B S I B s x 0 l a P A R T T ( 1 ,81g9 I lbaqbbl DBaaql}S I

BS812:Part118:1988

o B$l uDc t825.07+ 891.221: [620.1+ 543.217.6z 546,226]

C O N T R O L L ED
DO C U M E N T
NO. iLr -"i.
IF RED ORIGTNAL
O Britishstandards Instittnion,No part of ttis publicafionmay be photocopiedor o*ranrvisereproducedwirhoui the prior p€rmission
in writing of gsl

BritishStandard

o Testingaggregates
Part1 1B.Methodsfordetermination
of
sulphate'eontent

Essaisdesgranulats
Partie?18.M6thodesde dosagedessulfates

Priifungvon Zuschlagstoffen
Teil 118. Verfahrenzur Bestimmung
desSulfatgehalts

BritishStandards
Institution

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bytheBritishStandards
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1998
 . PARTXllA gA I l , b a q b b q0 0 e e q 1 e5 I
BSI BSsgI?
B S8 1 2I F ' a r1t 1 8I 1 9 B B

Foreword

ThisPartof BS812 hasbeenpreparedunderthe direction

of the Cement,Gypsum,Aggregates and OuarryProducts
Standards Committee, In the revisionof BS812 : Part2 t
1975,Part3 : 1975andPart4 : 1976eachtest,or collec'
tion of relatedtests,is beingrevisedseparately andis being
issued asa sepafate Partor Sectionof BS812.
ThisPartof BS812 contains methods for determination
of total sulphatecontentandwater-soluble sulphate
contento{ aggregates, neitherof which waspreviously
included in BS812,but areincludednow because of the
problems that mayariseif aggregates containinghigh
concentrations of sulphates areusedin concreteor placed
closeto concretestructures'
It is intended that otherBritishStandards shouldcallup
BS812tsstmethods asthe basisof compliance. Neverthe-
lessit isnot intsndedthat aggregates shouldbe subjected
regularly to all the listedtests.Specilications in other
standards, shouldcallup only relevant testmethods.
Adviceon the useof simplerqualitative testsisgivenfor a
preliminarvsortingof aggregates to seewhethermore
precise andexpensive testingis iustified.
Reference shouldbe madeto BS812 : Part101for general
guidance on testingaggregates, precisionof test methods
andvariance arising fromsampling errors,
Compliance a with British Standard doesnot of iaell
conferimmunityfrom legalobligations.

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 B s x g l E P A R T X l T B6 6 r t h e q r E l 0 0 e a { 9 1? I
B S8 1 2; P a r t1 1 8; 1 9 8 8

Contents

Page
Foreword lnsidefront cover
Committees
responslbls Backcover

Methods
1 Scope
2 Definitions
3 Principle 2
4 Sampling 2
5 Determination o{ the sulphatecontentof
a 2:1 water/aggregate extract 2
6 Determination of the total sulphate
content
by acid extraction 6
7 Precision I
8 Testr€port

Appendices
A Semi-quantitative
testfor the presence
of
sulphate
ions
B Detailsof experimentsfor determiningprecision
of testsfor water-solublesulphbteand total
sulphatecontentsof aggregates

Tables
1 M i n i m u m m a s so f p r e l i m i n a r ys u b . s a m p l teo r
watsr-solublesufphatemethod
2 Minimum massof preliminary sub-sampletor
total sulphatecontent method 6
3 Precisiondata,water-solublesuiphate
det€rmination 10
4 Precisiondata.total sulphatedetermination 10
5 Hesultsexcluded{rom calculationof precision
data in table 3 11
6 Resultsexcluded from calculation of precision
data in table 4 1l
Figure
1 lon-exchangecolumn for water.solublesulphates 4

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BsI BSxgIa PARTxllg
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Methods

3,2 Methodlor total sulphatocontent

1 Scope sampleof
from a crushed
Thgsulphates areextracted
f or aggregateby dllutehydrochloric Barium
acid. shloride
ThisPartof BS812 des*ibestwo methods
detormining the suIphate contentof aggregates. solutionisadded10the oxtract.The precipitate
o{ barium
sulohate dried
is collected, and weighedandthe total
Thefint methoddetermines the water-soluble sulphale
which applies to natural and sYnthetic sulphatecontentis calculated.
content of aggregates,
aggregates to be usedasdrainage materials or for fill or
hardeore,e,g.unboundroadbases or sub'bases or
foundations. 4 Sampling
Thesecond methoddetermines the total sulphate content
to beusedtor the test (thelaboratorysample)
o{ aggregatps. whichapplies to aggregates usedin concrete Thesample
shallbet€kenin accordance with the procedure described
andcementboundmaterials. i n cl ause5 of B S812 : P art102| 1984.
NOTE 1. The secondmethod {or the detefminationof total
sulphatebv acidextractionis speclfledas h is impracticalto Ensure that thesampleis representative of the moisture
producea methodlor the determinstlnof totol water-solubie contentaswell asthe solidsby preventing lossof moisture,
sulphatebecause of low hjatersolubility of calciumsulphste. exceptthroughevaporation, lhroughoutthe sampling
For practicalpurposeslor EggregEtes ln concretethe total !ulphatg
procedure stageup to the point
contsnt dotermingdby this method is taken to be the sameas the
andat anysubsequent
total vvater-soluble
suIphateognlenl. of test.
N O T E 2 . I n a p p s n d l xA t w o F r o c e d u r eI so r a s e m i - q u a n t i t a t ilvees t NOTE. This is nscessarv because wherethe aggregate to be tested
are described,lt is stronglv recommendedrh;1 one ot these is used carrlessurfacewater the sulphateswill normally be dissolved,
as a prgliminarvcheck betoreresortlngta the test describedln the at leostpartly, in both this and ths absorbsdu,/aterand hencethe
main text, vvhichmay b€ neededlor compliancewith a specification, sulphatecontentwill be affectedby migratiotiof ,,aaterthrough
the bulk matcri6ls,
NOTE 3. The titles of the publicationsre{erredto in this stsndard
6re li3tedon the insidoback cover.

