ISO/TS 13907:2012
(Main)Soil quality — Determination of nonylphenols (NP) and nonylphenol-mono- and diethoxylates — Method by gas chromatography with mass selective detection (GC-MS)
Soil quality — Determination of nonylphenols (NP) and nonylphenol-mono- and diethoxylates — Method by gas chromatography with mass selective detection (GC-MS)
ISO/TS 13907:2012 specifies a method for the determination of nonylphenols (NP), nonylphenol-monoethoxylates (NP1EO) and nonylphenol-diethoxylates (NP2EO) in sludge, treated biowaste and soil using GC-MS. For sludge, a limit of detection of 0,1 mg/kg and for soil and treated biowaste of 0,02 mg/kg (expressed as dry matter) may be achieved.
Qualité du sol — Détermination des nonyphénols (NP) et des nonylphénols monoéthoxylés et diéthoxylés — Méthode par chromatographie en phase gazeuse avec détection sélective de masse (CG-SM)
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TECHNICAL ISO/TS
SPECIFICATION 13907
First edition
2012-09-01
Soil quality — Determination of
nonylphenols (NP) and nonylphenol-
mono- and diethoxylates — Method
by gas chromatography with mass
selective detection (GC-MS)
Qualité du sol — Détermination des nonyphénols (NP) et des mono- et
di-éthoxylates de nonylphénol — Méthode par chromatographie en
phase gazeuse avec détection sélective de masse (CPG-SM)
Reference number
©
ISO 2012
© ISO 2012
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 either ISO at the
address below or ISO’s member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Interferences . 2
4.1 Interferences from sampling. 2
4.2 Interferences by GC-MS . 2
5 Reagents . 2
6 Apparatus . 4
7 Sample storage and sample pretreatment . 5
7.1 Sample storage . 5
7.2 Sample pretreatment . 5
8 Procedure. 5
8.1 Extraction . 5
8.2 Concentration (optional). 7
8.3 Clean-up (optional) . 7
8.4 Derivatization . 8
8.5 Blank test . 8
8.6 GC-MS analysis . 8
8.7 Calibration . 9
8.8 Analysis of samples and identification .10
9 Calculation and expression of results .10
9.1 General .10
9.2 Calibration .10
9.3 Calculation .11
10 Precision .11
11 Test report .11
Annex A (informative) Repeatability and reproducibility data .13
Annex B (informative) Example of chromatographic conditions and example of a chromatogram 15
Bibliography .17
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 2.
The main task of technical committees is to prepare International Standards. 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.
In other circumstances, particularly when there is an urgent market requirement for such documents, a
technical committee may decide to publish other types of document:
— an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical
experts in an ISO working group and is accepted for publication if it is approved by more than 50 %
of the members of the parent committee casting a vote;
— an ISO Technical Specification (ISO/TS) represents an agreement between the members of a
technical committee and is accepted for publication if it is approved by 2/3 of the members of the
committee casting a vote.
An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be confirmed for
a further three years, revised to become an International Standard, or withdrawn. If the ISO/PAS or
ISO/TS is confirmed, it is reviewed again after a further three years, at which time it must either be
transformed into an International Standard or be withdrawn.
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.
ISO/TS 13907 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3,
Chemical methods and soil characteristics.
iv © ISO 2012 – All rights reserved
Introduction
Nonylphenols (NP) are mainly found in the environment as degradation products of nonylphenol
polyethoxylates (NPEO). NPEO have many applications as non-ionic detergents in washing and
cleaning agents.
After use, NPEO are degraded by de-ethoxylation, resulting in polyethoxylates with fewer ethoxy-
groups. Nonylphenol-diethoxylates (NP2EO), nonylphenol-monoethoxylates (NP1EO) and nonylphenols
(NP) are the last three products in the degradation chain. Due to their significant presence in sewage
sludge, all three components are included in this Technical Specification.
This Technical Specification is applicable for several types of matrices and validated for municipal
sewage sludge (see also Annex A for the results of the validation).
