Iron ores -- Determination of lead content -- Flame atomic absorption spectrometric method

Minerais de fer -- Dosage du plomb -- Méthode par spectrométrie d'absorption atomique dans la flamme

Železove rude - Določevanje svinca - Metoda plamenske atomske absorpcijske spektrometrije

General Information

Status
Published
Publication Date
31-May-2000
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Jun-2000
Due Date
01-Jun-2000
Completion Date
01-Jun-2000

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INTERNATIONAL IS0
STANDARD 13311
First edition
1997-08-o 1
Iron ores - Determination of lead content -
Flame atomic absorption spectrometric
method
Minerais de fer - Dosage du plomb - M&hode par spectrom6trie
d ’absorption atomique dans la flamme
Reference number
IS0 13311:1997(E)
---------------------- Page: 1 ----------------------
IS0 13311:1997(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 13311 was prepared by Technical Committee
ISO/TC 102, iron ores, Subcommittee SC 2, Chemical analysis.
Together with IS0 13310, 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=40Onet; p=iso; o=isocs; s=central
Printed in Switzerland
---------------------- Page: 2 ----------------------
INTERNATIONAL STANDARD @ IS0 IS0 13311:1997(E)
Iron ores - Determination of lead 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

lead content of iron ores.

This method is applicable to lead 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 labora tory 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 ----------------------
0 IS0
IS0 13311:1997(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 sol ution.

Extraction of iron in the filtrate with 4-methyl-2-pentanone. Recovery of lead 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 lead 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,CO,), anhydrous.
4.2 4-methyl-2-pentanone (MIBK), high purity.
4.3 Hydrochloric acid, p 1 ,16 g/ml to 1 ,I 9 g/ml.
4.4 Hydrochloric acid, p 1,16 g/ml to 1 ,I9 g/ml, diluted 10 + 6.
4.5 Hydrochloric acid, p 1 ,I6 g/ml to 1 ,19 g/ml, diluted 1 + 1.
4.6 Hydrochloric acid, p 1 ,I6 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 1 ,I9 g/ml, 48 % (m/m).
4.9 Lead standard solutions
4.9.1 Lead stock standard solution

Dissolve 1,000 g of lead metal [of purity > 99,5 % (m/m)] in 40 ml of nitric acid (p I,4 g/ml, diluted 1 + 1). 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 lead.
4.9.2 Standard solution A

Transfer 10,O ml of lead stock standard solution (4.9.1) to a 100 ml volumetric flask. Dilute to volume and mix.

1 ml of this standard solution contains 100 pg of lead.
4.9.3 Standard solution B

Transfer 10,O ml of standard solution A (4.9.2) to a 100 ml volumetric flask. Dilute to volume and mix.

1 ml of this standard solution contains 100 pg of lead.
---------------------- Page: 4 ----------------------
@ IS0 IS0 13311:1997(E)
5 Apparatus

Ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying with the

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.

the slope of the calibration graph covering the .top 20 % of the concentration range

b) Graph linearity -

(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

c) Minimum stability -

that of the zero calibration solution, each being calculated from a sufficient number of repetitive measurements,

shall be less than 15 % and 0,5 % respectively of the mean value of the absorbance of the most concentrated

calibration solution.
NOTES

1 The use of a strip-chart recorder and/or digital readout is mended to evaluate criteria a), b) and c) and for all

subsequent 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
- Wavelength, nm 283,3
- Air flow rate, Vmin 14
- Acetylene flow rate, I/min 3

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 OC ,+ 2 OC as specified in

IS0 7764. (This is the predried test sample.)
---------------------- Page: 5 ----------------------
@ IS0
IS0 13311:1997(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

test, provided that the procedure is the same and the reagents are from the same reagent bottles.

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

---------------------- Page: 6 ----------------------
@ IS0 IS0 13311:1997(E)
these washings with the main solution. Add 50 ml of 4-methyl-2-pentanone
...

