METHODS OF SAMPLING AND TESTING &,J T44 /*? H

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4 In, by 4 tn, (100 by I00 mm) ~ n i a e ~ a a d of the & I C ~ C I I as rrcrrved at 110 f 5 C (230 &9 F) and each wdgh* to the nearest 0.1 g. The then be determ~ned to the nearest 0.01 I* (Q.25 mm) The wmght In

porrndsper cubtcfwt (kg/mm9 of each speclrnm shall be caiculatsd from t h h d$ammmons and the amcage werght reported.

Standard Methad of Testfir

AASHTO DESIGNATION. 7'44-81 (ASTM DESIGNATION: D2042-76)

1. SCOPE

1.l This method of test IS applrcable to the d c t m t n m d n of the degree of solubrlity rn argrnrc solvmts of bituminous mad matends such PI rOPd tars and paroleurn asphalts hawng little or no rnrnerd matter. The pmcedure to be followed for calculating the proportion of bitumen soluble In carbon tetrachloride IS PISO glvm.

2. SUMMARY OF METHOD

2.1 The sample 1s dtuolvcd in a spcafiad solvent and filtcrcd through a tilt- mat. The tnsolublc rnatcnal ts washed, dnsd and wetghed

I lt.+ 1Mkl hUDb Ok SAMPLING AND TESTING

33 Asbestar--Medium or long fiber (amphtbote), acld-washed for Gooch c m b l e s 3.4 Desrccaror--Of ttabls s ~ z z charged wrth an cffecttve descant U Ina ly~ica l Bala%-A cias A balance conforrntng to Oc rcqutremettts of AASHTO

Spectficatton M 231 3.6 Mujj7e Furnace-A furnace capable of obtatnrng temperatures of 650C (IZOOF) (Not

requmd when ustng the fiber glass filter drscs In I r a of asbestos ) 3 7 F~bcrglwjilter dkc-A filter made from extremely line borosrltcate glass fibers

4.1 The solvent to be used shall be spmfied Solvents suttrble for use In thrs method are as follows - ~

4.1.1 Carkn Dwulfdc. Rea~ent G m d e B y definltron, the matendsolubtc In carbon dtsulfde a bttumen, Thrs solvent ts surtobte for use mth both asphrltrc and tar mrtcnals.

4.1.2 Catbon Tetmchbndc. Reagent ~mdr-since tt n nonflunrnable thrs solvent IS genenllv destgnated for use rn detennrntng the degm of sotubtlrty of pmaleum asphalts tn lreu of the daermrnatlon of bttumen fdubtitty rn cubon dsulfide) It ts not appl~cable to tars or very htghlv cracked petroleum p d u m except as employed in Sectlon 10.

4 . i l Bcnzmc Rcagent Gmdc--Thu drcnt a sometimes uEed tn Irm of carbon dnulfrde and is surtable for use wrth asphalts Althou~h the solubrlrty of tar products tn benzene ts somctrmes rcqutred. the procedurcdescnbed rn t h ~ s methcd IS not recommended for such tests.

41.4 Tnchlomerhylcne Terhnrcd Grad-Tbts nonflammable solvent IS applicable to petrole. um asphalts as a substitute for carbon d~sulfide for detemtntng the dcgrcc of soluhltty. but IS not applrcable to tars or very h~ghly cracked petroleum products I t is Ias toxlc than carbon tarachlondc

5. SAFfSTY PRECAUTIONS

5.1 All organ~c solvents ate toxtc to some d e g m and good venttIabon should be provrded tn all cases Carbon dl-ulfide IS extmmely flammable: the vapor wrlt often Igndc spontnncousfy on contact wtrh a hot surface such as a hot plate or wen Therefore. when usrng thu solvent. be sum that the filtranon 1s conducted under a hood and well away from names or other sources of hu t . &fore pircmg cmcrbla orcantarners In theoven a11 traces of carbon drsulfidt should be removed (as mdrcnted by the drsappearance of all odor) O t h m s e . thevapan wrll tgntte Carbon dtsulfide u a h very rrntattng to the sktn and dlrecf contact should be avo~ded

6. PREPARATION OF COOCH CRUCIBLE

6.1 Thoroughly shake a portlon of the asbestos fiber tn dtstrlled water so ar to form a rhrn suspnslon In whtch the asbestos flbcn am evenly dupmed