TECHNICAL SPECIFICATION ISO/TS 13907:2012(E)
Soil quality — Determination of nonylphenols (NP) and
nonylphenol-mono- and diethoxylates — Method by gas
chromatography with mass selective detection (GC-MS)
WARNING — Persons using this Technical Specification should be familiar with usual laboratory
practice. This Technical Specification does not purport to address all of the safety problems, if
any, associated with its use. It is the responsibility of the user to establish appropriate safety and
health practices and to ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this Technical
Specification be carried out by suitably trained staff.
1 Scope
This Technical Specification specifies a method for the determination of nonylphenols (NP), nonylphenol-
monoethoxylates (NP1EO) and nonylphenol-diethoxylates (NP2EO) in sludge, treated biowaste and
soil using GC-MS.
For sludge, a limit of detection of 0,1 mg/kg and for soil and treated biowaste of 0,02 mg/kg (expressed
as dry matter) may be achieved.
Lower limits of detection may be achieved by concentrating the extract by solvent evaporation.
NOTE 4-tert-octylphenol can also be analysed with this method.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of performance
characteristics — Part 1: Statistical evaluation of the linear calibration function
ISO 11465, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric method
ISO 14507, Soil quality — Pretreatment of samples for determination of organic contaminants
ISO 16720, Soil quality — Pretreatment of samples by freeze-drying for subsequent analysis
ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography and
mass spectrometry
3 Principle
After pretreatment, the test sample is extracted by shaking with a mixture of acetone and petroleum ether
(1:1). If necessary, interfering compounds are removed from the extract by a clean-up on a suitable column.
The extract is treated with N-methyl-N-(trimethylsilyl)-trifluoracetamide (MSTFA) reagent for the
derivatization (silylation) of the analytes, and subsequently analysed by gas chromatography and mass
selective detection (GC-MS).
Nonylphenols and nonylphenol-mono- and diethoxylates are identified from the GC fingerprint, the
relative retention times and the relative intensities of two diagnostic ions. The quantification is based
13 13
on an internal standard procedure. The internal standards ( C-labelled 4-n-NP and C-labelled
4-n-NP2EO) are taken through the whole analytical procedure.
4 Interferences
4.1 Interferences from sampling
Use sampling containers of materials (preferably glass or steel) that do not significantly affect the
sample during the contact through sampling and storage. Plastic containers may be used if it has been
proven that they do not significantly affect the sample.
4.2 Interferences by GC-MS
Substances that co-elute with NP, NP1EO or NP2EO and give the same ion(s) may interfere with the
determination. This may have a large influence on the result, since all three analytes are determined
from the sum of a cluster of five to nine chromatographic peaks. It is essential that the interfering
peaks are not included in the calculations. A peak is excluded if the retention times are not the same
as expected from the calibration standard an
...
TECHNICAL ISO/TS
SPECIFICATION 13907
First edition
2012-09-01
Soil quality — Determination of
nonylphenols (NP) and nonylphenol-
mono- and diethoxylates — Method
by gas chromatography with mass
selective detection (GC-MS)
Qualité du sol — Détermination des nonyphénols (NP) et des mono- et
di-éthoxylates de nonylphénol — Méthode par chromatographie en
phase gazeuse avec détection sélective de masse (CPG-SM)
Reference number
©
ISO 2012
© ISO 2012
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 either ISO at the
address below or ISO’s member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Interferences . 2
4.1 Interferences from sampling. 2
4.2 Interferences by GC-MS . 2
5 Reagents . 2
6 Apparatus . 4
7 Sample storage and sample pretreatment . 5
7.1 Sample storage . 5
7.2 Sample pretreatment . 5
8 Procedure. 5
8.1 Extraction . 5
8.2 Concentration (optional). 7
8.3 Clean-up (optional) . 7
8.4 Derivatization . 8
8.5 Blank test . 8
8.6 GC-MS analysis . 8
8.7 Calibration . 9
8.8 Analysis of samples and identification .10
9 Calculation and expression of results .10
9.1 General .10
9.2 Calibration .10
9.3 Calculation .11
10 Precision .11
11 Test report .11
Annex A (informative) Repeatability and reproducibility data .13
Annex B (informative) Example of chromatographic conditions and example of a chromatogram 15
Bibliography .17
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 2.
The main task of technical committees is to prepare International Standards. 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.
