SIST ISO 5416:2000
(Main)Direct reduced iron -- Determination of metallic iron content -- Bromine-methanol titrimetric method
Direct reduced iron -- Determination of metallic iron content -- Bromine-methanol titrimetric method
Minerais de fer préréduits -- Dosage du fer métallique -- Méthode titrimétrique au brome-méthanol
Direktno reducirano železo - Določevanje kovinskega železa - Titrimetrijska metoda z brom-metanolom
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INTERNATIONAL IS0
STANDARD 5416
Second edition
1997-08-01
Direct reduced iron
- Determination of
metallic iron content - Bromine-methanol
titrimetric method
Minerais de fer prkrkduits - Dosage du fer m&allique - Mkthode
titrimhtrique au brome-mkthanol
Reference number
IS0 5416:1997(E)
---------------------- Page: 1 ----------------------
IS0 5416:1997(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 5416 was prepared by Technical Committee
ISO/TC 102, iron ores, Subcommittee SC 2, Chemical analysis.
This second edition cancels and replaces the first edition (IS0 5416:1987),
which has been technically revised.
Annex A form an integral part of this International Standard. Annexes B to E
are for information only.
0 IS0 1997
All rights resewed. 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
---------------------- Page: 2 ----------------------
INTERNATIONAL STANDARD 0 IS0 IS0 5416:1997(E)
- Determination of metallic iron
Direct reduced iron
- Bromine-methanol titrimetric method
content
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 titrimetric method for the determination of the metallic iron content of reduced
iron ores (direct reduced iron: DRI).
This method is applicable to metallic iron contents between 15 % (m/m) and 95 % (m/m) in DRI.
NOTE - The term “metallic iron” means those forms of iron not bonded to oxygen or not present as pyrite.
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 385-l :1984, Laboratory glassware - Burettes - Pat? 1: General requirements .
IS0 648: 1977, Laboratory glassware - One-mark pipettes.
IS0 1042: 1983, Laboratory glassware - One-mark volumetric flasks.
IS0 2596:1994, iron ores - Determination of hygroscopic moisture in analytical samples - Gravimetric and Karl
Fischer methods.
IS0 2597-l :1994, iron ores - Determination of total iron content - Part 1: Titrimetric method after tin(H) chloride
reduction.
IS0 3696: 1987, Water for analytical laboratory use - Specification and test methods.
IS0 10835:1995, Direct reduced iron - Sampling and sample preparation -
Manual methods for reduced pellets
and lump ores.
---------------------- Page: 3 ----------------------
@ IS0
IS0 5416:1997(E)
3 Principle
Dissolution of metallic iron by treatment with bromine-methanol solution. Separation of the insoluble residue by
filtration. Reduction of the iron in the filtrate to iron followed by titration with potassium dichromate solution.
manganese, nickel and vanadium are also dissolved by the
NOTE - Other metallic elements such as chromium, cobalt,
vanadium, they do not interfere with the titration procedure
bromine-methanol solution but, except for
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 Hydrochloric acid, p 1,16 g/ml to 1 ,19 g/ml.
4.2 Sulfuric acid, p 1,84 g/ml, diluted 1 + 1.
4.3 Methanol, Karl Fischer reagent grade, max. 0,l % H,O.
4.4 Bromine-methanol solution, 50 ml/l.
Dissolve 5 ml of bromine in 95 ml of methanol (4.3). This solution shall be freshly prepared and used immediately.
WARNING - The preparation of the bromine-methanol solution and all stages of the procedure where
bromine is present shall be carried out in an efficient fume cupboard.
4.5 Hydrogen peroxide solution, 30 % (V/V).
4.6 Tin(ll) chloride solution, 100 g/l.
Dissolve 119 g of tin(ll) chloride dihydrate (SnCI,-2H20) successively in small amounts with 200 ml of hydrochloric
acid (4.1) by warming. Cool, dilute to 1 litre and mix. Add 2 g of coarsely granulated tin and store the solution in a
brown bottle.
4.7 Mercury(ll) chloride solution, 50 g/l.
Dissolve 50 g of mercury(li) chloride (HgCl*) in 800 ml of hot water. Cool, dilute to 1 litre and mix.
4.8 Sulfuric acid-phosphoric acid mixture.
Add cautiously, while stirring, 150 ml of sulfuric acid (p 1,84 g/ml) and 150 ml of phosphoric acid (p 1,7 g/ml) to
600 ml of water. Cool, dilute to 1 litre and mix.