5 Determination of the sulphatecontentof

2 Definitions
F o r t h e p u r p o s eos f t h i s P a r to f B S 8 1 2 , t h e d e f i n i t i o n s
g i v e ni n B S8 1 2 : P a r t 1 0 1 a n d P a r t 1 0 2 a p p l y ,
a 2t1w ater/ aggregate extrast
NOTE. Calciumsulphateis relativelyharmlessbecauseof its limited
solubilityand th€ oxtractionconditionshavebeenchosengo that
aggregates containingonly calciumsLllphateare ciassitiedas tsJling
i n c l a s sI o f t a b l e6 . 1 i n B S8 1 ' 1 0: p a r t I : 1 9 3 5 .

3 Principle 5.1 Apparatus

3.1 Method{or wator-soluble sulphates 5.1.1 Apparatusfor preparationof testportion and

extractionof the sulphate(see5.4 and 5.5.1)
An aggregate sampleis extracted witlr twiceits own mass
of dis t illed
or de mi n e ra l i zweadte rto r€ mo vwe a te r-sol ubl e5,1,1,1Wellventilated oven,oapable of beingcontrolled
sulphate ions.Thewater-soluble 'C.
sulphate contentis to mai ntai an temperature o{ 105t 5
determined by eitheran ion-exchange methodor a gravi-
metricmethodin oneof the followingways. 5.1,1.2Ealance, capable of weighingup to 5 kg accurate
to 5 g. The balance shallbe regularlycalibrated asspecified
(a)Someof the extractlstransferred to an ion.exchangei n B S5781r P art1.
oolumnandthe eluateis titratedwith standardized
sodiumhydroxidesolution. 6,1,1,3Testsleve.20 mm squareholeperforated plate
compl yi ng
w i th B S410.
lb) Someof the extractis treatedwith dilutedhydro.
chloricacid.Barlumchloridesolutionis addedandthe 5,1,1,4 Pestleandmortar, or suita5lemechanicalcruslrer.
precipitate is colleoted,driedandweighed. N0TE, Thjs is not requlredfor sggregateall passingthe 20 mm sieve.
The ion-exchange methodmeasures tho presence of 6,1.1,5Two plastics or metalbottles,wide-mouthed,
sulphate ions.Whenotheranions{seenote)arepresenr this screw-capped,
The bottlesshallbe 5 L capacity when
methodis precluded. Thegravimetric methodis applicable
(i,e,slags) testing coarse aggregates or 2 L whentestingfine aggregate.
whenaggregates containing sulphides are being
analysed, 5.1,1.6 Mechanicalshakers or rollen. to take the extrac-
NOTE. Anion6o{ strongacidr,€.9.chlorides,njtratesand phos- ti onbottl es(5.1.1.5).
phates,Interferewlth tlre ion.sxchange
method and sre eppsrenlly
measurodassulphato,Howav€r,\ ,henchlorideis the only other lon 5,1,1.7 Twofilter funnels,of approximately
100mm
presenl,and it hasbEenquantitativelydetermined,the ion-exchange diamsterwith mediumgrade'filter papersof a diameter
method describsdcan be usedprovidedthe resull is correctedas to the sizeof the {unnel.
appropriate
shownin 5.6,2.

*WhatmanNo. 40 havebeenfound suitable.

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 B S I B S x A l , e P A R T * l , l , gA B I thaqtbl 00aeq15 0 I
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5.1,1.8Seakers. 5,22,4 Nitric acid {c(HNOa)= approximately 1 mol/L),

5,1.2 Apparatusfor the ion-exchange
rnethod(seeS.3 madeby dilutingl5 mL of concentratednitricacid
(relative
density1.42)to 100 mL with water..
and5.5.2,1)
5,1,2,1Pipette,S0mL slze.gtad€B in accordancB 5,2.2,5 Sodiumhydroxidesolution (c(NaOH)= approxi-
wit h B s 179 7 . mately0.1 mol/Ll. madeby dissolving 2 g of sodium
hvdroxidein 500 mL of water,Determine the exact
5,1.2,2 An ion'exchange
columnand reservoir. concentration(in mol/L) by titrationagainst potassium
NOTE.A iypical dosignis shown in ligure 1. hydrogenphthal€te or with a standardized acidsolution,
5,1,2,3Conica!ftasks,5oo andkeepthe solutionin an airtightplastics container
mL capacitv,At leasttwo
arerequ{red. { 5.1.4.1).

