ISO 22241-2:2019
(Main)Diesel engines — NOx reduction agent AUS 32 — Part 2: Test methods
Diesel engines — NOx reduction agent AUS 32 — Part 2: Test methods
This document specifies test methods required for determination of the quality and chemical characteristics of NOx reduction agent AUS 32 (aqueous urea solution) as specified in ISO 22241-1.
Moteurs diesel — Agent AUS 32 de réduction des NOx — Partie 2: Méthodes d'essai
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INTERNATIONAL ISO
STANDARD 22241-2
Second edition
2019-02
Diesel engines — NOx reduction agent
AUS 32 —
Part 2:
Test methods
Moteurs diesel — Agent AUS 32 de réduction des NOx —
Partie 2: Méthodes d'essai
Reference number
©
ISO 2019
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Specifications . 1
5 Sampling . 2
6 Precision and dispute . 2
Annex A (normative) Sampling . 3
Annex B (normative) Determination of urea content by total nitrogen . 5
Annex C (normative) Refractive index and determination of urea content by refractive index .9
Annex D (normative) Determination of alkalinity .12
Annex E (normative) Determination of biuret content .15
Annex F (normative) Determination of aldehyde content .20
Annex G (normative) Determination of insoluble matter content by gravimetric method .24
Annex H (normative) Determination of phosphate content by photometric method .27
Annex I (normative) Determination of trace element content (Al, Ca, Cr, Cu, Fe, K, Mg, Na, Ni,
P and Zn) by ICP-OES method .33
Annex J (informative) Determination of identity by FTIR spectrometry method .41
Annex K (informative) Precision of test method .43
Bibliography .44
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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso
.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 22, Road vehicles, Subcommittee SC 34,
Propulsion, powertrain and powertrain fluids.
This second edition cancels and replaces the first edition (ISO 22241-2:2006), which has been
technically revised. It also incorporates the Technical Corrigendum ISO 22241-2:2006/Cor. 1:2008. The
main changes compared to the previous edition are as follows:
— Major revisions to test methods of Annex C and Annex I,
— Precision values for all test methods were revised,
— Annex K was updated.
A list of all parts in the ISO 22241 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2019 – All rights reserved
INTERNATIONAL STANDARD ISO 22241-2:2019(E)
Diesel engines — NOx reduction agent AUS 32 —
Part 2:
Test methods
WARNING — The use of this document can involve hazardous materials, operations and
equipment. This document does not purport to address all the safety issues associated with its
use. It is the responsibility of users of this document to respond appropriately to ensure the
safety and health of personnel prior to application of the document.
1 Scope
This document specifies test methods required for determination of the quality and chemical
characteristics of NOx reduction agent AUS 32 (aqueous urea solution) as specified in ISO 22241-1.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 4259 (all parts), Petroleum and related products — Precision of measurement methods and results
ISO 12185, Crude petroleum and petroleum products — Determination of density — Oscillating U-tube
method
ISO 17034, General requirements for the competence of reference material producers
ISO 22241-1, Diesel engines — NOx reduction agent AUS 32 — Part 1: Quality requirements
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 22241-1 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
3.1
certified reference material
CRM
substance or material used to check the quality and metrological traceability of products, to validate
analytical measurement methods or for the calibration of instruments
4 Specifications
Conformance with the limits specified in ISO 22241-1 shall be determined by the test methods specified
in Annexes B through I of this document. If necessary, the identity of the product can be determined as
specified in Annex J.
5 Sampling
Samples shall be taken in accordance with Annex A.
6 Precision and dispute
Each of the test methods specified in Annex B through Annex I include a precision statement using
guidance from ISO 4259 (all parts). In cases of dispute, the procedures described in ISO 4259 (all parts)
shall be used for resolving the dispute, and interpretation of the results based on the test method
precision shall be used.
For the convenience of the user, the respective precision data are summarized in Table K.1.
2 © ISO 2019 – All rights reserved
Annex A
(normative)
Sampling
A.1 General
The sampling method specified in this annex is valid for each sampling of AUS 32 throughout the supply
chain after the shipment from the manufacturer’s site to the AUS 32 containers of the vehicles.
A.2 Principle
The limits for the quality characteristics of AUS 32, which are specified in ISO 22241-1, are the
representative analytical results that can only be obtained when the sample is protected from any
contamination before the analysis.
Therefore, suitable bottles shall be used for sampling, which do not contaminate the sample, especially
regarding the trace elements.
NOTE The sampling method specified in this annex is based on ISO 5667-3.
A.3 Possible contaminants
During the sampling process, foreign matter can lead to contamination of the sample. Under realistic
conditions, the following sources of contamination will pose a major hazard:
— residues of process aids used for the production of the sampling bottles;
— contaminants which have been deposited in the empty bottles during the time they are stored empty;
— contaminants from the air, i.e. dust or any foreign matter from the surrounding, during the sampling;
— residues of cleaning agents, which have been used for cleaning the sampling equipment and the
bottles as well;
— fuel.