4.9 Iron standard solution.
Dissolve 0,800 g of high purity iron(lll) oxide (Fe203 > 99 %) in 40 ml of hydrochloric acid (4.1). Dilute to 1 000 ml
and mix.
1 ml of this solution contains 0,558 mg of iron.
NOTE -
If the purity of the iron(lll) oxide is unknown, the solution should be standardized using a 100 ml aliquot evaporated
to a low volume.
2
---------------------- Page: 4 ----------------------
@ IS0
IS0 5416: 1997(E)
4.10 Potassium dichromate, standard volumetric solution, c(K,Cr,O,) = 0,016 67 mol/l.
Pulverize about 6 g of potassium dichromate in an agate mortar, dry at 140 OC to 150 OC for 2 h, then cool to room
temperature in a desiccator.
Weigh 4,903 g of the dried material, dissolve in water and transfer to a 1 000 ml volumetric flask. Dilute to volume
with water and mix.
4.11 Sodium diphenylamine sulfonate, 2 g/l solution.
Dissolve 0,2 g of sodium diphenylamine sulfonate (C,H,NHC,H,SO,Na) in 100 ml of water. Store the solution in a
brown glass bottle.
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 Burette, complying with the specifications of IS0 385-l.
5.2 Conical flask, of capacity 100 ml, diameter 50 mm to 60 mm, without concave base, for dissolving the
sample. A watch glass or reflux condenser is required if working outside a fume cupboard.
5.3 Magnetic stirrer (rotational frequency 200 min- 1 to 400 min-I), magnetic stirring bar without pivot ring,
polytetrafluoroethylene (PTFE) coated; diameter 5 mm, length 40 mm.
5.4 Filtering apparatus, with glass-fibre filters or plastics microfiltersl), in either case with a pore size of less than
1 pm.
6 Sampling and samples
6.1 Laboratory sample
For analysis, use a laboratory sample of minus 160 pm particle size which has been taken and prepared in
accordance with IS0 10835.
6.2 Preparation of test samples
Thoroughly mix the laboratory sample using non-magnetic materials. Taking multiple increments with a non-magnetic
spatula, extract a test sample of not less than 25 g in such a manner that it is representative of the whole contents
of the container. Prepare an air-equilibrated test sample in accordance with IS0 2596.
7 Procedure
7.1 Number of determinations
Carry out the analysis at least in duplicate in accordance with annex A, independently, on one air-equilibrated test
sample.
1) PVC filters or PVF filters.
---------------------- Page: 5 ----------------------
@ IS0
IS0 5416: 1997(E)
The expression “independently” means that the second and any subsequent result is not affected by the previous
NOTE -
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 using a non-magnetic spatula, weigh, to the nearest 0,000 2 g, approximately 0,50 g of
the air-equilibrated test sample (6.2).
Blank test and check test
7.3
In each run, one blank test and one analysis of a certified reference material of the same type of DRI shall be
carried out in parallel with the analysis of the sample(s) under the same conditions. A 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 used are from the same reagent bottles.
When the analysis is carried out on several samples of the same type of DRI at the same time, the analytical value
of one certified reference material may be used.
7.4 Determination of hygroscopic moisture content
Determine the hygroscopic moisture content in accordance with IS0 2596, simultaneously with the taking of the test
portion (7.2) for the determination of the metallic iron content.
7.5 Determination
7.5.1 Dissolution of metallic iron
Place the test portion (7.2) in a thoroughly dry 100 ml conical flask (5.2), add 50 ml of bromine-methanol solution
(4.4), cover with a watch glass or fit a reflux condenser and stir continuously with the magnetic stirrer for 30 min
(see the following note) at a temperature of 20 OC. Filter immediately through a glass-fibre filter or plastics microfilter
(5.4) under suction and collect the filtrate in a suction filter flask. Wash the filter with methanol (4.3) (e.g. six times
with 5 ml portions) until the washings are colourless (free from bromine), then wash a further three times with water
to remove the methanol. Transfer the solution to a 600 ml beaker, washing with water.
NOTE - A dissolution time of 30 min is usually adequate. To ensure complete dissolution, two different dissolution times
should be used. If 30 min has been taken for the first test portion, the replicate test portion should be digested for twice this
time, i.e. 60 min. This procedure should be repeated, increasing the digestion time until agreement is reached between
replicate determinations.
7.5.2 Determination of metallic iron
Add 20 ml of sulfuric acid (4.2) to the total filtrate, heat the solution cautiously until fumes o
...
