SIST EN ISO 11916-3:2022
(Main)Soil quality - Determination of selected explosives and related compounds - Part 3: Method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) (ISO 11916-3:2021)
Soil quality - Determination of selected explosives and related compounds - Part 3: Method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) (ISO 11916-3:2021)
This International Standard specifies the measurement of explosive and related nitrocompounds
compounds using liquid chromatography–tandem mass spectrometry (LC-MS/MS) in soil and soilmaterials. This method is applicable to 12 compounds (1,3-DNB, 1,3,5-TNB, 2,4-DNT, 2,6-DNT, 2,4,6-TNT, 4-A-2,6-DNT, 2-A-4,6-DNT, Tetryl, Hexyl, RDX, HMX, PETN) listed in ISO 11916-1(soil, HPLC/UV method) except nitrobenzene, 2-nitortoluene, 3-nitrotoluene and 4-nitrotoluene. In particular,this method is effective for the analysis of PETN, 1,3,5-TNB and tetryl which showed poor interlaboratory trial results with ISO 11916-1. Under the conditions specified in this document, concentrations as low as 0,005 mg/kg to 0,014 mg/kg-dry matter can be determined, depending on the substance.
Purpose and justification of the proposal*
Currently two ISO standards exist for the analysis of explosives and related compounds in soil: ISO 11916-1(HPLC/UV method), ISO 11916-2(GC-ECD or MS method). According to the results of interlaboratory trial with ISO 11916-1, it showed some problematic aspects to analyze PETN, 1,3,5-TNB and tetryl. In case of ISO 11916-2, it also gave poor inter-laboratory trial results for 1,3,5-TNB. Therefore, it is necessary to develop new method effectively applicable to the determination of PETN, 1,3,5-TNB and tetryl.
In addition to this, lower risk-based PRGs (Preliminary Remediation Goal), new regulatory concerns, and change of land use have created the atmosphere to apply more sensitive and selective instruments to determine explosive and related compounds. From the view of these aspects, liquid chromatography–tandem mass spectrometry (LC-MS/MS) is one of alternative methods for these purposes. LC-MS/MS method provides 10-20 times or much lower detection limit than that of HPLC/UV method and is recommendable to determine PETN, 1,3,5-TNB and tetryl.
Also LC-MS/MS method is getting more familiar in ISO standard development (e.g. ISO/CD22104 Water quality--Microcystins, ISO/NP21677 Water quality--HBCD, ISO/CD21675 Water quality--PFAS).
Consider the following: Is there a verified market need for the proposal? What problem does this
standard solve? What value will the document bring to end-users? See Annex C of the ISO/IEC
Directives part 1 for more information. See the following guidance on justification statements on ISO Connect:
https://connect.iso.org/pages/viewpage.action?pageId=27590861
Bodenbeschaffenheit - Bestimmung von ausgewählten Explosivstoffen und verwandten Verbindungen - Teil 3: Verfahren mittels Flüssigkeitschromatographie mit Tandem-Massenspektrometrie (LC-MS/MS) (ISO 11916-3:2021)
Dieses Dokument legt ein Verfahren zur Messung von Explosivstoffen und verwandten Nitroverbindungen (wie in Tabelle 1 angegeben) in Böden und Bodenmaterialien fest. Dieses Dokument ist für die Spurenanalyse von Explosivstoffen und verwandten Verbindungen mittels Flüssigkeitschromatographie mit Tandem Massenspektrometrie (LC MS/MS) vorgesehen. Im Allgemeinen zeigt die LC MS/MS Messung für jede Verbindung in Tabelle 1 die niedrigere Bestimmungsgrenze (LOQ) (en: limit of quantification) als bei der Verwendung von Hochleistungs Flüssigkeitschromatographie (HPLC) mit UV-Detektion (siehe Anhang B und Anhang C).
Unter den in diesem Dokument festgelegten Bedingungen können in Abhängigkeit von der jeweiligen Substanz Konzentrationen gleich oder größer als 0,005 mg/kg bis 0,014 mg/kg, bezogen auf die Trockenmasse, bestimmt werden. Ähnliche Verbindungen, insbesondere verschiedene Nitroaromaten, Nebenprodukte und Abbaupro¬dukte von Explosivstoffen, können nach diesem Verfahren analysiert werden, unter der Voraussetzung, dass die Anwendbarkeit im Einzelfall verifiziert wird.
[Tabelle 1]
Qualité du sol - Dosage d'une sélection d'explosifs et de composés apparentés - Partie 3: Méthode utilisant la chromatographie en phase liquide couplée à la spectrométrie de masse en tandem (CL-SM/SM) (ISO 11916-3:2021)
Le présent document spécifie la quantification de composés explosifs et nitrocomposés apparentés (indiqués dans le Tableau 1) dans le sol et les matériaux du sol. Le présent document est destiné à l’analyse de traces d’explosifs et de composés apparentés par chromatographie en phase liquide couplée à la spectrométrie de masse en tandem (CL-SM/SM). En général, la quantification par CL-SM/SM permet d’obtenir, pour chaque composé du Tableau 1, une LOQ (limite de quantification) inférieure à celle obtenue avec la chromatographie liquide à haute performance (CLHP) avec détection UV (voir l'Annexe B et l'Annexe C).
Dans les conditions spécifiées dans le présent document, des concentrations aussi faibles que 0,005 mg/kg à 0,014 mg/kg de matière sèche peuvent être déterminées, selon la substance. Des composés similaires, en particulier différents composés nitroaromatiques, sous-produits et produits de dégradation des composés explosifs, peuvent être analysés à l'aide de cette méthode à condition que l'applicabilité soit vérifiée au cas par cas.
Kakovost tal - Določevanje izbranih eksplozivov in podobnih spojin - 3. del: Metoda s tekočinsko kromatografijo s tandemsko masno spektrometrijo (LC-MS/MS) (ISO 11916-3:2021)
Ta mednarodni standard določa metodo za merjenje eksplozivnih in podobnih nitro spojin
s tekočinsko kromatografijo s tandemsko masno spektrometrijo (LC-MS/MS) v tleh in talnem materialu. Ta metoda se uporablja za 12 spojin (1,3-DNB, 1,3,5-TNB, 2,4-DNT, 2,6-DNT, 2,4,6-TNT, 4-A-2,6-DNT, 2-A-4,6-DNT, tetril, heksil, RDX, HMX, PETN), navedenih v standardu ISO 11916-1 (tla, metoda HPLC/UV), z izjemo nitrobenzena, 2-nitrotoluena, 3-nitrotoluena in 4-nitrotoluena. Metoda je zlasti učinkovita za analizo spojin PETN, 1,3,5-TNB in tetrila s slabimi rezultati medlaboratorijskega preskusa v skladu s standardom ISO 11916-1. Pod pogoji iz tega standarda je mogoče določiti že koncentracije od 0,005 mg/kg do 0,014 mg/kg suhe snovi, odvisno od snovi.
