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  • ISSN 0347-6049

    i V//särtryck 153

    Resilient modulus by indirect tensile testSafwat F. SaidPrepared for presentation and publication at the Fourth Inter-national Symposium RULEM, 24 - 26th October, 1990 inBudapest, Ungern

    Vag-och Trafik- Statens väg- och trafikinstitut (VT!) * 581 01 Linköping

    'Institutet swedish Road and Trattic Research Institute * S-581 01 Linköping Sweden

  • ISSN 0347-6049

    ___ K1/särtryck153 1990

    Resilient modulus by indirect tensile test

    Safwat F. Said

    Prepared for presentation and publication at the Fourth Inter-

    national Symposium RIÅLEM, 24 - 26th October, 1990 in

    Budapest, Ungern

    f, Väg"00h a /(' Statens vag- och trafikinstitut (VTI) * 581 01 Linkoping

    [ St]tlltet Swedish Road and Traffic Research Institute * S-581 01 Linkoping Sweden

  • Samhall Klintland Grafiska, Linköping

  • RESILIENT MODULUS BY INDIRECT TENSILE TEST"

    SAFWAT F. SAID

    Swedish Road and Traffic Research Institute

    Linköping, SWEDEN

    Abstract

    With developments in analytical design of pavement structu-

    re, there is an increasing demand for knowledge of the

    mechanical properties of various pavement elements under

    different conditions encountered in roads, such as tensile

    strength, stiffness modulus, and repeated-load fatigue re-

    sistance of the asphalt concrete mixtures. These parameters

    provide a good basis for analytical design and performance

    evaluation of flexible pavements.

    In this study, Indirect Tensile Test has been conducted

    because of its validity and simplicity. However, modifica-

    tions of the test apparatus and test procedure have been

    introduced.

    Three different types of asphalt concrete mixtures have

    been examined using indirect tensile method. Two of the

    mixes are blended with 3% rubber content by total weight.

    i.e. Rubit (RUBI2), which is a dense asphalt concrete used

    for surfacing, and a porous mix called Rubdrain (RUBD12) .

    The third mix is a conventional dense asphalt concrete

    (HAB12T) used for surfacing. The maximum size of the aggre-

    gate was 12 mm for all types.

    Stress-deformation-strain relationships have been estab-

    lished in order to examine the effect of stress and/or

    strain level on the resilient modulus found by the indirect

    tensile test and to define an approximate linear viscoelas-

    tic zone for bituminous mixtures at different temperatures.

    Resilient modulus has been measured using the modified in-

    direct tensile method for mixtures studied at four different

    temperatures.

    Keywords: Asphalt Material, Rubberized Asphalt, Indirect

    Tensile Test, Resilient Modulus, Linear Viscoelastic,

    Stress-Strain Relation, Temperature.

    *This job has been conducted by the Dept. of Highway

    Engineering, Royal Inst. of Technology in cooperation with

    the Swedish Road and Traffic Research Inst.

  • 1 Introduction

    With developments in analytical design of pavement structu-

    re, there is an increasing demand for knowledge of the

    mechanical properties of various pavement elements under

    different conditions encountered in roads, such as tensile

    strength, stiffness modulus, and repeated-load fatigue re-

    sistance of the asphalt concrete mixtures. These parameters

    provide a good basis for analytical design and performance

    evaluation of flexible pavement.

    In the last three decades a lot of research has been

    focused on the response of various layers and materials sub-

    jected to possible conditions in the field by using a wide

    variety of methods and apparatus, which have a provided

    valuable knowledge platform for further investigation.

    Indirect tensile test has been conducted in this study

    because of its validity and simplicity. However, modifica-

    tions of the test apparatus and test procedure have been

    introduced.

    Three different types of asphalt concrete mixtures have

    been examined using indirect tensile method. A conventional

    mix HABl2T, which is a dense asphalt concrete used for

    surfacing, Rubit (RUBI2)], which is a rubber granular blended

    asphalt mix with 3% rubber content, and a porous mix, called

    Rubdrain (RUBD12) also containing 3% rubber used as a drain-

    age layer, have been used. The maximum size of the aggregate

    was 12 mm for all types. Rubit and Rubdrain mixtures are

    marketed by the ABV (NCC) company. The specimens were

    supplied by the ABV laboratory.