6 3 Asscmbk the fikcnng apparatus as shown in R g I Frll the crucrble wtth some of the suspenston of asbestos tn water and allow tt partly tosettle rn thecrunbte Apply a ltght sudron todmw off the water. Icavrng a firm mat of asbestos In tha cruc~blc. Add more suspended asbestos and repeat the process untd a mat IS burlt up that after lgnltlon. wrtl wetgh 09 f 0.1 g (Note 2). Wash the arbatar mat thoroughly wtth water. dry In an oven. and tgnlte in a muffle furnace at 600 to 650 C 11 100 to l ZOO F) Cool the crucrble In a desrccator and wetgh to the neamt 0.1 mg. Repeat the rgnttton and coolrng until constant wnght k 0 . 3 mg) ts o b t a r d . Stom in a dcsmator untrl reedy for use.

NOTE I-In the datmrnrtlon, the aabeaos rppararrly trrcversrbly abmrbs asd tamoum of*dublc brrumm (usually I to 5 mg pcr gram of arbertm) The w u & u ornrbsms usod should, rhacforq k kept wllhtn the spm- frcd t~m~ts to mure rcproduc~ble resub

6J Wficn ustng a fiber glass filler drsc, drsrcgard Secttons 6 1 and 63. Assemble the tiltenng apparatus as shown In Wg 1 Motsten the d m wrth solvent and scat firmly In the bottom of the cruel- bla Place In an oven at 1 loo& 5 "C (230& 9'F) for at least 20 mnutes cool In desrccator and weigh Repeat the drytng and wetghmg unt~ l constant mass (zk 0 3 mg) e obtarncd Store In a dtstc- cator until ready for use

METHODS OF SAMPLING AND TESTING

FIG. I.-PiItmng Apparatus Assembly

7.1 Normally the temperature at wh~ch r h ~ s test IS run IS not cnt~cal and tt may be performed at the laboratory arr temperature. For refem? tests.. however, the flask and sample m solutron shall be placed In a water bath mamtamcd at 37 8 A025 C (100 ltsO 5 Fl for one hour before filtering Cautcon If carbon drsulfide IS the solvent uscd. run both normal and referee t a t s at laboratory alr ternperaturn It IS dangerous to heat carbon d~sulfide

8. PROCEDURE

8.1 Note safety prccautrons In Sectlon 5 and Sect~on 7 Transfer approx~marely 2 g of the ample Into a t a d 125 ml Erlenmeyer flask or other surtable contamer Wetgh accurately to the neamt mtll8gram. Add 100 ml of the specified solvent to the contamer In small portions wlth continuous agltatlon untrl all lumps drsappear and no und~ssolved sample adheres to the contamer Stopper the flask or othcnv~se cover the contamer and set aslde for at least 15 mtn (See Scet~on 71

82 Place the prevrously prepared and welghtcd Gooch cructble ~n the filtcnng tube Wet the mat wtth a small poruon of dean solvent and decant the solutton through the mat of the cruclMc w~th or wtthout hght suct~oo as may be necessary When the ~nsoluble matter IS apprmablc, retaln as much of rt as posstblc rn the contalner un t~ l the solut~on has drancd through the mat Wash the son- tamer w~th a small amount of solvent and, using a stream of solvent from a wash bottle. transfer all ~nsoiuble matter to the cructblc, Use a "pohccman" IT necessary to remove any tnsoluble matter adhenng to the contamer, rmse the pol~ceman and contalner thoroughly Wash the tnsolublc matter In the rmnble wlth solvent untd the filtrate IS substantrally colotlas, then apply strong suchon to remove the remarnlng solvent Remove the m a b l e from the tube, wash the bottom fa of any drs- solved matter, and place the crucible on top of an oven or on a steam bath unnl all odor of the solvent IS removed. (See safety prsautlons in Scctlon 5 ) Place In an oven at 1IOi; 5OC (230f gaF) for at least 20 mlnuta Cool In a d a m a t o r and wctgh Repeat the drymg and waghag unt11 constant mass (i 0 3 rng) IS obtatncd (Note 2 ) Except for referee tests, prevtously uscd aabestos mat cruc~bles may be used however, fiberglass tik d~scs should be used only one tlme

NOTE 2-In order lo obtsln pracuc results when usmg an asbatos mat the cdltng amc In the &laator must be apprommatdy the sama (w~rhm* 5 mm ) alta all hmunp For exarnplq if tho empty mnble a wnghtd after a 30 min d t n g tn the datcEaror. the emable contatntng the m~oluble matter must be waghni after 3[H 5 rnm cwllng m the datcgtor Eltha empty cructblts or crucibla contamnB insaluble matte that have rcmatned In a dg~ccator ovcm~ght should be reheated s an wen for at laut 30 m~n , then allowcd to cook before wc~ghmg.