Namen in utemeljitev predloga*
Za analizo eksplozivov in podobnih spojin v tleh trenutno obstajata dva standarda ISO: ISO 11916-1 (metoda HPLC/UV), ISO 11916-2 (metoda GC-ECD ali MS). Glede na rezultate medlaboratorijskega preskusa v skladu s standardom ISO 11916-1 je bilo ugotovljenih nekaj težavnih vidikov pri analizi PETN, 1,3,5-TNB in tetrila. V primeru standarda ISO 11916-2 so bili pridobljeni tudi slabi rezultati medlaboratorijskega preskusa za spojino 1,3,5-TNB. Zato je treba razviti novo metodo, ki bo omogočala učinkovito določevanje spojin PETN, 1,3,5-TNB in tetrila.
Poleg tega so cilji predhodne sanacije (PRG), ki temeljijo na nižjem tveganju, nova regulativna vprašanja in sprememba rabe zemljišč ustvarili ozračje za uporabo občutljivejših ter selektivnejših instrumentov za določevanje eksplozivov in podobnih spojin. Pri teh vidikih je tekočinska kromatografija s tandemsko masno spektrometrijo (LC-MS/MS) ena od alternativnih metod za te namene. Metoda LC-MS/MS zagotavlja od 10- do 20-krat nižjo ali še veliko nižjo mejo zaznavnosti kot metoda HPLC/UV in je priporočljiva za določanje spojin PETN, 1,3,5-TNB in tetrila.
Metoda LC-MS/MS postaja tudi vse bolj poznana na področju razvoja standardov ISO (npr. ISO/CD22104 Kakovost vode – mikrocistini, ISO/NP21677 Kakovost vode – HBCD, ISO/CD21675 Kakovost vode – PFAS).
Razmislite o naslednjem: Ali obstaja za predlog preverjena potreba na trgu? Katero težavo
odpravlja ta standard? Kakšno vrednost ima dokument za končne uporabnike? Za več informacij glej dodatek C
v 1. delu Direktiv ISO/IEC. Glej naslednje smernice o utemeljitvah na spletnem mestu ISO Connect:
https://connect.iso.org/pages/viewpage.action?pageId=27590861
General Information
Buy Standard
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 11916-3:2022
01-januar-2022
Kakovost tal - Določevanje izbranih eksplozivov in podobnih spojin - 3. del:
Metoda s tekočinsko kromatografijo s tandemsko masno spektrometrijo (LC-
MS/MS) (ISO 11916-3:2021)
Soil quality - Determination of selected explosives and related compounds - Part 3:
Method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) (ISO
11916-3:2021)
Bodenbeschaffenheit - Bestimmung von ausgewählten Explosivstoffen und verwandten
Verbindungen - Teil 3: Verfahren mittels Flüssigkeitschromatographie mit Tandem-
Massenspektrometrie (LC-MS/MS) (ISO 11916-3:2021)
Qualité du sol - Dosage d'une sélection d'explosifs et de composés apparentés - Partie
3: Méthode utilisant la chromatographie en phase liquide couplée à la spectrométrie de
masse en tandem (CL-SM/SM) (ISO 11916-3:2021)
Ta slovenski standard je istoveten z: EN ISO 11916-3:2021
ICS:
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN ISO 11916-3:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 11916-3:2022
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SIST EN ISO 11916-3:2022
EN ISO 11916-3
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2021
EUROPÄISCHE NORM
ICS 13.080.10
English Version
Soil quality - Determination of selected explosives and
related compounds - Part 3: Method using liquid
chromatography-tandem mass spectrometry (LC-MS/MS)
(ISO 11916-3:2021)
Qualité du sol - Dosage d'une sélection d'explosifs et de Bodenbeschaffenheit - Bestimmung von ausgewählten
composés apparentés - Partie 3: Méthode utilisant la Explosivstoffen und verwandten Verbindungen - Teil 3:
chromatographie en phase liquide couplée à la Verfahren mittels Flüssigkeitschromatographie mit
spectrométrie de masse en tandem (CL-SM/SM) (ISO Tandem-Massenspektrometrie (LC-MS/MS) (ISO
11916-3:2021) 11916-3:2021)
This European Standard was approved by CEN on 7 September 2021.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 11916-3:2021 E
worldwide for CEN national Members.
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SIST EN ISO 11916-3:2022
EN ISO 11916-3:2021 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 11916-3:2022
EN ISO 11916-3:2021 (E)
European foreword
This document (EN ISO 11916-3:2021) has been prepared by Technical Committee ISO/TC 190 "Soil
quality" in collaboration with Technical Committee CEN/TC 444 “Environmental characterization of
solid matrices” the secretariat of which is held by NEN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by April 2022, and conflicting national standards shall be
withdrawn at the latest by April 2022.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO 11916-3:2021 has been approved by CEN as EN ISO 11916-3:2021 without any
modification.
3
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SIST EN ISO 11916-3:2022
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SIST EN ISO 11916-3:2022
INTERNATIONAL ISO
STANDARD 11916-3
First edition
2021-09
Soil quality — Determination of
selected explosives and related
compounds —
Part 3:
Method using liquid chromatography-
tandem mass spectrometry (LC-MS/
MS)
Qualité du sol — Dosage d'une sélection d'explosifs et de composés
apparentés —
Partie 3: Méthode utilisant la chromatographie en phase liquide
couplée à la spectrométrie de masse en tandem (CL-SM/SM)
Reference number
ISO 11916-3:2021(E)
©
ISO 2021
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021
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
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Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 2
5 Interferences . 2
6 Reagents . 2
6.1 General . 2
6.2 Chemicals . 2
6.3 Standard substances and solutions . 3
6.3.1 Standard substances . 3
6.3.2 Standard solutions . 3
7 Apparatus . 4
7.1 General . 4
7.2 Equipment for extraction . 4
7.3 Liquid chromatograph-tandem mass spectrometer (LC-MS/MS) . 4
8 Procedure. 5
8.1 Sample pre-treatment, sample storage and determination of water content . 5
8.2 Extraction . 5
8.2.1 General. 5
8.2.2 Extraction using ultrasonic waves . 5
8.2.3 Extraction using mechanical shaking . 6
8.3 Storage of extract . 6
9 Liquid chromatography tandem mass spectrometry (LC-MS/MS) .6
9.1 General . 6
9.2 Identification and quantification . 6
9.3 Calibration . 7
10 Calculation of results . 7
11 Quality assurance/quality control (QA/QC) . 8
12 Expression of results . 9
13 Test report . 9
Annex A (informative) Conditions of high performance liquid chromatography tandem
mass spectrometry (LC-MS/MS) .10
Annex B (informative) Comparison of LC-MS and LC-MS/MS application for PETN, 1,3,5-TNB
and tetryl .13
Annex C (informative) Comparison of LOD and LOQ in the measurement of HPLC and LC-MS/MS .16
Annex D (informative) Comparison of extractive capability of acetonitrile and methanol
when using LC-MS/MS .19
Annex E (informative) Report of interlaboratory validation study for ISO 11916-3 .21
Bibliography .23
© ISO 2021 – All rights reserved iii
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(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.
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 of 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 190, Soil quality, Subcommittee
SC 3, Chemical and physical characterization, in collaboration with the European Committee for
Standardization (CEN) Technical Committee CEN/TC 444, Environmental characterization of solid
matrices, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna
Agreement).