    Stress-deformation-strain relationships have been estab-

    lished in order to examine the effect of stress and/or

    strain level on the resilient modulus found by the indirect

    tensile test and to define an approximate linear viscoelas-

    tic zone for bituminous mixtures at different temperatures.

    Resilient modulus has been measured using the modified

    indirect tensile method for mixtures studied at four

    different temperatures.

    2 Test apparatus

    Due to its simplicity and validity the Repeated-1load Indi-

    rect Tensile Test [1-8], with modification in test apparatus

    and test procedure, has been used to study the mechanical

    properties of bituminous mixtures. The principle of this

    test is that a cylindrical specimen is loaded in the verti-

    cal diametral plane, the compressive load is applied through

    a couple of curved loading strips. The resultant deformation

    is measured at horizontal diameter.

    The expressions given by Schmidt [2] andKennedy et .al.

    [1] for tensile stress at the center of specimen, resilient

    modulus, Poisson's ratio and strain across horizontal diame-

    ter are the following:

  • . + v v + + + + k k k k k k k k W k ok WoW k ok k k k k k ok k k k k d k k k k k k k k (1)Q [1

    5 11 3.4 [ÄH/AV]- 0427 4 v 4 4 v k kW kk kk kk k k k k k k k k k k k k k k k k k (2)

    (P/t. AH)[4/n+n-1] = P(n+0.27)/t.AH. . . .. . + + + ++ + ++. (3)Mr

    E. =(2P/MantD)[ (4D*n-16D?x2)/(D2+4x2)2+(1-n)]. .... . + +. (4 )

    Tensile stress (MPa)

    Applied load (N)

    specimen thickness (mm)

    specimen diameter (mm)

    Poisson's ratio

    Total resilient horizontal deformation (mm)

    Total resilient vertical deformation (mm)

    Resilient modulus (MPa)

    Tensile strain at horizontal diameter

    SU

    ctU

    Q

    AH

    NV

    Mr

    Ex

    d

    By substituting Equation (1) in Equation (3) and solving for

    resilient modulus:

    Mr = (KD/2) (0/AH)]) (n+0.27) i i i v v v v k k k k k k k k k k k k e k k k k k k a (5)

    To find the tensile strain at the center of the specimen

    (x=0), substituting Equation (3) in Equation (4) and solving

    for strain we get:

    Co = (2AH/D)[(I+3n)/(4+KM+T)] ] + + + + + + + + + + + * + & * k ok k k k k k k k a (6 )

    If n = 0.35 then

    Co = 2.1 (AH/D) ....................................... (7)

    where, AH and D are defined as before.

    The testing machine is capable of applying compressive

    pulse loads over a range of frequencies and load durations

    for repeated load testing.

    In this investigation the repeated load pulse was applied

    at a frequency of 0.33 Hz with 0.2 sec loading time and 2.8

    sec rest period. The load applied in the vertical diameter

    plane is sensed by a load cell under the specimen. Deforma-

    tion across the horizontal diameter of the specimen is

    sensed by one extensometer instead of two LVDTSs, which are

    normally used. Instron dynamic strain gauge (2620-601, with

    resolution of 20+*107-5 mm and weight 20 grams), and MTS

    extensometer (632-11l1c, resolution 8*10-7-5 mm and weight 25

    grams) have been shown to be adequate. The strain gauge is

    fixed to two curved zinc strips (2 mm thick, i0 mm wide and

    80 mm long) which are glued at opposite sides of the hori-

    zontal diameter. The total weight of extensometer and the

  • two deformation strips is less than 75 gm (See Plate 1 and

    Figure 1). However, a couple of LVDTs with the frame which

    carry out the two LVDTs is more than 700 gm which might

    influence the recorded deformation.

    Plate 1. Horizontal] extensiometer mounted on the specimen.

    _| (ts d US If 4)

    FPL

    /_/_ __J

    Fig.l. Deformation strips.

  • The deformation is measured at the same points where the

    two zinc strips are glued in order to avoid any error in re-

    cording deformations due to specimen movement or inadequate

    contact between extensometer (strain gauge) and specimen.

    Brown and Cooper [9] have mentioned the shortcomings of

    indirect tensile test, using LVDTs, in deformation measure-

    ment. The recorded deformation was found to be influenced

    by the strength of the spring used to keep the LVDT core in

    contact with the specimen, and by the vibration of the frame

    which carries the deformation transducers. In addition, it

    is easier to use just one extensometer rather than two

    LVDTS .

