SIST ISO 13310:2000
(Main)Iron ores -- Determination of zinc content -- Flame atomic absorption spectrometric method
Iron ores -- Determination of zinc content -- Flame atomic absorption spectrometric method
Minerais de fer -- Dosage du zinc -- Méthode par spectrométrie d'absorption atomique dans la flamme
Železove rude - Določevanje cinka - Metoda plamenske atomske absorpcijske spektrometrije
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INTERNATIONAL IS0
STANDARD 13310
First edition
1997-08-01
Iron ores - Determination of zinc content -
Flame atomic absorption spectrometric
method
Minerais de fer - Dosage du zinc - M&hode par spectrom6trie
d ’absorptior? atomique dans la flamme
Reference number
IS0 13310:1997(E)
---------------------- Page: 1 ----------------------
IS0 13310:1997(E)
Foreword
IS0 (the international Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work of
preparing International Standards is normally carried out through IS0
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. IS0
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
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 IS0 13310 was prepared by Technical Committee
lSO/TC 102, iron ores, Subcommittee SC 2, Chemical analysis.
Together with IS0 13311, it cancels and replaces IS0 8753:1987, of which
it constitutes a technical revision.
Annex A forms an integral part of this International Standard. Annexes B
and C are for information only.
0 IS0 1997
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 l CH-1211 Geneve 20 l Switzerland
Internet central @ iso.ch
x.400 c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
ii
---------------------- Page: 2 ----------------------
INTERNATIONAL STANDARD o Iso IS0 13310:1997(E)
Iron ores - Determination of zinc content - Flame atomic
absorption spectrometric method
WARNING - This International Standard may involve hazardous materials, operations and equipment. This
International Standard does not purport to address all of the safety issues associated with its use. It is the
responsibility of the user to establish appropriate health and safety practices and determine the
applicability of regulatory limitations prior to use.
1 Scope
This International Standard specifies a flame atomic absorption spectrometric method for the determination of the
zinc content of iron ores.
This method is applicable to zinc contents between 0,001 % (m/m) and 0,5 % (m/m) in natural iron ores, iron ore
concentrates and agglomerates, including sinter products.
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 IS0 maintain
registers of currently valid International Standards.
IS0 648:1977, Laboratory glassware - One-mark pipettes.
IS0 1042:1983, Laboratory glassware - One-mark volumetric flasks.
IS0 3081 :I 986, Iron ores - Increment sampling - Manual method.
IS0 3082: 1987, Iron ores - Increment sampling and sample preparation - Mechanical method.
IS0 3083:1986, Iron ores - Preparation of samples - Manual method.
IS0 3696:1987, Water for analytical laboratory use - Specification and test methods.
IS0 7764:1985, Iron ores - Preparation of predried test samples for chemical analysis.
3 Principle
Decomposition of the test portion and removal of silica by treatment with hydrochloric acid and hydrofluoric acid.
Oxidation with nitric acid.
---------------------- Page: 3 ----------------------
@ IS0
IS0 13310:1997(E)
Evaporation to dryness, followed by dilution and filtration. Ignition of the residue. Fusion with sodium carbonate.
Dissolution of the cooled melt with hydrochloric acid. Reservation of the solution.
Extraction of iron in the filtrate with 4-methyl-2-pentanone. Recovery of zinc extracted. Decomposition of 4-methyl-
2-pentanone with nitric acid. Evaporation to dryness and dissolution of salts with the reserved solution and
hydrochloric acid.
Aspiration of the solution into the flame of an atomic absorption spectrometer using an air-acetylene burner.
Comparison of absorbance values obtained for zinc with those obtained from the calibration solutions.
4 Reagents
During the analysis, use only reagents of recognized analytical grade and only water that complies with grade 2 of
IS0 3696.
4.1 Sodium carbonate (Na&O,), anhydrous.
4.2 4-methyl-2-pentanone (MIBK), high purity.
4.3 Hydrochloric acid, p 1 ,I6 g/ml to I,19 g/ml.
4.4 Hydrochloric acid, p 1 ,I6 g/ml to 1,19 g/ml, diluted IO + 6.
4.5 Hydrochloric acid, p I,16 g/ml to 1 ,I9 g/ml, diluted 1 + 1.
4.6 Hydrochloric acid, p 1 ,16 g/ml to 1 ,I 9 g/ml, diluted 2 + 98.
4.7 Nitric acid, p 1,4 g/ml.
4.8 Hydrofluoric acid, p 1 ,I3 g/ml, 40 % (m/m), or p I,19 g/ml, 48 % (m/m).
4.9 Zinc standard solutions
4.9.1 Zinc stock standard solution
Dissolve 1,000 g of zinc metal [of purity > 99,5 % (m/m)] in 40 ml of hydrochloric acid (4.5). Cool and dilute to
1 000 ml in a one-mark volumetric flask and mix.