5.1,2.4 Graduatedmeasuring
cylincler,capacity100 mL, 5,2,2.6 lndicator,givinga distinctcolourchangein the
gradeB in accordance pH range4 to 5.
with BS 1797.
NOTE. Scroenedmethyl orangeis suitable,
5,1.2,5B%ette,50mL size,gradeB in accordance
wirh Bs 1797. 5,2.2.7 Silvernitratesolution,madeby dissolving0.Sg
of silvernitratein 100mL of water.Storethe solutionin
5.1.2,6 Beakars. an amber-coloured glassreagentbottle{5.,1.4.2),
5,1.3 Apparatusfor the gravimetricmethod (see5,5,2,2)
5,3 Preparationof the ion"exchange
column
5,1,3.1Plpette,b0 mL size,gradeB in accordance
with NOTE. This procedursis not requiredif the ion-exchange
B S17S 7. column
method is not ured (ses8,11.
5,1.3.2Apparatus
aslist€din 6.1.2.1to 6.1.2.10, 5,3,1 Empty a quantity of cation-exchange resjn (b.2,2.1).
s u f { i c i e nt o h a l f . f i l lt h e c o l u m n ( 5 . 1 . 2 . 2 ) i,n t o a
5,7,4 Apparatusfor prcparationof reagents(seeS.2,2) beaker(5.1.2.6)and stir witn water. Empty this suspension
5,1,4.1 Plastics o f r e s i ni n w a t e r i n t o t h e c o l u m n s o t h a t w h e n t h e r e s i n
cantaineLaittight.
hassettl€d,there is approximately20 mm depth of water
5,1.4.2 Amber-coloured
glassreagentbottle, abovethe resinwhen the surpluswater has drainedawav.
Maintainthis depth of water abovethe resinat all times
5,2 Reagents as it is jmponant that the resin is not allowedto drv out.
5,2,1 General. Roagentsof recognized
analytical
quality 5,3.2 Activate the cation-exchange resin by leachingwith
andonly distilledwateror waterof equivalsnr
quatitytirall I00 mL of the hydrochloric acid solution lS,Z.Z,Z|
be used. followed by washingwith distilled wster, placethe acid
NOTE 1. Whereaccurarelystandardizedsolutionsare required in the reservoirand leavethe apparatusuntil the acid has
i1
may be morBconvenientto obtaln them 6lreadystandardjzed passedthrough the column. Fihse ahd fill the reservoir
- to
'-

o b€ usedin accordance with the manufscturor,sinstructions.

NOTE 2, ll the ion.excharg6cgrumn method ls not used,
ths reagemsdescribedin S.2,2.1to 8.2.2.7are not required.
with distilledwater and leavethe water to percolate
through until the liquid coming from the column givesno
turbidity when testedwith about 1 mL of silvernitrate
5,2,2 Reagents sofution (5,2.2.7j acidifiedwith about five drops of nitric
5,2.2,1 Cation"exchange acid (5.2.2.4).
resin,stronglyacid*.
5.2,2.2 HydrochlorJc 5.3,3 Regeneratethe cation-exchange resin in the m66ns1
acJdsolution (c{HCl)= approxi-
describedin 5.3.2 after it has been usedfor lour
mately4 mol/L).madeby diluting360 mL concentrated consecu_
tive determinations.
hydrochloricacid(relative
densityl.1g) to I Lwirh
water.
5.2,2.3 Hydrochloricacidsolution,madeby diluting
20-0-mL concentratedhydrochloricacid (relativedeniity
. 1,18)to 1 L with water.

'A sultablemsterial
is Zerolit 22S or Amberlite 1R -120.

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IilonJun0815:12:39'1998
 9 9 1 g 5 x A l , ? P A R T * 1 , 188S t lbeqbhl [oaeqlL a r
t 1 8: 1 9 8 8
B S8 1 2 ' :P a r 1

' 1 9 l 2 6s o c k e t
( n o t f e q u i f e di f
c o n s ta n fh e o di s
n o f u s e d)

o
E

(otion-exchonge =
resin

6 l q s s v io o l p o d

Rubbeb
f ung
bofed to toke
gtosstube

l a l l o l | - e l c h a n g ec o l u m n

2tt129slopper

R o u n db oi fo me d Glqsstubefused
f{ o s k 5 0 0 rn l sideof ftosk to
cqPoqry providestobilify

{bl Consrantheaddevicefor use!"vithion'exchange column

A l l d i m e n s i o nasr e i n m l l l i m e r . e s .

Figure1. lon-exchange
columnfor water-soluble
sulphates

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 B S I B s x 8 l e P A R T * I I AS A I theqbbl 0oeaqt? q I
B S8 1 2I P a r1t 1 8 :1 9 8 8

