ISO 15247:1999

Zinc sulfide concentrates — Determination of silver content — Acid dissolution and flame atomic absorption spectrometric method

Concentrés sulfurés de zinc — Dosage de l'argent — Méthode par dissolution acide et spectrométrie d'absorption atomique dans la flamme

Koncentrati cinkovega sulfida - Določevanje srebra - Metoda kislinskega raztapljanja in metoda plamenske atomske absorpcijske spektrometrije

General Information

• Status: Withdrawn
• Publication Date: 28-Apr-1999
• Withdrawal Date: 28-Apr-1999
• ICS: 73.060.99 - Other metalliferous minerals
• Technical Committee: ISO/TC 183 - Copper, lead, zinc and nickel ores and concentrates
• Drafting Committee: ISO/TC 183 - Copper, lead, zinc and nickel ores and concentrates
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 15-Jun-2015
• Ref Project: SIST ISO 15247:2001 - Zinc sulfide concentrates -- Determination of silver content -- Acid dissolution and flame atomic absorption spectrometric method

Relations

• Revised: ISO 15247:2015 - Zinc sulfide concentrates — Determination of silver content — Acid dissolution and flame atomic absorption spectrometric method
• Effective Date: 29-Dec-2012

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 15247
First edition
1999-04-15
Zinc sulfide concentrates — Determination
of silver content — Acid dissolution and
flame atomic absorption spectrometric
method
Concentrés sulfurés de zinc — Dosage de l'argent — Méthode par
dissolution acide et spectrométrie d'absorption atomique dans la flamme
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND USER
PURPOSES, DRAFT INTERNATIONAL STAND-
ARDS MAY ON OCCASION HAVE TO BE
CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
A
Reference number
WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. ISO/FDIS 15247:1999(E)

---------------------- Page: 1 ----------------------
ISO 15247:1999(E)
Contents Page
1 Scope .1
2 Normative references .1
3 Principle.1
4 Reagents.2
5 Apparatus .3
6 Sample .3
7 Procedure .3
8 Expression of results .5
9 Precision.5
10 Test report .7
Annex A (normative) Procedure for the preparation and determination of the mass of a predried test
portion.8
Annex B (normative) Flowsheet of the procedure for the acceptance of analytical values for test samples .10
Annex C (informative) Derivation of precision equations .11
©  ISO 1999
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic
or mechanical, including photocopying and microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet [e-mail]
Printed in Switzerland
ii

---------------------- Page: 2 ----------------------
© ISO
ISO 15247:1999(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
International Standard ISO 15247 was prepared by Technical Committee ISO/TC 183, Copper, lead and zinc ores
and concentrates.
Annexes A and B form an integral part of this International Standard, annex C is for information only.
iii

---------------------- Page: 3 ----------------------
INTERNATIONAL STANDARD  © ISO ISO 15247:1999(E)
Zinc sulfide concentrates — Determination of silver content —
Acid dissolution and flame atomic absorption spectrometric
method
1 Scope
This International Standard specifies an acid dissolution and flame atomic absorption spectrometric method for the
determination of silver content of zinc sulfide concentrates.
The method is applicable to the determination of silver in zinc sulfide concentrates containing up to 60 % (m/m) zinc
in the form of zinc blende and related materials.
The method is applicable to silver contents from 10 g/t to 500 g/t.
2 Normative references
The following standards contain provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of publication, the editions indicated were valid. All standards are subject to
revision, and parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain
registers of currently valid International Standards.
ISO 385-1:1984, Laboratory glassware — Burettes — Part 1: General requirements.
ISO 648:1977, Laboratory glassware — One mark pipettes.
ISO 1042:1998, Laboratory glassware — One-mark volumetric flasks.
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods.
ISO 4787:1984, Laboratory glassware — Volumetric glassware — Methods for use and testing of capacity.
ISO 9599:1991, Copper, lead and zinc sulfide concentrates — Determination of hygroscopic moisture in the analysis
sample — Gravimetric method.
3 Principle
Decomposition of the concentrate in hydrochloric and nitric acids. Dissolution of the digestion residue in
hydrochloric acid and measurement by flame atomic absorption at 328,1 nm.
1

