ISO 17992:2013
(Main)Iron ores — Determination of arsenic content — Hydride generation atomic absorption spectrometric method
Iron ores — Determination of arsenic content — Hydride generation atomic absorption spectrometric method
ISO 17992:2013 specifies a hydride generation atomic absorption spectrometric method for the determination of the arsenic content of iron ore. ISO 17992:2013 is applicable to mass fractions of arsenic between 0,000 66 % and 0,020 15 % in natural iron ores, iron ore concentrates and agglomerates, including sinter products.
Minerais de fer — Dosage de l'arsenic — Méthode par spectrométrie d'absorption atomique à génération d'hydrure
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INTERNATIONAL ISO
STANDARD 17992
First edition
2013-09-15
Iron ores — Determination of arsenic
content — Hydride generation atomic
absorption spectrometric method
Minerais de fer — Dosage de l’arsenic — Méthode par spectrométrie
d’absorption atomique à génération d’hydrure
Reference number
©
ISO 2013
© ISO 2013
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 2013 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 1
5 Apparatus . 3
6 Sampling and samples . 4
6.1 Laboratory sample . 4
6.2 Preparation of predried test samples . 4
7 Procedure. 4
7.1 Number of determinations . 4
7.2 Test portion . 4
7.3 Blank test and check test . 4
7.4 Determination . 5
8 Expression of results . 7
8.1 Calculation of mass fraction of arsenic content . 7
8.2 General treatment of results . 7
8.3 Oxide factor .10
9 Test report .10
Annex A (normative) Flow sheet of the procedure for the acceptance of analytical values for
test sample .13
Annex B (informative) Parameters of some instruments .14
Annex C (informative) Derivation of repeatability and permissible tolerance formulae .16
Annex D (informative) Precision data obtained by international analytical trials .17
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
The committee responsible for this document is ISO/TC 102, Iron ore and direct reduced iron, Subcommittee
SC 2, Chemical analysis.
iv © ISO 2013 – All rights reserved
INTERNATIONAL STANDARD ISO 17992:2013(E)
Iron ores — Determination of arsenic content — Hydride
generation atomic absorption spectrometric method
WARNING — This International Standard can involve hazardous materials, operations, and
equipment, and does not purport to address all of the safety issues associated with its use. 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 a hydride generation atomic absorption spectrometric method for
the determination of the arsenic content of iron ore.
This International Standard is applicable to mass fractions of arsenic between 0,000 66 % and 0,020 15 %
in natural iron ores, iron ore concentrates and agglomerates, including sinter products.
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 3082, Iron ores — Sampling and sample preparation procedures
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 7764, Iron ores — Preparation of predried test samples for chemical analysis
ISO Guide 35:2006, Reference materials — General and statistical principles for certification
3 Principle
The test portion is decomposed by treatment with hydrochloric and nitric acid. The residue is treated
with sodium peroxide and sodium carbonate. Potassium iodide reduces As(V) to As(III) and ascorbic
acid masks the effect of iron in the solution. At optimum acidity of around 26 %, the solution and sodium
borohydride react to generate gaseous arsenic hydride. An inert carrier gas is used to transport the
arsenic hydride to a quartz tube atomizer. The equipment is set to measure the absorbances at 197,3 nm.
The absorbances of the test and calibration solutions, including those of certified or other reference
materials, are compared to determine the arsenic content.
4 Reagents
During the analysis, use only reagents of recognized analytical grade and Grade 2 water in accordance
with ISO 3696.
Reagents are to be selected or purified for the lowest possible blank value.
4.1 Sodium peroxide (Na O ).
2 2
4.2 Sodium carbonate (Na CO ), anhydrous powder.
2 3
4.3 Sodium bicarbonate (NaHCO ).
4.4 Sodium hydroxide (NaOH).
4.5 Iron oxide (Fe O ).
2 3
4.6 Arsenic trioxide (As O ).
2 3
4.7 Hydrochloric acid, ρ 1,16 g/ml to 1,19 g/ml.
4.8 Nitric acid, ρ 1,42 g/ml.
4.9 Hydrochloric acid, ρ 1,16 g/ml to 1,19 g/ml, diluted 1+1.
4.10 Hydrochloric acid, ρ 1,16 g/ml to 1,19 g/ml, diluted 2+98.
4.11 Hydrochloric acid, ρ 1,16 g/ml to 1,19 g/ml, diluted 12+88.
4.12 Sodium hydroxide solution, 40 g/l.
Dissolve 2 g of sodium hydroxide to 10 ml of water; dilute to 50 ml.