A list of all parts in the ISO 11916 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 2021 – All rights reserved
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
Introduction
Currently two ISO standards exist for the analysis of explosives and related compounds in soil:
ISO 11916-1 (HPLC with UV detection method), ISO 11916-2 (GC-ECD or MS). According to the results
of inter-laboratory trial with ISO 11916-1, it showed some problematic aspects to analyze PETN,
1,3,5-TNB and tetryl. In case of ISO 11916-2, it also gave poor inter-laboratory trial results for 1,3,5-TNB.
Therefore, it is necessary to develop new method effectively applicable to the determination of PETN,
1,3,5-TNB and tetryl. In addition to this, lower risk-based PRGs (Preliminary Remediation Goal), new
regulatory concerns, and change of land use have created the atmosphere to apply more sensitive and
selective instruments to determine explosive and related compounds. From the view of these aspects,
liquid chromatography–tandem mass spectrometry (LC-MS/MS) is one of alternative methods for these
purposes. LC-MS/MS method provides 10-20 times or more lower detection limit than that of HPLC/UV
method. In this document, LC-MS/MS method is intended for the trace analysis of explosives and related
compounds and applicable to 12 compounds (1,3-DNB, 1,3,5-TNB, 2,4-DNT, 2,6-DNT, 2,4,6-TNT, 4-A- 2,6-
DNT, 2-A-4,6-DNT, Tetryl, Hexyl, RDX, HMX, PETN) listed in ISO 11916-1 (soil, HPLC with UV detection
method) except for nitrobenzene, 2-nitrotoluene, 3-nitrotoluene and 4-nitrotoluene (see Annex E).
In case of nitrobenzene and nitrotoluenes, they have the low sensitivity in LC-MS/MS measurement
than using HPLC with UV detection method. In particular LC-MS/MS measurement is effective for the
analysis of PETN, 1,3,5-TNB and tetryl when comparing with the method using HPLC with UV detection
method. Also LC-MS/MS method is getting more familiar in ISO standard development (e.g. ISO 22104
Water quality-Microcystins, ISO/NP 21677 Water quality-HBCD, ISO 21675 Water quality-PFAS).
© ISO 2021 – All rights reserved v
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SIST EN ISO 11916-3:2022
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SIST EN ISO 11916-3:2022
INTERNATIONAL STANDARD ISO 11916-3:2021(E)
Soil quality — Determination of selected explosives and
related compounds —
Part 3:
Method using liquid chromatography-tandem mass
spectrometry (LC-MS/MS)
1 Scope
This document specifies the measurement of explosives and related nitrocompounds (as given in
Table 1) in soil and soil materials. This document is intended for the trace analysis of explosives and
related compounds by liquid chromatography–tandem mass spectrometry (LC-MS/MS). Generally, LC-
MS/MS measurement shows the lower LOQ (limit of quantification) for each compound in Table 1 than
using high-performance liquid chromatography (HPLC) with UV-detection (see Annex B and Annex C).
Under the conditions specified in this document, concentrations as low as 0,005 mg/kg to 0,014 mg/kg-
dry matter can be determined, depending on the substance. Similar compounds, in particular various
nitroaromatics, by-products and degradation products of explosive compounds can be analysed using
this method provided that the applicability is checked on a case-by-case basis.
Table 1 — Explosive and related nitrocompounds for analysis
®1
Compound Abbreviation CAS-RN
1,3-Dinitrobenzene 1,3-DNB 99-65-0
1,3,5-Trinitrobenzene 1,3,5-TNB 99-35-4
2,4-Dinitrotoluene 2,4-DNT 121-14-2
2,6-Dinitrotoluene 2,6-DNT 606-20-2
2,4,6-Trinitrotoluene 2,4,6-TNT 118-96-7
4-Amino-2,6-dinitrotoluene 4-A-2,6-DNT 19406-51-6
2-Amino-4,6-dinitrotoluene 2-A-4,6-DNT 35572-78-2
N-Methyl-N-2,4,6-tetranitroaniline Tetryl 479-45-8
2,4,6-Trinitro-N-(2,4,6-trinitrophenyl)aniline Hexyl 131-73-7
1,3,5-Trinitrohexahydro-1,3,5-triazine RDX 121-82-4
1,3,5,7-Tetranitro-octahydro-1,3,5,7-tetrazocine HMX 2691-41-0
Pentaerythrityl tetranitrate PETN 78-11-5
1 ® ®
CAS Registry Number (CAS RN ) is a trademark of CAS corporation. This information is given for the convenience of
users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products may be
used if they can be shown to lead to the same results.
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 11465, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric
method
© ISO 2021 – All rights reserved 1
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
Explosive materials in soils are extracted with acetonitrile by using one of the following techniques:
— ultrasonic bath with ultrasonic waves as medium (USE);
— horizontal mechanical shaker at room temperature (MSE).
There are two further extraction procedures such as pressurized liquid extraction (PLE) and soxhlet
apparatus that works isothermically at boiling temperature (SOX). However, they might not be suitable
for PETN, tetryl and 1,3,5-TNB.
The extract containing the analytes is either injected directly, or if necessary diluted prior to injection,
into a reversed-phase high-performance liquid chromatograph–tandem mass spectrometer (LC-MS/
MS).
WARNING — Take care when transporting, storing or treating explosive materials. High
temperature, high pressure and static electricity shall be prevented when storing explosive
materials. Small amounts of explosive materials should be kept moist in a cool, dark place.
Soil samples containing explosives with a mass fraction of less than 1 % do not have a risk of
explosion.
5 Interferences
Solvents, reagents, glassware, and other hardware used for sample processing can yield artifacts and/
or elevated baselines, causing misinterpretation of the chromatograms. All of these materials shall
therefore be demonstrated to be free of contaminants and interferences through the analysis of method
blanks.
Samples containing 2,4,6-trinitrobenzoic acid should not be extracted with acetonitrile as it can
result in the overestimation of 1,3,5-TNB due to decarboxylation. To avoid this interference, methanol
extraction can be an alternative method for 1,3,5-TNB.
When comparing with acetonitrile, methanol has showed serious problem in the recovery test for HMX,
RDX and tetryl with LC-MS/MS detection (see Annex D). Also, it should be avoided to extract tetryl at
temperatures above room temperature.
6 Reagents
6.1 General
All reagents shall be blank-free and of recognized analytical grade.
6.2 Chemicals
6.2.1 Water, with an electrical conductivity of ≤ 0,01 mS/m (25 °C).
2 © ISO 2021 – All rights reserved
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
6.2.2 Acetonitrile, CH CN, HPLC grade or equivalent.
3
6.2.3 Methanol, CH OH, HPLC grade or equivalent.
3
6.2.4 Ammonium acetate in water, 2,5 mmol/l.
For the preparation, weigh 96,3 mg of ammonium acetate (C H NO ) into 500 ml measuring flasks
2 7 2
(scale: mg/ml), fill up to the mark with water (6.2.1). Prepare the reagent just before it is used. Before
using as a mobile phase, filter the reagent using filter paper (7.1.6). After filtration, degas the filtrate
using ultrasonic bath or other methods.
