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ORE RESEARCH & EXPLORATION PTY LTD
Unit 23, 993 North Road,Murrumbeena,Vic 3163 AUSTRALIA
Telephone:61-3-95705300 Facsimile:61-3-95705221

CERTIFICATE OF ANALYSN FOR

GOLD REFERENCEMATBRIAL

OREAS 2C BATCH 2D3

Recommended
valueand95o/o limits
confidence
Constituent Recommended 95% Gonfidencelim:its
value
Low High
Gold,Au (ppb) 371 354 388

Recommended
valueandtolerance
limits
Constituent Recommen:ded Tolerancelimits
value 1-a=0,99,p=0.95

Low High

Gold,Au (ppb) 371 352 390

Preporedby:
OreResearch& ExplorationPty Ltd
Mav, 1994

REPORT2D
INTRODUCTION

OREAS referencematerials(RM) are intendedto provide a low cost method of


evaluatingand improvingthe qualityof preciousand base metalanalysisof geological
samples. To the analyst they provide an effectivemeans of calibratinganalytical
equipment,
assessingnew techniques in-houseprocedures.
and routinelymonitoring To
the explorationist
they providean importantcontrolin analyticaldata sets relatedto
explorationfrom the grass roots levelthroughto prospectevaluation.

As a rule only sourcematerialsexhibitingan exceptionallevelof homogeneityof the


element(s)of interestare used in the preparationof these materials.This has enabled
Ore Research& Exploration
to producea rangeof gold RM exhibiting
homogeneity
that
matchesor exceedsthat of currentlyavailableinternational
referencematerials.In many
instancesRM producedfrom a singlesourceare sufficiently
homogeneousto produce
a relativelycoarse-grained
form designedto simulatedrillchip samples.Thesehave a
grainsize of minus3mm and are designatedwith a "C" suffixto the RM identification
number.Thesestandardsare packagedin 1kg unitsfollowinghomogenisation
and are
intendedfor submission
to analytical
laboratories
in subsamplesizesof as littleas 2509.
They offerthe addedadvantagesof providinga checkon both samplepreparationand
analyticalprocedureswhileactingas a transparentstandardto the assaylaboratoryThe
moreconventional
pulpedstandardshavea grainsizeof minus75 micronsand a higher
degreeof homogeneity.
Thesestandardsare distinguished
by a "P"suffixto the standard
identification
number.

SOURCEMATERIALS

The materialused to producegold-bearingstandardOREAS2C Batch2D3 was taken


from the flanksof a mineralisedshear zonewithin Ordovicianflyschsedimentsin the
Blackwoodarea of centralVictoria.The sedimentarysuccessionhostingthe shearzone
consists predominantlyof medium-grainedgreywackestogether with subordinate
interbeddedsiltstone and slate. Hydrothermalalterationin the vicinity of the
mineraf
isationis indicatedby the development
of phyllite.The shearzone,in whichgold
gradesattaina maximum,is manifested
by foliatedsericiticand chloriticfaultgougeand
goethiticquartzveins.

Althoughno ore mineragraphy has beenundertaken


or scanningelectronmicroscopy to
determinethe natureof occurrenceof the gold,the very homogeneousdistribution
on a
mesoscopicscaleand uniformconcentration
gradientawayfrom the ore zone suggests
the gold is extremelyfine-grained Limitedpercussiondrilling
and evenlydisseminated.
indicatesthat sulphidesare rare to absentin the shearzone.

The majorand traceelementcomposition


of thisoxidised,quartz-veined
metagreywacke
goldore standardOREAS2C Batch2D3 is givenin Table1. The constituents
comprising
SiO2to Zr are the means of duplicateXRF analysesdeterminedat the Universityof
Melbourneusinga low dilutionboratefusionmethod,whilethe remainingconstituents,
As to Zn, are meansof at leastten replicateanalysesdeterminedvia INAAat Becquerel
Laboratories.

