ISO 10378 Analisis Au y Ag

INTERNATIONAL ISO
STANDARD 10378
Third edition
15
2016-02-
Copper, lead and zinc sulfide concentrates

— Determination of gold and silver—
Fireassay gravimetric and flame atomic
absorption spectrometricmethod
Concentrés de sulfurede cuivre,de plomb et de zinc— Dosage de

l’oret de l’argent— Méthode gravimétriquepar essaiau feu et
spectrométrie d’absorption atomique dans la flamme
Reference number
ISO 10378:2016(E)
InternationalOrganization for Standardization © ISO 2016

ISO10378:2016(E)
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InternationalOrganization for Standardization
ISO10378:2016(E)
Contents
Pag
e
Foreword .................. ................................................................................................... v

Introduction.................................................................................................................. vi
1 Scope .................................................................................................................. 1
2 Normative references................................................................................................... 1
3 Principle............................................................................................................... 2
3.1 General ................................................................................................................... 2
3.2 Fusion ........................................................................................................... 2
3.3 Cupellation............................................................................................................ 2
3.4 Parting.......................................................................................................... 2
3.5 Retreatment .......................................................................................................... 2
3.6 Correctionfor blank contamination....................................................................... 2
4 Reagents ............................................................................................................... 2
5 Apparatus ............................................................................................................. 4
6 Sample ................................................................................................................. 5
6. 1 Test sample ........................................................................................................... 5
6. 2 Test portion .......................................................................................................... 5
7 Procedure............................................................................................................................. 6
7. 1 Number of determinations....................................................................................... 6
7. 2 Trialfusion ............................................................................................................ 6
7. 3 Blank tests............................................................................................................. 6
7. 4 Charge preparation....................................................................................... 6
7.5 Primary fusion ..................................................................................................... 7
7. 6 Cupellation............................................................................................................ 8
7. 7 Retreatment of residues.................................................................................... 8
7.8 Determination of gold in the primary bead .................................................. 9
7.9 Determination of gold and silverin secondary beads and blanks,and of silver ....nprills10
7. 10 Determinationof silverin the partingsolution................................................. 11
8 Expressionof results.................................................................................................... 12
8. 1 Mass fractionof gold ...................................................................................... 12
8. 2 Mass fractionof silver.................................................................................... 13
9 Precision.............................................................................................................................. 14
9.1 Expressionof precision................................................................................... 14
9.2 Method for obtainingthe finalresult(seeAnnex H) ............................................ 15
9.3 Precisionbetween laboratories............................................................................ 15
9.4 Check of trueness................................................................................................ 17
9.4.1 General.......................................................................................................... 17
9.4.2 Type of certified referencematerial(CRM) or referencematerial(RM) ................. 18
10 Test report ............................................................................................................. 18
Annex A (normative)Procedure for the preparationand determinationof the mass of a
predriedtestportion ................................................................................................... 19
Annex B (normative)Trialfusion ...................................................................................... 21
Annex C (normative)Blank determination............................................................................. 22
Annex D (normative)Inquartation...................................................................................... 23
Annex E (normative)Determinationof vaporizationlossof silverduring the
cupellationprocess ....................................................................................................... 24
Annex F (normative)Sulfuricacid— Parting................................................................................... 25
Annex G (normative)Determinationof impuritiesin partingsolutionsand washings ..................... 27
© ISO 2016 – Allrightsreserved iii

ISO 10378:2016(E)
Annex H (normative) Flowsheet of the procedure for the acceptance of analyticalvalues for
testsamples (see 9.2 ) .........................................................................................31 ...
Annex I (informative) Flowsheet of the method .......................................................................32 .
Annex J (informative)Roasting method ...............................................................33........ ..........
Annex K (informative) Guide to the preparationof dilutionsfor the determination of silver

in partingsolutionsand residues .......................................................................34 ........
Annex L (informative)Derivationof precisionequations ...............................................35 ...............

Bibliography .....................................................................................................50 ........
iv
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ISO 10378:2016(E)
Foreword
ISO (theInternationalOrganizationfor Standardization)isa worldwide federationof nationalstandards
bodies (ISO member bodies).The work of preparing InternationalStandards is normally carried out through ISO
technicalcommittees. Each member body interestedin a subject for which a technical
committee has been establishedhas the right to be represented on that committee. International
organizations,governmental and non-governmental, in liaisonwith ISO,also take part in the work.
ISO collaboratescloselywith the InternationalElectrotechnicalCommission (IEC) on allmatters of
electrotechnicalstandardization.
The procedures used to develop thisdocument and those intended for itsfurther maintenance are describedin
the ISO/IEC Directives,Part 1.In particularthe differentapproval criterianeeded for the differenttypes of ISO
documents should be noted. This document was drafted in accordance with the editorialrulesof the ISO/IEC
Directives,Part 2 (see www.iso.org/directives).
Attention isdrawn to the possibilitythat some of the elements of thisdocument may be the subjectof patent
rights.ISO shallnot be held responsiblefor identifyingany or allsuch patent rights.Detailsof any patent
rightsidentified during the development of the document willbe in the Introductionand/or
on the ISO listof patent declarationsreceived(see www.iso.org/patents).
Any trade name used in thisdocument isinformation given for the convenience of users and does not
constitutean endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’sadherence to the WTO principlesin the Technical
Barriersto Trade (TBT) see the followingURL: Foreword - Supplementary information
The committee responsiblefor this document is ISO/TC 183, Copper, lead, zinc and nickel ores and concentrates
.
This third editioncancelsand replacesthe second edition(ISO 10378:2005),in which 6.2 has been
technicallyrevised and the warning noticein A.3.1has been updated.
v
ISO 10378:2016(E)
Introduction
This InternationalStandard describesa method for the determination of the mass fractionof gold
and silver in copper, lead, and zinc sulfide concentrates. This International Standard was prepared
to enable laboratoriesto determine the mass fractionof gold and silverin suitablesamples using
instrumentalmethods.
vi
INTERNATIONAL STANDARD ISO 10378:2016(E)
Copper, lead and zinc sulfide concentrates — Determination of

gold and silver— Fireassay gravimetric and flame atomic
absorption spectrometric method
WARNING — This InternationalStandard may involve hazardous materials,operations, and equipment. It is the
responsibilityof the user of this InternationalStandard to establish appropriate health and safety practicesand
determine the applicabilityof regulatory limitations priorto use.
1 Scope
This International Standard specifies a fire assay gravimetric and flame atomic absorption
spectrometricmethod for the determinationof the mass fractionof gold and silverin copper,lead,and
zinc sulfide concentrates as follows.
— Copper concentrates
The method isapplicableto the determinationof mass fractionsof gold from 0,5g/t to 300 g/t and of mass
fractionsof silverfrom 25 g/t to 1 500 g/t in copper sulfide concentrates containing mass fractionsof copper
from 15 % to 60 %.
— Lead concentrates
fractionsof silverfrom 200 g/t to 3 500 g/t in lead sulfide concentrates containing mass fractionsof leadfrom
10 % to 80 %.
— Zincconcentrates
fractions of silverfrom 10 g/t to 800 g/t in zinc sulfide concentrates containing mass fractionsof zincup to 60
%.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application.For dated references, only the edition cited applies.For undated
references,the latesteditionof the referenced document (includingany amendments) applies.
ISO 385, Laboratoryglassware— Burettes
ISO 648, Laboratoryglassware— Single-volumepipettes
ISO 1042, Laboratoryglassware— One-mark volumetricf lasks
ISO 3696, Water for analyticallaboratoryuse — Specificationand testmethods
ISO 4787, Laboratoryglassware— Volumetricinstruments— Methods fortestingofcapacityand for use
ISO 9599, Copper, lead and zinc sulfide concentrates— Determinationof hygroscopicmoisture in the analysis
ample— Gravimetricmethod
© ISO 2016 – Allrightsreserved 1

ISO 10378:2016(E)
3 Principle
3.1 General
Fire assaying for the determination of gold and silvercomprises a seriesof steps to separate f irstlythe precious
metals from most of the associatedmetals,followed by separationof the gold from silverand other metals pre-
concentratedinto a precious-metalalloy.
The stagesthat comprise the determinationsare describedin 3.2 to 3.6 inclusive.
3.2 Fusion
The samples are fused in a crucibleafter mixing with a litharge-basedf lux which, under reducing
conditions,collectsthe preciousmetals in a metalliclead button.
3.3 Cupellation
The base metals present in the lead button are substantiallyseparated from the precious metals by
oxidizingfusion.Cupellationproduces a bead largelycomprising a silver-goldalloywith small quantities
of other metals.
3.4 Parting
Gold isseparated from the primary bead by treatment with nitricacid.The gold prillisweighed. Gold prillshaving
a mass lessthan 50 μg are dissolvedin aqua regia and the gold isdetermined by atomic absorption
spectrometry (AAS).Silverisdetermined in the parting solutionby AAS.
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Retreatment
All residues are retreated to maximize the recovery of gold and silver.The addition of collectorsfor either gold or
silveris not required,as both metals are present in sufficientamounts to be readily visibleafter the
cupellationstage.The second bead is dissolvedin acids followed by analysisof both metals by AAS.
3.6 Correction for blank contamination
Contamination by gold and silverimpuritiesin the reagents is corrected for by fusing the reagents
without the testportion.
4 Reagents
During the analysis,use only reagents of recognized analyticalgrade and water that complies with
grade 2 of ISO 3696.
4.1 Sodium carbonate ,anhydrous.
4. 2 Litharge (PbO),assay grade having a mass fractionof gold of lessthan 0,01 g/t and a mass fraction of
silverof lessthan 0,2g/t.
4. 3 Silica,precipitated.
4.4 Potassium nitrateor sodium nitrate
NOTE Ifsodium nitrateisused,the masses specified for potassium nitratewillhave to be modi fied:
2
ISO 10378:2016(E)
85 0
g of KNO 3 × = g of NaNO 3
101 1
4.5 Flour
4. 6 Borax ,fused anhydrous sodium tetraborate(borax glasspowder).
4. 7 Nitricacid,concentrated( ρ20 1,42g/ml),chlorideconcentration<0,5μg/ml.
4. 8 Nitricacid,diluted1+1.
Slowly add 500 ml of concentratednitricacid(4.7) to 500 ml of water,while stirring.
4. 9 Lead ,foil,having a mass fractionof gold of lessthan 0,01 g/t and a mass fractionof silverof less than 0,2g/t.
4.10 Silver,of minimum purity99,99 %.
4.11 Hydrochloric acid (ρ20 1,16g/ml to 1,19g/ml).
4.12 Thiourea ,10 g/lsolution.
Add 1 g of thioureato 100 ml of water.
4.13 Aqua regia
Mix three partsof hydrochloricacid(4.11) with one part of nitricacid(4.7).Prepare freshlyas required.
4.14 Standard solutions
Standard solutionsshould be prepared at the same ambient temperature as that at which the
determinationswillbe conducted.
4.14.1 Silver,standard stock solutionA (500 μg of Ag/ml).
Weigh 0,500 0 g of silvermetal to the nearest0,1mg. Transfer to a 100 ml beaker,add 20 ml of diluted

nitricacid(4.8),and warm to dissolveCool. and add 20 ml of concentratednitricacid (4.7).Transfer to
a 1 000 ml volumetricf lask,f illup with water nearly to the mark, mix and cool to room temperature; then fillup
exactlyto the mark and mix again.
4.14.2 Silver,standard solutionB (50 μg of Ag/ml).
Pipette10,00 ml of silverstandard stock solutionA (4.14.)1 into a 100 ml volumetric f lask,f illup with water
nearly to the mark, mix and cool to room temperature; then fillup exactlyto the mark
and mix again.
Prepare a freshsolutionper batch.
4.14.3 Gold,standard solution(1 000 μg of Au/ml).
Weigh 1,000g of gold metal to the nearest0,1mg. Transfer to a 200 ml beaker,add 25 ml of aqua regia
solution(4.13),and warm to dissolveCool. and transferto a 1 000 ml volumetric f lask.Add 75 ml of
hydrochloricacid (4.11),f illup nearly to the mark with water, mix and coolto room temperature;then fillup
exactlyto the mark and mix again.