4.13 Sodium borohydride solution, 8 mg/ml.
Dissolve 0,5 g of sodium hydroxide to 10 ml of water, then dissolve 0,8 g of sodium borohydride
[NaBH > 95 % (m/m)] in the 50 ml beaker contained sodium hydroxide solution; dilute to 100 ml. This
solution shall be freshly prepared and used immediately.
4.14 Potassium iodide solution, 100 mg/ml.
Dissolve 10 g of potassium iodide [KI > 98,5 % (m/m)] in 20 ml of water. Dilute to 100 ml.
4.15 Ascorbic acid solution, 100 mg/ml.
Dissolve 10 g of ascorbic acid [C H O > 99,5 % (m/m)] in 20 ml of water. Dilute to 100 ml. This solution
6 8 6
shall be freshly prepared and used immediately.
4.16 Background solution, 10 mg Fe/ml.
Dissolve 1,43 g of iron oxide (4.5) [minimum purity 99,99 % (m/m)] in 30 ml of hydrochloric acid (4.7).
Evaporate until a syrupy consistency is obtained, cool, add 10 ml of hydrochloric acid (4.9), and transfer
the solution to a 100 ml one-mark volumetric flask. Dilute to volume with water and mix.
4.17 Arsenic standard solution A, 100 μg/ml.
Dry several hundred milligrams of arsenic trioxide [As O > 99,95 % (m/m)] at 105 °C for 1 h. Dissolve
2 3
0,132 g of the dried product in 2 ml of sodium hydroxide solution (4.12), add 30 ml of water, neutralize
with hydrochloric acid (4.10), using methyl orange (4.21) indicator, and add 4 g of sodium bicarbonate
(4.3). Dilute in a volumetric flask to 1 000 ml with water and mix.
1 ml of standard arsenic solution A contains 100 μg of arsenic.
2 © ISO 2013 – All rights reserved
4.18 Arsenic standard solution B, 1 μg/ml.
Transfer 10 ml of arsenic standard solution A (4.17) to a 1 l volumetric flask, dilute to the mark with
water, and mix.
1 ml of standard arsenic solution B contains 1 μg of arsenic.
4.19 Arsenic standard solution C, 0,1 μg/ml.
Transfer 10 ml of arsenic standard solution B (4.18) to a 100 ml volumetric flask, dilute to the mark with
water, and mix.
1 ml of standard arsenic solution C contains 0,1 μg of arsenic.
4.20 Methyl orange, indicator.
4.21 Methyl orange solution, 1 mg/ml.
Dissolve 0,10 g of methyl orange in 20 ml of water. Dilute to 100 ml.
5 Apparatus
Use ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks
complying with the specifications of ISO 648 and ISO 1042 respectively, and the following.
5.1 Atomic absorption spectrometer, equipped with an arsenic hollow cathode lamp or electrodeless
discharge lamp.
WARNING — Follow the manufacturer’s instructions to avoid possible explosion hazards for
igniting and extinguishing the air-acetylene flame and possible burning for hot electric furnace.
Wear tinted safety glasses whenever the atomic absorption spectrometer is in operation. Good
ventilation of the flame is necessary to prevent poison by arsenic hydride.
The atomic absorption spectrometer used in this method shall meet the following criteria.
a) Minimum sensitivity: The absorbance of the highest concentration calibration solution (see 7.4.3) is
at least 0,25.
b) Graph linearity: The slope of the calibration graph covering the top 20 % of the concentration range
(expressed as a change in absorbance) is not less than 0,7 of the value of the slope for the bottom
20 % of the concentration range determined in the same way.
c) Minimum stability: The standard deviation of the absorbance of the most concentrated calibration
solution and that of the zero calibration solution, each being calculated from a sufficient number
of repetitive measurements, are less than 1,5 % and 0,5 %, respectively, of the mean value of the
absorbance of the most concentrated solution.
