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IS 15799 (2008): Methods for testing tar and bituminousmaterials - Determination of durability of bitumen [PCD 6:Bitumen Tar and their Products]

IS 15799 : 2008

C1R 3ih f~{1i* ffl.1i~1 cn1 -qU~ M~ ­~ Cf)f fcChId1Q'""! ~~

Indian Standard

METHODS FOR TESTING TAR AND BITUMINOUSMATERIALS - DETERMINATION OF

DURABILITY OF BITUMEN

ICS 75.100

© BIS 2008

BUREAU OF INDIAN STANDARDSMANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG

NEW DELHI 110002

July 2008 Price Group 4

Bitumen, Tar and Their Products Sectional Committee. PCD 6

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft final ized by the Bitumen, Tarand Their Products Sectional Committee had been approved by the Petroleum, Coal and Related Products Division

Council.

Durability can be defined as the ability of bitumen to maintain satisfactory rheology. cohesion and adhesion inlong term service. As a part of quality criteria, the following have been identified as the prime durability factors:

Oxidative hardening

- Evaporative hardening

- Compositional hardening

The Rolling Thin Film Oven (RTFO) test described in IS 9382 : 1979 'Methods for testing tar and bituminousmaterials - Determination of effect of heat and air by thin film oven tests ' measures hardening Doth by oxidationand evaporation. By adjusting the duration of test, the short term hardening (plant mixing) and long term hardening(hardening during service) can be obtained accurately. .

Large scale field trials have revealed that a paving grade bitumen is deemed to have outlived its useful life whenthe penetration value goes below 20 or the softening point is raised above 70°C. Since the penetration and thesoftening point tests do not define explicitly the rheological nature of bitumen, the viscosity value has beenchosen as a truly durability parameter. Using RTFO test and PAV test, the time of exposure needed to harden thebitumen to reach the Specified Apparent Viscosity Level (SAVL) of 5.65 log Pa-s at 45 °C at the rate of a shearrate of5 x 10.3 S·I as durability of bitumen. The durability of bitumen is expressed as number of days of exposurerequired to reach the SAVL level.

In reporting the results of a test or analysi s made in accordance with this standard, if the final value, observed orcalculated, is to be rounded off, it shall be done in accordance with IS 2 : 1960 ' Rules for rounding off numericalvalues (revised)'.

IS 15799 : 2008

Indian Standard

METHODS FOR TESTING TAR AND BITUMINOUSMATERIALS - DETERMINATION OF

DURABILITY OF BITUMEN

1 SCOPE

2 REFERENCES

3 TERMINOLOGY

3.1 For the purpose of this standard, the followingdefinition and those given in IS 334 shall apply.

3.2 Durability - It is the combined effect in propertiesof bitumen caused due to conventional hot-mixing atabout 160°C and in-service oxidative ageing that occursin bitumen binders during pavement service .

4 APPARATUS

4.1 Rolling Thin Film Oven

4.1.1 A double walled, electrically heated convention­type oven, interior dimensions shall be 381 nun high,483 mm wide, and 445 ± 13 mm deep (with the doorclosed). The oven is provided with a tightly fittedhinged door containing two sheets of heat resistantglass (window) of size 305 to 330 mm wide x 203 to229 mm high and separated by an air space. Thewindow should permit an unobstructed view of theinterior of the oven. The top of the upper heatingelement shall be 25 ± 3 mm below the oven floor. Theoven shall have vents at the bottom with an open areaof 15.0 ± 0.7 cm2 and shall be located symmetricallyto supply incoming air around the heating elements.The oven shall have vents at the top with an open areaof 9.3 ± 0.45 cm2•

4.1.2 The oven shall have an air plenum covering theside walls and ceiling . The air space shall be 38.1 mmdeep from walls and ceiling. At a midpoint in the widthof the oven and 152.4 nun from the face of the circularmetal carriage to its axis, a squirrel cage-type fan 133mm outer diameter (00) and 73 nun wide shall beturned at I 725 rpm by an externally mounted motor.The squirrel cage fan shall be set so that the fan turnsin an opposite direction to its vanes. The air flowcharacteristics of the fan-plenum system shall besuction from the floor of the oven through the wallplenums and exhaust of the air through the fan. FiguresI and 2 show details of this plenum system.

