T44

METHODS OF SAMPLING AND TESTING

METHODS OF SAMPLING A N D TESTING

T47

Sta&iard Method of Test for

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Loss on Heating of Oil and Asphaitic Compounds

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AASHTO DESIGNATION T47-821

(ASTM DESIGNATION D6-80)

1. SCOPE
1.1 Thrs method covers the determ~natronof the loss In mass (txclustve of water) of or1 and
asphalt~ccompounds whcn heated as heremafter pracrlbed

2 APPLICABLE WCUMENTS
21 ASTM Standards.
E l Spcaficat~onfor ASTM T h a m o m a a s
El45 Spcaficauon for Gravrty-Convatton and Ford-Yent~lauonOvcns

3. SUMMARY OF METHOD
3 1 Fihy grams of material. spread out In a dish 55 mrn in drameter. IS h m t d In movlng .ur for
5 h at 163'C (325'F) and the percent Loss of mass determ~nedalong w~tha cornpanson before ~ n d
after, of any other d u ~ r c dcharactensttu Thrs method provtde only
volat~htyof a rnaterral under t a t condrt~ons

rdattve measument of the

41 Oven-The oven shall be cluztncally hated and shall conform to the pcrrormancc rcqurremcnts of Spcclficatron El45 Type I. Grade B, for opcatrng temperatures up lo 180C (365F)
Dunng the teru lor complrance to Spcc~ficatronEl45 requirements the ovcn shelf. properly placed
shall be IU p l a a and rotalrng. In addrt~on.a shall also comply w ~ t hthe followmg rcqulremtnu.
41.1 Conrtnunon (Note I h T h c oven shall be rectangular wrth mmmum tntcrror d~mcns~ons
of 330 mm (13 In ) m each mracuon Thc ovcn shall have m front a t~ghtlyfittrng h~ngeddoor whrch
shall provrde a clear o p m ~ n gsubstant~allythe same as the mtenor hcrght and w ~ d hof the oven The
0 mm (4 by 4 In ). and with two
door may contam a wrndow with drmmstons of at Iwr 100 by 1
sheets of giau separated by ao air rpacc. through wh~cha v e r ~ ~ ctahl a m o m e t a lmzttcd as spcc~ficd
In Sectton 7, may be read w~thautopcnmg the door, or the oven may be prov~dcdw~than inner glass
door, through whrch the thamorneter may be obscrval on opmlng the out- door morncntarrly The
oven shatl be adequately vent~latcdby convectton currents of a r and for thrs purpose shall be ptovrdcd with opcnrngs for the entrance of air and for the a r t of heated alr and v a p r s Opntngs mav
be of any srze and arrangement provided the rqurrements of Spccrlicat~onE145, Type I. Grade B,
are met
4.13 Rotating Shelf-The oven shall be provldcd with a circular metal shelf havrng a mlntmum
d~ameterof 250 mm (9 8 in ) (A rccommendcd form of alumrnum shelf IS shown rn Frg. I ) The shelf
shall be suspcndcd by a vcnlcal shaft and centered w~thrapect to the horizontal Intenor d ~ m a s ~ o n s
f h e shelf shall be provlded wrth a mechanical means of rotatlng ~t at the rate of 5 to 6 rpm Thc
shclf shall be vertrcally located as close to the center of the oven as pcrmrtted by compl~ancewtrh the
rcqulrtments of 6 2 regardrng thermometer placcment
NOTE 1--Contmucd use of cxistmg rmallcr wms wrnplyrng mth the rcqummcnts of this t a t shall be p a rnrtted for an ~ndofirutapnod to pmvtde for normat amonlullon of prcmt eqtupmern Howcva, all new ovens
Putchawd should comply w~ththe mmrmum dtmcnsrons and rqwremcno of ths test method
At 77tmnomcter--An AST M Loss on Hcst Thermometer graduated m Cels~uadegrees. havmg
a range from 155 to 170C and conformmg to the rqulrements for Thermometer 13C as prcscrrbcd
In the Spcc~ficatronEl.

