METHODS OF SAMPLING AND TESTING T44

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T47 METHODS OF SAMPLING A N D TESTING

Sta&iard Method of Test for

Loss on Heating of Oil and Asphaitic Compounds AASHTO DESIGNATION T47-821

(ASTM DESIGNATION D6-80)

1. SCOPE

1.1 Thrs method covers the determ~natron of the loss In mass (txclustve of water) of or1 and asphalt~c compounds whcn heated as heremafter pracrlbed

2 APPLICABLE WCUMENTS

21 ASTM Standards. E l Spcaficat~on for ASTM T h a m o m a a s El45 Spcaficauon for Gravrty-Convatton and Ford-Yent~lauon Ovcns

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~ned along w~th a cornpanson before ~ n d after, of any other d u ~ r c d charactensttu Thrs method provtde only 3 rdattve measument of the volat~hty of a rnaterral under t a t condrt~ons

41 Oven-The oven shall be cluztncally hated and shall conform to the pcrrormancc rcqurre- mcnts of Spcclficatron El45 Type I. Grade B, for opcatrng temperatures up lo 180C (365F) Dunng the teru lor complrance to Spcc~ficatron El45 requirements the ovcn shelf. properly placed shall be IU p l a a and rotalrng. In addrt~on. a shall also comply w~th the 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~ghtly fittrng h~nged door whrch shall provrde a clear opm~ng substant~ally the same as the mtenor hcrght and w ~ d h of the oven The door may contam a wrndow with drmmstons of at Iwr 100 by 10 mm (4 by 4 In ). and with two sheets of giau separated by ao air rpacc. through wh~ch a ver~~ca l thamometa lmzttcd as spcc~ficd In Sectton 7, may be read w~thaut opcnmg the door, or the oven may be prov~dcd w~th an inner glass door, through whrch the thamorneter may be obscrval on opmlng the out- door morncntarrly The oven shatl be adequately vent~latcd by convectton currents of a r and for thrs purpose shall be pto- vrdcd 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~on E145, Type I. Grade B, are met

4.13 Rotating Shelf-The oven shall be provldcd with a circular metal shelf havrng a mlntmum d~ameter of 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~th rapect 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~ance wtrh 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 ~ndofiruta pnod to pmvtde for normat amonlullon of prcmt eqtupmern Howcva, all new ovens Putchawd should comply w~th the mmrmum dtmcnsrons and rqwremcno of ths test method

At 77tmnomcter--An AST M Loss on Hcst Thermometer graduated m Cels~ua degrees. havmg a range from 155 to 170C and conformmg to the rqulrements for Thermometer 13C as prcscrrbcd In the Spcc~ficatron El.

* 74 r t

METHODS OF SAMPLING AND TESTING T47

4 3 Conmner-The contalner In wh~ch the sample IS to be tested shall be of metal or glass, cylrndrrcal In sham 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 vola- tilrty may be tested at the same tlme Samples varyrng greatly In volatthty should be tested separate- ly When extreme accuracy IS rcqurrcd not morc than one matenal should be t s tcd at one time and duplrcate samples of rt should be placed srmultancously ~n the oven Such duplrcates shall check w~thrn the lim~ts of accuracy glven rn Section 8 Results obta~ned on 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~table methods of dehydrat~on before subjcctrng the matenat to the loss on heating ta 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~ghed sample on snd near the crrcumference of the crrcular shelf, rn one of the recesses ~f the rccommendcd shell IS used Close the oven and rotate the shelf during theentire test at a rate of 5 to 6 rpm Mantan 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~de the periphery of theshelf, and w~th the bottom of the thermometer bulb 6 mm (0 25 rn )above the shelf

NOTE 3-If addrtlonal penods of hcaung arc dnrrat 11 IS rccomrnunded that t h y bc made In successwe In- crements of 5 h each

NOTE W h e n rt IS qurrcd that the pmetrallon or other charactetrst~cs of the sample after hLatrng k detu- mlncd. the c ~ d u c should 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 rerr- due shall be brought to standard temperature and tested as prexr~bal ~n the 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~t of error rncrmses 0 01 for wery 0 5% increase In loss by volat111- zauon as shown in Table 1

S e c t ~ o n A-B

Top V t c w

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