of test portion
5,4 Preparation 5,5.2 Determinationol the sulphatein the extrccts
5.4.1 Dry the laboratorysampleat a temperature 5,5,2.1 lon-exchange method.With a pipette(5.1.2.1)
-C transfer50 mL o{ filteredextractto the top of the
of 105r 5 to removesurfacewaterso that the sample
isfreef lowing. ion-exchange columnandallowto drainthroughthe
resi n.
5.4,2 Beducethe laboratorysampleby the procedures
describedin clause6 of BS812 r Part102 : 1984to an Rinsethe resinwith two 75 mL increments of distllled
amountnot lessthanthe massgivenin tableI appropriate watercollecting all the solutionandwashingsin a conical
to the nominalsizeof the aggregate. flask(5.1,2,3)placedunderthe outletof the cojumn.
Add threeto {ivedropsof the indicator(5.2.2.6)ro rhe
contentsof the conicalflaskandtitrateto the colour
Table1. Minimummassof preliminary sub.sample change with the standardized sodiumhvdroxide
for water.soluble
sulphatemethod solution(5.2.2.5).
Notnih6lmaximum siz€ Minimum mEssof
Replace the flaskunderthe outletof the columnandpass
of 6ggregate Bub-sample a furth8r75 mL of distilledwaterthroughthe resin.lf the
ihdicatorcolourchanges to showthat moreacidhasbeen
mm ks washedfrom the resin,titrateagainto neutrality.
63 50 Recordthe total volumeof standardized sodiumhvoroxide
50 35 s o l u t i o nu s e d( v 1 ) .
40 15 Repeatwith another50 mL aliquotof the fjltrateand
28 or less F recordthe volumeof standardized sodiumhvdroxide'
sol uti onused(vr).
5 . 4 . 3 S i e v et h e s u b , s a m p lteh r o u g ha 2 0 m m s i e v e{ 8 , 1 . 1 . 3 ) Takethe rneanvalueof vr andh IVI,
and crush any oversizeaggregateto passthe sieveavoidino lf the valuesof v1 and rz2diffcr by morethan0.b mL
excessive grinding.Combine,mix thoroughly and by suita'ble repeatthe procedure.
samplereductiontechniquesproducetwo test oortions
Repeatth€ completeprocedure with a secondtestportion.
eachoi about 2 kg massfor coarseaggregate or two test
portionseachof about boo g nrassfor sand.Dry 5,5.2.2 Gravimetricmethod. TransfergOmL of lilter€d
the test
p o r t i o n sb y h e a t i n ga t a t e m p e r a t u r €
o f 1 0 St b . C t o extractto a 500 mL beaksr,diluteto 300 mL with ciistill€d
achieve a d r y m a s sw h i c h i s c o n s t a n t o w i r h i n 0 . 1 % . or demi neral ;zed
w ater,addl 0 mL of hydrochlor acid
ic
solution(5.2.2.3)and carryout the procedure
described in
5.5 Analytical procedure 6.4.2to 6.4.9.
5.5.1 Preparation of extracts NOTE,Whenaggregales containing
sulphide
arebeinganalysed
seethe noteto 6,4,?.
5.5,1,1 For coarseaggregates usethe two plasticsor metal Repeatthe procedurewith a secondtest portion.
bottlesof 5 L capacityand for frne aggregareusethe two
bottlesof 2 L capacity (8.1,1.S).Weigheachbottle 5.6 Calculationand expressionof results
and
record its massto the near€st E g.
5.6.1 lf no other anionsare present,calculatethe
6.5.1.2 Transferthe test portions obtainedasdescribed concentrationof sulphaleions, (asSO3 in g/L), present
in 5.4 to the bottles,weigh bottle and contentsand record in the extracts,from the equation:
their massto the nearestb g. Calculatethe massof
concentrationof SO. = g.g, y
aggregate in each bot e by difference.
where
S.5.1.3 Add to eachbottle a massof distilled or
V l s t h e v o l u m eo f s o d i u mh y d r o x i d es o l u t i o n( i n m L ) j
demineralizedwater equal to twice the massof the
test rn is the concentrationof sodium hydroxide solution
portion. Fastehthe water-light bottle
closuresand mix the
contentsby shakingor rolling continuouslyfor (in mol/L).
a minimum
ot 24 h, 5.6,2 lf chloridesare the only other ions pr€sent.calculate
NOTE.lf mochanicat agitationequipment is not used8ndthe the concentTationof sulphateions, (asSO3 in g/L), present
Sampleandwateraremerelyallowedto r€mainin contaotr^ith
occasio.nal in the extractsfrom the equation:
shaklng therelsa possibllity
(pErticularly If thesource
or.surpnate-
is,tor example, largecryst6lsof gypsuml.thatthe concentrationof SO3 = O.8mV - 5,64C
*n"n courdtheorolicav dissotve witi not a beexrracted
i;,51T: where
C is the chloride ion content as a percentagebV mass
5.5.1.4 Filter the extractsthrough dry. medium_grade
of dry aggregate.
filter papers(5.1,1,7)until at least 100 mL of cleir
filtrates
havebeencollectedin cleandry beakers(S,1.1.g).

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 BSI BSX81E PARTXll6 s6 I thaqtbS 0Baaqla b I
B S8 1 2 r P a r t1 1 8: l 9 B B

5,6.3 Whenthe gravimetric methodhasbeenused, 6.1.2.8 lgnition crucibles,approximately35 mm in