SLOVENSKI STANDARD
SIST ISO 13311:2000
01-junij-2000
äHOH]RYHUXGH'RORþHYDQMHVYLQFD0HWRGDSODPHQVNHDWRPVNHDEVRUSFLMVNH
VSHNWURPHWULMH

Iron ores -- Determination of lead content -- Flame atomic absorption spectrometric

method

Minerais de fer -- Dosage du plomb -- Méthode par spectrométrie d'absorption atomique

dans la flamme
Ta slovenski standard je istoveten z: ISO 13311:1997
ICS:
73.060.10 Železove rude Iron ores
SIST ISO 13311:2000 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST ISO 13311:2000
---------------------- Page: 2 ----------------------
SIST ISO 13311:2000
INTERNATIONAL IS0
STANDARD 13311
First edition
1997-08-o 1
Iron ores - Determination of lead content -
Flame atomic absorption spectrometric
method
Minerais de fer - Dosage du plomb - M&hode par spectrom6trie
d ’absorption atomique dans la flamme
Reference number
IS0 13311:1997(E)
---------------------- Page: 3 ----------------------
SIST ISO 13311:2000
IS0 13311:1997(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 13311 was prepared by Technical Committee
ISO/TC 102, iron ores, Subcommittee SC 2, Chemical analysis.
Together with IS0 13310, 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=40Onet; p=iso; o=isocs; s=central
Printed in Switzerland
---------------------- Page: 4 ----------------------
SIST ISO 13311:2000
INTERNATIONAL STANDARD @ IS0 IS0 13311:1997(E)
Iron ores - Determination of lead 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

lead content of iron ores.

This method is applicable to lead 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 labora tory 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 13311:2000
0 IS0
IS0 13311:1997(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 sol ution.

Extraction of iron in the filtrate with 4-methyl-2-pentanone. Recovery of lead 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 lead 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,CO,), anhydrous.
4.2 4-methyl-2-pentanone (MIBK), high purity.
4.3 Hydrochloric acid, p 1 ,16 g/ml to 1 ,I 9 g/ml.
4.4 Hydrochloric acid, p 1,16 g/ml to 1 ,I9 g/ml, diluted 10 + 6.
4.5 Hydrochloric acid, p 1 ,I6 g/ml to 1 ,19 g/ml, diluted 1 + 1.
4.6 Hydrochloric acid, p 1 ,I6 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 1 ,I9 g/ml, 48 % (m/m).
4.9 Lead standard solutions
4.9.1 Lead stock standard solution

Dissolve 1,000 g of lead metal [of purity > 99,5 % (m/m)] in 40 ml of nitric acid (p I,4 g/ml, diluted 1 + 1). 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 lead.
4.9.2 Standard solution A

Transfer 10,O ml of lead stock standard solution (4.9.1) to a 100 ml volumetric flask. Dilute to volume and mix.

1 ml of this standard solution contains 100 pg of lead.
4.9.3 Standard solution B

Transfer 10,O ml of standard solution A (4.9.2) to a 100 ml volumetric flask. Dilute to volume and mix.

1 ml of this standard solution contains 100 pg of lead.
---------------------- Page: 6 ----------------------
SIST ISO 13311:2000
@ IS0 IS0 13311:1997(E)
5 Apparatus

Ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying with the

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.

the slope of the calibration graph covering the .top 20 % of the concentration range

b) Graph linearity -

(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

c) Minimum stability -

that of the zero calibration solution, each being calculated from a sufficient number of repetitive measurements,

shall be less than 15 % and 0,5 % respectively of the mean value of the absorbance of the most concentrated

calibration solution.
NOTES

1 The use of a strip-chart recorder and/or digital readout is mended to evaluate criteria a), b) and c) and for all

subsequent 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
- Wavelength, nm 283,3
- Air flow rate, Vmin 14
- Acetylene flow rate, I/min 3

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 OC ,+ 2 OC as specified in

IS0 7764. (This is the predried test sample.)
---------------------- Page: 7 ----------------------
SIST ISO 13311:2000
@ IS0
IS0 13311:1997(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

test, provided that the procedure is the same and the reagents are from the same reagent bottles.

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 hydrochl
...

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