SLOVENSKI STANDARD
SIST ISO 5416:2000
01-junij-2000
'LUHNWQRUHGXFLUDQRåHOH]R'RORþHYDQMHNRYLQVNHJDåHOH]D7LWULPHWULMVND
PHWRGD]EURPPHWDQRORP
Direct reduced iron -- Determination of metallic iron content -- Bromine-methanol
titrimetric method
Minerais de fer préréduits -- Dosage du fer métallique -- Méthode titrimétrique au brome-
méthanol
Ta slovenski standard je istoveten z: ISO 5416:1997
ICS:
73.060.10 Železove rude Iron ores
SIST ISO 5416:2000 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST ISO 5416:2000
---------------------- Page: 2 ----------------------
SIST ISO 5416:2000
INTERNATIONAL IS0
STANDARD 5416
Second edition
1997-08-01
Direct reduced iron
- Determination of
metallic iron content - Bromine-methanol
titrimetric method
Minerais de fer prkrkduits - Dosage du fer m&allique - Mkthode
titrimhtrique au brome-mkthanol
Reference number
IS0 5416:1997(E)
---------------------- Page: 3 ----------------------
SIST ISO 5416:2000
IS0 5416:1997(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 5416 was prepared by Technical Committee
ISO/TC 102, iron ores, Subcommittee SC 2, Chemical analysis.
This second edition cancels and replaces the first edition (IS0 5416:1987),
which has been technically revised.
Annex A form an integral part of this International Standard. Annexes B to E
are for information only.
0 IS0 1997
All rights resewed. 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
---------------------- Page: 4 ----------------------
SIST ISO 5416:2000
INTERNATIONAL STANDARD 0 IS0 IS0 5416:1997(E)
- Determination of metallic iron
Direct reduced iron
- Bromine-methanol titrimetric method
content
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 titrimetric method for the determination of the metallic iron content of reduced
iron ores (direct reduced iron: DRI).
This method is applicable to metallic iron contents between 15 % (m/m) and 95 % (m/m) in DRI.
NOTE - The term “metallic iron” means those forms of iron not bonded to oxygen or not present as pyrite.
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 385-l :1984, Laboratory glassware - Burettes - Pat? 1: General requirements .
IS0 648: 1977, Laboratory glassware - One-mark pipettes.
IS0 1042: 1983, Laboratory glassware - One-mark volumetric flasks.
IS0 2596:1994, iron ores - Determination of hygroscopic moisture in analytical samples - Gravimetric and Karl
Fischer methods.
IS0 2597-l :1994, iron ores - Determination of total iron content - Part 1: Titrimetric method after tin(H) chloride
reduction.
IS0 3696: 1987, Water for analytical laboratory use - Specification and test methods.
IS0 10835:1995, Direct reduced iron - Sampling and sample preparation -
Manual methods for reduced pellets
and lump ores.
---------------------- Page: 5 ----------------------
SIST ISO 5416:2000
@ IS0
IS0 5416:1997(E)
3 Principle
Dissolution of metallic iron by treatment with bromine-methanol solution. Separation of the insoluble residue by
filtration. Reduction of the iron in the filtrate to iron followed by titration with potassium dichromate solution.
manganese, nickel and vanadium are also dissolved by the
NOTE - Other metallic elements such as chromium, cobalt,
vanadium, they do not interfere with the titration procedure
bromine-methanol solution but, except for
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 Hydrochloric acid, p 1,16 g/ml to 1 ,19 g/ml.
4.2 Sulfuric acid, p 1,84 g/ml, diluted 1 + 1.
4.3 Methanol, Karl Fischer reagent grade, max. 0,l % H,O.
4.4 Bromine-methanol solution, 50 ml/l.
Dissolve 5 ml of bromine in 95 ml of methanol (4.3). This solution shall be freshly prepared and used immediately.
WARNING - The preparation of the bromine-methanol solution and all stages of the procedure where
bromine is present shall be carried out in an efficient fume cupboard.
4.5 Hydrogen peroxide solution, 30 % (V/V).
4.6 Tin(ll) chloride solution, 100 g/l.
Dissolve 119 g of tin(ll) chloride dihydrate (SnCI,-2H20) successively in small amounts with 200 ml of hydrochloric
acid (4.1) by warming. Cool, dilute to 1 litre and mix. Add 2 g of coarsely granulated tin and store the solution in a
brown bottle.
4.7 Mercury(ll) chloride solution, 50 g/l.
Dissolve 50 g of mercury(li) chloride (HgCl*) in 800 ml of hot water. Cool, dilute to 1 litre and mix.