COMMINUTIOA
N N D H O M O G E N I S A T I OPNR O C E D U R E S

Approximately300k9 of the gold-bearinggreywackewas subjectedto the following


procedure:

a) primaryt crushing in a lurge (36 x 5Lt:m)jutr: t:ntsher


h) drying in a gasfred roturv drier
c) c:ru,sltingin u small (10 x 20cnt)jau, t:rusher
sec:ontdarv
d) tertiary crttshing in u pan mill
e) screening t0 mimts 3tnnt

Following
crushing,
the materialwas splitintoten equalsublotswhich
werehomogenised
separatelyin a tumble blenderfor two hours each A tenth splitfrom each sublotwas
then combinedand blendedfor a furthertwo hours,two 2509subsamplesset asidefor
assayand the remaindercollectedin a 40 litrecontainer.Thisprocesswas repeatednine
timesuntilallthe materialhadbeenrecombined,
homogenised,
subampled
and collected
in separate4A litre containers.The resultantmaterialconstitutesthe minus 3mm
gradesattaina maximum,is manifested
by foliatedsericiticand chloriticfaultgougeand
goethiticquartzveins.

Althoughno ore mineragraphy has beenundertaken


or scanningelectronmicroscopy to
determinethe natureof occurrenceof the gold,the very homogeneousdistribution
on a
mesoscopicscaleand uniformconcentration
gradientawayfrom the ore zone suggests
the gold is extremelyfine-grained Limitedpercussiondrilling
and evenlydisseminated.
indicatesthat sulphidesare rare to absentin the shearzone.

The majorand traceelementcomposition


of thisoxidised,quartz-veined
metagreywacke
goldore standardOREAS2C Batch2D3 is givenin Table1. The constituents
comprising
SiO2to Zr are the means of duplicateXRF analysesdeterminedat the Universityof
Melbourneusinga low dilutionboratefusionmethod,whilethe remainingconstituents,
As to Zn, are meansof at leastten replicateanalysesdeterminedvia INAAat Becquerel
Laboratories.

COMMINUTIOA
N N D H O M O G E N I S A T I OPNR O C E D U R E S

Approximately300k9 of the gold-bearinggreywackewas subjectedto the following


procedure:

a) primaryt crushing in a lurge (36 x 5Lt:m)jutr: t:ntsher


h) drying in a gasfred roturv drier
c) c:ru,sltingin u small (10 x 20cnt)jau, t:rusher
sec:ontdarv
d) tertiary crttshing in u pan mill
e) screening t0 mimts 3tnnt

Following
crushing,
the materialwas splitintoten equalsublotswhich
werehomogenised
separatelyin a tumble blenderfor two hours each A tenth splitfrom each sublotwas
then combinedand blendedfor a furthertwo hours,two 2509subsamplesset asidefor
assayand the remaindercollectedin a 40 litrecontainer.Thisprocesswas repeatednine
timesuntilallthe materialhadbeenrecombined,
homogenised,
subampled
and collected
in separate4A litre containers.The resultantmaterialconstitutesthe minus 3mm
werepulverised
referencematerialOREAS2C Batch2D3.Eachof the 25Ogsubsamples
for 5 minutesin a vibratoryringmilland splitinto 1009lotspriorto submission
for assay.

ANALYSISOF OREAS 2C BATCH2D3

Seven laboratoriesparticipatedin the analyticalprogramand are listedin Appendixl.

the lettercodes
havebeenrandomlydesignated
To ensureanonymitytheselaboratories
A through G (note: laboratoryA analysed gold by two different methods and is
designatedas A1 and A2 in Table 2). Materialwas submittedto each laboratory
A to F were instructedto carryout four
prepackagedin 1009 subsamples.Laboratories
Al, B, C and D used a fire
replicateassaysfor gold on 509 charges.Laboratories
rod AAS procedure,A1 employedfire assay/lCP-MS,
assay/carbon E fire assay/solvent
AAS, and F fire assay/flameAAS. LaboratoryG was instructedto
extraction/flame
complete10 replicateassayson 309 subsamplesfor gold, arsenic,antimonyand 26
neutronactivationanalysis.
additionalelementsusinginstrumental

were requestedto ensurerigorousanalyticalprocedures


ln all instanceslaboratories
were adheredto.