T44 METHODS OF SAMPLING AND TESTING 71

9 CALCULATIONS AND R~PORT

9 1 C.tlculdtc wher the total percentage of ~nsolublc matter or the percentage of the samplc wlt~blc In the wlvent used as tollows

A - total wetght ~nsoluble and B - lorn1 wtrght of sample

9 1 1 For percentages of rnsoluble less than l 0, report to the neamt 0 01 percent. for perrcntdgcr trl tnsoluble I 0 or more. report to the nearest 0 I percent When carbon dlsulfide IS uscd ,I\ rhc wlwnt Ihe pvrccntnge ot the~amplesolubk IS. by definitron the percentage of bttumcn

10. PROPORTION OF BITUMEN SOLUBLE IN CARBON TETRACHLORIDE

10.1 Scintc specr l ic~ t~on~ require the deterrnmat~on of proportion of bitumen! soluble In carbon tctrnchlorrde In wch crsa. ~ w o solubtl~ty t a t s shall be made. one w~th carbon drsulfidc iprccnt hltumunJand another usrng carbon retrachlor~de as the solvent The above praccdurc shall be followed t~ccpr that tor thn purpose the soiutlon of sample in carbon tctrachlonde shall be allowed to stand at least 12 h In subdued light before f~ l tcnng C~lculate the proportfort (percent) of bttumcn soluble tn cdrbon Ictrnchloridc as tollous

Prowrtton - --t x 100 LJ

where: C - percent +ample mlublc In urbon ramchlonde and D - percent umpls duUe m carbon drrdMe (baumcnl

I I PRECISION

11.1 Est~matcs ot standard devrat~ons ~ p ' l for thn p r a r d u r t and the mtena for judging the .~ccept.~bll~ty ol results(95 percent contrdence kvef)areas folfows

W~rhtn- Bat~rcm- Lbon tory Lbantory Vmubrl~cy* Varublltty~

Asphl~s. mlubtllly mom lhan 99 prnrnt (ap llublc when either urba f~sulllda cur- bcn ntnchlmdc tnchlora- ethylene or benzene arc urdl 0 035 0 10 0 090 0 26

Tars, 11qud mdcs (appl~cablc whnn urbon dlsdfide IS uud) 011 031 0 2 2 0 6 1

Tan. m i d i d (apphublc when urbon drrulfide IS ural) 0 17 0 48 0 83 2 34

For deflnttlon of terms and recommended uu of pnctuon tndcra a the Recommended Pnc~rcc for Uu of rho Terms Prslrran and Accuracy re ~pplled to Muavrantnt of a Pmpny of a Malon.1 (ASTM E 177)

METHODS OF SAMPLING AND TESTING

m+ eccmutu of jundard dewatron ate hlcd on (ha idlmwnl Semt-

AsphmIU Llqutd Sottd T a n Tars

' 7he rundrnl dewal~ons sham (s.3 rcprtxnt the &mated standard dcvullon of the morurrment proam for the ruled cond~umi They 1~ ol- cuhled by mulllply~nl the smn&rd b v u t l o n r of the appltuMe dam by the

Two rcrults obuined by an opntor on the same mmple rhovld be con- sidered suspect i f they differ b mom than the suted amount A defined In Recammended PT~CIICG E 177 t i { # IS the d61Teronca two - Ilmlcs for wnde- Irbontorr+pcn~or-mrchlne-mult~by prectslon

Two rcrtrts obuincd by opentom m differmt labontatin should be conudcmd surpct rf they d r k b more than the succd amount. As defined tn Recommended Pncllu 8 177 r i a IS !he dtUcmnce two dutu ' lrmw for

T47 METHODS OF SAMPLING A N D TESTING 7 3

Staddard Method of Test for Loss oa Heating of Oil an9 Asphaltic Compoaods

AASHTO DESlGNATlON f47-82' (ASTM DESIGNATION D6-80)

covcn the &em~nat~on of ~ h c IOU IB mass unds when heated as hcrc~naiter prcscnbcd.

3. SUMMARY OF METHO\ /I"

3.1 Fdty gnns of in d~mmlr r . 1% hmtd in moving .ur ror wtth a cornpanson before hnd

after. o f any other only 3 relattve measurement o i the

I APPARATUS