1 ml of the stock solution contains 1 000 pg of zinc.
4.9.2 Standard solution
Transfer 10,O ml of zinc stock standard solution (4.9.1) to a 1 000 ml one-mark volumetric flask. Dilute to volume
and mix.
1 ml of this standard solution contains 10 pg of zinc.
---------------------- Page: 4 ----------------------
@ IS0
5 Apparatus
Ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying
specifications of IS0 648 and IS0 1042 respectively, and
5.1 Polytetrafluoroethylene (PTFE) beaker, of capacity 250 ml, with a PTFE cover.
5.2 Atomic absorption spectrometer, equipped with an air-acetylene burner.
The atomic absorption spectrometer shall meet the following criteria.
WARNING - Follow the manufacturer ’s instructions for igniting and extinguishing the air-acetylene flame
to avoid possible explosion hazards. Wear tinted safety glasses whenever the burner is in operation.
a) Minimum sensitivity - the absorbance of the most concentrated calibration solution (see 7.4.4) shall be at least
0,25.
Graph linearity - the slope of the calibration graph covering the top 20 % of the concentration range
(expressed as a change in absorbance) shall not be less than 0,7 of the value of the slope for the bottom 20 %
of the concentration range determined in the same way.
the standard deviation of the absorbance of the most concentrated calibration solution and
Minimum stability -
that of the zero calibration solution, each being calculated from a sufficient number of repetitive measurements,
shall be less than I,5 % and 0,5 % respectively of the mean value of the absorbance of the most concentrated
calibration solution.
NOTES
and/or digital readout device is recommended to evaluate criteria a), b) and c) and for all
The use of a strip-chart recorder
su bsequent measurements
2 Instrument parameters will vary with each instrument. The following parameters were successfully used in several
laboratories and they can be used as guidelines.
- Hollow cathode lamp, mA 8
- Wavelength, nm 213,9
- Air flow rate, Vmin 14
3
- Acetylene flow rate, I/min
In systems where the values shown for gas flow rates do not apply, the ratio of the gas flow rates may still be a useful
guideline.
6 Sampling and samples
6.1 Laboratory sample
For analysis, use a laboratory sample of minus 100 pm particle size which has been taken in accordance with
IS0 3081 or IS0 3082 and prepared in accordance with IS0 3082 or IS0 3083. In the case of ores having
significant contents of combined water or oxidizable compounds, use a particle size of minus 160 pm.
NOTE - A guideline on significant contents of combined water and oxidizable compounds is incorporated in IS0 7764.
6.2 Preparation of predried test samples
Thoroughly mix the laboratory sample and, taking multiple increments, extract a test sample in such a manner that it
is representative of the whole contents of the container. Dry the test samples at 105 “C If: 2 “C as specified in
IS0 7764. (This is the predried test sample.)
---------------------- Page: 5 ----------------------
@ IS0
IS0 13310:1997(E)
7 Procedure
7.1 Number of determinations
Carry out the analysis at least in duplicate in accordance with annex A, independently, on one predried test sample.
NOTE - The expression “independently” means that the second and any subsequent result is not affected by the previous
result(s). For this particular analytical method, this condition implies that the repetition of the procedure is carried out either by
the same operator at a different time or by a different operator including, in either case, appropriate recalibration.
7.2 Test portion
Taking several increments, weigh, to the nearest 0,000 2 g, approximately 2 g of the predried test sample obtained
in accordance with 6.2.
NOTE - The test portion should be taken and weighed quickly in order to avoid reabsorption of moisture.
7.3 Blank test and check test
In each run, one blank test and one analysis of a certified reference material of the same type of ore shall be carried
out in parallel with the analysis of the ore sample(s) under the same conditions. A predried test sample of the
certified reference material shall be prepared as specified in 6.2.
NOTE - The certified reference material should be of the same type as the sample to be analysed and the properties of the
two materials should be sufficiently similar to ensure that, in either case, no significant changes in the analytical procedure
become necessary.