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© ISO
ISO 15247:1999(E)
4 Reagents
During the analysis, use only reagents of recognized analytical grade and water that complies with grade 2 of
ISO 3696.
4.1  Silver metal, minimum 99,99 % purity.
4.2  Nitric acid, (r 1,42 g/ml), chloride content < 0,5 mg/ml.
20
4.3  Nitric acid, (500 ml/l).
To 250 ml of water carefully add, with stirring, 250 ml of nitric acid (4.2).
4.4  Hydrochloric acid, (r1,16 g/ml to 1,19 g/ml).
20
4.5  Hydrochloric acid, (200 ml/l).
To 800 ml of water carefully add, with stirring, 200 ml of hydrochloric acid (4.4).
4.6  Ammonia solution, (r 0,89 g/ml).
20
4.7  Ammonia solution, (250 ml/l).
To 750 ml of water add, with stirring, 250 ml of ammonia solution (4.6).
4.8  Silver standard solutions
4.8.1  Silver standard solution, (1 000 mg/ml)
Weigh 0,500 0 g of silver metal (4.1) into a 250 ml conical beaker, add 50 ml of nitric acid (4.3), cover and heat
gently until the metal dissolves. Remove the cover and evaporate gently to near dryness. Add 250 ml of
hydrochloric acid (4.4) and warm until the solution clears. Cool, and transfer to a 500 ml volumetric flask. Dilute to
volume with water and mix thoroughly.
This solution should be freshly prepared, unless it is being used on a regular basis.
4.8.2  Silver standard solution, (100 mg/ml)
Pipette 10 ml of silver standard solution (4.8.1) into a 100 ml volumetric flask containing 45 ml of hydrochloric acid
(4.4). Dilute to volume with water and mix thoroughly.
NOTE 1 Standard solutions should be prepared at the same ambient temperature as that at which the determinations will be
conducted.
NOTE 2 Silver standard solutions should be stored in brown glass bottles.
4.9  Calibration solutions
To six 100 ml volumetric flasks, each containing 20 ml of hydrochloric acid (4.4), add from a burette (5.2) 0 ml, 1 ml,
2 ml, 3 ml, 4 ml and 5 ml of silver standard solution (4.8.2). Dilute to volume with water and mix thoroughly.
These standards contain 0 mg, 1 mg, 2 mg, 3 mg, 4 mg and 5 mg of silver per ml and shall be freshly prepared.
NOTE Calibration solutions should be prepared at the same ambient temperature as that at which the determinations will
be conducted.
2

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© ISO
ISO 15247:1999(E)
5 Apparatus
Ordinary laboratory apparatus and
5.1  Volumetric glassware, of class A complying with ISO 385-1, ISO 648 and ISO 1042 and used in accordance
with ISO 4787.
5.2  Burette, grade A 10 ml capacity, capable of being read to 0,02 ml.
5.3  Atomic absorption spectrometer (AAS), equipped with a glass bead in the spray chamber rather than a flow
spoiler.
5.4  Balance, precision analytical, capable of being read to 0,1 milligram.
6 Sample
6.1 Test sample
Prepare an air-equilibrated test sample in accordance with ISO 9599.
NOTE A test sample is not required if predried test portions are to be used (see annex A).
6.2 Test portion
Taking multiple increments, extract a test portion from the test sample in such a manner that it is representative of
the whole contents of the dish or tray. Weigh to the nearest 0,1 mg approximately 1 g of test sample. At the same
time as the test portion is weighed, 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 predried test portions directly from the
laboratory sample.
7 Procedure
7.1 Number of determinations
Carry out the determinations at least in duplicate and as far as possible under repeatability conditions, on each test
sample.
NOTE Repeatability conditions exist where mutually independent test results are obtained with the same method on
identical test material in the same laboratory by the same operator using the same equipment within short intervals of time.
7.2 Blank test
Carry out a blank test in parallel with the analysis using all reagents specified in the determination but omitting the
test portion. The purpose of the blank test in this method is to check the quality of the reagents. If a significant blank
value is obtained as a result of the blank test, check all reagents and rectify the problem.
7.3 Decomposition of test portion
Transfer the test portion to a 250 ml conical beaker and moisten with 1 ml of water.
NOTE 1 All glassware should be washed in ammonia (4.7) and rinsed with water prior to use to remove any silver adhering to
the glass surface.
Add 35 ml of nitric acid (4.3), cover with a watch glass and heat at a low temperature until the reaction ceases.
3