    The loading device is shown in Plate 2 and Figure 2. The

    upper steel loading strip is not fixed on the upper platen

    of loading device in order to bring a good contact between

    loading strips and specimen even at low stresses and high

    stiff asphalt specimens. An alignment bar is fixed to the

    upper aluminum platen to bring the loading strips into the

    same vertical plane. Figure 3 shows three different cases

    which could happen depending on the contact between loading

    strips and specimen when the loading strips are fixed on the

    platens. Case 1 shows a good contact, while cases 2 and 3

    show insufficient contact which is a result of a rough

    surface. For more details see reference 22.

    Plate 2. Loading device and specimen in place.

  • 0 :sug Z 12

    © organ %& / C J_

    © 7/77 NZ / . -/// /" , z* sär

    \ ( \| 22 _£ _/ __z Im

    O_ y k 0 | [

    Å,

    di / en

    _ _ /

    | \ // 9)

    GRK w ] & |- 1

    #NWM r®\\\ n Xskäl .

    o s I _._]

    |

    210

    All dimensions in mm

    1 Precision Pillar2 Ball Bushing3 Upper Plate4 Float Loading Strip

    Fig. 2.

    twCO

    -IOy

    Un SpecimenAlignment BarFixed Loading StripBottom PlateHardened Disk

    Loading device for indirect tensile test.

  • Case 1 0

    Case 2

    Case 3

    Fig.3. Contact between strips and specimen.

    3 Viscoelastic property of bituminous materials

    Various investigators have emphasized the effects of stress

    or strain levels on the modulus of asphalt concrete mixtures

    [2,10-21]. The increasing use of elastic theory in pavement

    evaluation and for comparing various asphalt materials in

    terms of their rheological characters makes the fundamental

    properties in stress-strain relationship an important param-

    eter [16]. With regard to the non-linear viscoelastic behav-

    ior of bituminous materials, the stress or strain level has

    an essential influence when measuring the moduli. Sayegh

    [17] does not exceed a strain value of 4.107* when measuring

    moduli. Monismith et. al. [11] consider the stiffness of

    asphalt mixtures independent of applied stress at strains

    less than 1.1073 in/in. Bonnaure et .al. [13] determine

    stiffness modulus for strains 5.107 at -159C and +92C;

    20.107 at +302C. Bonnaure et .al. also report that the phe-

    nomenon of non-linearity appears at strains close to

    100.107. Kennedy and Anagnos [1] and ASTM [3] recommend a

    load range to induce 10 to 50 percent of the tensile

  • strength as determined in the static indirect tensile test,

    or in lieu of tensile strength data, loads ranging from 4 Ib

    (25 Ib according to Kennedy) to 200 Ib per inch of specimen

    thickness can be used. Schmidt [2] uses a stress range from

    about 1 psi up to 15 psi at the specimen center at 73 PF (24

    °C). So a wide variety of limits have been recommended.

    Therefore, an approximate linear zone (the resilient

    modulus is independent of applied stress or strain level)

    should be well defined to make the modulus more reliable.

    4 Linearity

    The test series consist of testing three specimens from each

    type of asphalt mixture at temperatures of -10, +5, +25 and

    +40 degrees Celsius and at a loading frequency of 0.33 Hz.

    Totally, 36 specimens have been tested with this method.

    The test procedure is the following:

    * The test specimens were stored in a temperature cabinet

    for 24 hours at testing temperature. ( A dummy specimen

    has shown that it takes at least four hours to bring the

    specimen from room temperature to -10eC) .

    * Repeated-load pulse, at a frequency of 0.33 Hz, was ap-

    plied with 0.2 sec loading time and 2.8 sec rest period

    * The load level was increased gradually up to a level

    which resulted in a recordable deformation by

    extensometer.

    * -A minimum of 50 load repetitions were applied before the

    first reading.

    * The load level was increased gradually to a higher level

    with about 25 load repetitions at each load level. The

    maximum load level used was about 4000 N.

    * Stresses and strains were calculated at each load level,

    a curve was fitted by regression analysis for all three

    specimens, which represent the material response at de-

    fined temperature. The zero point has normally been ad-

    justed due to surface irregularities.