4.1.3 The oven shall be equipped with a proportionalcontrol thermostat capable ofmaintaining 163 ± O.5°Ctemperature. The sensing element of the thermostatshall be placed 25.4 mm from the left side andapproximately 38.1 nun from the ceiling of the interiorof the plenum-enclosed oven so that the end of thesensing element is at a point approximately 203.2 mmfrom the rear interior wall of the oven. The thermometershall be hung or affixed to a mounting in the ceiling,which is 50.8 nun from the right side of the oven at a

TitleGlossary of terms relating to bitumenand tar (third revision)Methods for testing tar andbituminous materials - Determina­tion of effect of heat and air by thinfilm oven tests

NOTE - Some modified bitumen binders may phase separateor form skins during RTFO conditioning or PAY ageing andthe results from subsequent testing of this residue may not berepresentative of modified bitumens short term aged under fieldconditions.

1.1 This standard covers a method to measure thedurability of bitumen. Durability of the bitumen isreflected by the thermo oxidative effect during hot mixand in-service oxidative ageing. The test methodmeasures the combined effect of Rolling Thin Film Oven(RTFO) (heat and air on a moving film ofbitumen) andPressurized Ageing Vessel (PAV) (accelerated ageing ofbitumen by means of pressurized air and elevatedtemperature) of semi-solid bituminous materials.

1.2 It is intended to simulate the type of changes. whichoccur in bituminous binders during hot mix and in­service oxidative ageing but may not accuratelysimulate the relative rates of ageing.

1.3 The ageing of bitumen binders during service isaffected by ambient temperature, air pressure and bymixtures associated variables, such as volumetricproportions of the mix, permeability of the mix,properties of aggregates and possibly other factors .

The following standards contain provisions which ,through reference in this text, constitute provisions ofthis standard. At the time of publication the editionsindicated were valid. All standards are subject torevision and parties to agreements based on thisstandard are encouraged to investigate the possibilityof applying the most recent editions of the standardsindicated below:

IS No.334: 2002

9382 :1979

IS 15799 : 2008

....- , /" DIRECTION

ffi~'\ OF THEROTATION

e> -~--..

~ ~TOP vIew OF FAN

I IIIII II I

VENT

OVEN

THERMOMETER

FIG. I SCHEMATIC DIAGRAM OF AIR FLOW FRONT VIEW

midpoint in the depth of the oven . The heating controlsshall becapable of bringing the fully loaded oven backto the test temperature within a 10 min period afterinsertion of the samples in a preheated oven.

4.1.4 The oven shall be provided within a 304 .8 mmdiameter vertical circular carriage which ismechanically driven through a 19 mm diameter shaftat a speed of 15 ± 0.2 rev/min. This carriage shall beprovided with the suitable openings and clip s for firmlyholding eight glass containers in a horizontal position.

4.1.5 The oven shall beequipped with an air jet havingoutlet orifice 1.016 mm diameter (No. 68 drill )positioned to blow heated air into each bottle at itslowest point of travel and connected to a 7.6 m lengthof 8 mm outs ide diameter refrigeration copper tubing.The tubing shall be coiled to lie flat on the bottom ofthe oven and lead to a source of fresh, dried. dust-freeregulated air.

NOTE - Activated silica gel treated with an indicator is asatisfactory desiccant for the dried air.

2

4.2 Flow Meter

The flow meter may be any suitable type capable ofaccurately measuring the air flow at a rate of4000 mlImin and shall be located downstream of all regulatingdevices and upstream of the copper coil. It shall becal ibrated periodically us ing wet test meter or otherdisplacement method based on air flow exiting the airjet with the oven off at room temperature.

4.3 Thermometer

Thermometer conforming to the requirements asspec ified in IS 9382 shall be used.

4.4 Container

The container in which the sample is to be tested shallbe of heat-resistant glass conforming to the dimensionsshown in Fig. 3.

4.5 Cooling Rack

A wire or sheet metal rack constructed ofstainless steel

3 Nos. 0305 X 3.17 THICKALUMINIUM DISC

FRONT VIEW

IS 15799 : 2008

292

228

OVEN

111.5

4 Nos. SPACER0 .0.12.7 xl .D.6.35 x54.6LG.

4 Nos. SPACER0 .0 .12.7 xI.D.6.35 x20.6 LG.

SIDE VIEW

All dimensions in millimetres.