calculatethesulphatsconcentration of sulphateions, diameterand40 mm in heightandca_pable of maintaining
(asSOr in g/L),prossntin the extractsfrom the eguation: a constantmasswhsnheatedto 800'c,
NOTE, These ar€notrequired
crucibl€s crucibles
il theliltering
concentrationof SOs= 6.86m2
areused-
1.6,1,2.7) silicaor platinumaresuitable
Porcslain.
wnsr6 forignltion
materials crucibles.
m2 ls the massof precipitate obtainedin 8.4.9(in g). 6.1,2.5 A suitahlemeansof ignitingthe Necipitate,
5.6,4 Express the meansulphate contentsof the 2:1 preferablyan electric-muffle furnacecapable of reaching
-c.
extracts 0.1 s/L. lf the individualresults
to the nearest andmaintaining 800
differby morethan0.1 g/L and11, (calculated from 8.5) 6,1,2,10D$sicator.
r€peatthet€ststartingwith newanalytical testportions
(see5,4). 6.1,3 Apparatusfor preparationof reagents(see6,2,2)
NOTE.With aggregates contsiningdiscretecrystalsot gYpsumit
6.1,3.1 Amber+olourcdglassreagentbottle,
rnay bo difficult to obtEincloseagreementbetweenindividusl
t€st portions.
6.2 Feagants
6.2,1 General. Reagentsof recognized qualitv
analytical
6 Determination of thetotal sulphate quality
andonly distilledwateror waterof equivalent
contentby acid extraction shallbeused.
6,2.2 Reagents
6.1 Apparatus
6.?.2,1Bariumchlorde,5 % solution,madeby dissolving
8,1,1 Apparatusfor preparationof testporflon (see6.3) 50 g of bariumchloridein 1 L of watsr,andfilteredbefore
6,1.1,1Wellvehtilatad oven,capable of beingcontrolled useif necessary.
a t em p e ra tuoref 1 0 5t 5 " C ,
to m aint s in 6.2.2,2 Dilutehydrochloricacid.madeby dilutinq 100 mL
6,1,1,2Ealance, capable of weighingup to 5 kg accurate of concentrated hydrochloric acid(relative
density1.18)
to 5 g. Thebalance shallberegularlycalibrated asspecifisd t o l L w i t hw a t e r ,
i n B S5781: P ar t1. 6.2.2.3 Silvernltratesolution,madeby dissolving0.5 g
6 ,1 . 1, 37' esstr ev e2q0 mm,5 mm, I mm a n d1 b 0u m of silvernitratein 100mL of water,Storeth€ solution
co m ply ingwit h B S4 1 0 . in anamber-coloured glassreagent
bo11le{6.L3.1).
6.1.1.4 Pestleandmortat,or suitablemechanical crusher. 6,3 Preparation of testportion
6.1.2 Apparatusfor analysisof testportion 6.3,1 Dry the laboratorysample6t a temperature
-C
6,1,2,1Balance, capableof weighingup to 100g accurate of 105t 5 to removesurface waterso that the samDl€
to 0,001g, Thebalance shallberegularlycalibrated
as isfreeflowing.
specifiedin BS5781: Partl. 6.3.2 Reduce the laboratorysampleby the procedures
8,1,2,2Beakers, capacity250 mL andb00 mL. described in clause 5 of BS812 : Part102 : l9B4 to an
amoufitnot lessthanthe massgivenin table2 approprlate
6,1,2,3 Electrichot-plate.capable
of beingcontrolledto to the hominalmaximumsizeof aggregate.
boilthecontents of beakerswithoutcausing undue
ovetheating, Table2. Minimummassof preliminary sub-sample
6,"1.2,4Fumecupboard. for total sulphatecont6ntmsthod

6.1,2.5Twofilter funnels, of approximately 100mm Nominrlmaximum

sirs Minimum mals of
diameter with mediumgrade*andfine gradeffilter papers of r!gr€0st6 sub-tsmFlo
of a diameterappropriateto the sizeof ths funnels.
6.1.2.6 Droppingpipette.capacity10 mL. kg
F.!

8,1,2,7 Sintercdsilicafilteringcruclb/ds,porositygrade4, OU 35
approximatelv 35 mm in diameterand40 mm in height, 40 t9
NOTE. Theseare not r6quiredif filtration through fine gradel z6
{ilter papersis preferred.
20 2
14 1
l0 0.5
5 or less o.2

'Whatman No.40 is suitable.

but fine filter papor,€.g.Wralman No,42 may tle necessary
if the tiltrate is not comptelelvcE4
tWhatmsn No, 42 is !uitable.

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 B S I B S x B l , A p A R T * l , l , gA B I t haqbbg 0Deeqlt I t
B S8 1 2: P a r t1 1 8: 1 9 8 8

