ISO 13547-1:2014

INTERNATIONAL ISO
STANDARD 13547-1
First edition
2014-11-01
Copper, lead, zinc and nickel sulfide
concentrates — Determination of
arsenic —
Part 1:
Iron hydroxide concentration and
inductively coupled plasma atomic
emission spectrometric method
Concentrés sulfurés de cuivre, de plomb et de zinc — Dosage de
l’arsenic —
Partie 1: Méthode par digestion acide, co-précipitation avec le fer et
plasma induit par haute fréquence
Reference number
©
ISO 2014
© ISO 2014
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2014 – All rights reserved

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 2
4 Reagents . 2
5 Apparatus . 3
6 Sample . 4
6.1 Laboratory sample . 4
6.2 Test sample . 4
6.3 Test portion . 4
7 Procedure. 4
7.1 Number of determinations . 4
7.2 Blank test . 4
7.3 Dissolution of the test portion . 4
7.4 Removal of lead sulfate . 5
7.5 Dissolution of the insoluble residue . 5
7.6 Separation of arsenic . 5
7.7 Preparation of test solutions . 6
7.8 Preparation of calibration solutions . 6
7.9 Preparation of arsenic calibration curve . 6
7.10 Determination of arsenic content in test solutions . 6
8 Expression of results . 7
9 Precision . 7
9.1 Expression of precision . 7
9.2 Procedure for obtaining the final result . 8
9.3 Between-laboratories precision . 8
9.4 Check of trueness . 9
10 Test report .10
Annex A (normative) Procedure for the preparation and determination of the mass of a pre-dried
test portion .11
Annex B (normative) Flowsheet of the procedure for the acceptance of analytical values
fortest samples .13
Bibliography .14
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any
patent rights identified during the development of the document will be in the Introduction and/or on
the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
ISO 13547 consists of the following parts, under the general title Copper, lead, zinc and nickel sulfide
concentrates — Determination of arsenic:
— Part 1: Iron hydroxide concentration and inductively coupled plasma atomic emission spectrometric
method
— Part 2: Acid digestion and inductively coupled plasma atomic emission spectrometric method
iv © ISO 2014 – All rights reserved

INTERNATIONAL STANDARD ISO 13547-1:2014(E)
Copper, lead, zinc and nickel sulfide concentrates —
Determination of arsenic —
Part 1:
Iron hydroxide concentration and inductively coupled
plasma atomic emission spectrometric 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
This International Standard specifies an iron hydroxide concentration and inductively coupled plasma
atomic emission spectrometric (ICP-AES) method for the determination of the mass fraction of arsenic
in copper, lead, zinc, and nickel sulfide concentrates as follows:
a) for copper sulfide concentrates, the method is applicable to the determination of mass fractions of
arsenic from 0,05 % to 2,0 %;
b) for lead sulfide concentrates, the method is applicable to the determination of mass fractions of
arsenic from 0,05 % to 1,0 %;
c) for zinc sulfide concentrates, the method is applicable to the determination of mass fractions of
arsenic from 0,05 % to 0,6 %;
d) for nickel sulfide concentrates, the method is applicable to the determination of mass fraction of
arsenic from 0,05 % to 1,0 %.
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 latest edition of the referenced document (including any amendments) applies.
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 4787, Laboratory glassware — Volumetric instruments — Methods for testing of capacity and for use
ISO 8466-2, Water quality — Calibration and evaluation of analytical methods and estimation of performance
characteristics — Part 2: Calibration strategy for non-linear second-order calibration functions
ISO 9599, Copper, lead and zinc sulfide concentrates — Determination of hygroscopic moisture in the
analysis sample — Gravimetric method
ISO 12743:2006, Copper, lead, zinc and nickel concentrates — Sampling procedures for determination of
metal and moisture content
ISO Guide 35:2006, Reference materials — General and statistical principles for certification
3 Principle
The test portion is decomposed in nitric and sulphuric acids. Arsenic is coprecipitated in ammonia
solution by the carriers of iron hydroxide to be separated from the matrix. The arsenic content is
determined by comparison against iron-matched standards using ICP-AES.
4 Reagents
During the analysis, use only reagents of recognized analytical grade and distilled water, or water of
equivalent purity.
4.1 Sodium hydroxide (NaOH), AR grade.
4.2 Arsenic trioxide (As O ), AR grade.
2 3
4.3 Iron(III) chloride hexahydrate (FeCl •6H O), AR grade (<0,000 05 % arsenic).
3 2
4.4 Ammonium chloride (NH Cl), AR grade.
4.5 Ammonium acetate, AR grade.
4.6 Nitric acid (ρ 1,42 g/mL), AR grade.
4.7 Nitric acid, dilute (1 + 1).
Slowly, add 50 ml of nitric acid (4.6) to 50 ml of water while stirring.
4.8 Hydrochloric acid (ρ 1,16 g/mL), AR grade.
4.9 Hydrochloric acid, dilute (1 + 1).
Slowly add 50 ml of hydrochloric acid (4.8) to 50 ml of water while stirring.
4.10 Sulphuric acid (ρ 1,840 g/mL), AR grade.
4.11 Sulphuric acid, dilute (1 + 1).
Slowly add 50 ml of sulphuric acid (4.10) to 50 ml of water while stirring.
4.12 Sulphuric acid, dilute (1 + 50).
Slowly add 20 ml of sulphuric acid (4.10) to 1 000 ml of water while stirring.
The addition of sulphuric acid to water generates heat and shall be performed with adequate precautions.
4.13 Hydrofluoric acid (ρ 1,13 g/mL).
4.14 Aqueous ammonia (ρ 0,91 g/mL).
4.15 Ammonia solution (1 + 99).
2 © ISO 2014 – All rights reserved

4.16 Iron(III) chloride solution (10 g/l).
Dissolve 48,4 g iron (III) chloride hexahydrate (4.3) in 200 ml of water. Add 10 ml of hydrochloric acid
(4.8) and make up to 1 000 ml with water and mix.
4.17 Sodium hydroxide solution (20 % w/v).
Weigh 20,0 g of sodium hydroxide (4.1) in a polytetrafluoroethylene beaker (5.6). Add 50 ml of water and
allow the solid to dissolve. Dilute the solution to 100 ml and store in a labelled polyethylene container.
4.18 Saturated solution of potassium chlorate in nitric acid.
Superfluous potassium chlorate is added into the nitric acid and then the d
...