The resultsare presentedin Table2 with the analyticalsubsampleweightand method


indicatedat the head of each columnand the mean,medianand two sigmastandard
deviations(absoluteand relative)given for each laboratorydata set. lnterlaboratory
agreementof the meansof eachdata set is generallygoodwiththe exceptionof E which
globalmean of 360ppbAu.
is 15.3%lowerthan the uncorrected

STATISTICALEVALUATIONOF ANALYTICALDATA
FOR OREAS 2C BATCH2D3

RecommendedValue and ConfidenceLimits


The recommended
valuewas determinedfrom the meanof meansof acceptedreplicate
valuesof acceptedlaboratorydata setsA to G (note:to eliminateover-representation
on
Table 1. Approximatemajorand lrace elementcornpositionof gold-bearirrgreferencernaterial

Constituenl Concentration Consliluent Concenlralion

si02 64.43 As 162


Ti02 0.7 Ba 1270
At203 20.36 Ce 114
Fe203 3.28 Co 2S
MnO 0.01 (- t" 116
Mgo 1.27 Cs to
CaO 0.04 Hf ^
Na2O 0.23 t ^
Ld 54
K20 Rb lDJ

P205 0.06 Sb B3
H2O+ 3.78 Qn 18
ioiat gB.t4 Sm 10
Nb 15 Th 1B
Pb ?6 Yb
J 65 Zn II

Sr 117
137
Y 41
Zr 130

Table 2. Analyticalresultsfor gold in OREAS2C Batch2D3 (FA"MS- fire assay/inductively coupledplasma- mass spectrometry;
FA-CR - fire assay/carbonrod atomic absorptionspectrometry;FA-AAS fire assay/atomicabsorptionspectrometry;
-
FA"EX fire assay/solventextraction/atomicabsorplion spec:trometry,INAA - inslrumentalneutron activalionanalysis;
sampleweight in parentheses;Std.Dev.(x2)- two sigma standarddeviation;RSD(x2)- two sigma relativestandard
deviation;outliersin botd)
;' Lab Al
11 Lab A2 Lab B Ltb C Lab D Lab E Lab F labGr
No. ]
]jReplicate FA.CR FA.MS FA.CR FA"CR FA.CR FA.EX FA.AAS INAA
it - (sgs) (sOs) (50s) (50g) (50s) (50s) (50s) (3og)
ll 1 350 354 400 400 364 300 365 36ell
)l 350 344 400 400 328 320 348 378]l
il 3 I 350 s37 seO 365 380 300 352 374i
ll 4 I 350 337 390 335 372 300 378 392
r5lsza JOO
ilo cql I

il 'i 3 7 7l
R ? R6 l
1;
rl"
""-i
364 i
i 10 I s60l
,mean I 350.0 343.0 395.0 375.0 373.5 s05.0 364.2 374.6'
llmedian 3s0.0 340.5 395.0 382.5 37s.0 300.0 365.0 325.5I
Dev.(x2) i
ilSld. 0.0 16.1 11.5 62.7 14.4 20.0 28.2 20.0l
.Fgn(x2)_=-- _q0 4l 2.5 16,7 3.8 o.() 53l

n
.+
the part of laboratory
A a weightingfactorof 0.5 was appliedto the meansof A1 and
42) accordingto the formulae

x i = i L1*gu

.. 1g-
X = - ) . f , -i=t '
P

where

x,, is the jth result reported h), luhoratory i;


p is the numher of purticipating luboratories;

n, is the numher of results reported hy luhorutory i;

I, is the mean for laboratory i;

i is the nuan of means.

The confidencelimitswere obtainedby calculationof the varianceof the consensus


value(meanof means)and referenceto Student's-f
distribution
with degreesof freedom
(p-1)

p
v ttl = ;=
ptp_t)I
(I,-i)'
7=t

Confidcnce linits = ixtl-sz@-1)(V 6))tt'

where tr-.oz(p'I) is the I-x/2 fractile oJ'the t-distrihution with (p-I) degrees oJ'freetktm.

The distribution
of the valuesare assumedto be symmetrical
about the mean in the
calculationof the confidencelimits.
Thetestfor rejection
of individual assayoutliers meanswas
laboratory
and of outlying
basedonz scores(rejected if I z,l ,2 5) computed of location
fromtherobustestimators
andscale,f and S, respectively, to the formulae
according

S : l-483 medianl*,r - metliun @ |


j=L"".n- i=t"""n

xi -T
&is

where
T is the medisn yalue in a dotu set;
.9 is the medisn o.full ahsolute deviatiortsfrom the sumple median multiplied bv 1.483,o correction factor
to make the estimator consistent with the usaal parilmeter of o normal distrihution.