6.2.5 Ammonium acetate in methanol, 2,5 mmol/l.
For the preparation, weigh 96,3 mg of ammonium acetate (C H NO ) into 500 ml measuring flasks
2 7 2
(scale: mg/ml), fill up to the mark with methanol (6.2.3). Prepare the reagent just before it is used.
Before using as a mobile phase, filter the reagent using filter paper (7.1.6). After filtration, degas the
filtrate using ultrasonic bath or other methods.
6.3 Standard substances and solutions
6.3.1 Standard substances
6.3.1.1 Reference substances
Reference substances are listed in Table 1.
6.3.1.2 Method-checking standards
Suitable compound(s) not found in the sample (i.e. 2,5-dinitrotoluene or 1,2-dinitrobenzene) can be
used as method-checking standards. It is recommended that the concentration of method-checking
standards in the final extract is ranged from 0,04 mg/l to 0,1 mg/l. Before selecting the method-
checking standards, confirm the applicability of those standards according to the analytical conditions
of each laboratory.
6.3.2 Standard solutions
6.3.2.1 General
All standard solutions used in this method shall be prepared as described below.
If commercially available certified standard stock solutions are used, calibration solutions are prepared
in volumetric flasks by diluting the stock solutions with acetonitrile (6.2.2).
All dilution steps shall not exceed the factor 100.
6.3.2.2 Single-substance stock solutions
For the preparation, weigh 50 mg ± 0,1 mg of the reference substances into 50 ml measuring flasks
(scale: mg/ml), fill up to the mark with acetonitrile (6.2.2) and let the reference substances dissolve
completely.
Transfer the stock solutions to amber-glass flasks and seal with polytetrafluoroethylene (PTFE)-coated
screw caps. The stock solutions can be kept in the refrigerator at 2 °C to 6 °C in the dark for up to
6 months.
© ISO 2021 – All rights reserved 3
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
6.3.2.3 Multi-component stock solutions
Prepare multi-component stock solutions of different concentrations from the various single-substance
stock solutions (6.3.2.2) by mixing and diluting with acetonitrile (6.2.2). At concentrations below 1 mg/
ml, solutions should be checked after one week as reference substances can decompose.
6.3.2.4 Calibration standard solutions
Calibration standard solutions are prepared by the dilution of multi-component stock solutions. The
working range of 0,01 mg/l to 0,2 mg/l is recommendable. A minimum of 5 concentration levels is
needed for the calibration.
7 Apparatus
7.1 General
Usual laboratory apparatus and the followings are used for this standard.
7.1.1 Amber glass containers with caps containing PTFE coated lining.
7.1.2 Amber glass vials with caps containing septa with PTFE coated lining.
7.1.3 Amber glass conical bottles with ground-in stopper.
7.1.4 Analytical balance, with a precision of at least 0,1 mg.
7.1.5 Laboratory centrifuge, capable of producing an acceleration of at least 1 000 g.
7.1.6 Membrane filter, 0,45 µm pore size.
Any adsorption of the target compounds shall be avoided. No interfering material shall be eluted. PTFE,
polyamide or an equivalent material is recommended.
7.2 Equipment for extraction
7.2.1 Temperature-controlled ultrasonic bath, 35 Hz, effective HF-power of at least 140 W.
Water bath capable of maintaining the temperature at (30 ± 5) °C or at (50 ± 5) °C during ultrasonic
extraction.
7.2.2 Horizontal mechanical shaker.
The shaker shall maintain a frequency of 100 cycles/min and offer a shaking width of about 10 cm.
7.3 Liquid chromatograph-tandem mass spectrometer (LC-MS/MS)
7.3.1 LC system, consisting of a pump that supports a pressure of at least 40 MPa (400 bar) and an
injection system with an appropriate loop capacity depending on injection volume.
7.3.1.1 LC-Column
Temperature-controlled columns packed with reversed phase material. The stainless column
(25 cm x 2,1 mm∼4,6 mm internal diameter) filled with silica gel (particle diameter, 5 μm) chemically
4 © ISO 2021 – All rights reserved
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
bonded with octadecylsilyl (ODS) group or those with an equivalent separating ability should be used.
If the applicability is verified, other types of column can be used.
For verification purposes, where applicable, repeat the chromatographic separation using a column
of different selectivity; CN reversed-phase column or phenyl-hexyl reversed-phase column are
recommended.
7.3.1.2 Mobile phase
A solution made b
...
SLOVENSKI STANDARD
SIST EN ISO 11916-3:2022
01-januar-2022
Kakovost tal - Določevanje izbranih eksplozivov in podobnih spojin - 3. del:
Metoda s tekočinsko kromatografijo s tandemsko masno spektrometrijo (LC-
MS/MS) (ISO 11916-3:2021)
Soil quality - Determination of selected explosives and related compounds - Part 3:
Method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) (ISO/FDIS
11916-3:2021)
Bodenbeschaffenheit - Bestimmung von ausgewählten Explosivstoffen und verwandten
Verbindungen - Teil 3: Verfahren mittels Flüssigkeitschromatographie mit Tandem-
Massenspektrometrie (LC-MS/MS) (ISO 11916-3:2021)
Qualité du sol - Dosage d'une sélection d'explosifs et de composés apparentés - Partie
3: Méthode utilisant la chromatographie en phase liquide couplée à la spectrométrie de
masse en tandem (CL-SM/SM) (ISO 11916-3:2021)
Ta slovenski standard je istoveten z: EN ISO 11916-3:2021
ICS:
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN ISO 11916-3:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 11916-3:2022
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SIST EN ISO 11916-3:2022
EN ISO 11916-3
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2021
EUROPÄISCHE NORM
ICS 13.080.10
English Version
Soil quality - Determination of selected explosives and
related compounds - Part 3: Method using liquid
chromatography-tandem mass spectrometry (LC-MS/MS)
(ISO 11916-3:2021)
Qualité du sol - Dosage d'une sélection d'explosifs et de Bodenbeschaffenheit - Bestimmung von ausgewählten
composés apparentés - Partie 3: Méthode utilisant la Explosivstoffen und verwandten Verbindungen - Teil 3:
chromatographie en phase liquide couplée à la Verfahren mittels Flüssigkeitschromatographie mit
spectrométrie de masse en tandem (CL-SM/SM) (ISO Tandem-Massenspektrometrie (LC-MS/MS) (ISO
11916-3:2021) 11916-3:2021)
This European Standard was approved by CEN on 7 September 2021.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 11916-3:2021 E
worldwide for CEN national Members.
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SIST EN ISO 11916-3:2022
EN ISO 11916-3:2021 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 11916-3:2022
EN ISO 11916-3:2021 (E)
European foreword
This document (EN ISO 11916-3:2021) has been prepared by Technical Committee ISO/TC 190 "Soil
quality" in collaboration with Technical Committee CEN/TC 444 “Environmental characterization of
solid matrices” the secretariat of which is held by NEN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by April 2022, and conflicting national standards shall be
withdrawn at the latest by April 2022.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO 11916-3:2021 has been approved by CEN as EN ISO 11916-3:2021 without any
modification.