The use of a strip-chart recorder and/or digital readout device is recommended to eva
...
INTERNATIONAL ISO
STANDARD 17992
First edition
2013-09-15
Iron ores — Determination of arsenic
content — Hydride generation atomic
absorption spectrometric method
Minerais de fer — Dosage de l’arsenic — Méthode par spectrométrie
d’absorption atomique à génération d’hydrure
Reference number
©
ISO 2013
© ISO 2013
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 2013 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 1
5 Apparatus . 3
6 Sampling and samples . 4
6.1 Laboratory sample . 4
6.2 Preparation of predried test samples . 4
7 Procedure. 4
7.1 Number of determinations . 4
7.2 Test portion . 4
7.3 Blank test and check test . 4
7.4 Determination . 5
8 Expression of results . 7
8.1 Calculation of mass fraction of arsenic content . 7
8.2 General treatment of results . 7
8.3 Oxide factor .10
9 Test report .10
Annex A (normative) Flow sheet of the procedure for the acceptance of analytical values for
test sample .13
Annex B (informative) Parameters of some instruments .14
Annex C (informative) Derivation of repeatability and permissible tolerance formulae .16
Annex D (informative) Precision data obtained by international analytical trials .17
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
The committee responsible for this document is ISO/TC 102, Iron ore and direct reduced iron, Subcommittee
SC 2, Chemical analysis.
iv © ISO 2013 – All rights reserved
INTERNATIONAL STANDARD ISO 17992:2013(E)
Iron ores — Determination of arsenic content — Hydride
generation atomic absorption spectrometric method
WARNING — This International Standard can involve hazardous materials, operations, and
equipment, and does not purport to address all of the safety issues associated with its use. 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 a hydride generation atomic absorption spectrometric method for
the determination of the arsenic content of iron ore.
This International Standard is applicable to mass fractions of arsenic between 0,000 66 % and 0,020 15 %
in natural iron ores, iron ore concentrates and agglomerates, including sinter products.
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 3082, Iron ores — Sampling and sample preparation procedures
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 7764, Iron ores — Preparation of predried test samples for chemical analysis
ISO Guide 35:2006, Reference materials — General and statistical principles for certification
3 Principle
The test portion is decomposed by treatment with hydrochloric and nitric acid. The residue is treated
with sodium peroxide and sodium carbonate. Potassium iodide reduces As(V) to As(III) and ascorbic
acid masks the effect of iron in the solution. At optimum acidity of around 26 %, the solution and sodium
borohydride react to generate gaseous arsenic hydride. An inert carrier gas is used to transport the
arsenic hydride to a quartz tube atomizer. The equipment is set to measure the absorbances at 197,3 nm.
The absorbances of the test and calibration solutions, including those of certified or other reference
materials, are compared to determine the arsenic content.
4 Reagents
During the analysis, use only reagents of recognized analytical grade and Grade 2 water in accordance
with ISO 3696.
Reagents are to be selected or purified for the lowest possible blank value.
4.1 Sodium peroxide (Na O ).
2 2
4.2 Sodium carbonate (Na CO ), anhydrous powder.
2 3
4.3 Sodium bicarbonate (NaHCO ).
4.4 Sodium hydroxide (NaOH).
4.5 Iron oxide (Fe O ).
2 3
4.6 Arsenic trioxide (As O ).
2 3
4.7 Hydrochloric acid, ρ 1,16 g/ml to 1,19 g/ml.
4.8 Nitric acid, ρ 1,42 g/ml.
4.9 Hydrochloric acid, ρ 1,16 g/ml to 1,19 g/ml, diluted 1+1.
4.10 Hydrochloric acid, ρ 1,16 g/ml to 1,19 g/ml, diluted 2+98.
4.11 Hydrochloric acid, ρ 1,16 g/ml to 1,19 g/ml, diluted 12+88.
4.12 Sodium hydroxide solution, 40 g/l.
Dissolve 2 g of sodium hydroxide to 10 ml of water; dilute to 50 ml.