ISO 10378:2016(E)
4.14.4 Gold and silver,standard solution(100 μg of Au/ml + 50 μg of Ag/ml).
Pipette10,00 ml of silverstandard stock solutionA (4.14.1) into a 100 ml volumetric flask.Add 40 ml of

hydrochloric acid (4.11).Pipette10,00 ml of gold standard solution(4.14.3) into the volumetric flask. Fillup nearly to
the mark with water, mix and cool to room temperature; then fillup exactly to the
mark and mix again.
4.15 Calibrationsolutions
Calibrationsolutionsshould be prepared at the same ambient temperature as that at which the

4.15.1 Gold/silvercalibrationsolutions
Pipette0,0ml, 1,00ml, 2,00ml, 5,00ml, and 10,00 ml of gold and silverstandard solution(4.14.4) intoa seriesof
100 ml one-mark volumetric flasks.
Add 40 ml of hydrochloric acid (4.11) to each flask,f illup nearly to the mark with water, mix and cool to room
temperature; then fillup exactlyto the mark and mix again.
These solutionscontain 0,0 μg of Au/ml, 1,00 μg of Au/ml, 2,00 μg of Au/ml, 5,00 μg of Au/ml, and 10,00 μg of
Au/ml; and 0,0 μg of Ag/ml, 0,50 μg of Ag/ml, 1,00 μg of Ag/ml, 2,50 μg of Ag/ml, and 5,00 μg of Ag/ml, and
shallbe freshlyprepared.
4.15.2 Silvercalibrationsolutions
Pipette0,0 ml, 1,00 ml, 2,00 ml, 4,00 ml, 6,00 ml, 8,00 m,l and 10,00 ml of silverstandard solutionB ( 4.14.2) into a seriesof 100 ml volumetric
flasks.Add 10 ml of nitricacid (4.7),f illup nearly to the mark with water, mix and GetcoolmoretoroomFREEtemperature;standardsfromthen
StandardfillupexactlySharingtotheGroupmark andand ourmixchatsagain.
These solutionscontain 0,0 μg of Ag/ml, 0,50 μg of Ag/ml, 1,00 μg of Ag/ml, 2,00 μg of Ag/ml, 3,00 μg of
Ag/ml, 4,00 μg of Ag/ml, and 5,00 μg of Ag/ml, and shallbe freshlyprepared.
Contamination by gold and silverimpurities in the reagents is corrected for by fusing the reagents without the
testportion.
5 Apparatus
5.1 Assay cruciblefurnace,with a maximum required operatingtemperature of 1 200 °C.
5.2 Muf fle furnace, with a maximum required operating temperature of 1 100 °C. Temperature
indication,automatic temperature control,and controlledairflow are preferable.
5.3 Assay crucibles,made of fire clay,of nominal capacity 200 ml to 600 ml, capable of withstanding
corrosion by the samples and fluxes at 1 100 °C.
The crucibleshallbe of such a sizethat the charge does not fillthe crucibleto a depth greater than 3/4
the depth of the crucible.
5.4 Cupels,made of magnesium oxide,or bone-ash cupels having a nominal capacity of 50 g of molten
lead.
The insidebottom of the cupel shallbe concave, as recommended in the fire assay texts referred to in
the Bibliography.
5.5 Conical mould ,made of cast iron,of sufficientcapacity to contain allof the molten lead plus slag
from the cruciblefusion.
4 © ISO 2016 – Allrightsreserved

ISO 10378:2016(E)
5.6 Analyticalbalance,sensitiveto 1 mg.
5.7 Microbalance,sensitiveto 1 μg or less.
5.8 Ordinary laboratoryglassware,washed freeof chlorides.
5. 9 Volumetric glassware, of classA complying with ISO 385, ISO 648, and ISO 1042, and used in accordance
with ISO 4787.
5.10 Atomic absorptionspectrometer (AAS),equipped with background correctionand a glassbead

in the spray chamber.
5.11 Inductivelycoupled plasma (ICP)atomic emission spectrometer .
5.12 Pulverizer.
5.13 Hotplate.
6 Sample
6.1 Test sample
Prepare an air-equilibratedtestsample in accordance with ISO 9599.
NOTE A testsample isnot requiredifpredriedtestportionsare to be used (seeAnnex A) .
6.2 Test portion
Taking multipleincrements,extracta testportion from the testsample in such a manner that itis
representativeof the whole contentsof the dish or tray.Weigh to the nearest1 mg approximately 10 g to 20 g of
the testsample.At the same time as testportionsare being weighed for analysis,weigh test portionsfor the
determinationof hygroscopicmoisture in accordance with ISO 9599.
NOTE 1 The precisionof determinationof the mass of contained gold in a lot is the sum of sampling and
analyticalprecisionThe. presence of particulategold in a concentratecontributesto imprecisionof the analytical
component of totalprecisionWhen. ithas been establishedthatthe presence of particulategold in a concentrate
causesunacceptableimprecision,the followingmixing and sampling methods are recommended.
a) Mix the sample by eitherof the followingpreferredmixing methods as describedin ISO 12743:2006:
— 15.3.2c),stripmixing;
— 15.3.2e),rifle,or rotarydivider.
Mixing methods in items a),b),and d) inISO 12743:2006,15.3.2are not recommended.
b) Extract a test portion from the test sampleitherusingofthe following methods described in43:2006:ISO127
— 15.4.1a),rotarysample division;
— 15.4.1f),ribbon division.
Methods in items b) to e) and g) in ISO 12743:2006,15.4.1are not recommended .
Alternatively,the method specified in Annex A may be used to prepare predriedtestportionsdirectly from the
laboratorysample.

ISO 10378:2016(E)
Ifa mass fractionof arsenicabove 2 % is present in the sample, thiselement should be removed by followingthe
procedure in Annex J;otherwise,interferencewith the cupellationstage may occur.
NOTE 2 Ifthe mass fractionof copper isgreaterthan 30 %, a 10 g or 15 g testportionispreferable(see the fourthparagraph of

7.4) .
For lead concentrates,the testportionshould be 10 g to ensure an adequate supply of lead.
7 Procedure
7.1 Number of determinations
Carry out the determinationsat leastin duplicate,as far as possibleunder repeatabilityconditions,on

each testsample.
NOTE 1 Repeatabilityconditionsexistwhere mutually independent testresultsare obtained with the same

method on identicaltestmaterialin the same laboratoryby the same operator using the same equipment, within
shortintervalsof time.
NOTE 2 In the case where the ratioof silverto gold does not exceed 2,5 to 1 and the procedure specified in
7.10iscarriedout for the silverdetermination,separatedeterminationsfor gold and silverwillbe necessary (see Annex D )
.Four testportions,therefore,are required, .etwo. for determinationsof gold and two for silver.
NOTE 3 Annex I containsa flowsheet of the method.
7.2 Trialfusion
Carry out a trialfusion as describedin Annex B, to ensure that the mass of the lead button isbetween
30 g and 45 g. Get more FREE standards from Standard Sharing Group and our chats
7.3 Blank tests
Carry out a reagent blank test as described in Annex C in parallelwith the analysis,using the same quantitiesof
allreagents,with the additionof sufficientf lour (4.5) to the flux to give a lead button of
between 30 g and 45 g. Omit the testportionand the potassium nitrateThe. totalblank should not
exceed 5 μg of gold or 100 μg of silver.
7.4 Charge preparation
Determine the mass of potassium nitrate(4.4) and flour (4.5) required in the charge,as indicatedby the
trialfusion(see Annex B ),and includethisreagent in the flux mixture.Typicalmasses of the flux components for
copper,lead,and zincconcentratesare shown in Tables1 to 3 respectively.
Thoroughly mix the testportionwith a flux.
Intimatemixing of flux components and the testportionisvery important.Allf lux components should be in a
finelydivided statewith a preferred particlesizeof lessthan 0,5mm.
6
ISO 10378:2016(E)
Table 1 — Typicalmasses of f lux components for copper concentrates
Mass
Flux components g
Sodium carbonate( 4.1) 30

Litharge( 4.2) 210
Silica( 4.3) 25
Potassium nitrate( 4 .4 ) —
Flour( 4.5) —
Test portion 20
Ifthe mass fractionof copper is greaterthan 30 %, the mass of lithargeshould be 30 times that of copper plus 35
g for the lead button.Alternatively, 10 g or 15 g testportion can be used while retaining the flux composition
given in Table 1.Ifthere are dificultiesexperienced in achieving a fluid melt, the amount of silicarecommended in
Table 1 can be reduced to 19 g,while including6 g borax.
Table 2 — Typicalmasses of f lux components for lead concentrates
Flux components Mass, g

Litharge( 4.2) 100
Silica( 4.3) 10
Borax (4.6 ) 10
Flour( 4.5) —
Test portion 10
Table 3 — Typicalmasses of f lux components for zincconcentrates
Flux components Mass, g

Litharge( 4.2) 120
Silica( 4.3) 10
Borax (4.6 ) 10
Flour( 4.5) —
Test portion 20
Place the mixture in an assay crucible(5.3).
7.5 Primary fusion
Placethe cruciblesin the furnace(5.1) preheated to approximately 900 °C.
Ifoilf-ired or gas-fired furnaces are used, the fuel should be turned off immediately before opening the
furnace.
Slowly raisethe furnace temperature to 1 000 °C to 1 050 °C.Maintain thistemperature untilthe fusion
has been tranquilfor at least10 min.

ISO 10378:2016(E)
The optimum furnace settingtemperature depends on the furnace structureand the positionof the
thermometer. Ifunfused materialremains in the bottom of assay crucibles,the settingtemperature of the furnace
should be raisedand the assay repeated.
To minimize cruciblecorrosionand build-upof impuritiesin the lead button,the overallfusiontime should not
exceed 40 min. However, should the fusiontake an extended time to settle,the fusiontime
may need to exceed 40 min.
Itisrecommended that a fire-claylidor a layerof saltor borax approximately 12 mm thickbe used with thisfusion
to prevent lossof material by dusting or ebullitionIfborax. isused as a cover,the amount used in the flux may be
reduced accordingly.Ifsome “shotting”of the lead isnoted in the slag (thisis common for
zincconcentrates),itisrecommended thatthe extraborax be retained.
Pour the mixture into a dry conicalmould (5.5),takingcare that no lossof lead or slagoccurs.Reserve the cruciblefor
retreatmentfusion.
Allow the mixture to cooland carefullyseparate the lead button from the slag.Hammer the lead button as
necessary to remove any small particlesof adhering slag.Reserve the slagfor retreatment.
Weigh the leadbutton.Ifthe button weighs lessthan 30 g or more than 45 g,discardthe button and slag
and repeat the assay afterappropriateadjustment of the oxidizingagent (see Annex B).
NOTE Buttons weighing lessthan 30 g may show poor collectionefficiencies,whereas those exceeding 45 g contain
may higher amounts of copper and other base metals.
7.6 Cupellation
Placethe leadbutton obtainedin 7.5intoa preheated cupel(5.4) in a muf flefurnace (5.2) at 900 °C.Allow the
cupellationto proceed at the lower muf fletemperature of approximately 860 °C with a steady airf low.
Variationsdepend on the cupel type and furnace conditions.In the case of cupels made of bone ash,a
cupellationtemperature of 820 °C isrecommended.
NOTE 1 In the case where only gold isbeing determined, itcould be effectiveto raisethe furnace temperature to 900 °C to
finishthe cupellationafter the visiblelead melt on the cupel is approximately 10 mm in diameter [approximately 80 % (mass
fraction)of lead absorbed] .
High cupellationtemperatures willcause higher silverlossesand low temperatures can cause “freezing” of the
bead and incomplete cupellationIt. is recommended that lossof silverduring the cupellation processbe determined,to
decideupon the furnace conditions(seeAnnex E).
Remove the cupelfrom the furnace and cool.
Carefullyextractthe primary bead and remove any adhering cupel material with a brush. Flattenthe bead
slightlyand place in a 30 ml porcelaincrucible.
NOTE 2 A testtube can be used insteadof a porcelaincrucible.
NOTE 3 Ifthe ratioof silverto gold in the primary bead isgreater than 2,5 to 1,the silvercan be determined
by the gravimetric method instead of the procedure specified in 7.10. For the gravimetricmethod, weigh the primary bead,
in micrograms, to the nearest 1 μg (m0),carry out the parting by the procedure specified in 7.8, and determine the
impuritiesin the partingsolutionsand washings by the procedure specified in Annex G .
NOTE 4 Ifitis dificultto recover the bead because of itssmall size,1 mg of palladium can be added before fusion.In
thiscase,the palladium bead isdissolvedand determined by the procedure specified in 7.9.
Reserve the cupelfor retreatmentof residues.
7.7 Retreatment of residues
Place both the cupel and the slag in a pulverizer(5.12) and pulverizefor about 20 s to reduce the
materialto minus 150 μm.