F IG. 2 CIRCULAR M ETAL C ARRI AGE

064:t 12

140

031 .75:t 1.5

I b1.5 ± 0.8 .....

:t 1.5 I MATERIAL

PYREX BRAND TUBINGSTANDARD WALL64 00 WALL THICKNESS2.4 :t 0.3

All dimensions in millimetres,

F IG. 3 S AMPL E B OTTLE

3

IS 15799 : 2008

or aluminium, which allows the sample containers tocool in a horizontal position and allows air to flowfreely around each container with at least 25 mmclearance between containers.

4.6 Pressure Ageing Vessel (see Fig. 4)

4.6.1 Pressure Vessel

A stainless steel pressure vessel designed to operateat 2.1 ± 0.1 MPa between 90° to110°C with interiordimensions adequate to hold a pan holder capable ofholding ten TFaf stainless steel pans in horizontal(level) position (see Fig. 5) such that the bitumen binderfilm thickness is reasonably uniform . The holder shallbe designed for easy insertion and removal from thevessel.

NOTE - 11Ievessel may be a separate unit to be placed in aforced draft oven for conditioning the bitumen binders or anintegral part of the temperature control system (for example,by direct heating of the vessel or by surrounding the vesselwith a permanently affixed heating unit forced air oven or liquidbath) . For practical purposes, it is recommended that the vesselhave the dimensions of 250 mm in diameter and 265 mm inheight.

4.6.2 Pressure and Temperature Controlling Devices

4.6.2.1 A pressure relief valve that prevents pressurein the vessel from exceeding the design pressure ofthe vessel. but in no case exceeding 2.5 MPa duringageing.

4.6.2.2 A pressure regulator or regulating systemcapable of controlling the pressure within the vesselto ± 0.02 MPa, and with a capacity adequate to reducethe pressure from the source of compressed air sothat the pressure within the loaded pressure vessel ismaintained at 2.1 ± 0 .1 MPa during the ageingprocess.

4.6.2.3 A slow release bleed valve that allows thepressure in the vessel at the completion of theconditioning procedure to be reduced from 2.1 MPato local atmospheric pressure within 8 to 15 min.

4.6.3 Temperature Controlling Devices

4.6.3.1 A digital temperature control device formaintaining the temperature during ageing within thepressure vessel at the ageing temperature of ± 0.5"c.

NEEDLEVALVE

QUICKDISCONNECT

BLEED VALVE

PRESSURERELIEF VALVE

PRESSUREVESSEL

PRESSURE GAUGEOR SENSOR

RTD

r-­IIIII

COMPRESSED AIR I P.A.V.CYLINDER I

TEMPERATURE )LCON~ 1 ---

FIG. 4 SCHEMATIC DIAGRAM OF PAY TEST SYSTEM

4

IS 15799 : 2008

b,;:~10

FROM INSIDE

TO TEMPERATURETRANSDUCER AND

TEMPERATURE READOUT SURFACE OFTHE P.A.v.

WALL CLEARANCE ~ 10 -/ i

~ ~10

FROM TOP OFASPHALT BINDER

///// V vt/ /// / V//V / /////~

PROVIDE AT LEAST 5 r'CLEARANCE TO I

NEAREST SURFACEI ---- --- ASSEMBLY TO INCLUDEI PANS AND SUPPORT

I~

I - t--10 Nos.TFOT PANSI SUPPORTED ON SHELF

IOR STANDARDS.ENTIREASSEMBLY SHALL BE

ASSEMBLY I I REMOVABLE AS ANSUPPORT POINT~ I INTEGRAL UNIT

aI

~

"-~

NOTES

1 Distance ' 0 ' controls the level of the pan. The assembly shall be supported at three or more support points. The dislance ' 0 ' measurefrom each assembl y support point to the bottom of the pan (top of shelf or pan support point ) shall be controlled 10 % 0.05 mm.

2 Distance b, and b, shall be such that any active port ion of the temperature transducer is ;::: 10 mm from any adjacent surface.

3 Distance 'c ' shall be z 12 mm.

All dimensions in millimetres.

