ISO 5073:1999

Brown coals and lignites — Determination of humic acids

Charbons bruns et lignites — Dosage des acides humiques

Rjavi premogi in ligniti - Določevanje huminskih kislin

General Information

• Status: Withdrawn
• Publication Date: 15-Dec-1999
• Withdrawal Date: 15-Dec-1999
• ICS: 73.040 - Coals
• Technical Committee: ISO/TC 27/SC 5 - Methods of analysis
• Drafting Committee: ISO/TC 27/SC 5/WG 7 - Brown coals and lignites
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 06-May-2013
• Ref Project: SIST ISO 5073:2002 - Brown coals and lignites -- Determination of humic acids

Relations

• Revised: ISO 5073:2013 - Brown coals and lignites — Determination of humic acids
• Effective Date: 10-Nov-2012
• Revises: ISO 5073:1985 - Brown coals and lignites — Determination of humic acids
• Effective Date: 15-Apr-2008

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 5073
Second edition
1999-12-01
Brown coals and lignites — Determination
of humic acids
Charbons bruns et lignites — Dosage des acides humiques
A
Reference number
ISO 5073:1999(E)

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ISO 5073:1999(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 5073 was prepared by Technical Committee ISO/TC 27, Solid mineral fuels,
Subcommittee SC 5, Methods of analysis.
This second edition cancels and replaces the first edition (ISO 5073:1985), which has been technically revised. It
uses the volumetric method, which is simpler than the gravimetric method (ISO 5073:1985) for determination of
humic acids.
Annex A forms a normative part of this International Standard.
©  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

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© ISO
ISO 5073:1999(E)
Introduction
In this International Standard, humic acids are determined by the volumetric method with titration of extracts.
The test is empirical and, in order to ensure producible results, it is essential that the composition of the extraction
solution, the temperature and the time of extraction should be carefully controlled. The value 0.59, which is the
average ratio of carbon content of humic acids for many brown coals and lignites, has been proved to be applicable.
Another value may also be used, predetermined as described in annex A, and applicable to different countries or
locations.
iii

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INTERNATIONAL STANDARD  © ISO ISO 5073:1999(E)
Brown coals and lignites — Determination of humic acids
1 Scope
This International Standard specifies volumetric methods for the determination of
a) total humic acids, and
b) free humic acid,
of brown coals and lignites.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publications do not apply. However, parties to agreements based on this International Standard are encouraged to
investigate the possibility of applying the most recent editions of the normative documents indicated below. For
undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC
maintain registers of currently valid International Standards.
ISO 1015:1992, Brown coals and lignites — Determination of moisture contents — Direct volumetric method.
ISO 1171:1997, Solid mineral fuels — Determination of ash.
ISO 1213-2:1992, Solid mineral fuels — Vocabulary — Part 2: Terms relating to sampling, testing and analysis.
ISO 5068, Brown coals and lignites — Determination of moisture content — Indirect gravimetric method.
ISO 5069-2:1983, Brown coals and lignites — Principles of sampling — Part 2: Sample preparation for deter-
mination of moisture content and for general analysis.
3 Terms and definitions
For the purposes of this International Standard, the following terms and definitions and those in ISO 1213-2 apply.
3.1
humid acids
a group of complex organic, amorphous compounds of high relative molecular mass which occur as free acid and
as metal salts (humates)
3.2
total humic acids
humic acids extracted by an alkaline sodium pyrophosphate solution
3.3
free humic acid
humic acid extracted by a sodium hydroxide solution
1