ISO 10378:2016(E)
Ifmagnesium cupels are used, itisrecommended that the slagand the cupel be retreated separately.
NOTE 1 Longer grindingcan cause caking of the materialand heatingof the grindingbarrel.
NOTE 2 The pulverizermay be cleaned between samples by grinding small portions of broken glassor quartz.
Thoroughly mix the ground residueswith a flux.Typical composition of the flux isshown in Table 4.
Table 4 — Typicalmasses of f lux components for the retreatment of residues
Mass, g
Flux components Magnesium oxide cupel Bone ash cupel
Sodium carbonate( 4.1) 50 to 60 40

Litharge( 4.2) 50 to 60 45
Silica( 4.3) 50 to 60 20
Flour( 4.4 ) 4 2 to 3
Borax (4.6 ) 30 to 50 15
The mass of flour shown in Table 4 is typical.The mass should be sufficientto produce a 30 g to 45 g lead
button.
The combined mass of slag and cupel of the primary fusion,in addition to the flux components given
in Table 4 ,may exceed the capacity of the assay crucibles,or the re-fusionmay be so reactivethat the
fusions may froth over. In these cases,itispermissibleto splitthe residues into equal halves and fuse separately
in two crucibles.The lead buttons obtained should be cupelled separately,or be scorified
togetherand the resultantleadbutton cupelled.
Place the mixture in the originalassay crucible.
Carry out the fusion as detailedin 7.5and discardthe crucibleand slag.
Cupel the leadbutton as detailedin 7.6to obtaina second bead and discardthe cupel.
7.8 Determination of gold in the primary bead
Add 10 ml of dilutenitricacid (4.8) to the primary bead in the porcelaincrucibleprepared in 7.6 and heat gently
on a hotplate (5.13) for 20 min or untilthe reactionceases.
NOTE 1 Itisessentialthat chloridebe absent during parting;otherwise,some of the gold may dissolve.
When the bead istreatedwith hot dilutenitricacid,silverwillstartto dissolveprovided thatthe ratio of silverto gold in
the bead exceeds 2,5to 1.The rate of dissolutionincreaseswith increasingmass fractionof silverof the bead.
Rapid attack of the bead should be avoided by further dilutionand slow heatingto prevent disintegrationofthe
gold.Should the ratioof silverto gold be lessthan 2,5to 1,as shown by failureto part in hot dilutenitricacid,the bead
should be inquarted (see Annex D ).
Ifthereisdanger of the gold sponge crumbling during the partingoperation,itisrecommended thatthe operationbe
carriedout with sulfuricacid(seeAnnex F).
Carefullypour the solutioninto a 200 ml beaker by decantation to avoid losses.
Add 15 ml of warm dilutenitricacid (4.8) to the porcelain crucibleand continue heating gently until parting
iscomplete. This should take approximately 25 min.

ISO 10378:2016(E)
Carefullypour the solutionintothe 200 ml beaker by decantationto avoid lossesWash. the crucibleand
gold with four 15 ml volumes of hot water.Collectallthe washings in the same 200 ml beaker.Reserve
the solutionfor the determinationof silveras specified in 7.10.
NOTE 2 The possibilityof gold particlesoccurring in the collectedparting and washing solutionscan be determined by
evaporatingthe solutionsslowly down to 2 ml to 3 ml, then continuingwith the determinationas specified in 7.9.
Dry the gold sponge in the porcelaincrucibleon the hotplate.
Placethe cruciblein the muf flefurnace (5.2) to anneal the gold at dullred heat for approximately5 min.
Cool and weigh the resultantgold prill,in micrograms, to the nearest1 μg ( m1).
Ifthe mass of the gold islessthan 50 μg, itisrecommended that the gold be dissolvedand determined by the
procedure specified in 7.9.
Ifthe mass of the gold islessthan 50 μg, repeat the fusionand cupellation,then dissolvethe prepared bead and
determine the gold and silverconcentrationas specified in 7.9 without the partingoperation. This
alternativeprocedure is recommended where there is a danger of the gold sponge crumbling during the
partingoperation.The procedure,however, cannot be appliedifthe product of mass of test
portionby mass fractionof silver,. emass. in testportion,islargerthan 7 500 μg.
NOTE 3 Ifthe sensitivityof the microbalance is0,1μg, the applicablerange of the gravimetricmethod can be extended to 5
μg of gold.In such a case,weigh the gold prill,in micrograms, to the nearest0,1μg (m1) .
Reserve the gold prillto determine silverin the prillThe. prillisdissolvedand the silverconcentration
is determined as specified in 7.9. Several of the weighed prillsof the same laboratorysample can be combined
for the determination.
Platinum and palladiumGetmoreare removedFREEstandardsfromthe fromprillduring StandardpartingSharingwithGroupnitricandcidour.Ifthechatsdetermination
of these elements remaining in the prillis considered necessary,determine these by the procedure specified in
7.9,followedby the additionof platinum and palladiumto the standard solutionsin relevant proportions.Ifa
sufficientdetectionlimitfor AAS or ICP cannot be obtained on a singleprillbasis, largenumber of prillsof the same
laboratorysample should be combined.
7.9 Determination of gold and silverin secondary beads and blanks,and of silverin prills
For blanks and samples determined by the procedure specifiedin the fourthlastparagraph of 7.8without the
partingoperation,the primary and secondary beads should be combined and treatedtogether.
Transfer the bead(s)or prill(s)to a testtube or a porcelaincrucibleAdd. 2 ml of nitricacid (4.7) and warm in a
heatingblock or a sand bath set at approximately 98 °C.Add 6 ml of hydrochloricacid ( 4.11) and heat again to
dissolvethe gold.Ifnecessary,add a further2 ml of nitricacid ( 4.7).Take the above solution,or that prepared
accordingto Annex C,and heat almost to dryness.
The solutionshould not be allowed to evaporate to dryness;otherwise,metallicgold willform.
Remove the testtube or the cruciblefrom the heating block or the sand bath and allow cooling.Add
10 ml of hydrochloricacid(4.11) and mix or swirlto dissolveany saltsTransfer.quantitativelyto a 50 ml
volumetricf lask,add 10 ml of hydrochloricacid(4.11),make up to the mark with water,and mix well.
Depending upon the mass fractionof silver(seeAnnex K ),itmay be necessaryto make dilutions o that the
concentrationof silverin the testsolutionsisin the range covered by the silvercalibrationsolutions
(4.15.)1.Hydrochloricacid(4.11) should be added so that40 ml of the acidiscontainedper 100 ml of the
dilutedtestsolutions.
Aspirate the test solutionsand gold/silvercalibrationsolutions(4.15.)1 into the atomic absorption spectrometer
(5.10) and measure the absorbance.As a guide,the atomic absorptionsettingsshown in Table 5 are
recommended; however, the instrument should be optimized to be free from any
interferenceand to give maximum sensitivityand as near as practicalto a linearrelationshipbetween
absorbance and concentration.

ISO 10378:2016(E)
Table 5 — Recommended atomic absorptionsettings
Parameter Gold Silver

Flame air/acetylene(oxidizing)
Wavelength 242,8nm 328,1nm
Lamp current 4 mA 5 mA
Background corrector on off
Aspirationrate optimizefor maximum signal
Integrationtime 3s
Number of integrations 5
Absorbance of 5 μg/ml calibrationsolution 0,17 0,55
Perform three measurements on each test solutionand calibrationsolution.Calculate,to three significantf

igures,the mean absorbance for each solution,provided that the range of values does not
exceed 0,003absorbance units.Ifthisrange isexceeded,repeatthe measurement.
In order to clean out the nebulizersystem, itisrecommended to aspiratea cleaningsolution,which is, for
instance,prepared by carefullyadding 500 ml of hydrochloricacid( 4.11) and 100 ml of concentrated nitricacid(4.7)
to 400 ml of water,between measurements.
Plot a calibrationgraph of absorbance versus concentrationand determine the gold and/or silver
concentrations,in micrograms per millilitre,inthe testsolutions,followed by calculationof the mass
(ma),in micrograms, of the gold and/or silverusing Formula (1):
ma = ρ × TDF (1)
where
ρ isthe mass concentrationof gold and/or silver;
TDF isthe totaldilutionfactor.
Alternatively,an ICP atomic emissionspectrometer (5.11) can be used for the determinationof gold and silverat the
appropriatewavelength.Typicalwavelengths are 242,8nm for gold and 328,1nm for silver; however, the
instrument should be optimized to be free from any interferenceand to give maximum sensitivityand as near as
practicalto a linearrelationshipbetween absorbance and concentration.In
order to improve the precision,itisrecommended that a simultaneousinternalstandard correctionbe
adopted.Yttrium isgenerallyused as an internalstandard.
During allAAS or ICP determinations,the testsolutionsand calibrationsolutions hould have the same
temperature,as well as the same acidconcentration.
7.10 Determination of silverin the parting solution

NOTE 1 This determinationisapplicablewhere the ratioof silverto gold isgreaterthan 2,5to 1 and the silver
has been parted from the gold as indicatedin 7.8.
NOTE 2 The silvercan be determined by the gravimetricmethod insteadof the procedure specified in this
subclause.For the gravimetricmethod, determine the impuritiesin the partingsolutionsand washings by the procedure
specified in Annex G .
Take the partingsolutionsand washings,which were reservedin7.8.Heat to evaporate to approximately

20 ml, cool,and then add 2 ml of nitricacid (4.8).Transfer quantitativelyto a 100 ml volumetricf lask, make up to
the mark with water,and mix well.
Ifthe solutionturns cloudy,add 1 % of thioureasolution(4.12) drop by drop, while stirringuntilthe

solutionisclear.Add 2 ml in excess,then diluteto volume.