When the analysis is carried out on several samples at the same time, the blank value may be represented by one
the same reagent bottles.
test, provided that the procedure is the same and the reagents are from
When the analysis is carried out on several samples of the same type of ore at the same time, the analytical value
of one certified reference material may be used.
7.4 Determination
7.4.1 Decomposition of the test portion
Transfer the test portion (7.2) to a 250 ml PTFE beaker (5.1). Moisten with a few millilitres of water, add 40 ml of
hydrochloric acid (4.3) and 10 ml of hydrofluoric acid (4.8), and cover with a PTFE cover. Heat on a hotplate at
100 OC, then increase the heat to 200 OC. Evaporate to dryness. Add 5 ml of nitric acid (4.7) and evaporate to nearly
1 ml. Dissolve the salts with 10 ml of hydrochloric acid (4.3) and evaporate to dryness again.
Dissolve the salts with 5 ml of hydrochloric acid (4.3). Add 10 ml of water and filter through a close-texture paper
into a 250 ml beaker. Remove all adhering particles from the beaker with a rubber-tipped rod, wash with
hydrochloric acid (4.6) until the paper is free from iron stains, and wash the paper three times with hot water.
Reserve the residue and combined filtrate and washings.
7.4.2 Treatment of residue
Place the paper and residue in a platinum crucible, dry and char the paper at a low temperature and ignite in a muffle
furnace at 550 OC. Add 0,5 g of sodium carbonate (4.1) and fuse over a Bunsen burner (about 900 OC to 1 000 OC)
until a clear melt is obtained. Dissolve the cooled melt with 5 ml of hydrochloric acid (4.5), heat to remove carbon
dioxide and reserve the solution.
7.4.3 Treatment of combined filtrate and washings
Evaporate the filtrate and washings (7.4.1) just to dryness. Dissolve the salts .with 20 ml of hydrochloric acid (4.4),
and transfer to a 200 ml separating funnel. Rinse the beaker with 20 ml of hydrochloric acid (4.4) and combine
4
---------------------- Page: 6 ----------------------
@ IS0 IS0 13310:1997(E)
these washings with the main solution. Add 50 ml of 4-methyl-2-pentanone (4.2) and shake thoroughly for 1 min.
Allow the l
...
SLOVENSKI STANDARD
SIST ISO 13310:2000
01-junij-2000
äHOH]RYHUXGH'RORþHYDQMHFLQND0HWRGDSODPHQVNHDWRPVNHDEVRUSFLMVNH
VSHNWURPHWULMH
Iron ores -- Determination of zinc content -- Flame atomic absorption spectrometric
method
Minerais de fer -- Dosage du zinc -- Méthode par spectrométrie d'absorption atomique
dans la flamme
Ta slovenski standard je istoveten z: ISO 13310:1997
ICS:
73.060.10 Železove rude Iron ores
SIST ISO 13310:2000 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST ISO 13310:2000
---------------------- Page: 2 ----------------------
SIST ISO 13310:2000
INTERNATIONAL IS0
STANDARD 13310
First edition
1997-08-01
Iron ores - Determination of zinc content -
Flame atomic absorption spectrometric
method
Minerais de fer - Dosage du zinc - M&hode par spectrom6trie
d ’absorptior? atomique dans la flamme
Reference number
IS0 13310:1997(E)
---------------------- Page: 3 ----------------------
SIST ISO 13310:2000
IS0 13310:1997(E)
Foreword
IS0 (the international Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work of
preparing International Standards is normally carried out through IS0
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. IS0
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
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 IS0 13310 was prepared by Technical Committee
lSO/TC 102, iron ores, Subcommittee SC 2, Chemical analysis.
Together with IS0 13311, it cancels and replaces IS0 8753:1987, of which
it constitutes a technical revision.
Annex A forms an integral part of this International Standard. Annexes B
and C are for information only.
0 IS0 1997
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 l CH-1211 Geneve 20 l Switzerland
Internet central @ iso.ch
x.400 c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
ii
---------------------- Page: 4 ----------------------
SIST ISO 13310:2000
INTERNATIONAL STANDARD o Iso IS0 13310:1997(E)
Iron ores - Determination of zinc content - Flame atomic
absorption spectrometric method
WARNING - This International Standard may involve hazardous materials, operations and equipment. This
International Standard does not purport to address all of the safety issues associated with its use. It is the
responsibility of the user to establish appropriate health and safety practices and determine the
applicability of regulatory limitations prior to use.
