AS 2917.

3—2008
ISO 10469:2006
AS 2917.3—2008

Australian Standard®
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Copper sulfide concentrates

Part 3: Determination of copper—

Electrogravimetric method
 This Australian Standard® was prepared by Committee MN-005, Copper, Lead, Zinc and
Nickel Ores and Concentrates. It was approved on behalf of the Council of Standards
Australia on 24 January 2008.
This Standard was published on 12 March 2008.

The following are represented on Committee MN-005:

• CSIRO Minerals
• Minerals Council of Australia

Additional Interests:
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• Minerals industry analytical laboratories

This Standard was issued in draft form for comment as DR 07041.

Standards Australia wishes to acknowledge the participation of the expert individuals that
contributed to the development of this Standard through their representation on the
Committee and through the public comment period.

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Standards Australia welcomes suggestions for improvements, and encourages readers to

notify us immediately of any apparent inaccuracies or ambiguities. Contact us via email at
mail@standards.org.au, or write to Standards Australia, GPO Box 476, Sydney, NSW 2001.
 AS 2917.3—2008

Australian Standard®
This is a free 7 page sample. Access the full version at http://infostore.saiglobal.com.

Copper sulfide concentrates

Part 3: Determination of copper—

Electrogravimetric method

Originated as AS 2917.3—1994.
Second edition 2008.

COPYRIGHT
© Standards Australia
All rights are reserved. No part of this work may be reproduced or copied in any form or by
any means, electronic or mechanical, including photocopying, without the written
permission of the publisher.
Published by Standards Australia GPO Box 476, Sydney, NSW 2001, Australia
ISBN 0 7337 8585 9
 ii
ii

PREFACE

This Standard was prepared by the Standards Australia Committee MN-005, Copper, Lead, Zinc
and Nickel Ores and Concentrates, to supersede AS 2917.3—1994, Copper sulfide concentrates,
Part 3: Determination of copper content—Electrogravimetric method.
The objective of this Standard is to provide those involved in the analysis of copper
concentrates with a standardized method for determining copper, supported by precision data
obtained from an interlaboratory test program.
The objective of this revision is to adopt the latest edition of the corresponding International
Standard.
This Standard is identical with, and has been reproduced from ISO 10469:2006, Copper,sulfide
concentrates—Determination of copper—Electrogravimetric method.
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As this Standard is reproduced from an International Standard, the following applies:

(a) Its number appears on the cover and title page while the International Standard number
appears only on the cover.
(b) In the source text ‘this International Standard’ should read ‘this Australian Standard’.
(c) A full point substitutes for a comma when referring to a decimal marker.
(d) Substitute ‘L’ for ‘l’ as the unit for litres.
References to International Standards should be replaced by references to Australian Standards,
as follows:
Reference to International Standard Australian Standard
AS ISO
9599 Copper, lead and zinc sulfide 2816 Copper, lead and zinc sulfide
concentrates—Determination of concentrates—Determination of
hygroscopic moisture in the hygroscopic moisture in the analysis
analysis sample—Gravimetric sample—Gravimetric method
method
Only international references that have been adopted as Australian Standards have been listed.
The terms ‘normative’ and ‘informative’ have been used in this Standard to define the
application of the annex to which they apply. A ‘normative’ annex is an integral part of a
Standard, whereas an ‘informative’ annex is only for information and guidance.
 iii
iii
Contents Page
CONTENTS
Foreword............................................................................................................................................................ iv
Page
Introduction ........................................................................................................................................................ v
1 Scope ..................................................................................................................................................... 1
2 Normative references ........................................................................................................................... 1
3 Principle ................................................................................................................................................. 1
4 Reagents ................................................................................................................................................ 2
5 Apparatus .............................................................................................................................................. 4
6 Sample ................................................................................................................................................... 5
6.1 Test sample ........................................................................................................................................... 5
6.2 Test portion ........................................................................................................................................... 5
7 Procedure .............................................................................................................................................. 5
7.1 Number of determinations ................................................................................................................... 5
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7.2 Blank test ............................................................................................................................................... 5

