ISO 13913:2014

INTERNATIONAL ISO
STANDARD 13913
First edition
2014-02-01
Soil quality — Determination of
selected phthalates using capillary
gas chromatography with mass
spectrometric detection (GC/MS)
Qualité du sol — Détermination de phthalates sélectionnés en
utilisant la chromatographie gazeuse capillaire avec détection par
spectrométrie de masse
Reference number
©
ISO 2014
© ISO 2014
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ii © ISO 2014 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Principle . 2
4 Interferences . 2
4.1 General . 2
4.2 Interferences during sampling . 2
4.3 Cross contamination . 2
4.4 Interferences in gas chromatography . 2
5 Reagents . 2
5.1 General . 2
6 Apparatus . 4
6.1 General . 4
7 Sampling and sample storage . 6
8 Procedure. 6
8.1 Preparation of glass apparatus . 6
8.2 Drying of the sample . 6
8.3 Extraction . 7
8.4 Clean-up . 7
8.5 Gas chromatography . 8
8.6 Blank monitoring . 8
8.7 Identification of individual compounds . 8
9 Calibration . 9
9.1 General . 9
9.2 Calibration with internal standard . 9
9.3 Verification of calibration .10
10 Calculation .11
11 Expression of results .12
12 Precision .12
13 Test report .12
Annex A (informative) Repeatability and reproducibility data .13
Annex B (informative) Example of a reference solution for multipoint calibration .16
Annex C (informative) Examples for gas chromatographic conditions .18
Annex D (informative) Flow scheme of the determination of phthalates .20
Bibliography .21
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
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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
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to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
methods and soil characteristics.
iv © ISO 2014 – All rights reserved

Introduction
This International Standard is applicable and validated for several types of matrices as indicated in
Table 1 (see also Annex A for the results of the validation).
Table 1 — Matrices for which this International Standard is applicable and validated
Matrix Materials used for validation
Sludge Municipal sludge
Biowaste Fresh compost
Soil Sludge amended soil
INTERNATIONAL STANDARD ISO 13913:2014(E)
Soil quality — Determination of selected phthalates using
capillary gas chromatography with mass spectrometric
detection (GC/MS)
WARNING — Persons using this International Standard should be familiar with usual laboratory
practice. This International Standard 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 International
Standard be carried out by suitably trained staff.
1 Scope
This International Standard specifies a method for the determination of selected phthalates in sludge,
treated biowaste, and soil, after extraction and gas chromatographic analysis with mass spectrometric
detection.
The method is applicable for the determination of phthalates (see Table 2) at the lowest mass content of
0,1 mg/kg to 0,5 mg/kg (expressed as dry matter), depending on the individual substance.
The applicability of the method to other phthalates not specified in Table 2 is not excluded except the
isomeric mixtures, e.g. DiNP (Di-isononylphthalate), but shall be verified in each case.
Table 2 — Phthalates that can be determined according to this International Standard
Molar mass
a
No Name Formula Abbreviation CAS-RN
g/mol
1 Dimethylphthalate C H O DMP 194,2 00131-11-3
10 10 4
2 Diethylphthalate C H O DEP 222,2 00084-66-2
12 14 4
3 Dipropylphthalate C H O DPP 250,3 00131-16-8
14 18 4
4 Di-(2-methyl-propyl)phthalate C H O DiBP 278,4 00084-69-5
16 22 4
5 Dibutylphthalate C H O DBP 278,4 00084-74-2
16 22 4
6 Butylbenzylphthalate C H O BBzP 312,4 00085-68-7
19 20 4
7 Dicyclohexylphthalate C H O DCHP 330,4 00084-61-7
20 26 4
8 Di-(2-ethylhexyl)phthalate C H O DEHP 390,6 00117-81-7
24 38 4
9 Dioctylphthalate C H O DOP 390,6 00117-84-0
24 38 4
10 Didecylphthalate C H O DDcP 446,7 00084-77-5
28 46 4
11 Diundecylphthalate C H O DUP 474,4 03648-20-2
30 50 4
a
Chemical Abstracts Service Registry Number.
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 5667-13, Water quality — Sampling — Part 13: Guidance on sampling of sludges
ISO 5667-15, Water quality — Sampling — Part 15: Guidance on the preservation and handling of sludge
and sediment samples
ISO 10381-2, Soil quality — Sampling — Part 2: Guidance on sampling techniques
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 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography and
mass spectrometry
3 Principle
The dried sample, dried by freeze drying or with sodium sulfate, is extracted with ethyl acetate on the
shaking device. An aliquot of the extract is cleaned with aluminium oxide (if necessary) followed by
gas chromatographic separation using capillary columns and identification and quantification of the
phthalates by mass spectrometry.
4 Interferences
4.1 General
Due to their use as plasticizer agents, phthalates are ubiquitous. The sources of phthalates are multiple
and shall be checked and reduced by every laboratory, itself. Therefore, special attention shall be paid
to avoid contamina
...