asphalts or asphalts with flash points of less than 79 °C. which are high-molecular-weight hydrocarbons soluble in carbon disulfide. and used to calculate the bitumen content as a percentage of the weight of the original asphalt. solubility in trichloroethylene. Flash point tests can also be used to detect contaminating materials such as gasoline or kerosine in an asphalt cement. An asphalt with a high flash point is more likely to have a lower hardening potential in the field.0 percent. is usually used in asphalt cement specifications. Due to the extreme flammability of carbon disulfide. Solubility Test on asphalt bitumen Asphalt consists primarily of bitumens. Procedure for Solubility test on Bitumen In the standard test for bitumen content (ASTM D4). In recent years. The standard solubility test using trichloroethylene is designated as ASTM D 2042.Tag Open Cup (ASTM D1310). There is a need to use a less hazardous and non-chlorinated solvent for this purpose. which tends to give more indicative results. Contamination of an asphalt cement by such materials can be indicated by a substantial drop in flash point.The Cleveland Open Cup (ASTM D92) 2. a small sample of about 2 g of the asphalt is dissolved in 100 ml of carbon disulfide and the solution is filtered through a filtering mat in a filtering crucible. the flash point test results have been related to the hardening potential of asphalt. The Cleveland Open-Cup method is used on asphalt cements or asphalts with relatively higher flash points. trichloroethylene has been identified as a carcinogen and contributing to the depletion of the earth’s ozone layer.

When the viscosity of an asphalt at a higher temperature (such as 135 °C) is to be determined. Ductility Test on Asphalt The ductility test (ASTM D113) measures the distance a standard asphalt sample will stretch without breaking under a standard testing condition (5 cm/min at 25 °C). The advantage of using the viscosity test as compared with the penetration test is that the viscosity test measures a fundamental physical property rather than an empirical value. the relationship between shear stress and shear rate is linear. the most commonly-used test is the Kinematic Viscosity Test (ASTM D2170). since the different methods might be measuring the viscosity at different shear rates. Viscosity Tests on Bitumen Asphalt The viscosity test measures the viscosity of an asphalt. Test 4. and thus the viscosity is constant at different shear rates or shear stress. which measures the kinematic viscosity in units of Stokes or centi-Stokes. especially at lower temperatures. Asphalts tend to behave as slightly non-Newtonian fluids.investigations have indicated that the solvent n-Propyl Bromide appears to be a feasible alternative to trichloroethylene for use in this application. Both the viscosity test and the penetration test measure the consistency of an asphalt at some specified temperatures and are used to designate grades of asphalts. It is generally considered that an asphalt with a very low ductility will have poor adhesive properties and thus poor performance in service. Kinematic viscosity is defined as: When viscosity is in units of Poise and density in units of g/cm. To convert from kinematic viscosity (in units of Stokes) to . for a non-Newtonian fluid. Read a detailed procedure of Bitumen Penetration Test with Sample Data Test 5. For a Newtonian fluid. The absolute viscosity test measures the viscosity in units of Poise. the test results might be significantly different. The viscosity at 60 °C represents the viscosity of the asphalt at the maximum temperature a pavement is likely to experience in most parts of the U. It is thus very important to indicate the test method used when viscosity results are presented. viscosity will be in units of Pascal-seconds. and shear stress in units of Pascal. the faster the asphalt will flow under the same stress. Viscosity is defined as the ratio between the applied shear stress and induced shear rate of a fluid. One Pascal-second is equal to 10 Poises. However. When shear rate is expressed in units of 1/sec. 3 the kinematic viscosity will be in units of Stokes. The most commonly used viscosity test on asphalt cements is the Absolute Viscosity Test by Vacuum Capillary Viscometer (ASTM D2171). Specifications for asphalt cements normally contain requirements for minimum ductility. The standard test temperature is 60 °C. the relationship between shear stress and shear rate is not linear. When different methods are used to measure the viscosity of an asphalt. and thus the apparent viscosity will change as the shear rate or shear stress changes.S. The lower the viscosity of an asphalt.

The carriage rotates within the oven while the 325°F (163°C) temperature ages the samples for 85 minutes.absolute viscosity (in units of Poises). Figure 1. Effect of Heat and Air on a Moving Film of Asphalt (Rolling Thin-Film Oven Test) Background . Rolling thin-film oven test. Test-6: Rolling Thin-Film Oven Overview The Rolling Thin-Film Oven (RTFO) procedure (Figure 1) provides simulated short term aged asphalt binder for physical property testing. The standard Rolling Thin-Film Oven test is:  AASHTO T 240 and ASTM D 2872. The basic RTFO procedure takes unaged asphalt binder samples in cylindrical glass bottles and places these bottles in a rotating carriage within an oven. The RTFO also provides a quantitative measure of the volatiles lost during the aging process. Samples are then stored for use in physical properties tests or the PAV. one simply multiplies the number of Stokes by the density in units of g/cm3. Asphalt binder is exposed to elevated temperatures to simulate manufacturing and placement aging.