7.3 Dissolution of test portion ................................................................................................................... 5
7.4 Separation of arsenic, antimony, tin, selenium and silver ............................................................... 5
7.5 Copper separation ................................................................................................................................ 6
7.5.1 Sulfide separation................................................................................................................................. 6
7.5.2 Hydroxide separation ........................................................................................................................... 7
7.6 Electrolytic deposition ......................................................................................................................... 7
7.7 FAAS determination of copper in the electrolyte, filter residues and sulfide precipitates........... 8
7.7.1 FAAS determination of copper in the filtrate of the sulfide precipitation....................................... 8
7.7.2 Treatment of hydroxide precipitate in sulfide separation ................................................................ 8
7.7.3 FAAS determination of copper in the electrolyte, filter residues and precipitates (sulfide
separation method)............................................................................................................................... 8
7.8 FAAS determination of copper in the electrolyte, filter residues and precipitates
(hydroxide separation method) ........................................................................................................... 9
8 Expression of results ......................................................................................................................... 10
9 Precision .............................................................................................................................................. 10
9.1 Expression of precision ..................................................................................................................... 10
9.2 Method for obtaining the final result (see Annex B) ....................................................................... 10
9.3 Precision between laboratories......................................................................................................... 11
9.4 Check of trueness............................................................................................................................... 11
9.4.1 Type of certified reference material (CRM) or reference material (RM) ........................................ 12
10 Test report ........................................................................................................................................... 12
Annex A (normative) Procedure for the preparation and determination of the mass of a predried
test portion .......................................................................................................................................... 13
Annex B (normative) Flowsheet of the procedure for the acceptance of analytical values for test
samples................................................................................................................................................ 15
Annex C (informative) Derivation of precision equations ............................................................................ 16

© ISO 2006 – All rights reserved iii

 ISO 10469:2006(E)

iv
iv

INTRODUCTION
Introduction
ISO 10469:1994 underwent periodical review in 1999. Although the decision was made to confirm the
International Standard at that time, significant comments were submitted by Japan. These comments were
considered at a meeting of ISO/TC 183 in 2000, where it was agreed that Japan would re-draft ISO 10469 to
indicate the proposed changes.

The most significant change was the elimination of the correction for impurities.

ISO/TC 183 agreed that the changes made do not warrant a new interlaboratory test programme. Details of
the changes are as follows:

a) Deletion of the determination of impurities in the deposited copper (7.9 in ISO 10469:1994).

b) Adjustment of the expression of dissolution of the test portion according to ISO 10258:1994, Copper
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sulfide concentrates — Determination of copper content — Titrimetric methods.

c) Adjustment of the expression of the sulfide separation method according to ISO 10258:1994.

d) In the case of contained bismuth or tellurium, modification of the sulfide separation procedure. The
method described in ISO 10469:1994 included a lot of copper in the iron hydroxide precipitation, which
will lead to incorrect results. The method described in ISO 13658:2000, Zinc sulfide concentrates —
Determination of zinc content — Hydroxide precipitation and EDTA titrimetric method has less copper in
the iron hydroxide precipitation than the method described in ISO 10469:1994, so the method described
in ISO 10469:1994 has now been modified with reference to ISO 13658.

e) The procedure of treatment of the iron hydroxide precipitation (contained copper) is not given in
ISO 10469:1994. The procedure of treatment has been added to the revised Standard.

Calibration solution A (4.34.1 in ISO 10469:1994) will be used in 7.7.1 (FAAS determination of copper in the
filtrate of the sulfide precipitation). This filtrate contains iron ion, so calibration solution A should contain iron to
achieve matrix matching. The preparation method of calibration solution A has been revised to include iron ion
in the revised Standard.

© ISO 2006 – All rights reserved v

 INTERNATIONAL STANDARD ISO 10469:2006(E)
1
1

AUSTRALIAN STANDARD

Copper sulfide concentrates

Copper
Part 3:
sulfide concentrates — Determination of copper —
Electrogravimetric method
Determination of copper—Electrogravimetric method

WARNING — This International Standard may involve hazardous materials, operations and equipment.
It is the responsibility of the user of this International Standard to establish appropriate health and
safety practices and determine the applicability of regulatory limitations prior to use.

1 Scope
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This International Standard specifies an electrogravimetric method for the determination of the mass fraction
of copper in copper sulfide concentrates in the range 15 % to 50 %.

2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.

ISO 385, Laboratory glassware — Burettes

ISO 648, Laboratory glassware — One-mark pipettes

ISO 1042, Laboratory glassware — One-mark volumetric flasks

ISO 4787, Laboratory glassware — Volumetric glassware — Methods for use and testing of capacity

ISO 9599, Copper, lead and zinc sulfide concentrates — Determination of hygroscopic moisture in the
analysis sample — Gravimetric method

3 Principle
The test portion is decomposed in nitric and sulfuric acids, and copper is separated from interfering elements:

⎯ from silver by precipitation of silver chloride;

⎯ from arsenic, antimony, selenium and tin by fuming with hydrobromic acid;

⎯ from iron by precipitation of copper sulfide with sodium thiosulfate or by precipitation of iron(III) oxide
hydrate (bismuth and tellurium are also separated in this way).

Electrogravimetric deposition of copper occurs in the presence of nitric acid, sulfuric acid and traces of
chloride. Under these conditions, coprecipitation of molybdenum does not occur.

Traces of copper in the electrolyte, the filtrate of the copper sulfide precipitation, all precipitates and residues
are determined by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma atomic
emission spectrometry.

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© ISO 2006 – All rights reserved 1
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AS 2917.3-2008, Copper sulfide concentrates

Determination of copper - Electrogravimetric
method
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