Copper, lead and zinc sulfide concentrates — Determination of cadmium — Part 2: Acid digestion and inductively coupled plasma atomic emission spectrometric method

This document specifies an acid digestion and inductively coupled plasma atomic emission spectrometric (ICP-AES) method for the determination of the mass fraction of cadmium in copper, lead and zinc sulfide concentrates as follows: a) for copper sulfide concentrates, the method is applicable to the determination of mass fractions of cadmium from 0,01 % to 0,30 %; b) for lead sulfide concentrates, the method is applicable to the determination of mass fractions of cadmium from 0,01 % to 0,30 %; c) for zinc sulfide concentrates, the method is applicable to the determination of mass fractions of cadmium from 0,05 % to 1,00 %.

Concentrés de sulfure de cuivre, de plomb et de zinc — Dosage du cadmium — Partie 2: Méthode par digestion acide et spectroscopie d’émission atomique à plasma à couplage inductif

General Information

Status
Published
Publication Date
18-Jul-2019
Current Stage
6060 - International Standard published
Start Date
30-Nov-2017
Due Date
27-May-2019
Completion Date
19-Jul-2019
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ISO 19976-2:2019 - Copper, lead and zinc sulfide concentrates -- Determination of cadmium
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INTERNATIONAL ISO
STANDARD 19976-2
First edition
2019-07
Copper, lead and zinc sulfide
concentrates — Determination of
cadmium —
Part 2:
Acid digestion and inductively
coupled plasma atomic emission
spectrometric method
Concentrés de sulfure de cuivre, de plomb et de zinc — Dosage du
cadmium —
Partie 2: Méthode par digestion acide et spectroscopie d’émission
atomique à plasma à couplage inductif
Reference number
ISO 19976-2:2019(E)
©
ISO 2019

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ISO 19976-2:2019(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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.
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Email: copyright@iso.org
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Published in Switzerland
ii © ISO 2019 – All rights reserved

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ISO 19976-2:2019(E)

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 2
5 Reagents . 2
6 Apparatus . 3
7 Sample . 3
7.1 Laboratory sample . 3
7.2 Test sample . 3
7.3 Test portion . 4
8 Procedure. 4
8.1 Number of determinations . 4
8.2 Blank test . 4
8.3 Dissolution of the test portion . 4
8.4 Preparation of test solutions . 4
8.5 Preparation of calibration solutions . 4
8.6 Preparation of cadmium calibration curve . 5
8.7 Determination of cadmium content in test solutions . 5
9 Expression of results . 5
10 Precision . 6
10.1 Expression of precision . 6
10.2 Method for obtaining the final result . 6
10.3 Between-laboratories precision . 7
10.4 Check of trueness . 7
10.4.1 General. 7
10.4.2 Type of CRM or reference material . 8
11 Test report . 8
Annex A (informative) Procedure for the preparation and determination of the mass of a
pre-dried test portion . 9
Annex B (normative) Procedure for obtaining the final result .11
Bibliography .12
© ISO 2019 – All rights reserved iii

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ISO 19976-2:2019(E)

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 of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso
.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 183, Copper, lead, zinc and nickel ores and
concentrates.
A list of all parts in the ISO 19976 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2019 – All rights reserved

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INTERNATIONAL STANDARD ISO 19976-2:2019(E)
Copper, lead and zinc sulfide concentrates —
Determination of cadmium —
Part 2:
Acid digestion and inductively coupled plasma atomic
emission spectrometric method
WARNING — The use of this document might involve hazardous materials, operations and
equipment. It is the responsibility of the user of this document to establish appropriate health
and safety practices.
1 Scope
This document specifies an acid digestion and inductively coupled plasma atomic emission
spectrometric (ICP-AES) method for the determination of the mass fraction of cadmium in copper, lead
and zinc sulfide concentrates as follows:
a) for copper sulfide concentrates, the method is applicable to the determination of mass fractions of
cadmium from 0,01 % to 0,30 %;
b) for lead sulfide concentrates, the method is applicable to the determination of mass fractions of
cadmium from 0,01 % to 0,30 %;
c) for zinc sulfide concentrates, the method is applicable to the determination of mass fractions of
cadmium from 0,05 % to 1,00 %.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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 — 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, zinc and nickel sulfide concentrates — Determination of hygroscopic moisture
content of the analysis sample — Gravimetric method
ISO 12743, Copper, lead, zinc and nickel concentrates — Sampling procedures for determination of metal
and moisture content
ISO Guide 35, Reference materials — Guidance for characterization and assessment of homogeneity and
stability
© ISO 2019 – All rights reserved 1