A.4 Apparatus
A.4.1 Sampling bottles.
1 000-ml wide neck bottles shall be used. Suited materials for these bottles are high density polyethylene
(HDPE), high density polypropylene (HDPP), polyvinylidene fluoride (PVDF) and perfluoroalkoxy
alkane (PFA).
Prior to the first use with AUS 32, the bottles shall be cleaned and finally rinsed with deionized water
followed by AUS 32.
A.4.2 Labels.
Each bottle shall be labelled using labels of approximately 10 cm by 5 cm. The labels and the writing on
these labels shall be resistant to water and to AUS 32.
A.5 Sampling
The locked wide-neck bottle shall be opened and the cap shall be placed on a clean surface with the
opening turned downward. After flushing the sampling pipe, the bottle shall be filled completely with
AUS 32 from the container. The first filling shall be discarded, and the bottle shall immediately be re-
filled with AUS 32 and closed tightly. The label shall be attached to the bottle (see A.4.2). During the filling
of the sample, maximum care shall be taken that neither dust nor liquid pollutants get into the bottle.
The filled bottle should reach the laboratory as soon as possible. During transportation and storage, the
sample should be kept at the lowest possible temperature, preferably between 0 °C and 15 °C.
It is recommended to conduct the analysis within three weeks in order to take into account possible
changes in the ammonia content.
A.6 Sample quantity
The minimum quantity of sample material depends on the type of analysis conducted. Whenever
possible, make sure that a sufficient volume of sample material is available (recommendation: 1 litre),
and at least double that which is required for complete verification of AUS 32 specifications. In case of
dispute, a sufficient number of samples shall be taken according to ISO 4259 (all parts).
A.7 Labelling
The label should contain the following information:
— product name;
1)
— name of the company which owns the sample product ;
1)
— address where the sample was taken from ;
1)
— manufacturer of the sample product ;
— batch or lot number;
1)
— container from which the sample was taken ;
1)
— part of the container where the sample was taken from (sampling point) ;
1)
— date and time of sampling ;
1)
— sample shipment date ;
1)
— name and signature of the person who took the sample .
1) Mandatory only in cases of dispute.
4 © ISO 2019 – All rights reserved
Annex B
(normative)
Determination of urea content by total nitrogen
B.1 General
This annex specifies the procedure for determining the urea content of AUS 32.
The method is applicable for the determination of the urea content in the range of 30 to 35 % (mass
fraction).
B.2 Principle
The sample is combusted at high temperatures in a stream of oxygen. Following the reduction of formed
nitrogen oxides to elemental nitrogen and removal of any interferin
...
INTERNATIONAL ISO
STANDARD 22241-2
Second edition
2019-02
Diesel engines — NOx reduction agent
AUS 32 —
Part 2:
Test methods
Moteurs diesel — Agent AUS 32 de réduction des NOx —
Partie 2: Méthodes d'essai
Reference number
©
ISO 2019
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Specifications . 1
5 Sampling . 2
6 Precision and dispute . 2
Annex A (normative) Sampling . 3
Annex B (normative) Determination of urea content by total nitrogen . 5
Annex C (normative) Refractive index and determination of urea content by refractive index .9
Annex D (normative) Determination of alkalinity .12
Annex E (normative) Determination of biuret content .15
Annex F (normative) Determination of aldehyde content .20
Annex G (normative) Determination of insoluble matter content by gravimetric method .24
Annex H (normative) Determination of phosphate content by photometric method .27
Annex I (normative) Determination of trace element content (Al, Ca, Cr, Cu, Fe, K, Mg, Na, Ni,
P and Zn) by ICP-OES method .33
Annex J (informative) Determination of identity by FTIR spectrometry method .41
Annex K (informative) Precision of test method .43
Bibliography .44
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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso
.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 22, Road vehicles, Subcommittee SC 34,
Propulsion, powertrain and powertrain fluids.
This second edition cancels and replaces the first edition (ISO 22241-2:2006), which has been
technically revised. It also incorporates the Technical Corrigendum ISO 22241-2:2006/Cor. 1:2008. The
main changes compared to the previous edition are as follows:
— Major revisions to test methods of Annex C and Annex I,
— Precision values for all test methods were revised,
— Annex K was updated.
A list of all parts in the ISO 22241 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2019 – All rights reserved
INTERNATIONAL STANDARD ISO 22241-2:2019(E)
Diesel engines — NOx reduction agent AUS 32 —
Part 2:
Test methods
WARNING — The use of this document can involve hazardous materials, operations and
equipment. This document does not purport to address all the safety issues associated with its
use. It is the responsibility of users of this document to respond appropriately to ensure the
safety and health of personnel prior to application of the document.
