Designation: D4402/D4402M − 15
Standard Test Method for
Viscosity Determination of Asphalt at Elevated Temperatures Using a Rotational Viscometer1 This standard is issued under the fixed designation D4402/D4402M; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon ( ´) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the U.S. Department of Defense.
3.1.1 apparent viscosity, n— the the ratio of shear stress to shear rate for a Newtonian or non-Newtonian liquid.
1. Sco Scope pe 1.1 This test method outlines outlines a procedure procedure for measuring measuring the apparent viscosity of asphalt from 38 to 260°C [100 to 500°F] using usi ng a rot rotatio ational nal vis viscom cometer eter and a temp tempera eratur ture-c e-cont ontrol rolled led thermal chamber for maintaining the test temperature.
3.1.2 filled asphalt, n— an an asphalt blend that contains finely dispersed insoluble mineral matter. 3.1.3 Newtonian Newtonian liquid liquid,, n— a liquid for which the rate of shear is proportional to the shearing stress. The constant ratio of the shearing stress to the rate of shear is the viscosity of the liquid liq uid.. The vis viscos cosity ity of a New Newton tonian ian liq liquid uid is the theref refore ore not dependent on its shear rate. If the ratio is not constant, the liquid is non-Newtonian. Many liquids exhibit both Newtonian
1.2 The values stated in either SI units or inch-pound inch-pound units are to be regarded separately as standard. The values stated in each system may not be exa exact ct equ equiva ivalen lents; ts; the theref refore ore,, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.
and non-Newtonian behavior, depending on the shear rate or temperature, or both.
1.3 This standar standard d doe doess not purport purport to add addre ress ss all of the safet sa fetyy co conc ncer erns ns,, if an anyy, as asso socia ciate ted d wi with th its us use. e. It is th thee responsibility of the user of this standard to establish appro priate safety and health practices and determine the applicability bili ty of re regul gulato atory ry limi limitati tations ons pri prior or to use use.. See 10.6 for specific precautionary information.
3.1.4 shear rate, n— the the measure of the speed at which the intermediate layers of the liquid move with respect to each other. Its unit of measure is the reciprocal second (sec -1). 3.1.5 shear shear str stress, ess, n— the the force per uni unitt are areaa req requir uired ed to produce the shearing action. Its SI unit of measurement is the pascal, and its cgs unit of measurement is dynes/cm 2.
2. Referenc Referenced ed Documents Documents 2.1 ASTM Standards: E644 Test E644 Test Methods for Testing Industrial Resistance Thermometers E1137 Specification E1137 Specification for Industrial Platinum Resistance Thermometers
3.1.6 viscosity, n— the the ratio between the applied shear stress and the rate of shear is called the coefficient of viscosity. This coefficient is a measure of the resistance to flow of the liquid. Thee SI un Th unit it of vi visc scos osity ity is th thee pa pasc scal al se seco cond nd (P (Pa·s a·s). ). Th Thee centime cen timetre tre gram sec second ond (cgs) unit of vis viscos cosity ity is the poise (dyne·s/cm2) and is equivalent to 0.1 Pa·s. Frequently, centi-
E2975 Test Method for Calibration of Concentric Cylinder E2975 Test Rotational Viscometers
poise (cP)—equal to one millipascal second (mPa·s)—is used as the viscosity unit.
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3.2 Definitions of Terms Specific to This Standard: 3.2.1 apparatust he pa part rt of th thee apparatus-measu measuring ring geome geometry try,, n— the equipment that is immersed in the asphalt sample, the dimensions sio ns of whi which ch are used, in con conjun junctio ction n wit with h the rotationa rotationall resisti res isting ng tor torque que,, to calc calcula ulate te the app appare arent nt vis viscos cosity ity.. Thi Thiss geometry may be referred to by the equipment manufacturer as a spindle, bob, inner concentric cylinder, vane, and so forth.