ISO 10378:2016(E)
Depending upon the mass fractionof silver(see Annex K),itmay be necessary to make dilutionsso that the
concentration of silverin the test solutionsis in the range covered by silvercalibrationsolutions
(4.15.)2.Nitricacid(4.7) should be added so that10 ml of the acidiscontainedper 100 ml of the diluted
testsolutions.
Aspirate the test solutionsand silvercalibrationsolutions(4.15.)2 into the atomic absorption spectrometer (5.10)
and measure the absorbance.As a guide,the atomic absorptionsettingsshown
in Table 5 are recommended; however, the instrument should be optimized to be free from any
interferenceand to give maximum sensitivity,and as near as practicalto a linearrelationshipbetween
absorbance and concentration.
Perform three measurements on each test solutionand calibrationsolution.Calculate,to three significant f

igures,the mean absorbance for each solution,provided that the range of values does not
exceed 0,003absorbance units.Ifthisrange isexceeded,repeatthe measurement.
Plota calibrationgraph of absorbance versusconcentrationand determine the silverconcentrations,in

micrograms per millilitre,in the testsolutions,followed by calculationof the mass ( ma),in micrograms, of the
silverusingFormula (1).
Alternatively,an ICP atomic emission spectrometer (5.11) can be used for the determinationof silver at the
appropriate wavelength. A typicalwavelength is 328,1 nm; however, the instrument should be optimized to be
free from any interferenceand to give maximum sensitivityand as near as practical
to a linearrelationshipbetween absorbance and concentrationIn. order to improve the precision,itis
recommended that a simultaneous internalstandard correctionbe adopted. Yttrium isgenerally used as an
internalstandard.
During allAAS or ICP determinations,the testsolutionsand calibrationsolutions hould have the same
temperature,as well as the same acidconcentration.
8 Expression of results
8.1 Mass fraction of gold
The mass fractionof goldof the testportion(wAu ),expressed in grams per tonne,isgiven by Formula (2):
m + m − m m m m
1 2 ( B + BR )− 5 + W 100
w Au = × (2)
H
m 100−
where
m1 isthe mass, in micrograms, of gold obtained in the primary bead (as weighed or as
determined by AAS);
m2 isthe mass, in micrograms, of gold in the secondary bead;
mB + mBR isthe mass, in micrograms, of gold in the primary blank bead combined with the mass
of gold in the secondary blank bead;
m5 isthe mass, in micrograms, of silver emaining in the prill(inthe case of AAS being
used to obtainm1,m5 = 0);
mW isthe mass, in micrograms, of gold in the parting and washing solutions;
m isthe mass, in grams, of the testportion;
H isthe hygroscopic moisture content,in percent,of the testportion (in the case of a pre -
driedtestportionbeing used,H = 0).
12
ISO 10378:2016(E)
8.2 Mass fraction of silver
If the silveris determined by the procedure specified in 7.10, the mass fractionof silverof the test
portion(wAg ),expressed in grams per tonne, isgiven by Formula (3):
+ m − m m m
m3 4 ( B + BR )+ 5 100
w Ag = × (3)
H
m 100−
where
m3 isthe mass, in micrograms, of silverin the parting and washing solutions;
m4 isthe mass, in micrograms, of silverin the residue recovered;
mB + mBR isthe mass, in micrograms, of silverin the blank primary bead combined with the mass
of silverin the blank determination of the residue recovered;
m5 isthe mass, in micrograms, of silverremaining in the prill;
H isthe hygroscopic moisture content,in percent,of the testportion (in the case of a pre - dried
testportionbeing used, H = 0).
Ifcomplete recovery of silverduring the cupellationprocess is not obtained, correct the mass fraction
of silverof the testportion(see Annex E ).
If the silveris determined by the gravimetric method instead of the procedure specified in 7.10, the mass
fractionof silverof the testportion(wAg ),expressed in grams per tonne, isgiven by Formula (4):
− m m m m
m0 − m1 + m4 ( B + BR )+ 5 −
imp 100
w Ag = × (4)
m 100 − H
where
m0 isthe mass, in micrograms, of the primary bead;
m1 isthe mass, in micrograms, of gold obtained in the primary bead (as weighed or as
determined by AAS);
m4 isthe mass, in micrograms, of silverin the residue recovered;
mB + mBR isthe mass, in micrograms, of silverin the blank primary bead combined with the mass
of silverin the blank determination of the residue recovered;
m5 isthe mass, in micrograms, of silverremaining in the prill;
mimp isthe totalmass, in micrograms, of impuritiesin the partingand washing solutions

obtained by the procedure specified in Annex G;
H isthe hygroscopic moisture content,in percent,of the testportion (in the case of a pre - dried
testportionbeing used, H = 0).
Ifcomplete recovery of silverduring the cupellationprocess is not obtained, correct the mass fraction
of silverof the testportion(see Annex E).

ISO 10378:2016(E)
9 Precision
9.1 Expression of precision
The precisionof thisanalyticalmethod isexpressed by the following formulae:
Zinc concentrates
Gold
Sr = 0 ,022 5 X + 0 ,032 5
SL =0,050 4 X + 0,0571 (5)
Silver (6)
Sr =0,0091 X +2,0575
SL =0,016 6 X +5,775 0 (7)
Lead concentrates (8)

Gold
Sr = 0 ,030 9 X + 0 ,033 6
Get more FREE standards from Standard Sharing Group and our chats SL =0,058 2
X + 0,0553 (9)
Silver (10)
Sr = 0 ,003 2 X + 5 ,843 8
SL = 0,003 2 X + 16,9747 (11)
Copper concentrates (12)

Gold
Sr = 0 ,004 4 X + 0 ,2 42 2
SL = 0,008 4 X + 0,2651 (13)
Silver (14)
Sr = 0 ,007 5 X + 0 ,968 8
SL =0,010 9 X + 2,155 8 (15)
where (16)
X isthe mean mass fractionof gold or silver,in grams per tonne, in the sample;
14
ISO 10378:2016(E)
Sr isthe within-laboratory standard deviation,in grams of gold or silverper tonne;
SL isthe between-laboratories tandard deviation,in grams of gold or silverper tonne.

NOTE Additionalinformationisgiven in Annex L .
9.2 Method for obtainingthe finalresult(seeAnnex H)
Calculatethe followingquantitiesfrom the duplicateresultsX1 and flowsheet X2 and process according to the
in Annex H :
Mean of duplicatesX = X1+X2 (17)

2
Within-laboratory standard deviation
Zinc concentrates
Gold determination
Sr = 0 ,022 5 X + 0 ,032 5 (18)
Silverdetermination
Sr 0,0091 X +2,0575
= (19)
Lead concentrates
Gold determination
Sr = 0 ,030 9 X + 0 ,033 6 (20)
Silverdetermination
Sr = 0 ,003 2 X + 5 ,843 8 (21)
Copper concentrates
Gold determination
Sr = 0 ,004 4 X + 0 ,2 42 2 (22)
Silverdetermination
Sr = 0 ,007 5 X + 0 ,968 8 (23)
Repeatabilitylimit
e = 2,8 S r (24)
9.3 Precisionbetween laboratories
The precisionbetween laboratoriesisused to determine the agreement between the resultsreported

by two (or more) laboratories.Itisassumed that allthe laboratoriesfollowed the same procedure.
Calculatethe followingquantities:

ISO 10378:2016(E)
Mean of finalresults
µ1 +µ2
µ
1,2 = 2
(25)
Between-laboratoriesstandard deviation
Zinc concentrates
Gold determination
SL =0,050 4 µ1,2 + 0,0571
(26)
Silverdetermination
SL =0,016 6 µ1,2 +5,775 0
(27)
Lead concentrates
Gold determination
SL =0,058 2 µ1,2 +0,0553
(28)
Silverdetermination
SL = 0,003 2 µ1,2 + 16,9747
(29)
Copper concentratesGet more FREE standards from Standard Sharing Group and our chats
Gold determination
SL =0,008 4 µ1,2 + 0,2651
(30)
Silverdetermination
SL =0,010 9 µ1,2 + 2,155 8
(31)
Within-laboratorystandard deviation
Zinc concentrates
Gold determination
Sr = 0 ,022 5 µ 1 ,2 + 0 ,032 5
(32)
Silverdetermination
Sr = 0 ,009 1 µ 1 ,2 + 2 ,057 5
(33)
Lead concentrates
16
ISO 10378:2016(E)
Gold determination
Sr = 0 ,030 9 µ 1 ,2 + 0 ,033 6 (34)
Silverdetermination
Sr = 0 ,003 2 µ 1 ,2 + 5 ,843 8 (35)
Copper concentrates
Gold determination
Sr = 0 ,004 4 µ 1 ,2 + 0 ,242 2 (36)
Silverdetermination
Sr = 0 ,007 5 µ 1 ,2 + 0 ,968 8 (37)
Permissibledifference
2
S
P =2,8 S2 +
r
(38)
L 2
Range
E= µ1 +µ2 (39)
where
μ1 isthe finalresult,in grams of gold or silverper tonne, reported by laboratory 1;
μ2 isthe finalresult,in grams of gold or silverper tonne, reported by laboratory 2 .
IfE islessthan or equal to P,the finalresultsare in agreement.
9.4 Check of trueness
9.4.1 General
The trueness of the analyticalmethod can be checked by applying itto a certified reference material
(CRM). The procedure isthe same as thatdescribedin Clause7 .When the precisionhas been con firmed,
the finallaboratory resultcan be compared with the certified value, Ac.
The followingtwo possibilitiesexist:

A C
µc − c ≤ (40)
Ifthisconditionexists,the differencebetween the reported resultand the certified value isstatistically insignificant.
A C
µc − c > (41)
If this condition exists,the difference between the reported result and the certified value is
statisticallysignificant.

ISO 10378:2016(E)
In Formulae (40) and (41),the symbols have the followingmeanings:
μc isthe finalresult,in grams of gold or silverper tonne,of the certified reference material;
Ac isthe certified value,in grams of gold or silverper tonne,of the certified reference material;
C isa quantity,in grams of gold or silverper tonne,depending on the type of the certified refer -ence
materialused,as de fined in 9.4.2.
9.4.2 Type of certified reference material (CRM) or reference material (RM)
The reference materials used for this purpose should be prepared and certified in accordance with
ISO Guide 35.
9.4.2.1 Reference material certified/characterizedby an interlaboratorytestprogramme
The quantity C (see 9.4.1),in grams of gold or silverper tonne,isgiven by Formula (24):
2
Sr
S2 A
C=2 SL
2
+ n + { c} (42)
where
2
S {Ac}isthe variance of the certified value;
n isthe number of replicatedeterminations.
9.4.2.2 Reference material certified/characterizedby one laboratory

The quantity C (see 9.4. 1),in grams of gold or silverper tonne,isgiven by Formula (43):
2
2 Sr
C=2 2 SL + n (43)
NOTE Itisrecommended that thistype of certified reference materialbe avoided,unlessthe particularCRM

isknown to have an unbiased certified value.
10 Test report
The testreport shallincludethe followinginformation:
a) identificationof the sample;
b) reference to thisInternationalStandard,i .eISO. 10378;
c) mass fractionof gold of the sample, expressed in grams per tonne;
d) mass fractionof silverof the sample, expressed in grams per tonne;
e) date on which the testwas carriedout;
f) any occurrences noticed during the determination that may have had an influence on the results.
18
ISO 10378:2016(E)
Annex A
(normative)
Procedure for the preparation and determination of the mass of a predried

testportion
A.1 General
This Annex specifies a method for the preparation and determination of the mass of a predried test portion in
the analysisof copper,lead,and zincsulfide concentrates.The method isapplicableto copper, lead, and zinc
sulfide concentrates not susceptibleto oxidation and having hygroscopic moisture contentsranging from 0,05% to
2 %.
A.2 Principle
The testportionto be used for analysisisdried in airin an oven maintained at 105 °C ± 5 °C.The dried test portion
isthen weighed and used for the analysisNo. correctionfor hygroscopic moisture isrequired.
A.3 Reagents
A.3.1 Desiccant, such as self-indicatingsilicagel or anhydrous magnesium perchlorate.
WARNING — Care needs to be taken whenever disposingof exhaustedmagnesium perchlorate and allother
laboratorychemicals.Environmentalregulationsoften apply.Users should seek specialist’sadvice to determine an
appropriate,effective,health-conscious,safety-conscious, and environmentally sound means of disposal.
A.4 Apparatus
Ordinary laboratoryequipment, and the following.
A.4.1 Analyticalbalance,sensitiveto 0,1mg.
A.4.2 Weighing vessels, of glass or silicaor corrosion-resistantmetal, with externallyf-itting

airtightcovers.
For small testportions(of mass lessthan 3 g),the mass of the vesselshallbe as small as possible,. e.
lessthan 20 g.
A.4.3 Laboratoryoven,capable of maintaining a temperature of 105 °C ± 5 °C.
A.5 Procedure
A.5.1 Preparation of the weighing vessel
Dry the weighing vesseland itscover ( A.4.2) by heating in the laboratory oven ( A.4.3) at 105 °C ± 5 °C for lh
.Transfer the vesseland itscover to a desiccatorcontaininga suitablefresh desiccant(A.3.1) and allow coolingto
ambient temperature.