6.3.3 Sievethe sub.sample througha 20 mm sieve{6.1.1.3) 6.4.3 Boil and add 10 mL barium chloride solurion
andcrushanyoversize aggregate to passthe sieve.Combine. (6.2.2.11dropwisewith constantstirring, Continue boilinq
mix thoroughlyandwherethe masso{ the sub-sample until the precipitateis properly formed and then let the
exceeds 2 kg reducethe sub-sample to 2 kg. Dry the sub- solution standat just below boiling point for at least
sample by heatingat a temperature of 10bt 5 oCto 30 min then leaveto cool for 24 h or overnight.
achieve a constantmassto within 0.i %.Crushall the
aggr€gate to passa 5 mm sieve,mix andreduceto not less 6.4.4 Transferthe precipltateof barium sulphatewith
than200 g, crushall the aggregate to passa 1 mm sieve extremecareto a previouslyignited and weighedsintered
andproducea sampleo{ approximately 100g andgrindall silicafilter crucible (6.1.2.7)usingsuction. Alternativelv
thrsto passa 150prnsieve.Th;s,sthe lest portion.Carry transferthe precipitatewith extremecareto a suitab,e
outall s a mp l i nre
g d u c ti obny th e m e th o ddescri bed
in filter paper in the glassfunn€l and filter.
c t aus6eo f BS8 1 2 : p a rt 1 0 2: 1 9 8 4 .
6,4.5 In eithei casewash the precipitateseveraltimeswith
NOTE. With suitablemechanic6lgrlndingequiprn€nt
it is possible hot distilledwater until the washingsare free from chloride
ro oy-passsome of thesestages.For example,a jaw_crusher
co!ld as indicatedby an absenceot turbidity when a drop is
Deusedto crush6ll the sub_sample to pass6 mm without the
prerrrninary sjevingand crushingat the 0 mm size.Simllarlv tesredwith rhe solurion of silvernluate it a
the 16.2.2,31.
zuu g sup-sampleportion passinFthe 5 mm s i n t e r e ds i l i c af i l t e r c r u c i b l ei s u s e dr e m o v ei t f r o m
sievecould be crushed tne
to pzss1.50pm, by-passing the 1-mmsizeoperation,i^. ;;;;;.;", f i l t e r t l a s ka n d d r y a t l O b r S . C f o r a p p r o x i m a t e l v
a discmill. The intention is to prooucea
test portion whicn is
S0 min
ru||y representative and graduallyraisethe temperatureto 900.C either
of the laboratorys6mpte. in an
electricmuffle furnace or by other suitablemeans
{6.1.2,9)
bC
6.4 Analyticalprocedurs u n t i l n o f u r t h e r l o s si n m a s so c c u r s ;I b m i h
at g00
should suffice.
6.4.1 Welghaccurately to the nearest 0,001g Ebout3 g
of the.testportion(prepared 6.4,6 Cool the crucible in a desiccator
asdescribed ln d.S)anO " 16.1.2.10)and
r ec or d
t h e m a s s(mrl . p l a c ei t i n a 2 S 0m L Ueater(e.t.Z,Z), weighto the nearest0.001 g, and calculateth. rna$ of rh.
t90 of the ditutedhydrochtoricacid16.2.i.2) precipitate{m, ) from the increasein
:11 sur.Ta massof the crucible-
ano Hspeatwith a secondduplicate3 g of the
te;t 6.4.7 lf the precjpitateis fjltored through
portlon,andfollowthe procedur€ a filter paper,
for bothl transferthe filler paper and precipitateto previousiv '
containrng a
,T1,15-l: T9:="", sisniticant amounts of csrbonates r g n l t e da n dw e i g h e dc r u c i b l e( 6 . 1 . 2 , 9 ) .
wfl.troth at this
stage.In thesecasesadd rhe ac;d slowly
conllnLtously wiriie-
stlrring. 6.4.8 lf an electricmuffls furnace is used,place
the
containinssutphidewlt reteaseH2s crucibleand content in it at room temperature
l-?,t,5 3:19"*:*
scrdrrication on and
and this vJillbe noticeableby ,c.
there is a dangerthat this pro6edure
its smelJ.In thesecases sraduallyraiserhe temperarureto 8o0 lil ir"""
will afi" ,rrpi"il o r o t h e r b u r n e ri s u s e d ,f i r s t d r y t h e
contentbecauseol sulphideoxidation. "**"rrn"," iilter p"p.;;;;
prectpttate s l o w l yo v e ra s m a l lf l a m et a k i n gc a r et o
lf aggregatescontain sulphide, placo char
,the 100mL of the the tilter paper slowly rather than to
dilutedhydrochloric acidin a ZSOmf- Oeat<er allow it to inflame,
anJtreai someof the precipitatemay be lost,
to boilingpoint. Remove lrom tho sourceot f.,.li,nJ, :]:,tti:'" y and
graqua raisethe temperatureto red heat.
whilestirrjngtheacidsolution,sprinkle
theweigheJ NOTE.lgnitionior about1Smin shourd
onalytical poftionof about3 gmasson besufficientin all csses,
to the acid.
6.4,2 Heatto boilingandsimmergently rh€ mass of the precipitate obtained (m,
for ?Em;n in a :,.:,.:.:^"',:1|-1,:
rrorl.tle rncreasein mass(to the nearest0.00,| )
fumecupboard(6.1.2.4i.Fitterthiough...oim
iiir.i' crucible. s) of The.
pa!.er(6,12.8).Ensure that the fiftr.r" ir.f."i.ll n.t,
refilterwith a fine filter paper.Wastr
ttrorougity*iii'i.,", 6.5 Galculationand expressiono{ resolts
y*. Coilectthe fittratsandwashinss in a
litli,ji
cuu.mL beaKer(6.1,2.2)anddilute
to 300 m L with C.l:11"" rotatsutphate
content,
asa percentase
distilledwater- 9:ll
by rnassof lhe
the dry aggregate,
ftom the equation;

ag^greg€ts
il*:i:,:'Jl;il:,,
ffi [irl*m,-",ifi""*H:,if *"
containr sutphides (e.g.stassl. Wf,un
,u.n Jgg;"s;u;'-
Percentageof SO. =
m2 x 34.3
n7r
are Derngtested,slsnd rhe solution
in a wur. ptacefli s6 min
afrersimm€,rihg.|| a \,,/hiteprecipitaruO*ufop,, tfft"iif,roug;i' 6,5.2 Express the meantotal sulphateaontentof the two
a mediumfilter paperand wash thofoughly test portionsto the nearestO.01% {asSOa ol
wirh hot distille"J
watet and continue os describedin 6.4.S. ' } tnu Jiy
massof aggregate. Repeatthe teststa*ingwith newi
portionsif the individualresultsdiffer 9
Lnuly]i"rt by mJre
than0.05% (SO3l.

lopyrightbytheBritishStandards Institution
Llon
J u n0 81 5 : 1 2 : 3 9 ' 1 9 9 8
 l h a q h b l 0 0 a e 5 B 00 I
e S f A S * A l , a P A R T x l , l , g8 8 I
B S8 1 2 : P a r t1 1 8 : 1 9 8 8

o
7 Precision I TestrePoft
Th€testreportshallaffirmthat the sulphate contentwas
experiment
7.1 A precision wascarriedout on five
Detailsof the experiment derermined in accordance with this Partof BS812 andstate
by 1o laboratories.
aggregates
whetheror not a certificate of samplingis available'
andthe precisiondataaregivenin appendixB'
(f avsilable,a copyof th€cortlficateof sampling shallbe
7,2 Theusesof the precision dataaredescribed 5
in clause provided. Thetestreportshallincludethe following
o f B S812I P ar t10 1I 1 9 8 4 . iniormation i
i a)sampl iedenti {i cati on;
(b) thesulphate contentin glL ol a 2:1 water/aggregate
exlractexprsssed in glL; and/or
(c)the total sulphate contentexpressed asa percentage
by massof the dry aggregats,

Copyright bytheBritishStandardsInstitution
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39 9 8
 B S I B S x g l e P A R T T l l AS g t l , h e q h L l0 0 a a 5 s I A I
B S8 1 2: P a r t1 1 8: 1 9 8 8