3. Terminology 3.1 Definitions:
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This test method is under the jurisdiction of ASTM Committee D08 Committee D08 on on Roofing and Waterproofi Waterproofing ng and is the direct respo responsibil nsibility ity of Subco Subcommitte mmitteee D08.03 on Surfacing Surfac ing and Bitum Bituminous inous Materials for Membra Membrane ne Waterpr aterproofing oofing and Built Built-up -up Roofing. Curren Cur rentt edi editio tion n app approv roved ed May 1, 201 2015. 5. Pub Publis lished hed May 201 2015. 5. Ori Origin ginall ally y approved in 1984. Last previous edition approved in 2013 as D4402/D4402M – 13. DOI: 10.1520/D4402_D4402M-15. 2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at
[email protected]. For Annual Book of ASTM Standards volume information, refer to the standard’s Document Summary page on
4. Summ Summary ary of Test Test Method 4.1 A rotati rotational onal viscometer viscometer,, as described in this test method, method, is used to measure the apparent viscosity of asphalt at elevated tempe tem perat ratur ures. es. Th Thee tor torqu quee on the ap appar paratu atuss-mea measu surin ring g geometr geo metry y, rot rotatin ating g in a the thermo rmosta statica tically lly con contro trolled lled sam sample ple
the ASTM website.
holder containing a sample of asphalt, is used to measure the
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D4402/D4402M − 15
relative resistance to rotation. The torque and speed are used to deter de termi mine ne th thee vi visco scosi sity ty of th thee as asph phalt alt in pa pasc scal al se seco cond nds, s, millipascal seconds, or centipoise.
9. Calibration and Standardizatio Standardization n
5. Sign Significan ificance ce and Use
9.2 The accuracy accuracy of the viscometer shall shall be checked at least annually using a certified reference fluid of known viscosity at various vario us temper temperatures atures,, using the proce procedure dure described in Test Method E2975. E2975. The The ref refere erence nce fluid sha shall ll be cer certifi tified ed to be Newton New tonian ian in beh behavi avior or ove overr the ful fulll ran range ge of exp expecte ected d tes testt tempera temp eratur tures es and she shear ar rat rates. es. The ref refere erence nce flui fluid d sha shall ll be certified at a temperature within 50°C [90°F] of the temperature(s) to be used during the test. The viscosity measured shall be within 62 % of the certified value, or else a calibration constant (viscosity of the calibration fluid/viscosity indicated by the apparatus) must be determined and applied.
9.1 The viscometer viscometer shall be zeroed before before use, or as needed, or both, according to the manufacturer’s instructions.
5.1 5. 1 Th This is te test st me meth thod od is us used ed to me meas asur uree th thee ap appa pare rent nt viscosity of asphalts at handling, mixing, or application temperatures. 5.2 Som Somee asp asphal halts ts may exh exhibit ibit non non-Ne -Newto wtonia nian n beh behavi avior or under the conditions of this test method, or at temperatures within with in the ran range ge of this tes testt met method hod.. Sin Since ce non non-Ne -Newto wtonia nian n viscos vis cosity ity val values ues are not abs absolu olute te pro proper perties ties,, but refl reflect ect the behavior of the fluid within the particular measurement system, it should be recognized that measurements made by this test method may not always predict field performance under the conditions of use.
9.3 The accuracy accuracy of the temperat temperature ure reading reading and the temperatu pera ture re sta stabi bilit lity y of th thee te temp mper erat atur uree co cont ntro rolle llerr ar aree to be checked at least every six months by placing an asphalt sample or high flash point oil in the test chamber, and equilibrating to a temperature within 50°C [90°F] of the temperature(s) to be used use d dur during ing the tes test. t. The sample temperat temperature ure shall then be measured to within 60.1°C [60.2°F] by using a NIST traceable measuring device, as described in Test Methods E644 E644.. If any temperature differential is indicated, the set point of the
5.3 Compa Comparison risonss betwee between n nonnon-Newto Newtonian nian viscosity values should be mad should madee onl only y for measurem measurement entss mad madee with similar similar conditions of temperature, shear rate, and shear history. 6. Appar Apparatus atus 6.1 Rotational Viscometer, capable of measuring the torque required to rotate the selected apparatus-measuring geometry at a se selec lected ted co cons nsta tant nt sp speed eed wh whil ilee su subm bmer erge ged d in as asph phalt alt at constant desired test temperature, and with the capability to convert the torque measurement to viscosity in pascal seconds, millipascal seconds, or centipoise. This calculation may need to be done manually for some instruments.
temperature controller shall be offset accordingly. 10. Procedur Proceduree 10.1 Follo Follow w the manufacturer’s manufacturer’s instructions instructions for the operation of the instrument.