FIG. 5 SCHEMATIC DIAGRAM SHOWING LOCATION OF PANS AND RTD WITHIN PAY

4.6.3.2 A heating device (forced-draft oven or fluidbath) capable of restoring the ageing temperaturewithin the vessel after loading the pans and the panholder and prior to pressurizing the vessel with in 2 hof placing the loading vessel in the heating device andmaintaining the temperature within the pressure vesselat the ageing temperature ± 0.5°C.

4.6.3.3 A pressure vessel with integral temperaturecontrolsystem that is capable of bringing the loaded pressurevessel to the desired conditioning temperature ± 0.5°ewithin 2 h as recorded by the RTD inside the loadedpressure vessel and maintaining the temperature withinthe pressure vessel at the ageing temperature ± 0.5°c.

NOTE - Preheating the pressure vessel may be necessary to

achieve the age ing temperature within (he requi red 2 h period.

4.6.4.2 A strip chart recorder or other data acquisitionsystem capable of recording temperature throughoutthe ageing process to ± 0.1"C, As an alternative. anelectronic device capable of reporting only maximumand minimum temperatures (accurate to ± 0.1"C) maybe used.

4.6.5 Pressure Gauge

A pressure gauge capable of measuring the pressurein the pressure vessel to within ± 0.02 MPa during theageing process.

4.7 Stainless Steel Pans

Ten standard stainless steel TFO pans meeting therequirements of IS 9382.

4.6.4 Temperature and Pressure Measurin g Devices

4.6.4.1 A platinum RTD accurate to the nearest 0.1-cfor measuring the temperature inside the pressurevessel. The RTD shall becalibrated as an integral unitwith its respective meter or electronic circuitry.

4.8 Vacuum Oven

A vacuum oven capable of maintaining temperatureup to 180°C with an accuracy of ± 5°C and vacuum of15± 1.0 kPa absolute shall be used . The pressure vesselitself may be used in lieu of a vacuum oven if it is

5

IS 15799 : 2008

capable of maintaining a temperature of 180°C and avacuum of 15.0 kPa.

4.9 Vacuum System

A vacuum system capable: o f generat in g andmaintaining pressure below 15.0 kPa absolute, Suitablevacuum systems include a vacuum pump. an airaspirator. or a house vacuum system.

5 CHEMICAL REQUIREMENT

Commercial bottled air or equivalent.

6 CALIBRATION AND STANDARDIZATION

6.1 Temperature Detector

Verify the calibration of RTD and its respecti ve meteror electronic circuitry to 0.1"C at least every six monthsusing a calibrated temperature indicator traceable to anational standard.

6.2 Pressure Gauge

Calibrate the pressure gauge to an accuracy of 0.02MPa at least every silt months.

6.3 For those vessels or PAV sy stems wherepressurization is operator-controlled. determine theoptimum temperature at which to apply pressure to thepressure vessel. Several ageing run s should beconducted. With the vessel loaded with pan rack andempty pans. increa se the: temperature inside the vesselto the ageing temperature, When the temperature insidethe vessel is within 10°C of the ageing temperature.apply an air pressure of 2.1 ± 0.1 MPa. Record thetemperature increase when pressure is applied. Performthe procedure at least three times and use the averagetemperature increase to establish the temperature atwhich to apply pressure to the vessel for performingthe ageing procedure.

7 PROCEDURE

7.1 Part A

7.1.1 Heat the sample in its container in an oven not toexceed 15O"C. Weigh 35 ± 0.5 g of sample into eachof the required glass containers providing sufficientmaterials for carrying out the ageing in the pressureageing vessel.

7.1.2 With the oven at operating temperature and theair flow set at 4 000 ± 200 ml/min, arrange thecontainers holding the bitumen in the carriage so thatthe carriage is balanced. Fill unu sed spaces in thecarriage withempty containers. Close the door and rotatethe carriage assembly at a rate of 15 ± 0.2 rev/min.Maintain the sample in oven with the air flowing and

6

the carriage rotating for 85 min. The test temperatureof 163 ± O.soC shall be reached within first 10 min.otherwise discontinue the test.

7.1.3 At the conclusion of the testing period. removeeach glass sample container. one at a time and transferthe contents into a bigger container and gently stir it tohomogenize it for further age ing in PAY.