lndividualassayand mean outliersare shown in bold type in Table2 and have been
omittedin the determination values.
of recommended

valuesand 95% confidencelimits


Table3. Recommended

Constituent Recommended 95% Confidencelimits


value
Low High
G o l d ,A u ( p p b ) 371 354 388

Statementof Homogenerty
The standarddeviationof each laboratorydata set includeserror due both to the
imprecisionof the analyticalmethodemployedand to possibleinhomogeneity
of the
materialanalysed.The standarddeviationof the pooled individualanalysesof all
participating
laboratories of eachanalyticalmethod,
includeserrordue to the imprecision
to possibleinhomogeneity
of the materialanalysedand, in particular,
to deficiencies
in
accuracyof eachanalytical the componentof
toleranceintervals
method.In determining
error attributable of the
to measurementinnaccuracywas eliminatedby transformation
grand mean)
individualresultsof each data set to a commonmean (the uncorrected
accordingto the formula

pn;

fi = 1 iE'u
xti = xti _;
'p
. =1

fni
i=1
where

tt b the jth raw result reported by laboratory i;

*,j b the jth transformcdresult reported by laboratory i;

n, is thc rwmber of resuls reported by laboraory i;

p is the numberof panfuipating Inboraories;


I, is the rsw meanfor laboratory i.

The homogeneity
was determinedfrom tablesof factorsfor two-sidedtolerancelimitsfor
normaldistributions
(tSO 3207)in which

Iawer lirnit is i - t4fu,p,1


-o)"/
Upperlimit is ; * kl@,p,1-o)"J

where

n is tlte numfur of results;


l-a rs the confidcncelevel;
p is the proportion of results expectedwithin the nlcrance limits;

t l * thefaaor for two-sided tolerancelimits (m,o ur*nown);

it the correctedgrand standard devi.ation.


"J

The correctedgrand standarddeviation,Sn",used to computethe toleranceintervalsis


the weightedmeansof standarddeviationsof all data sets for a particularconstituent
accordingto the formula
i t",t,-lll
"i=*
| {l --:1;
i=l s,

where

1 - ( 9 I is ttrc weightingfactor for labratory i;


4s;
t; it the grand sandard deviwion computcdfrom the tansformed (i.e. means-
adjusted)resuls
accordingto the formula

pni
l*
E E ('ii - x i
i=i i=i
)t
s8=

I ni-1
i=1

where *i X thc tarsformcd meanfor laboratorty i

The weightingfactorswere appliedto compensatefor the considerablevariationin


analyticalprecisionamongstparticipating Hence,weightingfactorsfor each
laboratories.
data set have been constructedso as to be inverselyproportionalto the standard
deviationof that data set.

No individualoutlierswere removedfrom the results prior to the calculationof tolerance


intervals,however,a weightingfactorof zero was appliedto laboratorydata sets where
(i.e.wherethe weightingfactor1-s,/4sn'<0)
s,/4sn'>1

for gold (referTable4), where


The meaningof thesetolerancelimitsmay be illustrated
lying
of 2509-sizedsubsampleswill have concentrations
99% of the time at least95o/o
this meansthat if the same numberof
between352 and 390ppm.Put more precisely,
subsampleswere taken and analysedin the same manner repeatedly,99% of the
of the total population,and
toleranceintervalsso constructedwould coverat least95o/o
1o/oof the toleranceintervalswould cover less than 95o/aof the total population(lS0
Guide35) Obviously,if OREAS2C Batch2D3 is subsampledin weightsless than or
greaterthan 2509, the anticipatedtoleranceintervalwill be greaterthan or less than,
respectively,
that of * 19ppb.

valuesand tolerancelimits(subsamplesize of 2509).


Table4. Recommended

Constituent Recommended Tolerancelimits


value 1-a=0.99,p=0.95

Low High

G o l d ,A u ( p p b ) 371 352 390


REFERENGES

of referencematerials- Generaland statistical


ISO Guide 35 (1985),Certification
principals.

ISO Guide3207 (1975),Statistical of data - Determination


interpretation of a statistical
toleranceinterval.

A P P E N D I XI

List of Participating
Laboratories:-

Analabs,Welshpool,WA, Australia
AustralianAssay Laboratories,
Balcatta,WA, Australia
AustralianLaboratoryServices,Stafford,QLD, Australia
BecquerelLaboratories,
Lucas Heights,NSW,Australia
ClassicLaboratories,
Thebarton,SA, Australia
GenalysisLaboratoryServices,Maddington,WA, Australia
SGS Australia,QueensPark,\VA, Australia

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