6.2 Apparatus-measuring geometry, of various shapes and sizes, for measurement of various viscosities of asphalt.
10.2 10. 2 All Allow ow the instrumen instrumentt elec electro tronic nicss to war warm m up for at least five minutes before conducting conducting any calibr calibrations ations or analyses.
6.3 Temperature-Controlled Temperature-Controlled Thermal Chamber Heater Heater,, for maintaining the sample of asphalt at the test temperature.
10.3 Set th 10.3 thee tem tempe pera ratu ture re co cont ntro rolle llerr to th thee de desi sire red d tes testt temperature, taking into account any offset determined in 9.3 in 9.3..
6.4 Sample Chambers, reusable or disposable. 6.5 Temperature capable le of mai mainta ntainin ining g the Temperature Controller Controller,, capab specimen temperatures to 61.0°C [62.0°F] for test temperatures between 38 and 150°C [100 to 300°F] and to 62.0°C [64.0°F] for test temperatures between 150 and 260°C [300 to 500°F].
10.4 Select an apparatus-measur apparatus-measuring ing geometry that will develop a resisting torque between 10 and 98 % of the instrument capacity at the selected speed. Generally, measurements will be more accurate at higher torque readings. 10.5 10. 5 Pre Prefer ferabl ably y, pre prehea heatt the sam sample ple cha chambe mberr and the selected apparatus-measuring geometry until temperature equilibrium has been obtained for at least 15 min. If filled asphalts are being measured, this step is mandatory.
6.6 Balance, readable to 0.1 g, for determining the mass of asphaltt sample asphal sample.. 6.7 Platinum Resistance Thermometer (PRT), with a probe which conforms to the requirements of Specification E1137, E1137, for mea measur suring ing the temp tempera eratur turee of the the therma rmall cha chambe mberr. The PRT shall have a 3- or 4-wire connection configuration and overall sheath length shall be at least 50 mm [2 in.] greater than the imm immers ersion ion dep depth. th. Cali Calibra brate te the PR PRT T sys system tem (pr (probe obe and readout) in accordance with Test Methods E644 Methods E644..
10.6 Add the volume of sample specified specified by the manufacturer for the apparatus-measuring geometry to be used to the sample chamber. A convenient way for measuring the volume is by weighing out the amount calculated from approximate density den sity data for the sam sample ple and the then n ret return urning ing the samp sample le chamber to the temperature controlled chamber heater. Thoroughly oug hly stir filled asp asphal halts ts to obt obtain ain a rep repres resent entativ ativee samp sample le before weighing.
7. Reag Reagents ents and Materials Materials 7.1 Solven Solvents ts for cleani cleaning ng sam sample ple cha chambe mber, r, app appara aratus tus-measuring geometry, and accessories.
NOTE 1—Exercise caution to avoid sample overheating, and to avoid the ignition of samples with low flash points.
8. Prepara Preparation tion of Apparatus Apparatus 8.1 The rotational rotational viscometer and thermal chamber heater shall be leveled and prepared as recommended by the instrument manufacturer.
10.7 Do not overfill overfill the sample chamber, chamber, but ensure that the measuring portion of the apparatus-measuring geometry will be completely immersed. Follow the manufacturer’s instructions tio ns.. Th Thee sam sampl plee vo volu lume me is cr criti itical cal to me meet et th thee sy syste stem m calibration standard. 2
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Insertt the selected prehe preheated ated apparatus-measur apparatus-measuring ing ge10.8 Inser ometry into the liquid in the chamber, and couple it to the viscomet visc ometer er,, fol followi lowing ng the man manufac ufactur turer’s er’s inst instruct ructions ions for proper alignment.