Appendices

AppendixA. Semi-quantitative
test for the mix. lf there is no turbidity or it has not formed within
S s,
presenceof sulphateions assumethat the aggregat€containslossthan 0.02 % sulphare
as SO3.
NOTE.ThebEriumchloridetestisverysensitive andanobservable
A.1 Apparatusand reagents will eventuay form (afte,approximarely
tu.rbidiry 1 mio),even
h/henthe SO3 content of the aggregete is only O.OO4 %. tt is also
A.1.1 Apparatus for m€thod1 or method2 (seeA.2.Zl necesSarytO ensurs that the Water used for tesling does not contain
sufficientsulphates(< 20 mg/L) ro give a posjtiveresult.
4.1.1.1 Pla.stics
bucket capacity10 L.
4,1.1.2 Beakeror plasticsdrinkingcup.
AppendixB. Detailsof experimentsfor
A.1.2 Additionalapparatus
for methodZ determiningprecisionof testsfor
4,1.2.'l Filterpaper,mediumgrade{. water-solublesulphateand total sulphate
4,1,2,2 Beaker,capacityb00 mL. contentsof aggregates
4.1,2.3 Testtube. 8.1 The precisiondata given in tabiesg and 4 were
determinedfrom an experimentconducted in 1994/b
A.1,3 Reagent
for methodl involving10 laboratories,The experimentwas designed,
and the data analysedfojlowing the princjplesset our
4.1,3.1 Sulphatereststzbst.
in BS 5497 : Parl 1 I 1979.
A,1.4 Reagents
Jof method2 8.2. The materialsusedwere approximately 200 kg lots.
With each material,twenty g kg to t0 kg iaborator-y
4.1,4.1 Hydrochlorjc acidsolution,madebydiluting samples
200 mL of concenirated were preparedand two sent to each laboratorv.
hydrochloricacid(iel3tive The laboratoriesdivided each laboratory sampleinto Jour
d e n s i t1y . 1 8t)o l L w i t h w a t e r
test portions: one was usedfor the chlorjde determination
4.1,4.2 Bariumchloridei o/o solution,madeby dissolving d e s c r i b e di n B S 8 1 2 : P a r t 1 1 7 , o n e f o r t h e w a t e r - s o l u b l e
50 g of bariumchloridein 1 L of lvater,andfilteredbefoie sulphatedeterminationand two for the total sulphate
use,if necessary, determination d e s c r i b e di n t h i s p a r t o f B S g 1 2 .
4.1,4.3 Measu
ring cvli nder. 8,3 The testsfor outliers given in BS b497 : part I : 197g
were appliedto the data. A summary of the resultsshown
4,1.4.4 Stopwatch.
to be outliersby thesetests is given in tables5 and 6.
B-4 Becauseof the small quantitiesof the aggregates
A,2 Procedure obtained for this experiment,the estimatesoi y" rnrurur"
only that variability which ariseswhen dividing iOO tg to
approximarely 200 kg of materialinro 5 kg to 10 kg laboratoiy r".pi",.
1'11 6 kg ot coarseaggregate or 1 kg Likewisethe contribution of
oTs a n,tl*:
drn th eb u c k e (A.1
t .1 .1a) n da d dan equi val ent samplereduction variabilitv
mass- to the estim8tesof V7, consiss only
of wat€rof low sulphatecontent.Agitatethe contents of the variability
Intermittently which ariseswhen div'rdingb kg to 10 kg laboratory samples
for 7 h andthen poursomesolutioninto a
DeaK eo r p ta s ti cdsri n k i n gc u p(A.1 ,1 ,2). into two test portions. In practiceone might expect ys
and perhapsyrt to be largerthan found in this
4.2,2 Carryout oneof the followingprocedures. expenment.
Method1. Allow anysolidsto settleandbriefly
dip the 8.5 The precisiondata Jrom table 3 (water-soluble
sllph€teteststrip{A.1.3,1}into the clearsupernatant sulphate)for four of the materials(limestone,shale.
liquld.After 2 min observe the colourationof the three graveland sand)fit the following relationships:
testzohes.lf noneof the testzoneshaschanged from rt = 0.02 + 0.05 i
redto.yellowthe sulphatein the aggregate canbetaken
to be lessthanO,O2yo. f r r = R r = 0 . 0 6+ 0 . 1 1i
Method2. Fjlterthe solutionthrougha mediumgrade Thesemay be usedto int€rpolatevaluesof rt , ,91 and g2
f ilt erp a p e (A
r .1 .2 .1u) n ti ta p p ro x i ma tel
50y mLi otuti on for levelsof sulphateion (FglL) betweenthose which
nasbeencollected.Measure S0 m L into a 500 m L appearin table 3. The blastfurnaceslaggavea higher value
beaker(A.1.2.2),add lb0 m L waterandstir rhoroughly. of 81 and ,92 rhat that predicted by the relationshiD.
Poursomeof the dilutedsolutioninto a testtube T h i s i s a t t r i b u t e dt o t h e p r e s e n c e
o f s u l p h i d e st:h i s d i f f i .
ta,f .'Z,gt
sothat it is half filled,add5 mL hydrochloric acid(A,1.4.11culty is overcomeby following the proceduredescribed
and5 to 10 dropsbariumchloridesolution(A,1.4.2) in the note to 6.4.2.
and

'Whatman
No. 40 hasbsen found suitable.
TMerckquant test stripshave beenfound suilable.