3
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SIST EN ISO 11916-3:2022
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SIST EN ISO 11916-3:2022
INTERNATIONAL ISO
STANDARD 11916-3
First edition
2021-09
Soil quality — Determination of
selected explosives and related
compounds —
Part 3:
Method using liquid chromatography-
tandem mass spectrometry (LC-MS/
MS)
Qualité du sol — Dosage d'une sélection d'explosifs et de composés
apparentés —
Partie 3: Méthode utilisant la chromatographie en phase liquide
couplée à la spectrométrie de masse en tandem (CL-SM/SM)
Reference number
ISO 11916-3:2021(E)
©
ISO 2021
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021
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
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 2
5 Interferences . 2
6 Reagents . 2
6.1 General . 2
6.2 Chemicals . 2
6.3 Standard substances and solutions . 3
6.3.1 Standard substances . 3
6.3.2 Standard solutions . 3
7 Apparatus . 4
7.1 General . 4
7.2 Equipment for extraction . 4
7.3 Liquid chromatograph-tandem mass spectrometer (LC-MS/MS) . 4
8 Procedure. 5
8.1 Sample pre-treatment, sample storage and determination of water content . 5
8.2 Extraction . 5
8.2.1 General. 5
8.2.2 Extraction using ultrasonic waves . 5
8.2.3 Extraction using mechanical shaking . 6
8.3 Storage of extract . 6
9 Liquid chromatography tandem mass spectrometry (LC-MS/MS) .6
9.1 General . 6
9.2 Identification and quantification . 6
9.3 Calibration . 7
10 Calculation of results . 7
11 Quality assurance/quality control (QA/QC) . 8
12 Expression of results . 9
13 Test report . 9
Annex A (informative) Conditions of high performance liquid chromatography tandem
mass spectrometry (LC-MS/MS) .10
Annex B (informative) Comparison of LC-MS and LC-MS/MS application for PETN, 1,3,5-TNB
and tetryl .13
Annex C (informative) Comparison of LOD and LOQ in the measurement of HPLC and LC-MS/MS .16
Annex D (informative) Comparison of extractive capability of acetonitrile and methanol
when using LC-MS/MS .19
Annex E (informative) Report of interlaboratory validation study for ISO 11916-3 .21
Bibliography .23
© ISO 2021 – All rights reserved iii
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(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.
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 of 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 190, Soil quality, Subcommittee
SC 3, Chemical and physical characterization, in collaboration with the European Committee for
Standardization (CEN) Technical Committee CEN/TC 444, Environmental characterization of solid
matrices, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna
Agreement).
A list of all parts in the ISO 11916 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 2021 – All rights reserved
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
Introduction
Currently two ISO standards exist for the analysis of explosives and related compounds in soil:
ISO 11916-1 (HPLC with UV detection method), ISO 11916-2 (GC-ECD or MS). According to the results
of inter-laboratory trial with ISO 11916-1, it showed some problematic aspects to analyze PETN,
1,3,5-TNB and tetryl. In case of ISO 11916-2, it also gave poor inter-laboratory trial results for 1,3,5-TNB.
Therefore, it is necessary to develop new method effectively applicable to the determination of PETN,
1,3,5-TNB and tetryl. In addition to this, lower risk-based PRGs (Preliminary Remediation Goal), new
regulatory concerns, and change of land use have created the atmosphere to apply more sensitive and
selective instruments to determine explosive and related compounds. From the view of these aspects,
liquid chromatography–tandem mass spectrometry (LC-MS/MS) is one of alternative methods for these
purposes. LC-MS/MS method provides 10-20 times or more lower detection limit than that of HPLC/UV
method. In this document, LC-MS/MS method is intended for the trace analysis of explosives and related
compounds and applicable to 12 compounds (1,3-DNB, 1,3,5-TNB, 2,4-DNT, 2,6-DNT, 2,4,6-TNT, 4-A- 2,6-
DNT, 2-A-4,6-DNT, Tetryl, Hexyl, RDX, HMX, PETN) listed in ISO 11916-1 (soil, HPLC with UV detection
method) except for nitrobenzene, 2-nitrotoluene, 3-nitrotoluene and 4-nitrotoluene (see Annex E).
In case of nitrobenzene and nitrotoluenes, they have the low sensitivity in LC-MS/MS measurement
than using HPLC with UV detection method. In particular LC-MS/MS measurement is effective for the
analysis of PETN, 1,3,5-TNB and tetryl when comparing with the method using HPLC with UV detection
method. Also LC-MS/MS method is getting more familiar in ISO standard development (e.g. ISO 22104
Water quality-Microcystins, ISO/NP 21677 Water quality-HBCD, ISO 21675 Water quality-PFAS).
© ISO 2021 – All rights reserved v
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SIST EN ISO 11916-3:2022
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SIST EN ISO 11916-3:2022
INTERNATIONAL STANDARD ISO 11916-3:2021(E)
Soil quality — Determination of selected explosives and
related compounds —
Part 3:
Method using liquid chromatography-tandem mass
spectrometry (LC-MS/MS)
1 Scope
This document specifies the measurement of explosives and related nitrocompounds (as given in
Table 1) in soil and soil materials. This document is intended for the trace analysis of explosives and
related compounds by liquid chromatography–tandem mass spectrometry (LC-MS/MS). Generally, LC-
MS/MS measurement shows the lower LOQ (limit of quantification) for each compound in Table 1 than
using high-performance liquid chromatography (HPLC) with UV-detection (see Annex B and Annex C).
Under the conditions specified in this document, concentrations as low as 0,005 mg/kg to 0,014 mg/kg-
dry matter can be determined, depending on the substance. Similar compounds, in particular various
nitroaromatics, by-products and degradation products of explosive compounds can be analysed using
this method provided that the applicability is checked on a case-by-case basis.
Table 1 — Explosive and related nitrocompounds for analysis
®1
Compound Abbreviation CAS-RN
1,3-Dinitrobenzene 1,3-DNB 99-65-0
1,3,5-Trinitrobenzene 1,3,5-TNB 99-35-4
2,4-Dinitrotoluene 2,4-DNT 121-14-2
2,6-Dinitrotoluene 2,6-DNT 606-20-2
2,4,6-Trinitrotoluene 2,4,6-TNT 118-96-7
4-Amino-2,6-dinitrotoluene 4-A-2,6-DNT 19406-51-6
2-Amino-4,6-dinitrotoluene 2-A-4,6-DNT 35572-78-2
N-Methyl-N-2,4,6-tetranitroaniline Tetryl 479-45-8
2,4,6-Trinitro-N-(2,4,6-trinitrophenyl)aniline Hexyl 131-73-7
1,3,5-Trinitrohexahydro-1,3,5-triazine RDX 121-82-4
1,3,5,7-Tetranitro-octahydro-1,3,5,7-tetrazocine HMX 2691-41-0
Pentaerythrityl tetranitrate PETN 78-11-5
1 ® ®
CAS Registry Number (CAS RN ) is a trademark of CAS corporation. This information is given for the convenience of
users of this document and does not constitute an endorsement by ISO of the product named. Equivalent products may be
used if they can be shown to lead to the same results.