1 Scope
This International Standard specifies a flame atomic absorption spectrometric method for the determination of the
zinc content of iron ores.
This method is applicable to zinc contents between 0,001 % (m/m) and 0,5 % (m/m) in natural iron ores, iron ore
concentrates and agglomerates, including sinter products.
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 IS0 maintain
registers of currently valid International Standards.
IS0 648:1977, Laboratory glassware - One-mark pipettes.
IS0 1042:1983, Laboratory glassware - One-mark volumetric flasks.
IS0 3081 :I 986, Iron ores - Increment sampling - Manual method.
IS0 3082: 1987, Iron ores - Increment sampling and sample preparation - Mechanical method.
IS0 3083:1986, Iron ores - Preparation of samples - Manual method.
IS0 3696:1987, Water for analytical laboratory use - Specification and test methods.
IS0 7764:1985, Iron ores - Preparation of predried test samples for chemical analysis.
3 Principle
Decomposition of the test portion and removal of silica by treatment with hydrochloric acid and hydrofluoric acid.
Oxidation with nitric acid.
---------------------- Page: 5 ----------------------
SIST ISO 13310:2000
@ IS0
IS0 13310:1997(E)
Evaporation to dryness, followed by dilution and filtration. Ignition of the residue. Fusion with sodium carbonate.
Dissolution of the cooled melt with hydrochloric acid. Reservation of the solution.
Extraction of iron in the filtrate with 4-methyl-2-pentanone. Recovery of zinc extracted. Decomposition of 4-methyl-
2-pentanone with nitric acid. Evaporation to dryness and dissolution of salts with the reserved solution and
hydrochloric acid.
Aspiration of the solution into the flame of an atomic absorption spectrometer using an air-acetylene burner.
Comparison of absorbance values obtained for zinc with those obtained from the calibration solutions.
4 Reagents
During the analysis, use only reagents of recognized analytical grade and only water that complies with grade 2 of
IS0 3696.
4.1 Sodium carbonate (Na&O,), anhydrous.
4.2 4-methyl-2-pentanone (MIBK), high purity.
4.3 Hydrochloric acid, p 1 ,I6 g/ml to I,19 g/ml.
4.4 Hydrochloric acid, p 1 ,I6 g/ml to 1,19 g/ml, diluted IO + 6.
4.5 Hydrochloric acid, p I,16 g/ml to 1 ,I9 g/ml, diluted 1 + 1.
4.6 Hydrochloric acid, p 1 ,16 g/ml to 1 ,I 9 g/ml, diluted 2 + 98.
4.7 Nitric acid, p 1,4 g/ml.
4.8 Hydrofluoric acid, p 1 ,I3 g/ml, 40 % (m/m), or p I,19 g/ml, 48 % (m/m).
4.9 Zinc standard solutions
4.9.1 Zinc stock standard solution
Dissolve 1,000 g of zinc metal [of purity > 99,5 % (m/m)] in 40 ml of hydrochloric acid (4.5). Cool and dilute to
1 000 ml in a one-mark volumetric flask and mix.
1 ml of the stock solution contains 1 000 pg of zinc.
4.9.2 Standard solution
Transfer 10,O ml of zinc stock standard solution (4.9.1) to a 1 000 ml one-mark volumetric flask. Dilute to volume
and mix.
1 ml of this standard solution contains 10 pg of zinc.
---------------------- Page: 6 ----------------------
SIST ISO 13310:2000
@ IS0
5 Apparatus
Ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying
specifications of IS0 648 and IS0 1042 respectively, and
5.1 Polytetrafluoroethylene (PTFE) beaker, of capacity 250 ml, with a PTFE cover.
5.2 Atomic absorption spectrometer, equipped with an air-acetylene burner.
The atomic absorption spectrometer shall meet the following criteria.
WARNING - Follow the manufacturer ’s instructions for igniting and extinguishing the air-acetylene flame
to avoid possible explosion hazards. Wear tinted safety glasses whenever the burner is in operation.
a) Minimum sensitivity - the absorbance of the most concentrated calibration solution (see 7.4.4) shall be at least
0,25.