In other circumstances, particularly when there is an urgent market requirement for such documents, a
technical committee may decide to publish other types of document:
— an ISO Publicly Available Specification (ISO/PAS) represents an agreement between technical
experts in an ISO working group and is accepted for publication if it is approved by more than 50 %
of the members of the parent committee casting a vote;
— an ISO Technical Specification (ISO/TS) represents an agreement between the members of a
technical committee and is accepted for publication if it is approved by 2/3 of the members of the
committee casting a vote.
An ISO/PAS or ISO/TS is reviewed after three years in order to decide whether it will be confirmed for
a further three years, revised to become an International Standard, or withdrawn. If the ISO/PAS or
ISO/TS is confirmed, it is reviewed again after a further three years, at which time it must either be
transformed into an International Standard or be withdrawn.
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.
ISO/TS 13907 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3,
Chemical methods and soil characteristics.
iv © ISO 2012 – All rights reserved
Introduction
Nonylphenols (NP) are mainly found in the environment as degradation products of nonylphenol
polyethoxylates (NPEO). NPEO have many applications as non-ionic detergents in washing and
cleaning agents.
After use, NPEO are degraded by de-ethoxylation, resulting in polyethoxylates with fewer ethoxy-
groups. Nonylphenol-diethoxylates (NP2EO), nonylphenol-monoethoxylates (NP1EO) and nonylphenols
(NP) are the last three products in the degradation chain. Due to their significant presence in sewage
sludge, all three components are included in this Technical Specification.
This Technical Specification is applicable for several types of matrices and validated for municipal
sewage sludge (see also Annex A for the results of the validation).
TECHNICAL SPECIFICATION ISO/TS 13907:2012(E)
Soil quality — Determination of nonylphenols (NP) and
nonylphenol-mono- and diethoxylates — Method by gas
chromatography with mass selective detection (GC-MS)
WARNING — Persons using this Technical Specification should be familiar with usual laboratory
practice. This Technical Specification does not purport to address all of the safety problems, if
any, associated with its use. It is the responsibility of the user to establish appropriate safety and
health practices and to ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this Technical
Specification be carried out by suitably trained staff.
1 Scope
This Technical Specification specifies a method for the determination of nonylphenols (NP), nonylphenol-
monoethoxylates (NP1EO) and nonylphenol-diethoxylates (NP2EO) in sludge, treated biowaste and
soil using GC-MS.
For sludge, a limit of detection of 0,1 mg/kg and for soil and treated biowaste of 0,02 mg/kg (expressed
as dry matter) may be achieved.
Lower limits of detection may be achieved by concentrating the extract by solvent evaporation.
NOTE 4-tert-octylphenol can also be analysed with this method.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of performance
characteristics — Part 1: Statistical evaluation of the linear calibration function
ISO 11465, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric method
ISO 14507, Soil quality — Pretreatment of samples for determination of organic contaminants
ISO 16720, Soil quality — Pretreatment of samples by freeze-drying for subsequent analysis
ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography and
mass spectrometry
3 Principle
After pretreatment, the test sample is extracted by shaking with a mixture of acetone and petroleum ether
(1:1). If necessary, interfering compounds are removed from the extract by a clean-up on a suitable column.
The extract is treated with N-methyl-N-(trimethylsilyl)-trifluoracetamide (MSTFA) reagent for the
derivatization (silylation) of the analytes, and subsequently analysed by gas chromatography and mass
selective detection (GC-MS).
Nonylphenols and nonylphenol-mono- and diethoxylates are identified from the GC fingerprint, the
relative retention times and the relative intensities of two diagnostic ions. The quantification is based
13 13
on an internal standard procedure. The internal standards ( C-labelled 4-n-NP and C-labelled
4-n-NP2EO) are taken through the whole analytical procedure.
4 Interferences
4.1 Interferences from sampling
Use sampling containers of materials (preferably glass or steel) that do not significantly affect the
sample during the contact through sampling and storage. Plastic containers may be used if it has been
proven that they do not significantly affect the sample.
4.2 Interferences by GC-MS
Substances that co-elute with NP, NP1EO or NP2EO and give the same ion(s) may interfere with the
determination. This may have a large influence on the result, since all three analytes are determined
from the sum of a cluster of five to nine chromatographic peaks. It is essential that the interfering
peaks are not included in the calculations. A peak is excluded if the retention times are not the same
as expected from the calibration standard an
...
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