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 11465, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric
method
© ISO 2021 – All rights reserved 1
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
Explosive materials in soils are extracted with acetonitrile by using one of the following techniques:
— ultrasonic bath with ultrasonic waves as medium (USE);
— horizontal mechanical shaker at room temperature (MSE).
There are two further extraction procedures such as pressurized liquid extraction (PLE) and soxhlet
apparatus that works isothermically at boiling temperature (SOX). However, they might not be suitable
for PETN, tetryl and 1,3,5-TNB.
The extract containing the analytes is either injected directly, or if necessary diluted prior to injection,
into a reversed-phase high-performance liquid chromatograph–tandem mass spectrometer (LC-MS/
MS).
WARNING — Take care when transporting, storing or treating explosive materials. High
temperature, high pressure and static electricity shall be prevented when storing explosive
materials. Small amounts of explosive materials should be kept moist in a cool, dark place.
Soil samples containing explosives with a mass fraction of less than 1 % do not have a risk of
explosion.
5 Interferences
Solvents, reagents, glassware, and other hardware used for sample processing can yield artifacts and/
or elevated baselines, causing misinterpretation of the chromatograms. All of these materials shall
therefore be demonstrated to be free of contaminants and interferences through the analysis of method
blanks.
Samples containing 2,4,6-trinitrobenzoic acid should not be extracted with acetonitrile as it can
result in the overestimation of 1,3,5-TNB due to decarboxylation. To avoid this interference, methanol
extraction can be an alternative method for 1,3,5-TNB.
When comparing with acetonitrile, methanol has showed serious problem in the recovery test for HMX,
RDX and tetryl with LC-MS/MS detection (see Annex D). Also, it should be avoided to extract tetryl at
temperatures above room temperature.
6 Reagents
6.1 General
All reagents shall be blank-free and of recognized analytical grade.
6.2 Chemicals
6.2.1 Water, with an electrical conductivity of ≤ 0,01 mS/m (25 °C).
2 © ISO 2021 – All rights reserved
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
6.2.2 Acetonitrile, CH CN, HPLC grade or equivalent.
3
6.2.3 Methanol, CH OH, HPLC grade or equivalent.
3
6.2.4 Ammonium acetate in water, 2,5 mmol/l.
For the preparation, weigh 96,3 mg of ammonium acetate (C H NO ) into 500 ml measuring flasks
2 7 2
(scale: mg/ml), fill up to the mark with water (6.2.1). Prepare the reagent just before it is used. Before
using as a mobile phase, filter the reagent using filter paper (7.1.6). After filtration, degas the filtrate
using ultrasonic bath or other methods.
6.2.5 Ammonium acetate in methanol, 2,5 mmol/l.
For the preparation, weigh 96,3 mg of ammonium acetate (C H NO ) into 500 ml measuring flasks
2 7 2
(scale: mg/ml), fill up to the mark with methanol (6.2.3). Prepare the reagent just before it is used.
Before using as a mobile phase, filter the reagent using filter paper (7.1.6). After filtration, degas the
filtrate using ultrasonic bath or other methods.
6.3 Standard substances and solutions
6.3.1 Standard substances
6.3.1.1 Reference substances
Reference substances are listed in Table 1.
6.3.1.2 Method-checking standards
Suitable compound(s) not found in the sample (i.e. 2,5-dinitrotoluene or 1,2-dinitrobenzene) can be
used as method-checking standards. It is recommended that the concentration of method-checking
standards in the final extract is ranged from 0,04 mg/l to 0,1 mg/l. Before selecting the method-
checking standards, confirm the applicability of those standards according to the analytical conditions
of each laboratory.
6.3.2 Standard solutions
6.3.2.1 General
All standard solutions used in this method shall be prepared as described below.
If commercially available certified standard stock solutions are used, calibration solutions are prepared
in volumetric flasks by diluting the stock solutions with acetonitrile (6.2.2).
All dilution steps shall not exceed the factor 100.
6.3.2.2 Single-substance stock solutions
For the preparation, weigh 50 mg ± 0,1 mg of the reference substances into 50 ml measuring flasks
(scale: mg/ml), fill up to the mark with acetonitrile (6.2.2) and let the reference substances dissolve
completely.
Transfer the stock solutions to amber-glass flasks and seal with polytetrafluoroethylene (PTFE)-coated
screw caps. The stock solutions can be kept in the refrigerator at 2 °C to 6 °C in the dark for up to
6 months.
© ISO 2021 – All rights reserved 3
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
6.3.2.3 Multi-component stock solutions
Prepare multi-component stock solutions of different concentrations from the various single-substance
stock solutions (6.3.2.2) by mixing and diluting with acetonitrile (6.2.2). At concentrations below 1 mg/
ml, solutions should be checked after one week as reference substances can decompose.
6.3.2.4 Calibration standard solutions
Calibration standard solutions are prepared by the dilution of multi-component stock solutions. The
working range of 0,01 mg/l to 0,2 mg/l is recommendable. A minimum of 5 concentration levels is
needed for the calibration.
7 Apparatus
7.1 General
Usual laboratory apparatus and the followings are used for this standard.
7.1.1 Amber glass containers with caps containing PTFE coated lining.
7.1.2 Amber glass vials with caps containing septa with PTFE coated lining.
7.1.3 Amber glass conical bottles with ground-in stopper.
7.1.4 Analytical balance, with a precision of at least 0,1 mg.
7.1.5 Laboratory centrifuge, capable of producing an acceleration of at least 1 000 g.
7.1.6 Membrane filter, 0,45 µm pore size.
Any adsorption of the target compounds shall be avoided. No interfering material shall be eluted. PTFE,
polyamide or an equivalent material is recommended.
7.2 Equipment for extraction
7.2.1 Temperature-controlled ultrasonic bath, 35 Hz, effective HF-power of at least 140 W.
Water bath capable of maintaining the temperature at (30 ± 5) °C or at (50 ± 5) °C during ultrasonic
extraction.
7.2.2 Horizontal mechanical shaker.
The shaker shall maintain a frequency of 100 cycles/min and offer a shaking width of about 10 cm.
7.3 Liquid chromatograph-tandem mass spectrometer (LC-MS/MS)
7.3.1 LC system, consisting of a pump that supports a pressure of at least 40 MPa (400 bar) and an
injection system with an appropriate loop capacity depending on injection volume.
7.3.1.1 LC-Column
Temperature-controlled columns packed with reversed phase material. The stainless column
(25 cm x 2,1 mm∼4,6 mm internal diameter) filled with silica gel (particle diameter, 5 μm) chemically
4 © ISO 2021 – All rights reserved
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SIST EN ISO 11916-3:2022
ISO 11916-3:2021(E)
bonded with octadecylsilyl (ODS) group or those with an equivalent separating ability should be used.
If the applicability is verified, other types of column can be used.
For verification purposes, where applicable, repeat the chromatographic separation using a column
of different selectivity; CN reversed-phase column or phenyl-hexyl reversed-phase column are
recommended.
7.3.1.2 Mobile phase
A solution m
...