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© ISO
ISO 5073:1999(E)
4 Principle
4.1 Total humic acids
Extraction of an analysis sample of coal is carried out with an alkaline sodium pyrophosphate solution. Carbon in
the humic acid extracts is oxidized with potassium dichromate followed by titration of the excess dichromate with
ammonium ferrous sulfate standard solution.
4.2 Free humic acid
Extraction of an analysis sample of coal is carried out with a sodium hydroxide solution. Carbon in the humic acid
extracts is oxidized with potassium dichromate followed by titration of the excess dichromate with ammonium
ferrous sulfate standard solution.
5 Reagents
5.1 Sodium pyrophosphate, alkaline extraction solution.
Dissolve 15 g of crystalline sodium pyrophosphate (Na P O 10H O) and 7 g of sodium hydroxide in 1 000 ml of
{
4 2 7 2
water.
5.2 Sodium hydroxide solution.
Dissolve 10 g of sodium hydroxide in 1 litre of water.
5.3 Potassium dichromate standard solution, c(1/6 K Cr O ) = 0,1 mol/l.
2 2 7
Dissolve 4,903 6 g of potassium dichromate, previously dried at 130 °C, in water. Transfer to a 1 litre volumetric
flask and dilute to the mark with water.
(1/6 K Cr O ) = 0,4 mol/l.
5.4 Potassium dichromate oxidizing solution, c
2 2 7
Dissolve 20 g of potassium dichromate in 1 litre of water.
5.5 Ammonium ferrous sulfate titration solution, c[(NH ) Fe(SO ) ] = 0,1mol/l.
4 2 4 2
Dissolve 40 g of ammonium ferrous sulfate in 1 litre of water. Add 20 ml of concentrated sulfuric acid. Store in a
dark bottle.
Standardize the ammonium ferrous sulfate titration solution against the c(1/6 K Cr O ) = 0,1 mol/l potassium
2 2 7
dichromate standard solution (5.3) for each batch of samples to be analysed.
Pipette 25 ml of potassium dichromate standard solution (5.3) into a 300 ml conical flask. Add 70 ml to 80 ml of
water. Carefully add 10 ml of concentrated sulfuric acid and 3 drops of 1,10-phenantholine indicator. After cooling,
titrate with the ammonium ferrous sulfate standard solution to a red colour.
Calculate the concentration, in moles per litre, of the ammonium ferrous sulfate solution as follows:
c = 0,1 ´ 25/V
where
c is the concentration, expressed in moles per litre, of the ammonium ferrous sulfate solution;
V is the volume of ammonium ferrous sulfate solution required for the titration.
2

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© ISO
ISO 5073:1999(E)
5.6 1,10-Phenanthroline indicator.
Dissolve 1,5 g of 1,10-phenanthroline and 1 g of ammonium ferrous sulfate in 100 ml of water. Store in a dark
bottle.
5.7 Sulfuric acid, concentrated, r = 1,84 g/ml.
20
6 Apparatus
6.1  Water bath, thermostatically controlled to (100 ± 1) °C, with four holes at least.
6.2  Balance, sensitive to 0,1 mg.
7 Sample
Prepare the sample for the determination of humic acids in accordance with clause 8 «sample preparation for
general analysis» of ISO 5069-2:1983.
For calculation to a dry basis, the moisture in the analysis sample shall be determined according to ISO 5068 or ISO
1015.
8 Procedure
8.1 Extraction of total humic acids
Weigh (0,2 ± 0,000 2) g of analysis sample into a conical flask. Add 150 ml of alkaline sodium pyrophosphate
extraction solution (5.1) and mix until the sample is th
...

SLOVENSKI STANDARD
SIST ISO 5073:2002
01-januar-2002
5MDYLSUHPRJLLQOLJQLWL'RORþHYDQMHKXPLQVNLKNLVOLQ
Brown coals and lignites -- Determination of humic acids
Charbons bruns et lignites -- Dosage des acides humiques
Ta slovenski standard je istoveten z: ISO 5073:1999
ICS:
73.040 Premogi Coals
SIST ISO 5073:2002 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST ISO 5073:2002

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SIST ISO 5073:2002
INTERNATIONAL ISO
STANDARD 5073
Second edition
1999-12-01
Brown coals and lignites — Determination
of humic acids
Charbons bruns et lignites — Dosage des acides humiques
A
Reference number
ISO 5073:1999(E)

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SIST ISO 5073:2002
ISO 5073:1999(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 5073 was prepared by Technical Committee ISO/TC 27, Solid mineral fuels,
Subcommittee SC 5, Methods of analysis.
This second edition cancels and replaces the first edition (ISO 5073:1985), which has been technically revised. It
uses the volumetric method, which is simpler than the gravimetric method (ISO 5073:1985) for determination of
humic acids.
Annex A forms a normative part of this International Standard.
©  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 5073:2002
© ISO
ISO 5073:1999(E)
Introduction
In this International Standard, humic acids are determined by the volumetric method with titration of extracts.
The test is empirical and, in order to ensure producible results, it is essential that the composition of the extraction
solution, the temperature and the time of extraction should be carefully controlled. The value 0.59, which is the
average ratio of carbon content of humic acids for many brown coals and lignites, has been proved to be applicable.
Another value may also be used, predetermined as described in annex A, and applicable to different countries or
locations.
iii