---------------------- Page: 6 ----------------------
© ISO
ISO 15247:1999(E)
Add 10 ml of hydrochloric acid (4.4), raise the cover slightly and evaporate to dryness. Remove from the hotplate
and cool.
Add a further 10 ml of hydrochloric acid (4.4) and again evaporate to dryness.
NOTE 2 Rapid heating may cause samples to splatter or spit. Care should be taken to ensure that this does not occur.
Redissolve in 25 ml of hydrochloric acid (4.5). Heat to boiling, remove from the hotplate and cool.
Transfer the solution to the volumetric flask indicated in Table 1 by washing and diluting to volume with hydrochloric
acid (4.5).
Table 1 — Volumetric flask size
Ag content Volumetric flask
g/t ml
10 to 250 50
250 to 500 100
7.4 Determination of silver
Determine the silver content of the test portion by flame atomic absorption spectrometry using calibration solutions
(4.9). As a guide, the following atomic absorption settings are recommended; however, the instrument should be
optimized to give maximum sensitivity and as near as practical to a linear relationship between absorbance and
concentration.
 Flame: air-acetylene (oxidizing)
 Wavelength: 328,1 nm
 Lamp current: 5 mA
 Background correction: none
 Aspiration rate: optimize for maximum signal
 Integration time: 3 s
 Number of integrations: 5
Perform three measurements on each standard solution. Calculate, to three significant figures, the mean
absorbance for each standard solution, provided that the range of values does not exceed 0,003 absorbance units.
If this range is exceeded, repeat the calibration.
The test solutions should
...

SLOVENSKI STANDARD
SIST ISO 15247:2001
01-junij-2001
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UD]WDSOMDQMDLQPHWRGDSODPHQVNHDWRPVNHDEVRUSFLMVNHVSHNWURPHWULMH
Zinc sulfide concentrates -- Determination of silver content -- Acid dissolution and flame
atomic absorption spectrometric method
Concentrés sulfurés de zinc -- Dosage de l'argent -- Méthode par dissolution acide et
spectrométrie d'absorption atomique dans la flamme
Ta slovenski standard je istoveten z: ISO 15247:1999
ICS:
73.060.99 Druge rude Other metalliferous minerals
SIST ISO 15247:2001 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST ISO 15247:2001

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SIST ISO 15247:2001
INTERNATIONAL ISO
STANDARD 15247
First edition
1999-04-15
Zinc sulfide concentrates — Determination
of silver content — Acid dissolution and
flame atomic absorption spectrometric
method
Concentrés sulfurés de zinc — Dosage de l'argent — Méthode par
dissolution acide et spectrométrie d'absorption atomique dans la flamme
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND USER
PURPOSES, DRAFT INTERNATIONAL STAND-
ARDS MAY ON OCCASION HAVE TO BE
CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
A
Reference number
WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. ISO/FDIS 15247:1999(E)

---------------------- Page: 3 ----------------------

SIST ISO 15247:2001
ISO 15247:1999(E)
Contents Page
1 Scope .1
2 Normative references .1
3 Principle.1
4 Reagents.2
5 Apparatus .3
6 Sample .3
7 Procedure .3
8 Expression of results .5
9 Precision.5
10 Test report .7
Annex A (normative) Procedure for the preparation and determination of the mass of a predried test
portion.8
Annex B (normative) Flowsheet of the procedure for the acceptance of analytical values for test samples .10
Annex C (informative) Derivation of precision equations .11
©  ISO 1999
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic
or mechanical, including photocopying and microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet [e-mail]
Printed in Switzerland
ii