rt

METHODS OF SAMPLING AND TESTING

74

T47

4 3 Conmner-The contalner In wh~chthe sample IS to be tested shall be of metal or glass,

cylrndrrcal In s h a m and shall have a flat bottom Its rnstdc drmensrons shall be substantrally as
follows dlamcter, 55 mm (2 17 In ). depth. 35 mm (1 38 ln )
NOTE 2-Conurners known in the dtug trade as seamlus "omlmcnt b o x 6 'may be obtamd lo drmens~ons
conformrng to the above rcqurrernents
5 PRECAUTIONS

5.1 Under ordinary ctrcumstanca a number of samples havrng about the same degcc of volatilrty may be tested at the same tlme Samples varyrng greatly In volatthty should be tested separately When extreme accuracy IS rcqurrcd not morc than one matenal should be t s t c d at one time and
duplrcate samples of rt should be placed srmultancously ~n the oven Such duplrcates shall check
w~thrnthe lim~tsof accuracy glven rn Section 8 Results obta~nedon samples showlng evrdenccs of
foamtng durrng the l e t shall be rejected
6. PREPARATION OF SAMPLE
6 1 Heat the sample wrth care, surnng as necessary, to prevent locnl overheatrng untll ~t has
become sufticrently fluid to pour In no case shoutd the temperature be rarsed to morc than 80 to
1 10 C (I45 to 200 F) above the expccled softcnmg pomt
4.2 Frrst test the matenal under enamrnatlon for water and, rf water rs pruent, remove ~t by
su~tablemethods of dehydrat~onbefore subjcctrng the matenat to the loss on heating t a t . or. obtam
another sample that 1s free of water

7. PROCEDURE

7 1 Place 50Of 0 5 g of the sample of the water-free matenal to bc tutcd In a tared contalner
conforming to thc requirements of 4 3. and weigh to the nearest 001 g If the material has been
heated to facilitate transfer, cool the sample to room temperature before makrng thrs rnrtral werghrng
Bnng the oven to a temperature of 163"C (32SF), and placc the container wrth the we~ghedsample
on snd near the crrcumference of the crrcular shelf, rn one of the recesses ~fthe rccommendcd shell
IS used Close the oven and rotate the shelf during theentire test at a rate of 5 to 6 rpm M a n t a n the
tempcrature at 163& 1' C (325h 1 8F) For 5 h after the sample has b a n rntroduced and the ovcn
has agam reached that tcmpcrature The 5-h pcrtod shall start when the tempcrature reaches 162'C
(324"F), and in no case shall the total tlmc that a sample IS In the oven be more than 5 h and 15 mln
At thc conclusron of the heatrng penod. remove the sampk from the ovcn, cool to room tcmpcraturc
weigh to the nearest 001 g, and calculate the loss due to heating
73 Detcrmrne temperatures by means of the sp*crficd thermometer. whtch shall be supported
from the shaft of the crrcular shelf in a vertrcal posltron approxtmatcly 19 mm (0 75 m ) lns~dethe
periphery of theshelf, and w~ththe bottom of the thermometer bulb 6 mm (0 25 rn )above the shelf
NOTE 3-If addrtlonal penods of hcaung arc dnrrat 11IS rccomrnunded that t h y bc made In successwe Increments of 5 h each
NOTE W h e n rt IS qurrcd that the pmetrallon or other charactetrst~csof the sample after hLatrng k detumlncd. the c ~ d u should
c
be mclted In the mntarnu at the lowest parstblt tcmpuature and thoroughly mxcd by
stlrnng, taking care to avod lncorporatlng slr bubbles In the mattrlat For h a pcnemtron tat, the well-rntxed rerrdue shall be brought to standard temperature and tested as prexr~bal~nthe Ttst for Penetratron of Btlurnrnrous
Matenah (AASHTO T49) For other tests. thc well-mnxed ratduo should be tcstcd acwrdmg to slnndard con&tlms as rqu~ral
by the test procedure ~nvolvcd

8 1 Up to 5% loss ro mass, the rerults obtalned may be consrdercd as correct wrthln 0 5 Above
5% loss In mass, the numcncal llm~tof error rncrmses 0 01 for wery 0 5% increase In loss by volat111zauon as shown in Table 1

S e c t ~ o nA-B

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FIG 1

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