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SIST ISO 5073:2002

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

SIST ISO 5073:2002
INTERNATIONAL STANDARD  © ISO ISO 5073:1999(E)
Brown coals and lignites — Determination of humic acids
1 Scope
This International Standard specifies volumetric methods for the determination of
a) total humic acids, and
b) free humic acid,
of brown coals and lignites.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publications do not apply. However, parties to agreements based on this International Standard are encouraged to
investigate the possibility of applying the most recent editions of the normative documents indicated below. For
undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC
maintain registers of currently valid International Standards.
ISO 1015:1992, Brown coals and lignites — Determination of moisture contents — Direct volumetric method.
ISO 1171:1997, Solid mineral fuels — Determination of ash.
ISO 1213-2:1992, Solid mineral fuels — Vocabulary — Part 2: Terms relating to sampling, testing and analysis.
ISO 5068, Brown coals and lignites — Determination of moisture content — Indirect gravimetric method.
ISO 5069-2:1983, Brown coals and lignites — Principles of sampling — Part 2: Sample preparation for deter-
mination of moisture content and for general analysis.
3 Terms and definitions
For the purposes of this International Standard, the following terms and definitions and those in ISO 1213-2 apply.
3.1
humid acids
a group of complex organic, amorphous compounds of high relative molecular mass which occur as free acid and
as metal salts (humates)
3.2
total humic acids
humic acids extracted by an alkaline sodium pyrophosphate solution
3.3
free humic acid
humic acid extracted by a sodium hydroxide solution
1

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SIST ISO 5073:2002
© ISO
ISO 5073:1999(E)
4 Principle
4.1 Total humic acids
Extraction of an analysis sample of coal is carried out with an alkaline sodium pyrophosphate solution. Carbon in
the humic acid extracts is oxidized with potassium dichromate followed by titration of the excess dichromate with
ammonium ferrous sulfate standard solution.
4.2 Free humic acid
Extraction of an analysis sample of coal is carried out with a sodium hydroxide solution. Carbon in the humic acid
extracts is oxidized with potassium dichromate followed by titration of the excess dichromate with ammonium
ferrous sulfate standard solution.
5 Reagents
5.1 Sodium pyrophosphate, alkaline extraction solution.
Dissolve 15 g of crystalline sodium pyrophosphate (Na P O 10H O) and 7 g of sodium hydroxide in 1 000 ml of
{
4 2 7 2
water.
5.2 Sodium hydroxide solution.
Dissolve 10 g of sodium hydroxide in 1 litre of water.
5.3 Potassium dichromate standard solution, c(1/6 K Cr O ) = 0,1 mol/l.
2 2 7
Dissolve 4,903 6 g of potassium dichromate, previously dried at 130 °C, in water. Transfer to a 1 litre volumetric
flask and dilute to the mark with water.
(1/6 K Cr O ) = 0,4 mol/l.
5.4 Potassium dichromate oxidizing solution, c
2 2 7
Dissolve 20 g of potassium dichromate in 1 litre of water.
5.5 Ammonium ferrous sulfate titration solution, c[(NH ) Fe(SO ) ] = 0,1mol/l.
4 2 4 2
Dissolve 40 g of ammonium ferrous sulfate in 1 litre of water. Add 20 ml of concentrated sulfuric acid. Store in a
dark bottle.
Standardize the ammonium ferrous sulfate titration solution against the c(1/6 K Cr O ) = 0,1 mol/l potassium
2 2 7
dichromate standard solution (5.3) for each batch of samples to be analysed.
Pipette 25 ml of potassium dichromate standard solution (5.3) into a 300 ml conical flask. Add 70 ml to 80 ml of
water. Carefully add 10 ml of concentrated sulfuric acid and 3 drops of 1,10-phenantholine indicator. After cooling,
titrate with the ammonium ferrous sulfate standard solution to a red colour.
Calculate the concentration, in moles per litre, of the ammonium ferrous sulfate solution as follows:
c = 0,1 ´ 25/V
where
c is the concentration, expressed in moles per litre, of the ammonium ferrous sulfate solution;
V is the volume of ammonium ferrous sulfate solution required for the titration.
2

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SIST ISO 5073:2002
© ISO
ISO 5073:1999(E)
5.6 1,10-Phenanthroline indicator.
Dissolve 1,5 g of 1,10-phenanthroline and 1 g of ammonium ferrous sulfate in 100 ml of water. Store in a dark
bottle.
5.7 Sulfuric acid, concentrated, r = 1,84 g/ml.
20
6 Apparatus
6.1  Water bath, thermostatically controlled to (100 ± 1) °C, with four holes at least.
6.2  Balance, sensitive to 0,1 mg.
7 Sample
Prepare the sample for the determination of humic acids in accordance with clause 8 «sample preparation for
general analysis» of ISO 5069-2:1983.
For c
...