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ISO 19976-2:2019(E)

3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
4 Principle
The test sample is dissolved in hydrochloric acid, nitric acid and hydrofluoric acid with a final stage
perchloric acid digestion. Yttrium is added as an internal standard to solutions of dissolved samples,
reference materials and calibration solutions and cadmium determined by ICP-AES.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and distilled water or water of
equivalent purity.
5.1 Hydrochloric acid, concentrated (ρ 1,19 g/ml).
20
5.2 Hydrochloric acid, dilute 1+1. Slowly add 500 ml of concentrated hydrochloric acid (5.1) to
500 ml of water while stirring.
5.3 Hydrochloric acid, dilute 1+9. Slowly add 50 ml of concentrated hydrochloric acid (5.1) to 450 ml
of water while stirring.
5.4 Nitric acid, concentrated (ρ 1,42 g/ml).
20
5.5 Hydrofluoric acid, concentrated (ρ 1,15 g/ml).
20
5.6 Perchloric acid, concentrated (ρ 1,70 g/ml).
20
5.7 Cadmium metal, minimum purity 99,99 %.
5.8 Cadmium, standard solution, 1 ml contains 1 mg of Cd.
Weigh, to the nearest 0,1 mg, 1,000 0 g of cadmium metal (5.7) into a 250 ml beaker. Add 10 ml of water
and 5 ml of nitric acid (5.4). Cover and warm gently (if necessary) until the cadmium metal is dissolved.
Heat to remove nitrogen oxides, then allow to cool, and add about 50 ml of water. Transfer the solution to
a 1 000 ml one-mark volumetric flask, add 40 ml of hydrochloric acid (5.2), fill up nearly to the mark with
water, mix and cool to room temperature. Then fill up exactly to the mark with water and mix again.
5.9 Cadmium, standard solution, 1 ml contains 100 μg of Cd.
Pipette 10,00 ml of cadmium standard solution (5.8) into a 100 ml one-mark volumetric flask. Add 20 ml
of hydrochloric acid (5.2), fill up nearly to the mark with water, mix and cool to room temperature.
Then fill up exactly to the mark with water and mix again.
2 © ISO 2019 – All rights reserved

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ISO 19976-2:2019(E)

5.10 Cadmium, standard solution, 1 ml contains 10 μg of Cd.
Pipette 10,00 ml of cadmium standard solution (5.9) into a 100 ml one-mark volumetric flask. Add 18 ml
of hydrochloric acid (5.2), fill up nearly to the mark with water, mix and cool to room temperature.
Then fill up exactly to the mark with water and mix again.
5.11 Yttrium, standard solution, 1 ml contains 1 mg of Y.
Weigh, to the nearest 0,1 mg, 1,269 9 g of yttrium trioxide (≥99,99 %) and transfer to a 250 ml
beaker. Add 100 ml of hydrochloric acid (5.3) and heat gently until the metal is dissolved, then cool
to room temperature. Transfer to a 1 000 ml one-mark volumetric flask, fill up nearly to the mark
with hydrochloric acid (5.3), mix and cool to room temperature, then fill up exactly to the mark with
hydrochloric acid (5.3) and mix again.
5.12 Yttrium, standard solution, 1 ml contains 200 μg of Y.
Pipette 50,00 ml of yttrium standard solution (5.11) into a 250 ml one-mark volumetric flask. Add 40 ml
of hydrochloric acid (5.2), fill up nearly to the mark with water, mix and cool to room temperature, then
fill up exactly to the mark with water and mix a
...

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