ISO 10378:2016(E)
A.5.2 Test portion
Tare the dried weighing vesseland itscover (A.5.1) .Immediately add the mass of laboratory sample specified
for analysis.An accurate totalmass of the testportion and weighing vesselisnot required
at thispoint.
A.5.3 Determination of the dry mass of testportion
Transfer the uncovered weighing vessel containing the test portion and the vessel cover to the
laboratoryoven (A.4.3) and dry at 105 °C ± 5 °C for 2 h.After the 2 h period,remove the weighing vessel and dry
testportion from the oven, replacethe vesselcover,and allow coolingto ambient temperature in the
desiccator.When cool,remove the weighing vesselcontainingthe dry testportion and the vessel cover from the
desiccatorand weigh to the nearest 0,1 mg (m6 ),after slightlyliftingthe cover and quicklyreplacingit.Transfer the
testportion intothe appropriateanalyticalapparatus and immediately reweigh the empty weighing vesseland
itscover.Record the mass (m7 ) to the nearest 0,1mg.
For new concentrates of unknown characteristics,itisadvisableto repeat the drying for another 2 h at 105 °C ±
5 °C and to reweigh the weighing vesselcontainingthe testportion and the vesselcover to the
nearest 0,1 mg ( 6 ) . The mass of the testportion can be considered to be constant ifthe difference
between and ′ is lessthan or equal to 0,5 mg. Ifthiscondition is not achieved,the drying and
6 6
weighing steps should be repeated.
A.6 Calculationof the dry mass of the testportion

The dry mass of the testportion ( 8 ),in grams, isgiven by Formula (A.1):
8= 6− 7 (A.1)
where
6 isthe mass, in grams, of the dried testportion plus the weighing vesseland itscover;
7 isthe mass, in grams, of the empty weighing vesselplus itscover.
The mass of the dry testportion isthe mass to be used to calculatethe mass fractionof element in the
laboratorysample on a dry basis.No correctionfor hygroscopic moisture isrequired.
20
ISO 10378:2016(E)
Annex B
(normative)
Trialfusion
B.1 General
The mass of oxidizingagent,potassium nitrateor sodium nitrate(4.4) in the charge depends on the reducing
power of the testsample.
A trialfusion iscarried out to ensure that the testfusion yieldsa lead button of mass between 30 g and
45 g.
B.2 Procedure
Mix a test portion with the appropriate masses of flux components. Typical masses of flux components for
copper,lead,and zincconcentratesare shown in Tables 1 to 3 ,respectively.
Carry out the fusion as specified in 7.5.
Weigh the lead button obtained from the fusion.Ifthe button weighs lessthan 30 g or more than 45 g,an
adjustment of the oxidizing/reducing properties of the fusion mixture may be made using the following
approximations:
a) the addition of 1 g of potassium nitratewilldecrease the button mass by 4 g;
b) variationsin the mass of the test portion will affect the button size according to the following approximation:
1 g of sulfur in the testportion willyieldapproximately 19 g of lead;
c) for roasted samples or other samples not giving at least30 g of lead button, f lour ( 4.5) may be added to
increase the reducing propertiesof the charge; the flour shallbe thoroughly mixed with the other
components in the charge (for information, 1 g of flour gives approximately 10 g to 12 g of lead) .

ISO 10378:2016(E)
Annex C
(normative)
Blank determination
C.1 General
A blank determination is carried out to determine the mass fraction of gold and silverof the assay
reagents,principallylithargeIt.isrecommended that the blank determination be performed in duplicate.
C.2 Procedure
Thoroughly mix the flux components with sufficientf lour (4.5).Typical masses of flux components for
copper,lead,and zincconcentratesare shown in Tables 1 to 3,respectively,and potassium nitrate( 4.4 )
should be omitted from the components. The amount of flour (4.5) is usually 3 g to 4 g, as a reducing
agent to produce a lead button of 30 g to 45 g.
Continue the blank determination in accordance with 7.5 to 7.7.
Combine the primary and secondary blank beads and determine the gold and silverconcentration of
the blank solutionsin accordance with 7.9.
22
ISO 10378:2016(E)
Annex D
(normative)
Inquartation
D.1 General
To ensure complete partingof the bead,the ratioof silverto gold has to exceed 2,5to 1.Beads in which thisratiois
not reached,i .ethose. in which the mass fractionof gold exceeds 30 % are inquarted.
However, in caseswhere the silverisdetermined by AAS or ICP,the silvercannot be determined in the inquarted
bead, and so separatedeterminationsfor gold and silverwillbe necessary.The gold should be determined by
inquartationin accordance with thisannex, and the silverby the dissolutionmethod specified in 7.9without the
partingoperation.
Ifthe silverisdetermined by the gravimetricmethod insteadof the procedure specified in 7.10,weigh the primary
bead before the inquartationInquart. the bead in accordance with thisannex, carry out the partingby the
procedure specified in 7.8,and determine the impuritiesin the partingsolutionand washing by the procedure
specified in Annex G.
NOTE 1 Ifthe approximate silverto gold ratioisknown to be lessthan 2,5to 1,the appropriatemass of silver
to give a ratioof 4 to 1 can be added priorto the f irstfusion.
NOTE 2 Ifthe mass of the gold islessthan 50 μg, the bead can be dissolvedwithout partingand the gold and
silverconcentrationcan be determined as specified in 7.9.In such cases,inquartationisnot necessary.
Silvershould be determined by the method in 7.9 without parting,provided that the product of mass of the
testportionby mass fractionof the silver,. emass. in the testportion,issmallerthan 7 500 μg.
The testportionof 20 g,therefore,istoo much to determine the silver,where the mass fractionof the element
exceeds325 g/t.
D.2 Procedure
Weigh the bead priorto any attempt at parting(m0).
Add a mass of silver(4 .10) sufficient o obtaina silverto gold ratioof 4 to 1.
Wrap the bead and the silvertogetherin 0,5g of leadfoil(4 .9),cupelin accordancewith 7.6 to obtaina silver-
richbead and determine the mass fractionof gold as specified in 7.8.

ISO 10378:2016(E)
Annex E
(normative)
Determination of vaporizationlossof silverduring the

cupellationprocess
E.1 General
To prevent loss of silverduring the cupellation process, itisvery important that furnace conditions be as
specified in 7.6.Itisrecommended that the lossof silverduring the cupellationprocessbe determined, to decideupon
the furnace conditions.
Ifcomplete recovery is not obtained, the mass fraction of silverof the test portion shallbe corrected.
E.2 Procedure
Weigh the same mass of silver(4 .10) as the mass fractionof silverin the testportion.Wrap itin 40 g of lead
foil(4.9) and cupel in accordance with 7.6 to obtaina silverbead.Retreat the cupel in accordance
with 7.7 and combine the primary and secondary beads in the porcelain crucible.
Add 10 ml of dilutenitricacid(4.8) to the beads in the porcelain crucible and heat gently on a hotplate
( 5.1 3) for 20 min, or untilthe reactionceases.
Determine silverconcentrationof the solutionsin accordance with 7.10.
E.3 Calculationof lossof silverduring the cupellationprocess

Loss of silverduring the cupellationprocess(LAg ),expressed in percent, is given by Formula (E.1):
m−m1
L = × 100 (E.1)
Ag m
where
m1 is the mass, in micrograms, of silverin the solutions;
m isthe mass, in micrograms, of the silvermetal weighed.
E.4 Correction of mass fractionof silverof the testportion

Ifsufficientrecovery of silverduring the cupellation process is not obtained, the mass fraction of silver
′
of the testportion( w ) ,expressed in grams per tonne, should be corrected by Formula (E .2):
Ag
w
Ag ×
w′ = 100 (E.2)
Ag −L
100
Ag
where
′
w is the mass fraction of silver,in grams per tonne, of test portion calculated by Formula (3);
Ag
LAg is the loss of silver,in percent, calculated by Formula (E .1) .

ISO 10378:2016(E)
Annex F
(normative)
Sulfuricacid — Parting
F.1 General
Ifthereisdanger of the gold sponge crumbling during the partingoperation,itisrecommended thatthe operationbe
carriedout with sulfuricacid.
F.2 Reagent
F.2.1 Sulfuricacid,concentrated(ρ20 1,84g/ml),chloridecontent <0,5μg/ml.
F.2.2 Sulfuricacid,diluted1 + 5.
Slowly add 200 ml of concentratedsulfuricacid(F.2 .)1 to 1 000 ml of water,while stirring.
F.3 Apparatus
F.3.1 Parting flask,of capacity60 ml.
F.4 Procedure
Transferthe bead prepared in 7.6to a partingf laskand add 5 ml to 20 ml of sulfuricacid(F.2 .)1.Dissolve the
silverby gentlyheatingfor 5 min to 10 min.
NOTE 1 Itisessentialthat chloridebe absent during parting;otherwise,some of the gold may dissolve.
When the bead is treated with hot sulfuricacid,silverwillstartto dissolve,provided that the ratio of silverto gold in
the bead exceeds 2,5 to 1. The rate of dissolutionincreaseswith increasingmass
fractionof silverof the bead. Rapid attack of the bead should be avoided by furtherdilutionand slow
heating to prevent disintegrationof the gold.Should the ratioof silverto gold be lessthan 2,5to 1 as
shown by failureto part in hot sulfuricacid,the bead should be inquarted(seeAnnex D).
After cooling,carefullypour the solutionintoa 200 ml beaker by decantationto avoid losses.
Wash the flaskand gold with several10 ml to 20 ml volumes of dilutesulfuricacid ( F.2 .),2followed by several10
ml to 20 ml volumes of hot water, and carefullypour the solutionsintothe 200 ml beaker by decantationto avoid
lossesCollect.allthe washings in the same 200 ml beaker.
Reserve the solutionfor the determinationof silveras specified in 7.10.
For the determination of silverin 7.10, prepare the calibrationsolutionsto contain the same concentrationsof
sulfuricacidas the testsolutions.
NOTE 2 The possibilityof gold particlesoccurring in the collectedparting and washing solutionscan be determined by
evaporatingthe solutions lowly down to 2 ml to 3 ml, then continuingwith the determinationas specified in 7.9.
Fillthe partingf laskwith water and cover with a 30 ml porcelaincrucibleTurn. the flaskupside down in order to
sink the gold into the crucibleRemove. the flask and discardthe water in the crucibleby
carefuldecantation.