13. Pre Precisi cision on and Bias 13.1 Unfilled Roofing Asphalt— The The following criteria shall be us used ed fo forr ju judg dgin ing g th thee ac accep ceptab tabili ility ty of an any y re resu sult lt (9 (95 5% confidence level). 13.1.1 Sing Single-O le-Opera perator tor Pr Precisi ecision on (Rep (Repeata eatabilit bility)— y)— Duplica Dup licate te val values ues by the same ope operat rator or usi using ng the same test equipm equ ipment ent,, in the sho shortes rtestt pra practic ctical al per period iod of time shall be considered not equivalent if the difference in the two results, expressed as a percent of their mean, exceeds 3.5 %.
10.9 10. 9 Brin Bring g the asp asphal haltt sam sample ple to the des desired ired temperatu temperature re within 30 min and allow it to equilibrate at the desired test temperature for a minimum of 10 min before beginning the measure meas uremen ment. t. In the cas casee of fille filled d asp asphal halts, ts, star startt the mot motor or rotation immediately.
13.1.2 Multilaborato Multilaboratory ry Precision (Repr (Reproducibility)— oducibility)— The values reported by each of two laboratories, representing the arithmetic average of duplicate determinations, shall be considered not equivalent if they differ by more than 14.5 %.
10.10 Start the motor rotation rotation of the viscometer viscometer at a speed that will develop a resisting torque that is between 10 and 98 % of the full-scale instrument capacity. Maintain this speed and allow all ow th thee sam sampl plee to eq equi uilib libra rate te fo forr an ad addi ditio tiona nall 5 mi min. n. Temperature should not deviate more than 61.0°C [62.0°F] during durin g this condit conditioning ioning period.
13.2 Filled Roofing Asphalt— An An interlaboratory study was conducted in 2004 comparing three filled roofing asphalts from three different suppliers, tested in triplicate at 205°C [400°F] by nine different laboratories. The data was used to calculate precision precis ion estimates for filled asphalt. The follow following ing criteria shall be used for judging the acceptability of any result (95 % confidence level). 13.2.1 The single-operator precision (repeatability) standard deviation has been determined to be 21.0 %. Therefore, two results obtained in the same laboratory, by the same operator using the same equipment, in the shortest practical period of time, should be considered not equivalent if the difference in the two results, expressed as a percent of their mean, exceeds 59.4 %. 13.2.2 13.2. 2 The multila multilaborat boratory ory precision (reproducibility (reproducibility)) standard deviation has been determined to be 33.2 %. Therefore, two res result ultss sub submit mitted ted by two dif differ ferent ent ope operat rators ors test testing ing the same material in different laboratories shall be considered not equivalent if the difference in the two results, expressed as a percent of their mean, exceeds 94.0 %.
10.11 Mea 10.11 Measur suree eith either er the viscosity viscosity or the tor torque que at 1-m 1-min in interva inte rvals ls for a tot total al of thr three ee min minute utes. s. The ins instru trumen mentt may perform this measurement automatically. 10.12 Repeat steps steps 10.9 – 10.11 for each test temperature required. If filled asphalts are being measured, a new, freshly stirred sample will be required for each test temperature. 10.13 If torque readings readings are above 98 % of the instrument instrument capacity at the test temperature, decrease the speed of rotation rotatio n of thelowest apparatus-m appar atus-measuri easuring ng geomet geometry ry and continue contin ue with wit h th thee tes test, t, or re repe peat at st step epss 10.5 10.5 – 10. 10.11 11 with with a sm small aller er diameter geometry and the appropriate volume of sample. 10.14 If the torque reading reading is below 10 % of the instrument instrument capacity at the highest test temperature, increase the speed of rotation of the apparatus geometry, or repeat steps 10.5 steps 10.5 – 10.11 with a larger diameter geometry and the appropriate volume of sample. 10.15 If the instrument instrument does not read out directly in viscosviscosity units, multiply the torque readings by the appropriate factor to obtain the viscosity values.