    The isochronous stress-horizontal deformation-strain

    diagrams were produced for bituminous mixtures to study the

    stress and strain effect on resilient modulus using repeated

    load indirect tensile test. Figure 4 shows isochronous dia-

    gram for HABl27T mix. Similar curves have been found for the

    other two mixtures (See Figure 5 and 6). The stress was

    calculated at the center of the specimen by Equation 1.

    These diagrams are represented by stress-deformation-strain

  • 0.40aoe | //l

    | +5 °C0.35 s

    l/ /// "(u gset 0.30

    TENS

    ILE

    STRE

    SS(M

    Pa)

    "7 a

    | \ 0.20

    sl |/ _-

    |/ s

    I

    //+40°C

    0.10

    |

    pameM

    . //// ///////,/

    /

    /

    o L-- . -o ul

    0 50, 100. 150, 200. 250, 300 x10

    OEFORMATION (mm)

    (0 " 200 / 5,00 " 600 x 10%

    STRAIN

    Fig.4. Stress-deformation-strain relationships for HABl27T.

    curves and not only by the more familiar stress-strain

    curves, hence the deformation distribution on the horizontal

    diameter is not uniform [2,4,5,23]. This is done in order

    to eliminate the effect of using an assumed value for the

    Poissons ratio for strain calculation at the center of the

    specimen, which might affect the strain value. However, for

    the sake of comparison, the tensile strain at the center of

    the specimen is calculated by Equation 7.

    The correlation coefficients (R) are higher than 0.94,

    except for the porous graded mix tested at 25 degrees

    Celsius, which is 0.83. In all the cases, the stress-

    deformation relationships show curves which are concave

    downwards. This means that strain increases faster than

    stress and results in a reduction in resilient modulus. The

    nonlinearity relationships are obvious even at low stress

    and deformation levels. The non-linear viscoelastic rela-

    tionships confirm the importance of stress and deformation

    levels when measuring the resilient moduli of asphalt

    mixtures .

    The above discussion shows the dominance of viscous prop-

    erties at high strain and stress levels. Therefore, and in

    order to measure the resilient moduli of bituminous materi-

    als with consistent in results, a viscoelastic linear zone

    should be defined in which the effect of stress or strain

    levels on the resilient modulus is negligible. If resilient

    modulus is measured at higher stresses or strains, it could

    be justified in some cases in order to simulate field

  • - 0.40

    &

    0 0.35

    E 3 n 10°C //+S°C / -

    § 0.30 o

    % / *ZSOC

    - 025 /////,////

    0.15 A/ ///

    I| | aoe_|_0.10 7 Tee|__---*x

    0.05 // / ////; * A ___/_l",//

    0- -4

    0 50 100 150. 200. 250, 300. 350 400. x 10

    JEFORMATION (mm)

    -- } + i } -6

    0 200 400 600 800 x10

    STRAIN

    Fig.5. Stress-deformation-strain relationships for RUB1l2.

    0.40

    0.35

    0.30

    TENSILE

    STRESS

    (MPa)

    0.25

    0 20

    0 15

    0 10

    0 05

    Fig.6. Stress-deformation-strain relationships

    10

    |

    1~10°C

    /

    ¥ +5 °C// /////

    // / e/

    _- 25°C

    / _l

    /| / cV/

    // 7/

    ________._ 4|U

    / // ---|_| see/ / nonafuse

    //L-/"/ Louk

    0 50 100 150. 200, 250 300 350 500 x 10

    DE FOR2MATION (mm)

    0 200 400 600 800 = 10

    STR AIN

    for RUBD12 .

  • p Linear zone is at

    o=A/B *100 © 10%

    Fig.7. Isochronous stress-deformation curve.

    conditions, in this case the stress or strain level should

    be reported.

    The viscoelastic linear zone is defined, in this study,

    as the zone where stress in the stress-deformation curve

    divergqges with less than 10 percent from the rectilinear

    stress-deformation relation shown in Fiqure 7. The recti-

    linear stress-deformation relation is represented by the

    slope of the curve at the origin.

    The 10 percent divergence of stress cause a 10 percent

    reduction in resilient modulus from the initial modulus

    value (modulus at origin). This variation is believed to be

    acceptable because of the hetrogeneity and unisotropy of

    asphalt concrete mixtures.

    Figure 4 through 6 also show the limits of deformations

    and stresses at 10 percent reduction of resilient modulus.