ISO 10378:2016(E)
Dry the gold sponge in the porcelaincrucibleon the hotplate.
Place the cruciblein the muf flefurnace (5.2) to anneal the gold at dullred heat for approximately 5 min.
Cool and weigh the gold,in micrograms, to the nearest 1 μg ( m1) .
Ifthe mass of the gold islessthan 50 μg, itisrecommended that the gold be dissolvedand determined by the
procedure specified in 7.9.
Ifthe mass of the gold islessthan 50 μg, repeat the fusion and cupellation,then dissolvethe prepared bead and
determine the gold and silverconcentrations as specified in 7.9 without parting.This procedure, however, cannot
be applied ifthe product of mass of testportion by mass fractionof silver, i.emass. in testportion,islargerthan 7
500 μg.
Ifthe sensitivityof the microbalance is0,1 μg, the applicablerange of the gravimetric method can be extended
to 5 μg of gold.In such cases,weigh the gold prill,in micrograms, to the nearest 0,1μg ( m1).
Reserve the gold prillto determine silverin the prillby combining severalof the weighed prillsof the same
laboratorysample, dissolvingthese and determining the silverconcentrationas specified in 7.9.
Platinum and palladiumare removed from the prillduring partingwith nitricacid.Ifthe determination
of these elements remaining in the prillis considered necessary,determine these by the procedure specified in
7.9 followed by the additionof platinum and palladium to the standard solutionsin relevant proportions.Ifa
sufficientdetection limitfor AAS or ICP cannot be obtained on a singleprillbasis,a largenumber of prillsof the
same laboratorysample should be combined.
26
ISO 10378:2016(E)
Annex G
(normative)
Determination of impuritiesin partingsolutionsand washings
G.1 General
Ifthe mass fractionof silverin the sample is high,the gravimetricmethod is recommended for the
accurate determination of silverFor. thismethod, itisnecessary to determine impuritiesin the parting
solutionand washing in accordance with thisAnnex.
G.2 Reagent
G.2.1 Hydrochloricacid,diluted1 + 1.
Slowly add 500 ml of concentrated hydrochloricacid ( 4.11) to 500 ml of water,while stirring.
G.2.2 Bismuth ,minimum purity 99,99 %.
G.2.3 Lead,minimum purity 99,99 %.
G.2.4 Palladium,minimum purity 99,99 %.
G.2.5 Platinum,minimum purity 99,99 %.
G.2.6 Magnesium oxide,minimum purity 99 %.
G.2.7 Calcium carbonate ,minimum purity 99,99 %.
G.2.8 Standard solutions.
Standard solutionsshould be prepared at the same ambient temperature as that at which the
G.2.8.1 Bismuth ,standard stock solutionA (500 μg of Bi/ml).
Weigh 0,5000 g of bismuth metal (G.2 .2) to the nearest0,1mg. Transferto a 100 ml beaker,add 20 ml of
dilutenitricacid (4.8) and warm to dissolve.Cool and transferto a 1 000 ml volumetric f lask,f ill up with water
nearly to the mark, mix and cool to room temperature; then fillup exactlyto the mark and mix again.
G.2.8.2 Bismuth ,standard solutionB (20 μg of Bi/ml).
Pipette10,00ml of bismuth standard stock solutionA (G.2 .8.)1into a 250 ml volumetric f lask,f illup with water
nearly to the mark, mix and cool to room temperature; then fillup exactly to the mark and mix again.

ISO 10378:2016(E)
G.2.8.3 Lead ,standard stock solutionA (500 μg of Pb/ml).
Weigh 0,5000 g of leadmetal (G.2.)3 to the nearest0,1mg. Transferto a 100 ml beaker,add 20 ml of dilute
nitricacid(4.8) and warm to dissolveCool. and transferto a 1 000 ml volumetric f lask,f illup with water nearly to
the mark, mix and cool to room temperature; then fillup exactlyto the mark and mix again.
G.2.8.4 Lead ,standard solutionB (10 μg of Pb/ml).
Pipette10,00 ml of lead standard stock solutionA (G.2 .8.)3into a 500 ml volumetric flask,f illup with water
G.2.8.5 Palladium,standard stock solutionA (200 μg of Pd/ml).
Weigh 0,1000 g of palladiummetal (G.2 .)4 to the nearest0,1mg. Transferto a 100 ml beaker,add 10 ml of aqua
regia(4.13) and warm to dissolveCool. and transferto a 500 ml volumetric f lask,f illup with water nearly to the
mark, mix and cool to room temperature; then fillup exactlyto the mark and mix again.
G.2.8.6 Palladium,standard solutionB (10 μg of Pd/ml).
Pipette10,00 ml of palladium standard stock solutionA (G.2 .8.)5into a 200 ml volumetric flask,f ill up with water
and mix again.
G.2.8.7 Platinum ,standard stock solutionA (1 000 μg of Pt/ml).
Weigh 0,1000 g of platinum metal (G.2 .5) to the nearest0,1mg. Transferto a 100 ml beaker,add 10 ml of
aqua regia(4.13) and warm to dissolveCool. and transferto a 100 ml volumetric f lask,f illup with water Get more FREE standards from Standard
Sharing Group and our chats
nearly to the mark, mix and cool to room temperature; then fillup exactlyto the mark and mix again.
G.2.8.8 Platinum ,standard solutionB (50 μg of Pt/ml).
Pipette10,00 ml of platinum standard stock solutionA (G.2 .8.)7to a 200 ml volumetric flask,f illup with water
G.2.8.9 Magnesium ,standard stock solutionA (500 μg of Mg/ml).
Weigh 0,829g of magnesium oxide (G.2 .6) to the nearest0,1mg. Transferto a 100 ml beaker,add 20 ml of
dilutehydrochloric acid (G.2 .),1and warm to dissolveCool. and transferto a 1 000 ml volumetric flask,f illup with
water nearly to the mark, mix and cool to room temperature; then fillup exactlyto the mark and mix again.
G.2.8.10Magnesium ,standard solutionB (5 μg of Mg/ml).
Pipette10,00ml of magnesium standard stock solutionA (G.2 .8.)9into a 1 000 ml volumetric f lask,f ill up with
water nearly to the mark, mix and cool to room temperature; then fillup exactlyto the mark and mix again.
G.2.8.11Calcium,standard stock solutionA (500 μg of Ca/ml).
Weigh 1,249 0 g of calcium carbonate (G.2 . 7) to the nearest 0,1 mg. Transfer to a 100 ml beaker,
add 20 ml of dilutehydrochloric acid (G.2 . ),1and warm to dissolveCool. and transferto a 1 000 ml
volumetric f lask,f illup with water nearly to the mark, mix and cool to room temperature; then fillup exactlyto
the mark and mix again.
28
ISO 10378:2016(E)
G.2.8.12Calcium,standard solutionB (20 μg of Ca/ml).
Pipette10,00ml of calcium standard stock solutionA (G.2 .8.11)into a 250 ml volumetric f lask,f ill up with water
and mix again.
G.2.9 Bismuth/lead/palladium/platinum/magnesium/calciumcalibrationsolutions
Calibrationsolutionsshould be prepared at the same ambient temperature as that at which the

Pipette0,0 ml, 1,00 ml, 2,00 ml, 3,00 ml, and 5,00 ml of bismuth standard solution(G.2 .8.),2lead
standardsolution(G .2 .8.),4palladiumstandardsolution(G .2 .8.),6platinumstandardsolution(G .2 .8.),8
magnesium standardsolution(G .2 .8.10),and calciumstandardsolution(G .2 .8.12)intoa seriesof 50 ml
one-mark volumetric f lasks.
Add 5 ml of aqua regia(4.13) to each flask,f illup nearly to the mark with water, mix and cool to room
temperature;then fillup exactlyto the mark and mix again.
These solutionscontain0,0μg of Bi,Ca/ml, 0,40 μg of Bi,Ca /ml, 0,80 μg of Bi,Ca /ml, 1,20μg of Bi,Ca / ml and
2,00 μg of Bi,Ca /ml; 0,0 μg of Pb, Pd/ml, 0,20 μg of Pb, Pd /ml, 0,40 μg of Pb, Pd /ml, 0,60 μg of Pb, Pd /ml
and 1,00 μg of Pb,Pd /ml; 0,0μg of Pt/ml,1,00 μg of Pt/ml,2,00μg of Pt/ml,3,00μg of Pt/ml and 5,00 μg of Pt/ml;
and 0,0 μg of Mg/ml, 0,10 μg of Mg/ml, 0,20 μg of Mg/ml, 0,30 μg of Mg/ml, and 0,50 μg of Mg/ml,
respectively,and shallbe freshlyprepared.
G.3 Procedure
Take the partingsolutionsand washings thatwere reservedin7.8.Heat to evaporate to dryness.Add 5 ml of
aqua regia(4.13) and warm to dissolveCool. and transferto a 50 ml volumetricf lask,f illup with water nearly to
the mark, mix and coolto room temperature;then fillup exactlyto the mark and mix again.
Aspirate the test solutionsand bismuth/lead/palladium/platinum/magnesium/calciumcalibration solutions(G .2 .)9

into the atomic absorptionspectrometer(5.10) and measure the absorbance.As a guide,the atomic
absorptionsettings hown in Table G.1 are recommended. However, the instrument
should be optimized to be free from any interferenceand to give maximum sensitivityand as near as
practicalto a linear elationshipbetween absorbanceand concentration.
Table G.1— Recommended atomic absorptionsettings
Parameter Bismuth Lead Palladium Platinum Magnesium Calcium

Flame air/acetylene(oxidizing) N 2O/acetylene
Wavelength 223,1nm 283,3nm 244,8nm 265,9nm 285,2nm 422,7nm
Lamp current 10 mA 5 mA 5 mA 10 mA 4 mA 10 mA
Background corrector on on on on on on
Aspirationrate optimizefor maximum signal
Integrationtime 3s
Number of integrations 5
Absorbance of 1 μg/ml 0,02 0,04 0,05 0,003 0,15(0,1μg of 0,25
calibrationsolution Mg/ml)
NOTE 1 The measurements of elements that are impossibleto be contained in the parting solutionand washings can be
skipped.
NOTE 2 Ifsilverchlorideprecipitates,the top clearlayersolutioncan be used as the testsolution.