4.8 Sulfuric acid-phosphoric acid mixture.
Add cautiously, while stirring, 150 ml of sulfuric acid (p 1,84 g/ml) and 150 ml of phosphoric acid (p 1,7 g/ml) to
600 ml of water. Cool, dilute to 1 litre and mix.
4.9 Iron standard solution.
Dissolve 0,800 g of high purity iron(lll) oxide (Fe203 > 99 %) in 40 ml of hydrochloric acid (4.1). Dilute to 1 000 ml
and mix.
1 ml of this solution contains 0,558 mg of iron.
NOTE -
If the purity of the iron(lll) oxide is unknown, the solution should be standardized using a 100 ml aliquot evaporated
to a low volume.
2
---------------------- Page: 6 ----------------------
SIST ISO 5416:2000
@ IS0
IS0 5416: 1997(E)
4.10 Potassium dichromate, standard volumetric solution, c(K,Cr,O,) = 0,016 67 mol/l.
Pulverize about 6 g of potassium dichromate in an agate mortar, dry at 140 OC to 150 OC for 2 h, then cool to room
temperature in a desiccator.
Weigh 4,903 g of the dried material, dissolve in water and transfer to a 1 000 ml volumetric flask. Dilute to volume
with water and mix.
4.11 Sodium diphenylamine sulfonate, 2 g/l solution.
Dissolve 0,2 g of sodium diphenylamine sulfonate (C,H,NHC,H,SO,Na) in 100 ml of water. Store the solution in a
brown glass bottle.
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 Burette, complying with the specifications of IS0 385-l.
5.2 Conical flask, of capacity 100 ml, diameter 50 mm to 60 mm, without concave base, for dissolving the
sample. A watch glass or reflux condenser is required if working outside a fume cupboard.
5.3 Magnetic stirrer (rotational frequency 200 min- 1 to 400 min-I), magnetic stirring bar without pivot ring,
polytetrafluoroethylene (PTFE) coated; diameter 5 mm, length 40 mm.
5.4 Filtering apparatus, with glass-fibre filters or plastics microfiltersl), in either case with a pore size of less than
1 pm.
6 Sampling and samples
6.1 Laboratory sample
For analysis, use a laboratory sample of minus 160 pm particle size which has been taken and prepared in
accordance with IS0 10835.
6.2 Preparation of test samples
Thoroughly mix the laboratory sample using non-magnetic materials. Taking multiple increments with a non-magnetic
spatula, extract a test sample of not less than 25 g in such a manner that it is representative of the whole contents
of the container. Prepare an air-equilibrated test sample in accordance with IS0 2596.
7 Procedure
7.1 Number of determinations
Carry out the analysis at least in duplicate in accordance with annex A, independently, on one air-equilibrated test
sample.
1) PVC filters or PVF filters.
---------------------- Page: 7 ----------------------
SIST ISO 5416:2000
@ IS0
IS0 5416: 1997(E)
The expression “independently” means that the second and any subsequent result is not affected by the previous
NOTE -
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 using a non-magnetic spatula, weigh, to the nearest 0,000 2 g, approximately 0,50 g of
the air-equilibrated test sample (6.2).
Blank test and check test
7.3
In each run, one blank test and one analysis of a certified reference material of the same type of DRI shall be
carried out in parallel with the analysis of the sample(s) under the same conditions. A 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 used are from the same reagent bottles.
When the analysis is carried out on several samples of the same type of DRI at the same time, the analytical value
of one certified reference material may be used.
7.4 Determination of hygroscopic moisture content
Determine the hygroscopic moisture content in accordance with IS0 2596, simultaneously with the taking of the test
portion (7.2) for the determination of the metallic iron content.
7.5 Determination
7.5.1 Dissolution of metallic iron
Place the test portion (7.2) in a thoroughly dry 100 ml conical flask (5.2), add 50 ml of bromine-methanol solution
(4.4), cover with a watch glass or fit a reflux condenser and stir continuously with the magnetic stirrer for 30 min
(see the following note) at a temperature of 20 OC. Filter immediately through a glass-fibre filter or plastics microfilter
(5.4) under suction and collect the filtrate in a suction filter flask. Wash the filter with methanol (4.3) (e.g. six times
with 5 ml portions) until the washings are colourless (free from bromine), then wash a further three times with water
to remove the methanol. Transfer the solution to a 600 ml beaker, washing with water.
NOTE - A dissolution time of
...
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