    The stress limits decrease with increased temperatures but

    for deformations it is the opposite, i.e., the deformation

    limits increase with increased temperatures. A similar con-

    clusion is reported by other investigators [24,25 ,26] when

    exposing asphalt mixture specimen to different deformation

    rates, using the tensile strength method, higher elongation

    is reported at lower deformation (high temperatures

    correspond to low deformation rates) and vice versa. At low

    temperatures the bituminous mixtures are stiff and brittle.

    They tolerate low strains with high stresses. At high

    temperatures these mixtures have low stiffness and high

    flexibility. They tolerate high strains but with very low

    stresses.

    Figure 8 shows a relation between temperatures and the

    logarithm of deformation limits, as defined before for

    1 1

  • - 1000

    600 - I 300

    Log(D) = exp(0.0138T+0.313) &g | e00

    2007 -400

    mm

    -6TE

    NSIL

    EST

    RAIN

    x10

    - - 20080 -

    D]x

    10

    60 7

    - 1000 7

    - 80

    DEFO

    RMAT

    ION

    (

    60

    ad - 40

    - 30 - 10 0 10 20 e

    TEMPERATUR (T) 2C

    Fig.8. Relationship betweenn the logarithm of deformation

    and temperature.

    tested mixtures (with 0.2 sec loading time, and a frequency

    of 20 cycle/min.).The correlation coefficient (R) for all

    materials together is 0.986, using regression Equation 8.

    Log(D) = exp(0.0138T+0.,313) . | / . v v v v v & v k k v k k k k k k k k k k a k a (8 )

    where

    D= Horizontal deformation in mm x 107-74

    T= Temperature in Celsius.

    5 Resilient modulus

    In accordance with the discussion in the above section

    regarding stress-strain relationships and the effect of

    irregularites of specimen surface the following procedure

    has been used for resilient modulus measurement. Indirect

    tensile test has been used on cylindrical bituminous sample.

    * The test specimens were stored in a temperature cabinet

    to the proper temperature.

    * Repeated-load pulses at a frequency of 0.33 Hz were

    applied with 0.2 sec loading time.

    12

  • Ä minimum of 50 load repetitions were applied before the

    first reading and until the resilient deformation became

    constant .

    The resilient horizontal deformation were measured at

    the maximum allowable load level and at 50 and 75% of

    this value. The test began at the lowest load level and

    increased gradually to higher load levels with about 25

    load repetitions at each load level.

    After the test had been completed, the tensile stress

    was calculated at each load level according to Equation

    (1) .

    Stress-resilient horizontal deformation curve was

    plotted. Curve fitting by linear regression analysis

    was used. In such cases, the zero point was adjusted as

    shown in Figure 9 to compensate for surface irregulari-

    ties and insufficient contact between loading strips and

    specimen .

    The resilient modulus was calculated with constant

    Poisson'!s ratio according to Table 1 at different

    temperatures by Equation 5:

    /

    LN

    Fig.9. Correction of the stress-strain curve.

    1 3

  • Table 1. Constant Poisson's ratio

    TeC n

    - 1 0 0 . 20

    d- 55 0 . 25

    +2 0 0 . 35

    +4 ( 0 . 4 0

    10000 +

    8000 -

    6000 -

    $ 4000 -£

    92)

    -3DCM

    2- 2000 +

    C

    gä[I x

    1900 ---HAB12T n

    1000 - - - RUBA2 ä

    - - -RUBD 12 *xgjxx

    500 he~10 0.0 +10 +20 +30 +40

    TEMPERATURE °C

    Fig.l10. Effect of temperature on resilient modulus.

    14

  • Figure 10 shows the resilient modulus at different

    temperatures. The relationship between temperature and the

    log of resilient modulus is not linear. The rubberized mix

    (RUB1I2) shows lower moduli than conventional mix (HABl27T), a

    fact which indicates the higher flexibility of the rubber-

    ized mix. The porous mix (RUBD12) has shown, as expected,

    the lowest moduli. Furthermore, there were no problems in

    measuring resilient modulus for the porous mix.

    Conclusions

    An approximate linear viscoelastic zone for practical use

    has been defined for asphalt mixtures at different

    temperatures (with 0.2 loading time and 20 cycles/min.).

    The upper loading strip should be free in order to create

    satisfactory contact between loading strips and specimen

    even at low stresses and stiff asphalt specimens.