1 Scope
This document specifies test methods required for determination of the quality and chemical
characteristics of NOx reduction agent AUS 32 (aqueous urea solution) as specified in ISO 22241-1.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 4259 (all parts), Petroleum and related products — Precision of measurement methods and results
ISO 12185, Crude petroleum and petroleum products — Determination of density — Oscillating U-tube
method
ISO 17034, General requirements for the competence of reference material producers
ISO 22241-1, Diesel engines — NOx reduction agent AUS 32 — Part 1: Quality requirements
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 22241-1 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
3.1
certified reference material
CRM
substance or material used to check the quality and metrological traceability of products, to validate
analytical measurement methods or for the calibration of instruments
4 Specifications
Conformance with the limits specified in ISO 22241-1 shall be determined by the test methods specified
in Annexes B through I of this document. If necessary, the identity of the product can be determined as
specified in Annex J.
5 Sampling
Samples shall be taken in accordance with Annex A.
6 Precision and dispute
Each of the test methods specified in Annex B through Annex I include a precision statement using
guidance from ISO 4259 (all parts). In cases of dispute, the procedures described in ISO 4259 (all parts)
shall be used for resolving the dispute, and interpretation of the results based on the test method
precision shall be used.
For the convenience of the user, the respective precision data are summarized in Table K.1.
2 © ISO 2019 – All rights reserved
Annex A
(normative)
Sampling
A.1 General
The sampling method specified in this annex is valid for each sampling of AUS 32 throughout the supply
chain after the shipment from the manufacturer’s site to the AUS 32 containers of the vehicles.
A.2 Principle
The limits for the quality characteristics of AUS 32, which are specified in ISO 22241-1, are the
representative analytical results that can only be obtained when the sample is protected from any
contamination before the analysis.
Therefore, suitable bottles shall be used for sampling, which do not contaminate the sample, especially
regarding the trace elements.
NOTE The sampling method specified in this annex is based on ISO 5667-3.
A.3 Possible contaminants
During the sampling process, foreign matter can lead to contamination of the sample. Under realistic
conditions, the following sources of contamination will pose a major hazard:
— residues of process aids used for the production of the sampling bottles;
— contaminants which have been deposited in the empty bottles during the time they are stored empty;
— contaminants from the air, i.e. dust or any foreign matter from the surrounding, during the sampling;
— residues of cleaning agents, which have been used for cleaning the sampling equipment and the
bottles as well;
— fuel.
A.4 Apparatus
A.4.1 Sampling bottles.
1 000-ml wide neck bottles shall be used. Suited materials for these bottles are high density polyethylene
(HDPE), high density polypropylene (HDPP), polyvinylidene fluoride (PVDF) and perfluoroalkoxy
alkane (PFA).
Prior to the first use with AUS 32, the bottles shall be cleaned and finally rinsed with deionized water
followed by AUS 32.
A.4.2 Labels.
Each bottle shall be labelled using labels of approximately 10 cm by 5 cm. The labels and the writing on
these labels shall be resistant to water and to AUS 32.
A.5 Sampling
The locked wide-neck bottle shall be opened and the cap shall be placed on a clean surface with the
opening turned downward. After flushing the sampling pipe, the bottle shall be filled completely with
AUS 32 from the container. The first filling shall be discarded, and the bottle shall immediately be re-
filled with AUS 32 and closed tightly. The label shall be attached to the bottle (see A.4.2). During the filling
of the sample, maximum care shall be taken that neither dust nor liquid pollutants get into the bottle.
The filled bottle should reach the laboratory as soon as possible. During transportation and storage, the
sample should be kept at the lowest possible temperature, preferably between 0 °C and 15 °C.
It is recommended to conduct the analysis within three weeks in order to take into account possible
changes in the ammonia content.
A.6 Sample quantity
The minimum quantity of sample material depends on the type of analysis conducted. Whenever
possible, make sure that a sufficient volume of sample material is available (recommendation: 1 litre),
and at least double that which is required for complete verification of AUS 32 specifications. In case of
dispute, a sufficient number of samples shall be taken according to ISO 4259 (all parts).
A.7 Labelling
The label should contain the following information:
— product name;
1)
— name of the company which owns the sample product ;
1)
— address where the sample was taken from ;
1)
— manufacturer of the sample product ;
— batch or lot number;
1)
— container from which the sample was taken ;
1)
— part of the container where the sample was taken from (sampling point) ;
1)
— date and time of sampling ;
1)
— sample shipment date ;
1)
— name and signature of the person who took the sample .
1) Mandatory only in cases of dispute.
4 © ISO 2019 – All rights reserved
Annex B
(normative)
Determination of urea content by total nitrogen
B.1 General
This annex specifies the procedure for determining the urea content of AUS 32.
The method is applicable for the determination of the urea content in the range of 30 to 35 % (mass
fraction).
B.2 Principle
The sample is combusted at high temperatures in a stream of oxygen. Following the reduction of formed
nitrogen oxides to elemental nitrogen and removal of any interferin
...
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