---------------------- Page: 4 ----------------------

SIST ISO 15247:2001
© ISO
ISO 15247:1999(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
International Standard ISO 15247 was prepared by Technical Committee ISO/TC 183, Copper, lead and zinc ores
and concentrates.
Annexes A and B form an integral part of this International Standard, annex C is for information only.
iii

---------------------- Page: 5 ----------------------

SIST ISO 15247:2001

---------------------- Page: 6 ----------------------

SIST ISO 15247:2001
INTERNATIONAL STANDARD  © ISO ISO 15247:1999(E)
Zinc sulfide concentrates — Determination of silver content —
Acid dissolution and flame atomic absorption spectrometric
method
1 Scope
This International Standard specifies an acid dissolution and flame atomic absorption spectrometric method for the
determination of silver content of zinc sulfide concentrates.
The method is applicable to the determination of silver in zinc sulfide concentrates containing up to 60 % (m/m) zinc
in the form of zinc blende and related materials.
The method is applicable to silver contents from 10 g/t to 500 g/t.
2 Normative references
The following standards contain provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of publication, the editions indicated were valid. All standards are subject to
revision, and parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain
registers of currently valid International Standards.
ISO 385-1:1984, Laboratory glassware — Burettes — Part 1: General requirements.
ISO 648:1977, Laboratory glassware — One mark pipettes.
ISO 1042:1998, Laboratory glassware — One-mark volumetric flasks.
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods.
ISO 4787:1984, Laboratory glassware — Volumetric glassware — Methods for use and testing of capacity.
ISO 9599:1991, Copper, lead and zinc sulfide concentrates — Determination of hygroscopic moisture in the analysis
sample — Gravimetric method.
3 Principle
Decomposition of the concentrate in hydrochloric and nitric acids. Dissolution of the digestion residue in
hydrochloric acid and measurement by flame atomic absorption at 328,1 nm.
1

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SIST ISO 15247:2001
© ISO
ISO 15247:1999(E)
4 Reagents
During the analysis, use only reagents of recognized analytical grade and water that complies with grade 2 of
ISO 3696.
4.1  Silver metal, minimum 99,99 % purity.
4.2  Nitric acid, (r 1,42 g/ml), chloride content < 0,5 mg/ml.
20
4.3  Nitric acid, (500 ml/l).
To 250 ml of water carefully add, with stirring, 250 ml of nitric acid (4.2).
4.4  Hydrochloric acid, (r1,16 g/ml to 1,19 g/ml).
20
4.5  Hydrochloric acid, (200 ml/l).
To 800 ml of water carefully add, with stirring, 200 ml of hydrochloric acid (4.4).
4.6  Ammonia solution, (r 0,89 g/ml).
20
4.7  Ammonia solution, (250 ml/l).
To 750 ml of water add, with stirring, 250 ml of ammonia solution (4.6).
4.8  Silver standard solutions
4.8.1  Silver standard solution, (1 000 mg/ml)
Weigh 0,500 0 g of silver metal (4.1) into a 250 ml conical beaker, add 50 ml of nitric acid (4.3), cover and heat
gently until the metal dissolves. Remove the cover and evaporate gently to near dryness. Add 250 ml of
hydrochloric acid (4.4) and warm until the solution clears. Cool, and transfer to a 500 ml volumetric flask. Dilute to
volume with water and mix thoroughly.
This solution should be freshly prepared, unless it is being used on a regular basis.
4.8.2  Silver standard solution, (100 mg/ml)
Pipette 10 ml of silver standard solution (4.8.1) into a 100 ml volumetric flask containing 45 ml of hydrochloric acid
(4.4). Dilute to volume with water and mix thoroughly.
NOTE 1 Standard solutions should be prepared at the same ambient temperature as that at which the determinations will be
conducted.
NOTE 2 Silver standard solutions should be stored in brown glass bottles.
4.9  Calibration solutions
To six 100 ml volumetric flasks, each containing 20 ml of hydrochloric acid (4.4), add from a burette (5.2) 0 ml, 1 ml,
2 ml, 3 ml, 4 ml and 5 ml of silver standard solution (4.8.2). Dilute to volume with water and mix thoroughly.
These standards contain 0 mg, 1 mg, 2 mg, 3 mg, 4 mg and 5 mg of silver per ml and shall be freshly prepared.
NOTE Calibration solutions should be prepared at the same ambient temperature as that at which the determinations will
be conducted.
2

