As 2678.2-2008 Zinc Sulfide Concentrates - Chemical Analysis Determination of Zinc - Ion-Exchange EDTA Titrim
As 2678.2-2008 Zinc Sulfide Concentrates - Chemical Analysis Determination of Zinc - Ion-Exchange EDTA Titrim
2—2008
ISO 12739:2006
AS 2678.2—2008
Australian Standard®
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• CSIRO Minerals
• Minerals Council of Australia
Additional Interests:
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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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using a current Standard, which should include any amendments that may have been
published since the Standard was published.
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Australian Standard®
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Originated as AS 2678.2—1999.
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 8587 5
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PREFACE
This Standard was prepared by the Standards Australia Committee MN-005, Copper, Lead, Zinc
and Nickel Ores and Concentrates, to supersede AS 2678.2—1999.
The objective of this Standard is to provide those responsible for the analysis of zinc
concentrates with a standardized method of determining zinc, 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 12739:2006, Zinc sulfide
concentrates—Determination of zinc—Ion-exchange/EDTA titrimetric method.
As this Standard is reproduced from an International Standard, the following applies:
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(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
ISO AS
9599 Copper, lead and zinc sulfide 2816 Copper, lead and zinc sulfide
concentrates—Determination of concentrates—Determination of
hygroscopic moisture in the analysis hygroscopic moisture in the analysis
sample—Gravimetric method sample—Gravimetric 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.
ISO 12739:2006(E)
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CONTENTS
Contents Page
Page
1 Scope .................................................................................................................................................... 1
2 Normative references .......................................................................................................................... 1
3 Principle ................................................................................................................................................ 1
4 Reagents ............................................................................................................................................... 1
5 Apparatus ............................................................................................................................................. 3
6 Sample .................................................................................................................................................. 3
6.1 Test sample .......................................................................................................................................... 3
6.2 Test portion .......................................................................................................................................... 3
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7 Procedure ............................................................................................................................................. 3
7.1 Number of determinations .................................................................................................................. 3
7.2 Blank test ............................................................................................................................................. 4
7.3 Dissolution of test portion .................................................................................................................. 4
7.4 Preparation of the ion-exchange column .......................................................................................... 4
7.5 Adsorption of zinc on ion-exchange column .................................................................................... 5
7.6 Elution of zinc from ion-exchange column ....................................................................................... 5
7.7 Titration ................................................................................................................................................ 5
7.8 Determination of the titration factor of the EDTA standard volumetric solution ........................... 5
8 Expression of results .......................................................................................................................... 6
9 Precision ............................................................................................................................................... 7
9.1 Expression of precision ...................................................................................................................... 7
9.2 Procedure for obtaining the final result ............................................................................................ 7
9.3 Between-laboratories precision ......................................................................................................... 7
9.4 Check of trueness ............................................................................................................................... 8
10 Test report ............................................................................................................................................ 9
Annex A (normative) Ion-exchange resins and columns ....................................................................... 10
Annex B (normative) Procedure for the preparation and determination of the mass of a predried test
portion ......................................................................................................................................................... 12
Annex C (normative) Determination of cadmium by atomic absorption spectrometry ....................... 14
Annex D (normative) Flowchart of the procedure for the acceptance of analytical values for test
samples ....................................................................................................................................................... 16
Annex E (informative) Effect of potentially interfering elements ........................................................... 17
Annex F (informative) Derivation of precision equations ....................................................................... 18
Bibliography ............................................................................................................................................... 23
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NOTES
INTERNATIONAL STANDARD ISO 12739:2006(E)
1
1
AUSTRALIAN STANDARD
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 ion-exchange/EDTA titrimetric method for the determination of the
mass fraction of zinc in zinc concentrates. The method is applicable to zinc sulfide concentrates having a mass
fraction of zinc in the range from 11 % to 62 %.
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 3696, Water for analytical laboratory use — Specification and test methods
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 of zinc concentrate is dissolved in hydrochloric, nitric and sulfuric acids. The acidity is adjusted
to about 2 mol/l with respect to hydrochloric acid. Zinc is adsorbed on a strongly basic anion-exchange resin.
Some interfering ions are removed by elution with 2 mol/l dilute hydrochloric acid. Zinc is eluted with an
ammonia/ammonium chloride solution. Zinc is determined in the eluate by titration with EDTA at a pH of
approximately 5,6 using xylenol-orange indicator.
4 Reagents
During the analysis, only reagents of recognized analytical grade and water that complies with grade 2 of
ISO 3696 shall be used.
4.1 Zinc, 99,99 % minimum purity, free from oxide prior to use.