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 13547-1:2014(E)
©
ISO 2014

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ISO 13547-1:2014(E)

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ISO 13547-1:2014(E)

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
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ISO 13547-1:2014(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
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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
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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
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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
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ISO 13547-1:2014(E)

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
4.5 Ammonium acetate, AR grade.
4.6 Nitric acid (ρ 1,42 g/mL), AR grade.
20
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.
20
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.
20
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).
20
4.14 Aqueous ammonia (ρ 0,91 g/mL).
20
4.15 Ammonia solution (1 + 99).
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ISO 13547-1:2014(E)

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 deposited solution is allowed
to form the saturated solution.
4.19 Ammonium acetate (25 % w/v).
Dissolve 25,0 g of ammonium acetate (4.5) into 100 ml water.
4.20 Arsenic standard solution, 1 ml contains 1 mg of As.
Weigh 1 320,3 g of arsenic trioxide (4.2) to the nearest 0,1 mg, Transfer to a 400 ml beaker and add 5 ml
of sodium hydroxide solution (4.17). Warm slightly to dissolve. When dissolution is complete, cool and
add 40 ml of nitric acid (4.6). Transfer to a 1 000 ml volumetric flask containing 60 ml of nitric acid (4.6).
Fill up nearly to the mark with water, mix, and equilibrate at room temperature then fill up exactly to
the mark and mix again. Store in a labelled container.
Alternatively, purchase a suitable high quality prepared standard.
Before use, compare this International Standard against a traceable National Standard to ensure
suitability for use.
4.21 Arsenic standard solution, 1 ml contains 0,2 mg of As.
Pipette 40 ml of arsenic standard solution (4.20) into a 200 ml volumetric flask containing 2 ml
hydrochloric acid (4.8). Fill up nearly to the mark with water, mix, and equilibrate at room temperature
then fill up exactly to the mark and mix again. Store in a labelled glass container.
5 Apparatus
All laboratory glassware and equipment shall be shown to be free of arsenic contamination.
5.1 Balance, sensitive to ±0,000 1 g.
5.2 Ordinary laboratory glassware, complying with ISO 648 and ISO 1042 and used in accordance
with ISO 4787.
5.3 Inductively coupled plasma atomic emission spectrometer (ICP-AES).
The emission wavelength should be set to 193,696 nm or 197,197 nm.
1)
5.4 Insoluble filter paper, Whatman® No. 40 or equivalent.
1)
5.5 Coprecipitation filter paper, Whatman® No. 1 or equivalent.
1) This information is given for the convenience of users of this International Standard and does not constitute an
endorsement by ISO.
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ISO 13547-1:2014(E)

5.6 Polytetrafluoroethylene beaker, 200 ml capacity.
6 Sample
6.1 Laboratory sample
Laboratory samples shall be taken and prepared in accordance with the procedures described in
ISO 12743.
As arsenic may evaporate from samples at elevated temperatures, consideration should be given to
preparing a separate chemical analysis sample as described in ISO 12743:2006, 16.2.
6.2 Test sample
Prepare an air-equilibrated test sample and a hygroscopic moisture test sample in accordance with
ISO 9599.
NOTE A test sample is not required if pre-dried test portions are to be used (see Annex A).
6.3 Test portion
Taking multiple increments, extract approximately 0,5 g from the test sample and weigh to the nearest
0,1 mg. At the same time, as test portions are being weighed for analysis, weigh test portions for the
determination of hygroscopic moisture in accordance with ISO 9599.
Alternatively, the method specified in Annex A may be used to prepare pre-dried test portions directly
from the laboratory sample.
Obtain an approximate concentration for the iron in the sample as required in step 7.6.
7 Procedure
7.1 Nu
...