Copyright by the BritishStandards Institution

M o nJ u n0 81 5 : 1 2 : 3 9 1 9 9 8
 BSI BSx6Ia P A R T x I ' l , g8 8 I l,beqbhl 00piS0e q I
B S8 1 2r F a r t1 1 8: 1 9 8 8

8.6 Theprecision data{romtable4 {totalsulphate}

fit R2 = 0.05+ 0'58x
the followingrelatlonshiPs: Thesemaybe usedto interpolatevaluesof 11, B I and82
r r = 0. 03+ 0. 01r for levels thosewhich
ion {x %) b€tween
of sulphate
B, =0.06+0.49F appear in table4.

sulphatedetsrmination
data,water-soluble
Table3. Precision

Aggr€0a1q Sulphatolon g/L

n rl 81 R2 ,/ v"
nn?
1 4 m m lightgr eyl i m e s to n(D e) I 0.01 0,01 0.03 0.003 0.010 0,003
1 4m ms ea' dr ed ggera d v eal n ds a n d(B l I 0 . 1 4 0.04 0.05 0,06 0 . 0 1 5 0 , 0 1 2 0.004
5 mm mediumgreylimestone crushed
sand/shell mixture(E) s o . 1 7 0.03 0.13 0 , 0 1 1 0.045 0,000
1 4m m blas t f ur n asclea g(A) I t.rt I 0.10 0.60 0.62 0.035 0.210 0.065
28 m mc ollier sy h a l e{ C } 8 2,13 0.12 nto o.29 0.041 0.095 0.000

NOTE.n is lhe numberot laboratorieswhoseresultswere includ€din the calculationoJ the precisiondata, Definitlonsoi I, rl
R 1 ,R 2 , V r , , t / L a n d t / s a r eg i v e ni n 5 . 2 o f B S 8 1 2 i P a r t 1 0 1 ; 1 9 8 4 ,

Tdble 4. Precisiondata,total sulphatedeiermination

Aggr€0ato S!lphoto i on %

rl R1 Ra

14m m lightgr eyli m e s to n(D

e) I 0.02 u,uz 0.06 0,06 0,008 0 , 0 1 9 0,006
gravelandsand(B)
14mm sea-dredged
5 mm mediumgrey(imestone
m ix t ur e(E)
s and/ s hell
crushed
9

I
0.08

0,28
0.05

0.03
0.18 0.18

0,14 0,' 14
0.017 0.062 0.000

0.012 0.049 0.014

o
14 mm blastfurnace slag{A) I 0.52 0.04 0.28 U.OU 0 . 0 1 5 0 . 1 0 0 0.034
28 m m c ollier s
y h a l e(C ) 0.80 0.04 0.50 u.c/ 0.015 0 , 1 7 7 0,098

NOTE,n is the numberof laboratoricswhole resultswere incl!ded in the calculationof the proci3iondata, Dofinitiongo{ t fr
R 1 , 8 7 , V r | V 1 a n d V g a r eg i v e ni n 6 , 2 o f B S 8 1 2 ; P a r t1 0 1 : 1 9 8 4 .

Copyright bytheBritishStandatds Institution

M o nJ u n0 8 1 5 : 1 2 :13999 8
 B S I B S x S t , e p A R T x l , l ,8AS I l b e q b b j 0 0 a a 5 0 3h
B S8 1 2I P a r t1 1 8:

Table5, Resultsexcludedlrom calculationof preclslondatain table3

L2
L3 Alsoexcluded
l2
tl Outlier
rl
LJ Outlier
L3 D Alsoexcluded
L3 Outlisr
L4 E Outl i er
LI D UUIIIET
L9 A O u t li e r ( 6 p o i l e ds a r n p l e s )

Table 6, Resultsexcludedfrom calculationot ptecision

dato in table 4

L1
L3 A Ou tl i e r
L.' o Alsoexcluded
t3 c Alsoexcluded
O u tl i e r
ta
E O u tl i e r
110
Outlier

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Publications
referredto
BS4 10 Speclticationfor tEst siev€s
SS 812 Testingaggr€gat€r
*Pan 2 Msthods
for determlnstionof physlcElproperties
+Psrt3 Methods
for datermlns on of mecf,"ni"affi-p.rii.,
rPart 4
MEthods for determlnation of chemicot propeities
Port 1O1Guids to samplingand tesringaggregites
part 102 Msthodstor sampling
Part 117 Mcthod for determinatlonof wat€r-solublachloride
-- -salts
9! 1197 Tablsslor useih the calibrqtionof votum"tii" gi"""#-
BS 5497 Preclsionof test methods
*psatabilitvandreproducibifity
ror€ standard
tesrmethodby interlaboraiory
BssTsl i,Xjrlr*iT,iTJ::,fffi,Ti"."J::J-"rt 1est,
Part1 Spscificstion tor syst€mrequirementu
BS 8110 Slructuraluseof conciete
part 1 Codeof praoticefor
designand construction

rReferr€dto in
the foreword only. Under revision.

Copyrighlby the BritishStandards Institution

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8S812:Part118:1988
ThisBritishSlEndard, havlng besnprepar€d undsrths dir€ction
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of necessary dotailssuch6s symbolsand
the Cement Gypsum, AggregatesandouarryProducts Standards lize, typs or gradedesighations, Enquiriesshouldbe addressed to
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@
@
issuedsincepublication
Amendments
N
D a t eo f i s s u e Text a1{ected
"|-'
o)
3

:
(o
@
@

h t a n d a rIdnss t i t u t i o' n2 P a r kS t r e eLt o n d oW

B r i t i sS n 1 A2 B S, T e l e p h o n
0e1 - 6 2 9 0 0 0. T e l e x2 6 6 9 3 3

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