13.3 Unfi precis cision ion est estima imates tes Unfilled lled Pavi Paving ng Asph Asphalt— alt— The pre given are based on the analysis of test results from eight pairs of AMRL proficiency proficiency samples. The data analyzed consisted of results from 142 to 202 laboratories for each of the eight pairs of samples. The details of this analysis are in NCHRP Final
11. Calculation 11.1 11 .1 If the instrument does not automatically automatically average three readings, then calculate the result as the arithmetic average of the three readings taken at 1-min intervals, rounded to three signifi sig nifican cantt figu figures res.. If the rot rotatio ational nal vis viscom cometer eter has a dig digital ital output out put dis displa playin ying g vis viscos cosity ity in cen centip tipois oisee (cP (cP), ), mul multipl tiply y by 0.001 0.0 01 to obt obtain ain the vis viscos cosity ity in pas pascal cal sec second ondss (Pa (Pa·s) ·s).. For instr in strum umen ents ts th that at of offe ferr au auto tomat matio ion, n, th thee re resu sults lts of a 33-min min integration shall be acceptable. If required, multiply the average reading by the calibration constant determined in 9.2 9.2..
Report,, NCH Report NCHRP RP Pro Project ject No. 9-2 9-26, 6, Pha Phase se 3. The fol follow lowing ing criteriaa shall be used for judging the accepta criteri acceptability bility of any resul resultt (95 % confidence level). 13.3.1 13.3. 1 The singl single-oper e-operator ator precis precision ion (repea (repeatability tability)) coef coeffficientt of var cien variati iation on (1s %) has been det determ ermine ined d to be 1.2 %. Therefore, two results obtained in the same laboratory, by the same sa me op oper erat ator or us usin ing g th thee sa same me eq equi uipm pmen ent, t, in th thee sh shor ortes testt practical period of time, should be considered not equivalent if the difference in the two results, expressed as a percent of their mean, exceeds 3.5 % (d2s %). 13.3.2 The multilaboratory precision (reproducibility) coefficient of variation (1s %) has been determined to be 4.3 %. Therefore, Theref ore, two result resultss submi submitted tted by two dif different ferent operators operators testing test ing the sam samee mat materia eriall in dif differ ferent ent labo laborat ratori ories es sha shall ll be considered not equivalent if the difference in the two results,
12. Repor Reportt 12.1 Report test temper temperature, ature, apparatus-measur apparatus-measuring ing geometry type and size, torque in mNm or percent of instrument capacity, and speed in sec-1 or r/min with viscosity results in pascal seconds (Pa·s), millipascal seconds (mPa·s), or centipoise (cP). For example, Viscosity at 135°C = 0.455 Pa·s with Bohlin 25 mm bob, 8.3 mNm of torque at 10 sec-1 or Viscosity at 400°F = 240 cP with Brookfield spindle number 31, 48 % torque at 60 r/min.
expressed as a percent of their mean, exceeds 12.1 % (d2s %). 13.4 Bias— No No information can be presented on the bias of this test method for measuring apparent viscosity because no material having an accepted reference value is available. 3
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14. Keyw Keywords ords 14.1 asphal asphalts; ts; rotati rotational onal viscometers; viscometers; viscos viscosities ities ASTM International International takes no positi position on respecting the validi validity ty of any patent rights assert asserted ed in connec connection tion with any item mentio mentioned ned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of infringement of such rights, are entirely their own responsibility. This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible respon sible technical technical committee, which you may attend. If you feel that your comments have not receiv received ed a fair hearing you should make your views known to the ASTM Committee on Standards, at the address shown below. This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above address addr ess or at 610610-832832-9585 9585 (pho (phone), ne), 610610-832832-9555 9555 (fax (fax), ), or serv service@ ice@astm astm.org .org (e-m (e-mail) ail);; or thro through ugh the ASTM webs website ite (www.astm. (www .astm.org). org). Permission Permission rights to photocopy the standa standard rd may also be secure secured d from the Copyri Copyright ght Clearance Center, Center, 222 Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/
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