SLOVENSKI STANDARD
oSIST prEN ISO 11916-3:2020
01-april-2020
[Not translated]
Soil quality - Determination of selected explosives and related compounds - Part 3:
Method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) (ISO/DIS
11916-3:2020)
Bodenbeschaffenheit - Bestimmung von ausgewählten Explosivstoffen und verwandten
Verbindungen - Teil 3: Verfahren mittels Flüssigkeitschromatographie mit Tandem-
Massenspektrometrie (LC-MS/MS) (ISO/DIS 11916-3:2020)
Qualité du sol - Dosage d'une sélection d'explosifs et de composés apparentés - Partie
3: Méthode utilisant la chromatographie en phase liquide couplée à la spectrométrie de
masse en tandem (CL-SM/SM) (ISO/DIS 11916-3:2020)
Ta slovenski standard je istoveten z: prEN ISO 11916-3
ICS:
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
oSIST prEN ISO 11916-3:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 11916-3:2020
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oSIST prEN ISO 11916-3:2020
DRAFT INTERNATIONAL STANDARD
ISO/DIS 11916-3
ISO/TC 190/SC 3 Secretariat: DIN
Voting begins on: Voting terminates on:
2020-02-18 2020-05-12
Soil quality — Determination of selected explosives and
related compounds —
Part 3:
Method using liquid chromatography-tandem mass
spectrometry (LC-MS/MS)
ICS: 13.080.10
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
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ISO/DIS 11916-3:2020(E)
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PROVIDE SUPPORTING DOCUMENTATION. ISO 2020
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oSIST prEN ISO 11916-3:2020
ISO/DIS 11916-3:2020(E)
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oSIST prEN ISO 11916-3:2020
ISO/DIS 11916-3:2020(E)
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Contents Page
Introduction . v
1 Scope .1
2 Normative references .2
3 Principle .2
4 Interferences .2
5 Reagents .2
5.1 General .2
5.2 Chemicals .3
5.2.1 Water, with a electrical conductivity of ≥ 0.01 mS/m (25°C). .3
5.2.2 Acetonitrile, CH3CN, HPLC grade or equivalent. .3
5.2.3 Methanol, CH3OH, HPLC grade or equivalent. .3
5.2.4 Ammonium acetate in water, 2,5 mmol/l. .3
5.2.5 Ammonium acetate in methanol, 2,5 mmol/l. .3
5.3 Standard substances and solutions .3
5.3.1 Standard substances .3
5.3.2 Standard solutions .3
6 Apparatus .4
6.1 General .4
6.1.1 Amber glass containers with caps containing PTFE coated lining. .4
6.1.2 Amber glass vials with caps containing septa with PTFE coated lining. .4
6.1.3 Amber glass conical bottles with ground-in stopper. .4
6.1.4 Analytical balance, with a precision of at least 0,1 mg. .4
6.1.5 Laboratory centrifuge, capable of producing an acceleration of at least 1 000 G. .4
6.1.6 Membrane filter, 0,45 µm pore size. .4
6.2 Equipment for extraction.4
6.2.1 Temperature-controlled ultrasonic bath, 35 Hz, effective HF-power of at least 140 W. .4
6.2.2 Horizontal mechanical shaker. .4
6.3 Liquid chromatograph-tandem mass spectrometer (LC-MS/MS) .5
6.3.1 LC system, consisting of a pump that supports a pressure of at least 40 MPa (400
bar) and an injection system with an appropriate loop capacity depending on
injection volume. .5
6.3.2 Tandem mass spectrometer .5
7 Procedure .5
7.1 Sample pretreatment, sample storage and determination of water content .5
7.2 Extraction .5
7.2.1 General .5
7.2.2 Extraction using ultrasonic waves .6
7.2.3 Extraction using mechanical shaking .6
7.3 Storage of extract .6
8 Liquid chromatography tandem mass spectrometry (LC-MS/MS) .7
8.1 General .7
8.2 Identification and quantification .7
8.3 Calibration .7
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9 Calculation of results . 8
10 Quality assurance/quality control (QA/QC) . 8
11 Expression of results . 9
12 Test report . 9
Annex A (informative) Conditions of high performance liquid chromatography tandem
mass spectrometry (LC-MS/MS) . 11
Annex B (informative) Comparison of LC-MS and LC-MS/MS application for PETN, 1,3,5-TNB
and tetryl . 14
B.1 Descriptions of experiment . 14
B.2 Ion chromatogram of LC-MS (SIM) and LC-MS/MS (MRM) . 14
Annex C (informative) Comparison of LOD and LOQ in the measurement of HPLC and LC-
MS/MS. 17
C.1 Analytical conditions of HPLC . 17
Annex D (informative) Comparison of extractive capability of acetonitrile and methanol
when using LC-MS/MS . 20
D.1 Descriptions of experiment . 20
D.2 Results . 20
Bibliography . 22
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Introduction
Currently two ISO standards exist for the analysis of explosives and related compounds in soil: ISO
11916-1(HPLC/UV method), ISO 11916-2(GC-ECD or MS). According to the results of inter-laboratory
trial with ISO 11916-1, it showed some problematic aspects to analyze PETN, 1,3,5-TNB and tetryl. In
case of ISO 11916-2, it also gave poor inter-laboratory trial results for 1,3,5-TNB. Therefore, it is
necessary to develop new method effectively applicable to the determination of PETN, 1,3,5-TNB and
tetryl. In addition to this, lower risk-based PRGs (Preliminary Remediation Goal), new regulatory
concerns, and change of land use have created the atmosphere to apply more sensitive and selective
instruments to determine explosive and related compounds. From the view of these aspects, liquid
chromatography–tandem mass spectrometry (LC-MS/MS) is one of alternative methods for these
purposes. LC-MS/MS method provides 10-20 times or more lower detection limit than that of HPLC/UV
method. In this document, LC-MS/MS method is intended for the trace analysis of explosives and related
compounds and applicable to 12 compounds (1,3-DNB, 1,3,5-TNB, 2,4-DNT, 2,6-DNT, 2,4,6-TNT, 4-A-
2,6-DNT, 2-A-4,6-DNT, Tetryl, Hexyl, RDX, HMX, PETN) listed in ISO 11916-1(soil, HPLC/UV method)
except for nitrobenzene, 2-nitrotoluene, 3-nitrotoluene and 4-nitrotoluene. In case of nitrobenzene and
nitrotoluenes, they have the low sensitivity in LC-MS/MS measurement. In particular, this method is
effective for the analysis of PETN, 1,3,5-TNB and tetryl when comparing with the method using HPLC.
Also LC-MS/MS method is getting more familiar in ISO standard development (e.g. ISO/CD22104 Water
quality--Microcystins, ISO/NP21677 Water quality--HBCD, ISO/CD21675 Water quality--PFAS).
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DRAFT INTERNATIONAL STANDARD ISO/DIS 11916-3:2020(E)
Soil quality — Determination of selected explosives and
related compounds — — Part 3: Method using liquid
chromatography-tandem mass spectrometry (LC-MS/MS)
1 Scope
This part of ISO 11916 specifies the measurement of explosives and related nitrocompounds (as given
in Table 1) in soil and soil materials. This document is intended for the trace analysis of explosives and
related compounds by liquid chromatography–tandem mass spectrometry (LC-MS/MS). Generally, LC-
MS/MS measurement shows the lower LOQ (limit of quantification) for each compound in Table 1
than that of high-performance liquid chromatography (HPLC) measurement.