Graph linearity - the slope of the calibration graph covering the top 20 % of the concentration range
(expressed as a change in absorbance) shall not be less than 0,7 of the value of the slope for the bottom 20 %
of the concentration range determined in the same way.
the standard deviation of the absorbance of the most concentrated calibration solution and
Minimum stability -
that of the zero calibration solution, each being calculated from a sufficient number of repetitive measurements,
shall be less than I,5 % and 0,5 % respectively of the mean value of the absorbance of the most concentrated
calibration solution.
NOTES
and/or digital readout device is recommended to evaluate criteria a), b) and c) and for all
The use of a strip-chart recorder
su bsequent measurements
2 Instrument parameters will vary with each instrument. The following parameters were successfully used in several
laboratories and they can be used as guidelines.
- Hollow cathode lamp, mA 8
- Wavelength, nm 213,9
- Air flow rate, Vmin 14
3
- Acetylene flow rate, I/min
In systems where the values shown for gas flow rates do not apply, the ratio of the gas flow rates may still be a useful
guideline.
6 Sampling and samples
6.1 Laboratory sample
For analysis, use a laboratory sample of minus 100 pm particle size which has been taken in accordance with
IS0 3081 or IS0 3082 and prepared in accordance with IS0 3082 or IS0 3083. In the case of ores having
significant contents of combined water or oxidizable compounds, use a particle size of minus 160 pm.
NOTE - A guideline on significant contents of combined water and oxidizable compounds is incorporated in IS0 7764.
6.2 Preparation of predried test samples
Thoroughly mix the laboratory sample and, taking multiple increments, extract a test sample in such a manner that it
is representative of the whole contents of the container. Dry the test samples at 105 “C If: 2 “C as specified in
IS0 7764. (This is the predried test sample.)
---------------------- Page: 7 ----------------------
SIST ISO 13310:2000
@ IS0
IS0 13310:1997(E)
7 Procedure
7.1 Number of determinations
Carry out the analysis at least in duplicate in accordance with annex A, independently, on one predried test sample.
NOTE - The expression “independently” means that the second and any subsequent result is not affected by the previous
result(s). For this particular analytical method, this condition implies that the repetition of the procedure is carried out either by
the same operator at a different time or by a different operator including, in either case, appropriate recalibration.
7.2 Test portion
Taking several increments, weigh, to the nearest 0,000 2 g, approximately 2 g of the predried test sample obtained
in accordance with 6.2.
NOTE - The test portion should be taken and weighed quickly in order to avoid reabsorption of moisture.
7.3 Blank test and check test
In each run, one blank test and one analysis of a certified reference material of the same type of ore shall be carried
out in parallel with the analysis of the ore sample(s) under the same conditions. A predried test sample of the
certified reference material shall be prepared as specified in 6.2.
NOTE - The certified reference material should be of the same type as the sample to be analysed and the properties of the
two materials should be sufficiently similar to ensure that, in either case, no significant changes in the analytical procedure
become necessary.
When the analysis is carried out on several samples at the same time, the blank value may be represented by one
the same reagent bottles.
test, provided that the procedure is the same and the reagents are from
When the analysis is carried out on several samples of the same type of ore at the same time, the analytical value
of one certified reference material may be used.
7.4 Determination
7.4.1 Decomposition of the test portion
Transfer the test portion (7.2) to a 250 ml PTFE beaker (5.1). Moisten with a few millilitres of water, add 40 ml of
hydrochloric acid (4.3) and 10 ml of hydrofluoric acid (4.8), and cover with a PTFE cover. Heat on a hotplate at
100 OC, then increase the heat to 200 OC. Evaporate to dryness. Add 5 ml of nitric acid (4.7) and evaporate to nearly
1 ml. Dissolve the salts with 10 ml of hydrochloric acid (4.3) and evaporate to dryness again.
Dissolve the salts with 5 ml of hydrochloric acid (4.3). Add 10 ml of water and filter through a close-texture paper
into a 250 ml beaker. Remove all adhering particles from the beaker with a rubber-tipped rod, wash with
hydrochloric acid (4.6) until the paper is free from iron stains, and wash the paper three times with hot water.
Reserve the residue and combined filtrate and washings.
7.4.2 Treatment of residue
Place the paper and residue in a platinum crucible, dry and char the paper at a low temperature and ignite in a muffle
furnace at 550 OC. Add 0,5 g of sodium carbonate (4.1) and fuse over a Bunsen burner (about 900 OC to 1 000 OC)
until a clear melt is obtained. Dissolve the cooled melt with 5 ml of hydrochloric acid (4.5), heat to remove carbon
dioxide and re
...
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