    One extensometer may be used instead of two LVDTs with

    carryirig frame. In that case the recorded deformation

    will not be influenced by the following: (1) the strength

    of the spring that keeps the LVDT cores in contact with

    the specimen, (2) the vibration of the frame which car-

    ries the deformation transducers, and (3) the extensive

    load on the specimen.

    References

    Kennedy T.W and Anagnos J.N, "Procedures for the Static

    and Repeated-Load Indirect Tensile Tests, "Research Re-

    port 183-14, Center for Transportation Research, The Uni-

    versity of Texas at Austin, 1983.

    Schmidt R.J, "A Practical Method for Measuring the Resil-

    ient Modulus of Asphalt-Treated Mixes", Highway Research

    Record, 404, 1972 .

    ; American Society for Testing and Materials,ASTM D 4123-82, Method of Indirect Tension Test for Re-silient Modulus of Bituminous Mixtures, 1984.

    Wallace K. and Monismith C.L, "Diametral Modulus Testingon Nonlinear Pavement Materials", Proceedings, The Asso-ciation of Asphalt Paving Technologists, Vol. 49, 1980,p. 633.

    . Kennedy T.W, "Characterization of Asphalt Pavements Mate-

    15

  • 1 0

    1 1

    1 2

    1 3

    1 4

    15

    16

    rials Using the Indirect Tensile Test" Proceedings of the

    Association of Asphalt Paving Technologists, Vol. 46.

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    Baladi G.Y., Harichandrun R. and De Foe J.H., "The Indi-

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    . Pell P.58 and Taylor I.F, "Asphaltic Road Materials in

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    . Kallas B.F. and Riley C., "Mechanical Properties of As-

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    . Kallas B.F and Puzinauskas V.P, "Flexure Fatigue Tests on

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    16

  • 17 .

    18 .

    19

    20

    21

    22 .

    23

    24

    25 .

    26

    Sayegh G., "Viscoelastic Properties of Bituminous

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    .Lee M.A. and Emery J.J., "Improved Methods for Character-

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    .Vinson T. "Fundamentals of Resilient Modulus Testing"

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    . Linde S. "Investigations on the Cracking Behavious of

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    Polymerteknik, Borås 1988.

    17

  • L" ANALYSE D'EXTENSION INDIRECTE DES MODULES RESILIENTS

    SAFWAT FP. SAID

    L' Institut National Suédois de Recherches Routiéres et de la

    Circulation

    Linképing, Suéde

    Résumé

    Les progrés faits dans le domaine du design analitique des

    structures de pavé ont rendu necessaire un croissant besoin

    de connaissances sur les propriétés mécanique des différents

    composants du pavé dans les conditions des routes; telles que

    la résistance a l'extension; la rigidité des modules et la

    résistance a plusieures réprises des mélanges de pavé en bé-

    ton. Ces paramétres constituent une base convenable pour le

    design analytique et l'évaluation des performances du pavé

    flexible.

    Dans ce rapport-ci on a choisi l'analyse d'extension indi-

    recte a cause de sa validité et simplicité. En tout cas; on a

    éffectué des modifications de l' appareillage et des

    procedures d'analyse.

    On a examiné trois types différents de mélanges de pavé en

    béton par utilisant la méthode d'extension indirecte. Deux

    d'entre les mélanges sont mélés a 3% de contenu de caoutchouc

    par le poids total, c'est a dire le Rubit (RUB12), qui est un

    asphalt dense en béton, utilisé pour la réféction des routes,

    et un mélange poreux appéllé Rubdrain (RUBD12) . Le troisiéme

    mélange est un asphalt dense conventionnel en béton (HABI2T),

    utilisé pour la réféction des routes. La dimension maximum de

    l' aggrégat a été 12 mm pour tous les types.

    La relation entre la tension et la déformation (stress-de-

    formation-strain) a été établie pour examiner l' influence du

    niveau de la tension et/ou la déformation sur le module rési-

    lient trouvé par l'analyse d'extension indirecte et pour dé-

    finir une zone viscoélastique approximativement linéaire pour

    les mélanges de bitume a temperatures différentes. Les modu-

    les résilients ont été mésurés par utilisant la méthode d'ex-

    tension indirecte, modifiée pour les mélanges analysés a 4

    temperatures différentes.