ISO 19976-1:2019

INTERNATIONAL ISO
STANDARD 19976-1
First edition
2019-07
Copper, lead and zinc sulfide
concentrates — Determination of
cadmium —
Part 1:
Flame atomic absorption
spectrometric method
Concentrés de sulfure de cuivre, de plomb et de zinc — Dosage du
cadmium —
Partie 1: Spectrométrie d'absorption atomique dans la flamme
Reference number
©
ISO 2019
© ISO 2019
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ii © ISO 2019 – All rights reserved

Contents Page
Foreword .iv
1 Scope . 1
2 Normative reference . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
6 Apparatus . 3
7 Samples . 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 Determination . 4
8.3.1 Dissolution of test portion . 4
8.3.2 Preparation of test solutions . 4
8.3.3 Adjustment of the AAS . 5
8.3.4 Atomic absorption measurements . 5
8.4 Check test . 5
9 Expression of results . 5
10 Precision and accuracy . 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 . 8
10.4.1 General. 8
10.4.2 Type of CRM or reference material . 8
11 Test report . 9
Annex A (informative) Procedure for the preparation and determination of the mass of a
predried test portion .10
Annex B (normative) Procedure for obtaining the final result .12
Bibliography .13
Foreword
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concentrates.
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iv © ISO 2019 – All rights reserved

INTERNATIONAL STANDARD ISO 19976-1:2019(E)
Copper, lead and zinc sulfide concentrates —
Determination of cadmium —
Part 1:
Flame atomic absorption 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 a flame atomic absorption spectrometric 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 0,30 %.
2 Normative reference
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 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
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
Dissolve the test portion in hydrochloric acid and nitric acid. Add hydrofluoric acid to remove silicon.
Then add perchloric acid and determine the iron concentration in the test portion using an atomic
absorption spectrometer (AAS) with a deuterium lamp for background correction at 228,8 nm.
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).
5.2 Hydrochloric acid, diluted 1+1.
Slowly add 500 ml of concentrated hydrochloric acid (5.1) to 500 ml of water, while stirring.
5.3 Hydrochloric acid, diluted 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).
5.5 Hydrofluoric acid, concentrated (ρ 1,15 g/ml).
5.6 Perchloric acid, concentrated (ρ 1,70 g/ml).
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.
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.
2 © ISO 2019 – All rights reserved

5.11 Cadmium calibration solutions.
Prepare a series of calibratio
...