7.2 Part B

7.2.1 Place the pan holder inside the pressure vessel.If an oven is used, place the pressure vessel inside theoven. select an ageing temperature and preheat thepressure vessel to the ageing temperature. If anintegrated temperature control pressure vessel is used.one should select an ageing temperature and followthe manufacturer's instruction for preheating thepressure vessel.

NOTE - For vessels placed in an oven , preheat ing the vesselto 10° to 15°C above the ageing temperature ca n be used [0

reduce the drop in PAYtemperature dur ing (he load ing processand minimize the time required to stabilize the system. afterloading to attain the required temperature.

7.2.2 Weigh 50 ± 0.5 g of above residue (obtainedfrom Part A) into a TFOT pan which will yieldapproximately 3.2 mm thick film of residue.

7.2.3 Place the filled pans in the pan holder and placethe pan holder inside the pressure vessel and close it.If an oven is used, place the pressure vessel inside theoven. Wait until the temperature inside the vessel iswithin 10°C of the ageing temperature (100°C). Then,apply an air pressure of 2.10 ± 0.1 MPa and then starttiming the test. If the temperature inside the vessel hasnot reached the desired temperature for applyingpressure within 2 h of loading the pan holder and pans.discontinue the procedure and discard the residuesamples.

7.2.4 Maintain the temperature and air pressure insidethe vessel for 20 h ± 10 min . If the temperature risesabove and falls below the target ageing temperature± OS C for more than a total of 60 min during the 20h ageing period, discard the material. Also. if thepressure at the end of ageing period is outside of therange. discard the material.

7.2.5 At the end of 20 h ageing period. begin the slowreduction of the internal pressure of the PAY, using theair pressure bleed valve. The bleed valve is adjusted toan opening such that it equalizes the internal andexternal pressures on the PAY within 8-15 min, thusavoiding excessive bubbling and foaming of residue.

7.2.6 Vacuum De-gas the Aged Samples

7.2.6.1 Remove the pan holder and pans from the PAYand place the pan in an oven set to 163"C for 15 ± I min.

NOTE - PAY residue may be healed in the TFOT pans al163°C and sti rred to rem ove air bubbles. The se precautionswill help avoid oxida tive harden ing and volatile loss thai willharden the sa mple . During the heat ing proce ss. the sampleshould be covered and st irred occasionally scraping the bouo mof the pan s 10 ensure homogeneity.

7.2.6.2 Pre-heat the vacuum oven to 170 ± 5°C.

7.2.6.3 Remove the pans from the oven and pour thehot residue from the pan s cont aining a single sampleinto a single container. Select a container of dimensionsuch that the depth of the res idue in the container isbetween 15 mm and 40 mm . After the last pan isscraped. tran sfer the container to the vacuum ovenwithin 1min . Maintain the temperature of vacuum ovenat 170 ± 5°C for 10 ± 1 min .

7.2.6.4 Open the vacuum valve as rapidly as possible toreduce the pressure to 15 ± 2.5 kPa absolute . Maintainabsolute pres sure at 15 ± 2.5 kPa for 30 ± I min. Releasethe vacuum and remove the container. If any bubblesremain on the surface of the residue . remo ve them byflashing the surface of the residue with a torch or hotknife .

7

IS 15799 : 2008

7.2.6.5 If test s to determine the propert ie s ofdegas sed PAY re sidue are not performedimmediately. it is permissible to cover and store thesamples in their cont ainers at room temperature forfuture testing.

8 REPORT

The following information shall he reponed:

a) Sample identification;

b) Ageing test temperature. neare st to 0.5°(';

c) Max imum or the min imum age ingtemperature , recorded neare st to 0.1°C;

d ) Total time during ageing that temperature wasoutside the specified range . nearest minute ;and

e) Total ageing time. hours and minutes.

9 PRECISION

Sin ce this is a practice and material is not testedprecision and bias statements are not needed.

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Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Stand ards are also reviewedperiodically ; a standard along with amendm ents is reaffirmed when such review indicates that no changes areneeded; if the review indicates that changes are needed , it is taken up for revision . Users of Indian Standardsshould ascerta in that they are in possession of the latest amendments or edition by referring to the latest issue of'BIS Catalogue ' and 'Standards: Monthl y Additions' .

This Indian Standard has been developed from Doc : No. PCD 6 (1336 ).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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