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SIST ISO 15247:2001
© ISO
ISO 15247:1999(E)
5 Apparatus
Ordinary laboratory apparatus and
5.1  Volumetric glassware, of class A complying with ISO 385-1, ISO 648 and ISO 1042 and used in accordance
with ISO 4787.
5.2  Burette, grade A 10 ml capacity, capable of being read to 0,02 ml.
5.3  Atomic absorption spectrometer (AAS), equipped with a glass bead in the spray chamber rather than a flow
spoiler.
5.4  Balance, precision analytical, capable of being read to 0,1 milligram.
6 Sample
6.1 Test sample
Prepare an air-equilibrated test sample in accordance with ISO 9599.
NOTE A test sample is not required if predried test portions are to be used (see annex A).
6.2 Test portion
Taking multiple increments, extract a test portion from the test sample in such a manner that it is representative of
the whole contents of the dish or tray. Weigh to the nearest 0,1 mg approximately 1 g of test sample. At the same
time as the test portion is weighed, 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 predried test portions directly from the
laboratory sample.
7 Procedure
7.1 Number of determinations
Carry out the determinations at least in duplicate and as far as possible under repeatability conditions, on each test
sample.
NOTE Repeatability conditions exist where mutually independent test results are obtained with the same method on
identical test material in the same laboratory by the same operator using the same equipment within short intervals of time.
7.2 Blank test
Carry out a blank test in parallel with the analysis using all reagents specified in the determination but omitting the
test portion. The purpose of the blank test in this method is to check the quality of the reagents. If a significant blank
value is obtained as a result of the blank test, check all reagents and rectify the problem.
7.3 Decomposition of test portion
Transfer the test portion to a 250 ml conical beaker and moisten with 1 ml of water.
NOTE 1 All glassware should be washed in ammonia (4.7) and rinsed with water prior to use to remove any silver adhering to
the glass surface.
Add 35 ml of nitric acid (4.3), cover with a watch glass and heat at a low temperature until the reaction ceases.
3

---------------------- Page: 9 ----------------------

SIST ISO 15247:2001
© ISO
ISO 15247:1999(E)
Add 10 ml of hydrochloric acid (4.4), raise the cover slightly and evaporate to dryness. Remove from the hotplate
and cool.
Add a further 10 ml of hydrochloric acid (4.4) and again evaporate to dryness.
NOTE 2 Rapid heating may cause samples to splatter or spit. Care should be taken to ensure that this does not occur.
Redissolve in 25 ml of hydrochloric acid (4.5). Heat to boiling, remove from the hotplate and cool.
Transfer the solution to the volumetric flask indicated in Table 1 by washing and diluting to volume with hydrochloric
acid (4.5).
Table 1 — Volumetric flask size
Ag content Volumetric flask
g/t ml
10 to 250 50
250 to 500 100
7.4 Determination of silver
Determine the silver content of the test portion by flame atomic absorption spectrometry using calibration solutions
(4.9). As a guide, the following atomic absorption settings are recommended; however, the instrument should be
optimized to give maximum sensitivity and as near as practical to a linear relationship between absorbance and
concentration.
 Flame: air-acetylene (oxi
...