METHODS OF SAMPLING AND TESTING

&,J
/*?

T44

I lt.+

1Mkl hUDb Ok SAMPLING

A N D TESTING

33 Asbestar--Medium o r long fiber (amphtbote), acld-washed for Gooch c m b l e s

3.4 Desrccaror--Of
ttabls s ~ z zcharged wrth an cffecttve descant
U I n a l y ~ i c a lBa%
lA
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~bcrglwjilterdkc-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~entG 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~cableto 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 f o r use wrth asphalts Althou~hthe solubrlrty of tar products tn benzene ts somctrmes
IS not recommended for such tests.
rcqutred. the procedurcdescnbed rn t h ~ methcd
s
41.4 Tnchlomerhylcne Terhnrcd Grad-Tbts
nonflammable solvent IS applicable to petrole.
um asphalts as a substitute for carbon d~sulfidefor detemtntng the dcgrcc of soluhltty. but IS not
applrcable to tars or very h~ghlycracked petroleum products It is Ias toxlc than carbon tarachlondc
-

-4 In, by 4 tn, (100 by I00 mm) ~ n i a e ~ a aofdthe & I C ~ C IasI rrcrrved

at 110f5 C (230&9 F)and each wdgh* to the nearest 0.1 g. The
then be determ~nedto 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.

StandardMethad of Testfir

5. SAFfSTY PRECAUTIONS

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 tilttnsolublc rnatcnal ts washed, dnsd and wetghed

mat. The

5.1 All organ~csolvents 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 o r other sources of h u t . &fore pircmg
cmcrbla orcantarners In theoven a11 traces of carbon drsulfidt should be removed (asmdrcnted 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 f0.1 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 n e a m t 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 a s d t a m o u m of*dublc brrumm
(usually I to 5 mg pcr gram of arbertm) The w u & u ornrbsms usod should, rhacforq k kept wllhtn the spmfrcd t ~ m ~to
t s m u r e rcproduc~bleresub
6J Wficn ustng a fiber glass filler drsc, drsrcgard Secttons 6 1 and 6 3 . Assemble the tiltenng
apparatus as shown In Wg 1 Motsten the d m wrth solvent and scat firmly In the bottom of the cruelbla Place In an oven at 1loo& 5 "C (230& 9'F) for at least 20 mnutes cool In desrccator and
weigh Repeat the drytng and wetghmg u n t ~ constant
l
mass (zk 0 3 mg) e obtarncd Store In a dtstc-

cator until ready for use

METHODS OF SAMPLING AND TESTING

T44

METHODS OF SAMPLING AND TESTING

71

CALCULATIONS AND R ~ P O R T

9 1 C.tlculdtc w h e r the total percentage of ~nsolublcmatter or the percentage of the samplc

wlt~blcIn the wlvent used as tollows

A
B

-- lorn1
total wetght ~nsoluble
wtrght of sample

and

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~amplesolubkIS. by definitron the percentage of bttumcn
10. PROPORTION OF

FIG.I.-PiItmng

BITUMEN SOLUBLE IN CARBON TETRACHLORIDE

10.1 Scintc s p e c r l i c ~ t ~ orequire

n ~ the deterrnmat~onof proportion of bitumen! soluble In carbon
tctrnchlorrde In wch crsa. ~ w osolubtl~tyt a t s shall be made. one w~thcarbon drsulfidc iprccnt
hltumunJand another usrng carbon retrachlor~deas the solvent The above praccdurc shall be followed
t ~ c c p rthat 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 t c n n gC~lculatethe proportfort (percent) of bttumcn soluble tn
cdrbon Ictrnchloridc as tollous

Apparatus Assembly

s IS run IS not cnt~caland tt may be performed at

7.1 Normally the temperature at wh~chr h ~ test
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

Prowrtton

--t x 100
LJ

where:
C percent +amplemlublc In urbon ramchlonde and
D percent umpls d u U e m carbon drrdMe (baumcnl

--

I I PRECISION
8. PROCEDURE
8.1 Note safety prccautrons In Sectlon 5 and Sect~on7 Transfer approx~marely2 g of the
a m p l e 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~ssolvedsample adheres to the contamer
Stopper the flask or othcnv~secover the contamer and set aslde for at least 15 mtn (See Scet~on71
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 ~ t h
or wtthout hght suct~ooas may be necessary When the ~nsolublematter IS apprmablc, retaln as
much of rt as posstblc rn the contalner u n t ~ the
l solut~onhas drancd through the mat Wash the sontamer w ~ t ha small amount of solvent and, using a stream of solvent from a wash bottle. transfer
all ~nsoiublematter to the cructblc, Use a "pohccman" IT necessary to remove any tnsoluble matter
adhenng to the contamer, rmse the pol~cemanand 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 f
a of any drssolved 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
(i0 3 rng) IS obtatncd (Note 2 ) Except for referee tests, prevtously uscd aabestos mat cruc~bles
may be used however, fiberglass tik d~scsshould 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~olublematter 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~ccatorovcm~ghtshould be reheated s an wen for at laut 30 m ~ n, then allowcd to cook before wc~ghmg.

l thn p r a r d u r t and the mtena for judging the

11.1 Est~matcsot standard devrat~ons~ p ' for
.~ccept.~bll~ty
ol results(95 percent contrdence kvef)areas folfows

W~rhtnL b o n tory
Vmubrl~cy*

Asphl~s.mlubtllly mom lhan

99 prnrnt (ap llublc when
either urba f~sulllda curbcn ntnchlmdc tnchloraethylene or benzene arc
urdl
0 035
Tars, 11qud mdcs (appl~cablc
whnn urbon dlsdfide IS
uud)
011
Tan. m i d i d (apphublc
when urbon drrulfide IS

Bat~rcm-

Lbantory
Varublltty~

0 10

0 090

0 26

031

022

061

0 17
0 48
0 83
2 34
For deflnttlon of terms and recommended uu of pnctuon tndcra a
the Recommended Pnc~rccfor U u of rho Terms Prslrran and Accuracy re
~pplledto Muavrantnt of a Pmpny of a Malon.1 (ASTM E 177)

ural)

METHODS OF SAMPLING A N D TESTING

T47

METHODS OF SAMPLING A N D TESTING

Staddard Method of Test for

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

AsphmIU

Llqutd
Tan

73

SemtSottd
Tars

Loss oa Heating of Oil an9 Asphaltic Compoaods

AASHTO DESlGNATlON f47-82'

(ASTM DESIGNATION D6-80)

covcn the &em~nat~onof ~ h cIOU

unds when heated as hcrc~naiterprcscnbcd.

'

7he rundrnl dewal~onssham (s.3 rcprtxnt the &mated standard

dcvullon of the morurrment proam for the ruled cond~umiThey 1~ olcuhled by mulllply~nlthe smn&rd b v u t l o n r of the appltuMe dam by the

IB mass

Two rcrults obuined by an o p n t o r on the same mmple rhovld be considered 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~byprectslon
Two rcrtrts obuincd by opentom m differmt labontatin should be
conudcmd s u r p c t rf they d r k b more than the succd amount. As defined tn
Recommended P n c l l u 8 177 r i a IS !he dtUcmnce two dutu ' lrmw for

3. SUMMARY OF METHO\
3.1

Fdty gnns of

after. o f any other

I APPARATUS

/I"

in d ~ m m l r r .1% hmtd in moving .ur ror

wtth a cornpanson before hnd
only 3 relattve measurement o i the