One of the basic tenets of the Superpave PG binder specification is that tests should be as closely tied with field performance as possible. a method to simulate the aging is important in investigating and predicting early age HMA pavement behavior and distresses. Asphalt Binder aging by Loss of Volatiles Although many different factors contribute to asphalt binder aging. often termed “volatiles” increases an asphalt’s viscosity. the Superpave PG binder specification calls for short term aged asphalt binder to be tested at high temperatures to determine fatigue and rut resistance. The loss of smaller molecules from the asphalt binder. 1975[1]). the key component of concern for the RTFO is the loss of volatiles. Specifically. Field tests have shown that in-place asphalt binder does not lose a significant amount of volatiles over its life (Corbett and Merz. Loss of Volatiles Occurrence Asphalt binders typically lose volatiles during the manufacturing and placemen processes. Figure 2: HMA placement. Seeing as the constituent asphalt binder in HMA undergoes significant aging during the manufacturing and placement processes (Figure 2). Aging Simulation . The elevated temperature of these processes ages the asphalt binder by driving off a substantial amount of volatiles.

asphalt binder tests concerned with mix and placement properties (such as the DSR) are conducted on RTFO aged samples.  Asphalt binder modifiers.The RTFO aging procedure is used to simulate aging during mixing and placement. usually remain dispersed in the asphalt binder due to the rolling action of the carousel (Figure 3). Test Origins The RTFO was developed as an improvement to the Thin-Film Oven Test (TFOT) for short term asphalt binder aging.. while asphalt binder tests concerned with in-service performance (such as the DSR. Therefore. The TFOT placed asphalt binder samples in shallow pans (of the same dimensions as those used for the PAV) and then heated them in an oven for an extended period of time to accomplish simulated aging. if used. BBR and DTT) are performed on samples first aged in the RTFO and then in the PAV. some polymer modified asphalt binders and PG 70-XX and higher) because they do not flow properly in the bottles as they are rotated. RTFO Aging of Modified Asphalt Binders The RTFO has problems with highly viscous binders (e. The RTFO is an improvement over the TFOT because:  Fresh asphalt binder is continuously exposed to heat and air flow due to the rolling action of the carousel (Video 1). while the PAV aging procedure is used to simulate aging during in-service life. .g. Video 1: RTFO rotating. Notice the small air nozzle on the bottom blowing on the bottles as they rotate by.

which is then placed in a carousel inside a specially designed oven. The oven is heated to 325°F (163°C) and the carrousel is rotated at 15 RPM for 85 minutes. The bottle at left is after the RTFO test. forms on the asphalt binder because of the rolling action of the carousel. the bottle in the middle is before the test. . It is not a complete procedure and should not be used to perform the test.Figure 3: RTFO bottles. Test Description The following description is a brief summary of the test.  The test is reasonably short at 85 minutes. Figure 4 shows major RTFO equipment.  No surface skin. The carousel rotation continuously exposes new asphalt binder to the heat and air flow and slowly mixes each sample. The complete procedure can be found in:  AASHTO T 240 and ASTM D 2872: Effect of Heat and Air on a Moving Film of Asphalt (Rolling Thin-Film Oven Test) Summary Unaged asphalt binder is placed in a cylindrical jar. which inhibits aging.

Heat a sample of asphalt binder until it is fluid to pour.Figure 4: RTFO equipment. If a determination of mass change is desired. label two RTFO bottles and weigh them empty. Immediately after pouring each bottle. turn the bottles on their side without rotating or twisting and place them on a cooling rack.23 oz (35 g) of asphalt binder into each bottle (Figure 5). Basic Procedure 1. Pour 1. Approximate Test Time 3 hours from sample preparation to scraping of final bottle. 2. Record the weights. Stir sample to ensure homogeneity and remove air bubbles. 3. . These are designated as the “mass change” bottles.

There is no standard scraping utensil but at least 90 percent of the asphalt binder should be removed from the bottle. Residue from the remaining bottles should be transferred to a single container. Remove residue from each bottle by first pouring as much material as possible. Allow all bottles to cool 60 to 180 minutes. then scraping the sides of the bottle to remove any remaining residue (Video 3).Figure 5. After cooling. . 5. Remove the bottles one at a time from the carousel. Place the bottles in the RTFO oven carousel (Video 2). close the door. Record the weights. setting the mass change bottles aside. maintain the oven temperature at 325°F (163°C) and the airflow into the bottles at 244 in3/min (4000 ml/min). 1. During this time. Pouring hot asphalt binder into the RTFO bottle 4. weigh the two mass change bottles again. 6. and rotate carousel at 15 RPM for 85 minutes . RTFO residue should be tested within 72 hours of aging. Video 2: Inserting a bottle in the RTFO.