4.13 Sodium borohydride solution, 8 mg/ml.
Dissolve 0,5 g of sodium hydroxide to 10 ml of water, then dissolve 0,8 g of sodium borohydride
[NaBH > 95 % (m/m)] in the 50 ml beaker contained sodium hydroxide solution; dilute to 100 ml. This
solution shall be freshly prepared and used immediately.
4.14 Potassium iodide solution, 100 mg/ml.
Dissolve 10 g of potassium iodide [KI > 98,5 % (m/m)] in 20 ml of water. Dilute to 100 ml.
4.15 Ascorbic acid solution, 100 mg/ml.
Dissolve 10 g of ascorbic acid [C H O > 99,5 % (m/m)] in 20 ml of water. Dilute to 100 ml. This solution
6 8 6
shall be freshly prepared and used immediately.
4.16 Background solution, 10 mg Fe/ml.
Dissolve 1,43 g of iron oxide (4.5) [minimum purity 99,99 % (m/m)] in 30 ml of hydrochloric acid (4.7).
Evaporate until a syrupy consistency is obtained, cool, add 10 ml of hydrochloric acid (4.9), and transfer
the solution to a 100 ml one-mark volumetric flask. Dilute to volume with water and mix.
4.17 Arsenic standard solution A, 100 μg/ml.
Dry several hundred milligrams of arsenic trioxide [As O > 99,95 % (m/m)] at 105 °C for 1 h. Dissolve
2 3
0,132 g of the dried product in 2 ml of sodium hydroxide solution (4.12), add 30 ml of water, neutralize
with hydrochloric acid (4.10), using methyl orange (4.21) indicator, and add 4 g of sodium bicarbonate
(4.3). Dilute in a volumetric flask to 1 000 ml with water and mix.
1 ml of standard arsenic solution A contains 100 μg of arsenic.
2 © ISO 2013 – All rights reserved
4.18 Arsenic standard solution B, 1 μg/ml.
Transfer 10 ml of arsenic standard solution A (4.17) to a 1 l volumetric flask, dilute to the mark with
water, and mix.
1 ml of standard arsenic solution B contains 1 μg of arsenic.
4.19 Arsenic standard solution C, 0,1 μg/ml.
Transfer 10 ml of arsenic standard solution B (4.18) to a 100 ml volumetric flask, dilute to the mark with
water, and mix.
1 ml of standard arsenic solution C contains 0,1 μg of arsenic.
4.20 Methyl orange, indicator.
4.21 Methyl orange solution, 1 mg/ml.
Dissolve 0,10 g of methyl orange in 20 ml of water. Dilute to 100 ml.
5 Apparatus
Use ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks
complying with the specifications of ISO 648 and ISO 1042 respectively, and the following.
5.1 Atomic absorption spectrometer, equipped with an arsenic hollow cathode lamp or electrodeless
discharge lamp.
WARNING — Follow the manufacturer’s instructions to avoid possible explosion hazards for
igniting and extinguishing the air-acetylene flame and possible burning for hot electric furnace.
Wear tinted safety glasses whenever the atomic absorption spectrometer is in operation. Good
ventilation of the flame is necessary to prevent poison by arsenic hydride.
The atomic absorption spectrometer used in this method shall meet the following criteria.
a) Minimum sensitivity: The absorbance of the highest concentration calibration solution (see 7.4.3) is
at least 0,25.
b) Graph linearity: The slope of the calibration graph covering the top 20 % of the concentration range
(expressed as a change in absorbance) is not less than 0,7 of the value of the slope for the bottom
20 % of the concentration range determined in the same way.
c) Minimum stability: The standard deviation of the absorbance of the most concentrated calibration
solution and that of the zero calibration solution, each being calculated from a sufficient number
of repetitive measurements, are less than 1,5 % and 0,5 %, respectively, of the mean value of the
absorbance of the most concentrated solution.
The use of a strip-chart recorder and/or digital readout device is recommended to eva
...
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