ISO 10378:2016(E)
In order to clean out the nebulizersystem, itisrecommended to aspiratethe cleaningsolution,which is, for
instance,prepared by carefullyadding 500 ml of hydrochloricacid ( 4.11) and 100 ml of concentrated nitricacid (4.7)
to 400 ml of water, between measurements.
Plot a calibrationgraph absorbance versus concentrationand determine the bismuth, lead,palladium,

platinum,magnesium, and/or calcium concentrations,in micrograms per millilitre,inthe testsolutions, followed by
calculationof the mass (ma),in micrograms, of the metals using Formula (G.1):
ma = ρ × 50 (G.1)
where ρ isthe mass concentrationof each metal.
Sum up the mass of allelements determined to calculatethe amount of impuritiesin the partingsolution and
washings (mimp ).
Alternatively,an ICP atomic emission spectrometer (5.11) can be used for the determination of bismuth,
lead,palladium,platinum,magnesium, and calcium at the appropriate wavelength. Typical wavelengths
are 223,06 nm for bismuth, 220,35 nm for lead,340,46 nm for palladium,214,42 nm for platinum, 279,55 nm for
magnesium, and 393,37 nm for calcium.However, the instrument should be optimized to be free from any
interferenceand to give maximum sensitivityand as near as practicalto a linear relationshipbetween absorbance
and concentration.
During allAAS or ICP determinations,the testsolutionsand calibrationsolutionsshould have the same

temperature as well as the same acid(s)concentration.
30
ISO 10378:2016(E)
Annex H
(normative)
Flowsheet of the procedure for the acceptance of analyticalvalues for

testsamples (see 9.2)
Perform X1 ,X 2
Yes
X1 X2 |≤ r X X + X 2 )/2
| , ഥ =( 1
No
Yes Range of Yes

| , |≤ 1,2 3 X X X r X X X X
X1 X 2 r Perform X 1 , , ,≤ 1,2
2 3 ഥ=( 1+ 2 + )/3
3
No
No
X X
Perform 3 , 4 Perform X4
Range of Yes X X X X X
X1,X 2,X 3,X 4,≤ 1,3r ഥ =(1+ 2 + 3 + 4 )/4
Xഥ = Median of X1,X 2,X 3,X 4

ISO 10378:2016(E)
Annex I
(informative)
Flowsheet of the method
7.4Charge preparation
In case bead istoo smallto recover
Add 1 mg of Pd
Insteadof inquartation
Add Ag
Slag
7.5Primary fusion
Lead button
Cupel
7.6Cupellation 7.7Retreatment of residues
Primary bead Secondary bead
Au <50 g Yes or In case of added 1 mg of Pd

Ag <7 500 g Combine
For Ag determination
No/Yes 7.9Dissolutionof bead
In case of Ag <7 500 g
Method for Ag Gravimetricmethod

7.6Weighing of bead
detemination
ASSGetor ICPmoremthodFREE standards from Standard Sharing Group and our chats
Primary bead 7.9Measurement of
No Au, Ag by ASS of ICP
Ag/Au >2,5 Ag/Au >2,5
Annex D Inquartation
for Au determination
Yes Yes
Except inquartation
7.8Parting 7.8Parting
Ag solution Ag solution
Au prill Au prill
7.10Ag measurement Annex G Determination
by ASS or ICP of impurities
Yes Yes
Au <50 g Au <50 g
No/Yes No/Yes
7.8Weighing of prill 7.8Weighing of prill
7.9Dissolutionof prill
Ag, (Pt,Pd) Au,Ag Ag, (Pt,Pd)

7.9Measurement by ASS or ICP
Figure I.1— Flowsheet of the method
32
ISO 10378:2016(E)
Annex J
(informative)
Roasting method
J.1 General
Ifarsenicispresent in the sample at a mass fractionabove 2 %, thismay cause interferencewith the
cupellationprocedure. The followingroastingprocedure willremove thiselement by volatilizingitas sulfide.
J.2 Procedure
Weigh the testportion(6.2) intoa roastingdish that has been coated with chalk or lithargeto prevent
stickingSpread. the testportion evenly on the coating.
Place the dish in the muf flefurnace ( 5.2) maintained at 450 °C for 2 h.
Gradually increasethe temperature of the muf fle furnace to 600 °C and heat for another 2 h. Stirthe
testportion every 30 min during roasting.
Remove the dish from the muf fle furnace and cool.Transfer the testportion and thoroughly mix with the flux
components, using part of the lithargeas a coating.
Continue with the primary fusion (7.5),but in thiscase determine the amount of flour required in the charge.

ISO 10378:2016(E)
Annex K
(informative)
Guide to the preparationof dilutionsfor the determination of silverin

partingsolutionsand residues
See TablesK .1 and K.2.
Table K.1 — Gold and silverin testsolutionsin 7.9
Total
Mass in testpotion Original Aliquotto Final
dilution
μg volume take volume
factor
Gold Silver ml ml ml 50
<50 <250 50 50 50 50
— 250 to 500 50 20 50 125
— 500 to 1 200 50 10 50 250
— 1 200 to 2 400 50 10 100 500
— 2 400 to 4 800 50 10 200 1 000
— 4 800 to 7 500 50 10 500 2 500
Table K.2 — Silverin testsolutionsin 7.10
Mass of silverin test Original Aliquotto Final Total

portion volume take volume dilution
μg ml ml ml factor
<500 100 100 100 100
500 to 1 000 100 20 50 250
1 000 to 2 000 100 20 100 500
2 000 to 4 000 100 10 100 1 000
4 000 to 8 000 100 10 200 2 000
8 000 to 20 000 100 10 500 5 000
20 000 to 40 000 100 10 1 000 10 000
NOTE The mass in the testportionisthe product of the mass of testportionand the concentrationof
gold and silver.
34
ISO 10378:2016(E)
Annex L
(informative)
Derivation of precisionequations
L.1 General
This internationalStandard was tested in an interlaboratorytestprogramme involving 5 countries and 16
laboratories.The following samples were analysed.
a) Five samples of zinc concentrate covering the range 0,1 g/t to 2,3 g/t of gold and 42 g/t to 780 g/t of silver.
b) Six samples of lead concentrate covering the range 0,1 g/t to 6,7 g/t of gold and 390 g/t to
3 200 g/t of silver.
c) Five samples of copper concentrate covering the range 0,3 g/t to 200 g/t of gold and 60 g/t to 680 g/t of
silver.
The test programme was designed to determine the repeatabilityand within-laboratory and between-
laboratoriesreproducibilitiesingeneral,using the principlesof ISO 5725-2 .
L.2 Design of the testprogramme

The analyticaltest programme was designed with the aim of providing maximum information. Each
laboratory used two samples (two bags) of each concentrate and each sample was analysed twice
independently.
L.3 Test samples

This test programme used five samples of zinc concentrate, six samples of lead concentrate, and five
samples of copper concentrate.The composition of these samples isgiven in Tables L.1,L .2,and L.3.
L.4 Statisticalevaluation
The procedure for statisticalevaluation is illustratedschematically inFigure L.1 . The resultsof the
statisticalevaluationare summarized in Tables L.4 .to L.9 .
The estimated precisions( Sr, SL , r,and P) are plottedagainsttheircorresponding sample means on a graph as
shown in Figures L.2 to L.7,and the regressionequations of these precisionsagainstsample means were
computed and are presented in Tables L.4 to L.9.

ISO 10378:2016(E)
Table L.1— Composition of zinc concentrate samples
Sample numbers
Element
2001-Zn-1 2001-Zn-2 2001-Zn-3 2001-Zn-4 2001-Zn-5
Zn % (m/m) 49 50 54 36 49
Pb % (m/m) 3 0,9 1 15 3
Cu % (m/m) 0,3 0,6 1 0,6 0,3
Au g/t <0,1 <0,1 2 0,1 0,4
Ag g/t 160 79 43 790 520
S % (m/m) 30 33 32 28 31
As % (m/m) 0,01 0,03 0,03 0,31 0,06
Sb % (m/m) 0,01 <0,01 <0,01 0,23 0,02
Sn % (m/m) <0,01 <0,01 <0,01 0,35 <0,01
Bi % (m/m) <0,01 <0,01 <0,01 0,10 <0,01
Fe % (m/m) 8 10 6 10 10
SiO2 % (m/m) 3 1 1 2 2
Al2O 3 % (m/m) 0,6 0,2 0,2 0,5 0,09
CaO % (m/m) 0,9 0,1 0,1 0,1 0,2
MgO % (m/m) 0,5 0,2 0,03 0,05 0,5
Cd % (m/m) 0,2 0,1 0,3 0,2 0,3
Ni % (m/m) <0,01 <0,01 <0,01 <0,01 <0,01
Co % (m/m)Get more FREE<0,01 standards from0,02 Standard Sharing<0,01 Group <0,01andour chats <0,01
36
ISO 10378:2016(E)
Table L.2— Composition of lead concentrate samples
Sample numbers
Element
2001-Pb-1 2001-Pb-2 2001-Pb-3 2001-Pb-4 2001-Pb-5 2001-Pb-6
Pb % (m/m) 65 33 65 57 50 72
Zn % (m/m) 6 5 10 12 7 4
Cu % (m/m) 1 2 0,8 0,07 0,2 0,3
Au g/t 70 3 4 <0,1 <0,1 0,5
Ag g/t 2200 660 1300 390 1100 3200
S % (m/m) 17 30 17 19 23 14
As % (m/m) 0,3 0,5 0,1 0,03 0,03 0,03
Sb % (m/m) 0,2 0,2 0,3 0,1 0,09 0,2
Sn % (m/m) <0,01 <0,01 <0,01 <0,01 <0,01 <0,01
Bi % (m/m) 0,4 0,02 0,02 <0,01 <0,01 <0,01
Fe % (m/m) 4 20 3 5 11 3
SiO2 % (m/m) 2 0,5 0,7 3 2 3
Al2O 3 % (m/m) 0,3 0,07 0,3 0,1 0,5 0,1
CaO % (m/m) 0,9 0,7 0,04 0,06 0,5 0,3
MgO % (m/m) 0,3 0,2 0,06 0,01 0,3 0,7
Cd % (m/m) 0,03 0,01 0,03 0,2 0,03 0,02
Ni % (m/m) <0,01 <0,01 <0,01 <0,01 <0,01 <0,01
Co % (m/m) <0,01 <0,01 <0,01 0,02 0,01 <0,01

ISO 10378:2016(E)
Table L.3— Composition of copper concentrate samples
Sample numbers
Element
2001-Cu-1 2001-Cu-2 2001-Cu-3 2001-Cu-4 2001-Cu-5
Cu % (m/m) 33 24 37 26 37
Zn % (m/m) 0,2 0,06 0,1 4 0,08
Pb % (m/m) 0,04 0,02 0,03 4 0,02
Au g/t 54 53 0,9 0,4 200
Ag g/t 69 62 120 670 590
S % (m/m) 27 27 27 32 21
As % (m/m) <0,02 0,04 0,08 <0,02 0,1
Sb % (m/m) <0,02 <0,02 <0,02 0,1 <0,02
Sn % (m/m) <0,02 <0,02 <0,02 <0,02 <0,02
Bi % (m/m) <0,02 <0,02 <0,02 <0,02 <0,02
Fe % (m/m) 22 23 20 28 16
SiO2 % (m/m) 10 16 9 2 11
Al2O 3 % (m/m) 2 4 2 0,4 1
CaO % (m/m) 0,6 1 0,7 0,09 9
MgO % (m/m) 0,5 0,6 0,1 0,09 1
Cd % (m/m) <0,02 <0,02 <0,02 <0,02 <0,02
Ni % (m/m) <0,02 <0,02 <0,02 <0,02 <0,02
Co % (m/m) Get more<0,02FREE standards <0,02from Standard Sharing<0,02 Group and0,02our chats 0,02
38
ISO 10378:2016(E)
Raw data
Yes
Chemical ouliers? Rejectoutliers
No
Yes
Statisticaloutliers? Rejectoutliers
No
Perform two-way
ANOVA
Test sample Yes Combine analyticalresults

homogeneous? submittedby each laboratory
Yes
Statisticaloutliers? Rejectoutliers
No No
Outliersfound? Yes Perform one-way

ANOVA
No
Use precisionsestimated
from two-way ANOVA
Regressionsof
precisionvs level
Presentraw data and regression

Report
linesand in graphicalform
Figure L.1— Flowsheet of procedure for statisticalevaluationof analyticaldata resultingfrom internationaltests

ISO 10378:2016(E)
Table L.4— Summary of precisionsfor zincconcentratesamples — Gold
Sample number
K0 k n0 n X r P Sr SL SL /Sr
(see Table L.1 )
2001-Zn-1 8 8 31 31 0,044 0,082 0,130 0,029 0,042 1,415
2001-Zn-2 8 8 31 31 0,901 0,226 0,327 0,081 0,102 1,262
2001-Zn-3 8 8 31 31 2,292 0,207 0,502 0,074 0,171 2,313
2001-Zn-4 8 8 31 31 0,107 0,082 0,131 0,029 0,042 1,445
2001-Zn-5 8 8 31 31 0,160 0,079 0,299 0,028 0,105 3,724
The regression formulae are Correlationcoefficient
0,8052
r = 0,063 0 X + 0,0911
0,9087
P = 0,1476 X + 0,1745
0,8052
Sr = 0,0225 X + 0,0325
0,8947
SL = 0,0504 X + 0,0571
K0 Totalnumber of participatinglaboratories.
k Number of participatinglaboratoriesused for computation of precision.
n0 Total number of analyticalresults.

n Number of analyticalresultsused for computation of precision.
X Overallmean of the mass fractionof gold,in grams per tonne,of the sample.
r Permissiblewithin-laboratorytolerance(repeatability),in grams of gold per tonne.
P Permissiblebetween-laboratoriestolerance,in grams of gold per tonne.
Sr Within-laboratorystandard deviation,in grams of gold per tonne.