Kandhal. Typical Values Typical mass loss is in the range of 0. F. P. Corbett. The RTFO is primarily used to simulate short term asphalt binder aging for use in other tests.. Results Parameters Measured Mass change of a sample as a percent of initial mass. Brown. D.C. Mixture Design. (1996). D.L.05 to 0. 27-34. WARNING Any scraping tool may be used but an average of 90% of the residue must be removed from the sample bottles. weigh them and discard their residue. Hot Mix Asphalt Materials.E.R. Lee.5 percent. there is currently no limit on mass gain.↵ 2. (1975). Transportation Research Record 544. and Kennedy. National Research Council. 1. L. Roberts. R. Lanham. After cooling the two mass change bottles for 60 – 180 minutes. Record the weights..0% Note 1 Although some samples can gain weight due to the oxidative products formed during the test (Roberts et al. It has been found that circumferential scraping is usually more effective than lengthwise scraping.Video 3: Scraping the asphalt residue out of a RTFO bottle. Asphalt Binder Hardening in the Michigan Test Road After 18 Years of Service. Specification Table 1: Performance Graded Asphalt Binder RTFO Specification Material Value 1 Specification Property of Concern None Unaged binder Mass loss ≤ 1. and Merz.W.↵ . Transportation Research Board. T. E. MD. Footnotes (↵ returns to text) 1. Washington. and Construction. National Asphalt Pavement Association Education Foundation.Y..S..W. pp. 1996[2]).

From the surge drum the blown product is passed through heat exchangers to achieve the desired "rundown" temperatures and to provide an economical means of preheating the short residue. Asphalt Air Blowing Process Pilot Test Plant The physical properties of asphalts may further be modified by 'air blowing'. This is an oxidation process which involves the blowing of air through the asphalts. before pumping the product to storage. thereby increasing the surface area and rate of reaction. Oxygen is consumed by the bitumen as the air ascends through the material.3. Air is blown through the bitumen by means of an air distributor located at the bottom of the column. Therefore close temperature . increasing the overall molecular size of the asphaltenes already present in the feed and forming additional asphaltenes from the maltene phase. Description of the continuous blowing process After preheating. In this way the minimum level of product in the blowing column is controlled. the former to suppress foaming and dilate the oxygen content of waste gases and the latter cools the vapours to prevent after-burning. The "blown" product flows from the bottom of the blowing column into a surge drum via an external draw-off line. Steam and water are sprayed into the vapour space above the bitumen level. The air is not only the reactant but also serves to agitate and mix the bitumen. the short residue is introduced into the blowing column just below the normal liquid level. with the short residue at a temperature of 240°C to 320°C. either on a batch or a continuous basis. resulting in oxidation and polycondensation. The reaction is exothermic. The penetration and softening point of the blown bitumen are affected by: model registered © * the viscosity of the feedstock * the temperature in the blowing column * the residence time in the blowing column * the origin of the crude oil used to manufacture the feedstock * the air-to-feed ratio The blowing process dehydrogenates the short residue.

Fully blown bitumens Fully blown or oxidised bitumens are produced by vigorous air-blowing of short residue or short residue blended with a heavy distillate. occurs because the actual molecules are thermally broken apart. This damage. ie increase its penetration index. Three phenomena can be identified: * Reactions during which the size of the molecules increases. pipe coatings. 2007 | Author: Pavement Interactive The spot test is used to determine whether or not an asphalt cement has been damaged during processing due to overheating. called “cracking”. Air-rectified or semi-blown bitumens To produce penetration grade bitumens suitable for road construction. separation of side branches from the molecules with blown distillate produced as a side product. formation of cyclic hydrocarbons by means of dehydrogenation with H2O as a side product * Reactions during which the size of the molecule decreases. Used judiciously. Spot Test Publish date: August 16. which is achieved by regulating the air-to-short residue ratio in the blowing column. Thus by controlling the viscosity of the feed and the conditions in the column all the blown grades of bitumen can be manufactured. The position of the blowing curve is primarily dependent on the viscosity of the feed. ie the softer the feed the higher the curve. this mechanism results in an increase in the asphaltene content and a change in the colloid-chemical constitution and rheological properties of the bitumen * Reactions during which the size of the molecule is unchanged. they not only account for about 60% of the oxygen in blown bitumen but also link up two different molecules and thus contribute to the formation of material of higher molecular weight. etc. The chemistry of the blowing process The aim of the blowing process is theformation of asphaltenes. and are specified and designated by both softening point and penetration tests. The severity of blowing depends on the temperature in the column and to a lesser extent on the residence time. eg roofing. formation of esters is particularly important.control of this process is required. semi-blowing can be applied to reduce the temperature susceptibility of the bitumen. bitumens manufactured from some crudes require a limited amount of air blowing. eg 85/40 is an oxidized grade bitumen with a softening point of 85+-5 ºC and a penetration of 40 +. This process is termed semi-blowing or air rectification. Oxidized bitumens Oxidized bitumens are used almost entirely for industrial applications. paints. Cracked asphalt cements tend to be less ductile and more susceptible to .5. flooring mastics.

aging effects. the spot test is a form of paper chromatography (a method for analyzing complex mixtures by separating them into the chemicals from which they are made). the spot test is not often specified. the spot test is rarely used. Today. A small drop of prepared asphalt cement is dropped onto a filter paper. . If the spot formed is uniformly brown then the test is negative. Basically. Since modern refining practices rarely cause cracking. If the spot formed is brown with a black center then the test is positive.