SL Between-laboratories tandard deviation,in grams of gold per tonne.
X Mean mass fractionof gold,in grams per tonne,of the sample.
40
ISO 10378:2016(E)
Table L.5— Summary of precisionsfor zincconcentrate samples — Silver
Sample number
K0 k n0 n X r P Sr SL SL/Sr
(see Table L.1 )
2001-Zn-1 8 7 31 27 150,03 10,484 21,281 3,744 7,124 1,903
2001-Zn-2 8 8 31 31 76,34 7,038 18,966 2,514 6,536 2,600
2001-Zn-3 8 8 31 31 42,34 3,170 20,833 1,132 7,397 6,534
2001-Zn-4 8 7 31 27 780,16 19,639 52,277 7,014 18,000 2,566
2001-Zn-5 8 7 31 27 503,96 28,098 47,803 10,035 15,528 1,547
0,8092
r= 0,0255 X + 5,7611
0,9708
P = 0,0496 X + 16,8383
0,8092
Sr = 0,009 1 X + 2,0575
0,9791
SL = 0,0166 X + 5,7750

X Overallmean of the mass fractionof silver,in grams per tonne,of the sample.
r Permissiblewithin-laboratorytolerance(repeatability),in grams of silverper tonne.
P Permissiblebetween-laboratoriestolerance,in grams of silverper tonne.
Sr Within-laboratorystandard deviation,in grams of silverper tonne.

SL Between-laboratories tandard deviation,in grams of silverper tonne.
X Mean mass fractionof silver,in grams per tonne,of the sample.

ISO 10378:2016(E)
Table L.6— Summary of precisionsfor lead concentratesamples — Gold
Sample number
(see Table L.2)
2001-Pb-1 8 7 31 27 6,786 0,781 1,332 0,279 0,433 1,551
2001-Pb-2 8 8 31 31 2,542 0,327 0,530 0,117 0,170 1,461
2001-Pb-3 8 6 31 23 4,170 0,284 0,991 0,102 0,347 3,414
2001-Pb-4 8 8 31 31 0,121 0,138 0,243 0,049 0,079 1,611
2001-Pb-5 8 8 31 31 0,103 0,115 0,146 0,041 0,044 1,065
0,9334
r= 0,086 6 X + 0,0942
0,9909
P = 0,1749 X + 0,1704
0,9334
Sr = 0,0309 X + 0,0336
0,9829
SL = 0,0582 X + 0,0553


42
ISO 10378:2016(E)
Table L.7— Summary of precisionsfor lead concentratesamples — Silver
Sample number K0 k n0 n X r P SL SL/Sr

Sr
(see Table L.2)
2001-Pb-1 8 5 31 19 2 199,23 18,207 96,745 6,502 34,245 5,266
2001-Pb-2 8 7 31 27 649,64 21,932 44,944 7,833 15,066 1,923
2001-Pb-3 8 6 31 23 1 316,89 30,814 59,256 11,005 19,680 1,788
2001-Pb-4 8 7 31 27 393,42 23,660 63,949 8,450 22,044 2,609
2001-Pb-5 8 6 31 23 1 098,75 27,881 50,124 9,958 16,458 1,653
2001-Pb-6 8 6 31 23 3 215,64 55,572 73,819 19,847 22,318 1,124
0,7073
r= 0,009 0 X + 16,3626
0,6346
P = 0,0112 X + 48,206 1
0,7073
Sr = 0,0032 X + 5,843 8
0,4869
SL = 0,0032 X + 16,9747



ISO 10378:2016(E)
Table L.8— Summary of precisionsfor copper concentratesamples — Gold
Sample number
Table L.3) K0 k n0 n X r P Sr SL SL/Sr
(see
2001-Cu-1 11 11 43 43 53,800 2,178 3,399 0,778 1,082 1,391
2001-Cu-2 11 8 32 35 53,618 1,932 2,580 0,690 0,782 1,133
2001-Cu-3 11 11 43 43 0,822 0,207 0,431 0,074 0,145 1,957
2001-Cu-4 11 10 39 39 0,298 0,116 0,237 0,041 0,079 1,916
2001-Cu-5 11 11 41 41 198,371 2,734 5,436 0,976 1,814 1,858
0,8331
r= 0,0123 X + 0,6781
0,9365
P = 0,0250 X + 0,8791
0,8331
Sr = 0,004 4 X + 0,2422
0,9494
SL = 0,0084 X + 0,2651


44
ISO 10378:2016(E)
Table L.9— Summary of precisionsfor copper concentrate samples — Silver
Sample number
(see Table L.3)
2001-Cu-1 11 10 43 39 70,25 4,139 6,971 1,478 2,260 1,529
2001-Cu-2 11 9 43 36 64,34 3,059 6,985 1,093 2,372 2,171
2001-Cu-3 11 10 43 39 127,33 6,519 13,825 2,328 4,655 2,000
2001-Cu-4 11 10 42 38 681,97 16,759 27,249 5,986 8,763 1,464
2001-Cu-5 11 10 41 39 581,95 15,056 28,164 5,377 9,312 1,732
0,9926
r= 0,0210 X + 2,7127
0,9715
P = 0,0338 X + 6,3231
0,9926
Sr = 0,007 5 X + 0,9688
0,9642
SL = 0,0109 X + 2,1558



ISO 10378:2016(E)
Key
X mean mass fractionof gold (g/t) Y
precision(g of Au/t)
Figure L.2— Least-squaresfitof precisionagainstthe mean mass fractionof gold in zinc concentrate
Key
X mean mass fractionof silver(g/t) Y
precision(g of Ag/t)
Figure L.3— Least-squaresfitof precisionagainstthe mean mass fractionof silverin zinc concentrate
46
ISO 10378:2016(E)
Key
Figure L.4 — Least-squaresfitof precisionagainstthe mean mass fractionof gold in lead concentrate
Key
Figure L.5— Least-squaresfitof precisionagainstthe mean mass fractionof silverin lead concentrate

ISO 10378:2016(E)
Key
Figure L.6 — Least-squaresfitof precisionagainstthe mean mass fractionof gold in copper

Get more FREE standardsconcentrfromStandardte Sharing Group and our chats
48
ISO 10378:2016(E)
Key
Figure L.7 — Least-squaresf itof precisionagainst the mean mass fractionof silverin copper
concentrate

ISO 10378:2016(E)
Bibliography
[1] ISO 12743:2006, Copper, lead, zinc and nickel concentrates — Sampling procedures for determination of
metal and moisture content
[2] ISO 5725-2, Accuracy (trueness and precision)of measurement methods and results— Part 2: Basic
method for the determinationof repeatabilityand reproducibilityof a standard measurement method
[3] ISO Guide 35, Reference materials— Generaland statisticalprinciplesfor certification
50
ISO 10378:2016(E)
ICS 73.060.99
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ISO 10378 Analisis Au y Ag

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INTERNATIONAL ISO

Copper, lead and zinc sulfide concentrates

Concentrés de sulfurede cuivre,de plomb et de zinc— Dosage de

InternationalOrganization for Standardization © ISO 2016

COPYRIGHT PROTECTED DOCUMENT

ISO copyright office

ii © ISO 2016 – Allrightsreserved

Foreword .................. ................................................................................................... v

© ISO 2016 – Allrightsreserved iii

Annex I (informative) Flowsheet of the method .......................................................................32 .

Annex J (informative)Roasting method ...............................................................33........ ..........

Annex K (informative) Guide to the preparationof dilutionsfor the determination of silver

Annex L (informative)Derivationof precisionequations ...............................................35 ...............

Copper, lead and zinc sulfide concentrates — Determination of

ISO 385, Laboratoryglassware— Burettes

ISO 648, Laboratoryglassware— Single-volumepipettes

ISO 1042, Laboratoryglassware— One-mark volumetricf lasks

ISO 3696, Water for analyticallaboratoryuse — Specificationand testmethods

ISO 4787, Laboratoryglassware— Volumetricinstruments— Methods fortestingofcapacityand for use

© ISO 2016 – Allrightsreserved 1

The stagesthat comprise the determinationsare describedin 3.2 to 3.6 inclusive.

3.6 Correction for blank contamination

4.1 Sodium carbonate ,anhydrous.

4.4 Potassium nitrateor sodium nitrate

4. 6 Borax ,fused anhydrous sodium tetraborate(borax glasspowder).

4. 7 Nitricacid,concentrated( ρ20 1,42g/ml),chlorideconcentration<0,5μg/ml.

Slowly add 500 ml of concentratednitricacid(4.7) to 500 ml of water,while stirring.

4.10 Silver,of minimum purity99,99 %.

4.11 Hydrochloric acid (ρ20 1,16g/ml to 1,19g/ml).

4.12 Thiourea ,10 g/lsolution.

Add 1 g of thioureato 100 ml of water.

4.13 Aqua regia

4.14 Standard solutions

4.14.1 Silver,standard stock solutionA (500 μg of Ag/ml).

Weigh 0,500 0 g of silvermetal to the nearest0,1mg. Transfer to a 100 ml beaker,add 20 ml of diluted

4.14.2 Silver,standard solutionB (50 μg of Ag/ml).

Prepare a freshsolutionper batch.

4.14.3 Gold,standard solution(1 000 μg of Au/ml).

© ISO 2016 – Allrightsreserved 3

4.14.4 Gold and silver,standard solution(100 μg of Au/ml + 50 μg of Ag/ml).

Pipette10,00 ml of silverstandard stock solutionA (4.14.1) into a 100 ml volumetric flask.Add 40 ml of

Calibrationsolutionsshould be prepared at the same ambient temperature as that at which the

5.1 Assay cruciblefurnace,with a maximum required operatingtemperature of 1 200 °C.

4 © ISO 2016 – Allrightsreserved

5.6 Analyticalbalance,sensitiveto 1 mg.

5.7 Microbalance,sensitiveto 1 μg or less.

5.8 Ordinary laboratoryglassware,washed freeof chlorides.

5.10 Atomic absorptionspectrometer (AAS),equipped with background correctionand a glassbead

5.11 Inductivelycoupled plasma (ICP)atomic emission spectrometer .

6.1 Test sample

Prepare an air-equilibratedtestsample in accordance with ISO 9599.

NOTE A testsample isnot requiredifpredriedtestportionsare to be used (seeAnnex A) .

6.2 Test portion

Mixing methods in items a),b),and d) inISO 12743:2006,15.3.2are not recommended.

Methods in items b) to e) and g) in ISO 12743:2006,15.4.1are not recommended .

© ISO 2016 – Allrightsreserved 5

NOTE 2 Ifthe mass fractionof copper isgreaterthan 30 %, a 10 g or 15 g testportionispreferable(see the fourthparagraph of

For lead concentrates,the testportionshould be 10 g to ensure an adequate supply of lead.

7.1 Number of determinations