Under the conditions specified in this document, concentrations as low as 0,005 mg/kg to 0,014 mg/kg-
dry matter can be determined, depending on the substance. Similar compounds, in particular various
nitroaromatics, by-products and degradation products of explosive compounds may be analyzed using
this method. However, the applicability should be checked on a case-by-case basis.
Table 1 — Explosive and related nitrocompounds for analysis
a
Compound Abbreviation CAS-RN
1,3-Dinitrobenzene 1,3-DNB 99-65-0
1,3,5-Trinitrobenzene 1,3,5-TNB 99-35-4
2,4-Dinitrotoluene 2,4-DNT 121-14-2
2,6-Dinitrotoluene 2,6-DNT 606-20-2
2,4,6-Trinitrotoluene 2,4,6-TNT 118-96-7
4-Amino-2,6-dinitrotoluene 4-A-2,6-DNT 19406-51-6
2-Amino-4,6-dinitrotoluene 2-A-4,6-DNT 35572-78-2
N-Methyl-N-2,4,6-tetranitroaniline Tetryl 479-45-8
2,4,6-Trinitro-N-(2,4,6-trinitrophenyl)aniline Hexyl 131-73-7
1,3,5-Trinitrohexahydro-1,3,5-triazine RDX 121-82-4
1,3,5,7-Tetranitroo ctahydro-1,3,5,7-tetrazocine HMX 2691-41-0
Pentaerythrityltetranitrate PETN 78-11-5
a
CAS-RN: Chemical Abstract Service-Registry Number
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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 11465, Soil quality — Determination of dry matter and water content on a mass basis —
Gravimetric method
3 Principle
Explosive materials in soils are extracted with acetonitrile by using one of the following techniques:
— ultrasonic bath with ultrasonic waves as medium (USE);
— horizontal mechanical shaker at room temperature (MSE);
There are two further extraction procedures such as pressurized liquid extraction (PLE) and soxhlet
apparatus that works isothermically at boiling temperature (SOX). However, they might not be suitable
for PETN, tetryl and 1,3,5-TNB.
The extract containing the analytes is either injected directly, or if necessary diluted prior to injection,
into a reversed-phase high-performance liquid chromatograph–tandem mass spectrometer (LC-
MS/MS).
WARNING — Take care when transporting, storing or treating explosive materials. High
temperature, high pressure and static electricity shall be prevented when storing explosive
materials. Small amounts of explosive materials should be kept moist in a cool, dark place. Soil
samples containing explosives with a mass fraction of less than 1 % do not have a risk of
explosion.
4 Interferences
Solvents, reagents, glassware, and other hardware used for sample processing may yield artifacts
and/or elevated baselines, causing misinterpretation of the chromatograms. All of these materials shall
therefore be demonstrated to be free of contaminants and interferences through the analysis of method
blanks.
Samples containing 2,4,6-trinitrobenzoic acid should not be extracted with acetonitrile as it may result
in the overestimation of 1,3,5-TNB due to decarboxylation. To avoid this interference, methanol
extraction can be an alternative method for 1,3,5-TNB.
5 Reagents
5.1 General
All reagents shall be blank-free and of recognized analytical grade.
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5.2 Chemicals
5.2.1 Water, with a electrical conductivity of ≥ 0.01 mS/m (25°C).
5.2.2 Acetonitrile, CH3CN, HPLC grade or equivalent.
5.2.3 Methanol, CH3OH, HPLC grade or equivalent.
5.2.4 Ammonium acetate in water, 2,5 mmol/l.
For the preparation, weigh 96,3 mg of ammonium acetate(C H NO ) into 500 ml measuring flasks
2 7 2
(scale: mg/ml), fill up to the mark with water (5.2.1). Prepare the reagent just before it is used. Before
using as a mobile phase, filter the reagent using filter paper (6.1.7). After filtration, degas the filtrate
using sonic bath or other methods.
5.2.5 Ammonium acetate in methanol, 2,5 mmol/l.
For the preparation, weigh 96,3 mg of ammonium acetate(C2H7NO2) into 500 ml measuring flasks
(scale: mg/ml), fill up to the mark with methanol (5.2.3). Prepare the reagent just before it is used.
Before using as a mobile phase, filter the reagent using filter paper (6.1.7). After filtration, degas the
filtrate using sonic bath or other methods.
5.3 Standard substances and solutions
5.3.1 Standard substances
5.3.1.1 Reference substances
Compounds listed in Table 1.
5.3.1.2 Method-checking standards
Suitable compound(s) not found in the sample (i.e. 2,5-dinitrotoluene or 1,2-dinitrobenzene). It is
recommended that the concentration of method-checking standards in the final extract is ranged from
0,04 mg/l to 0,1 mg/l. Before selecting the method-checking standards, confirm the applicability of
those standards according to the analytical conditions of each laboratory.
5.3.2 Standard solutions
5.3.2.1 General
All standard solutions used in this method shall be prepared as described below.
NOTE If commercially available certified standard stock solutions are used, calibration solutions are
prepared in volumetric flasks by diluting the stock solutions with acetonitrile (5.2.2).
All dilution steps shall not exceed the factor 100.
5.3.2.2 Single-substance stock solutions
For the preparation, weigh 50 mg ± 0,1 mg of the reference substances into 50 ml measuring flasks
(scale: mg/ml), fill up to the mark with acetonitrile (5.2.2) and let the reference substances dissolve
completely.
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Transfer the stock solutions to amber-glass flasks and seal with polytetrafluoroethylene (PTFE)-coated
screw caps. The stock solutions can be kept in the refrigerator at 2 °C to 6 °C in the dark for up to 6
month.
5.3.2.3 Multi-component stock solutions
Prepare multi-component stock solutions of different concentrations from the various single-substance
stock solutions (5.3.2.2) by mixing and diluting with acetonitrile (5.2.2).At concentrations below 1
mg/ml, solutions should be checked after one week as reference substances may decompose.
5.3.2.4 Calibration standard solutions
Calibration standard solutions are prepared by the dilution of multi-component stock solutions. The
working range of 0,01 mg/l to 0,2 mg/l is recommendable. A minimum of 5 concentration levels is
needed for the calibration.
6 Apparatus
6.1 General
Usual laboratory apparatus and the followings.
6.1.1 Amber glass containers with caps containing PTFE coated lining.
6.1.2 Amber glass vials with caps containing septa with PTFE coated lining.
6.1.3 Amber glass conical bottles with ground-in stopper.
6.1.4 Analytical balance, with a precision of at least 0,1 mg.
6.1.5 Laboratory centrifuge, capable of producing an acceleration of at least 1 000 G.
6.1.6 Membrane filter, 0,45 µm pore size.
Any adsorption of the target compounds shall be avoided. No interfering material shall be eluated.
PTFE, polyamide or an equivalent material is recommended.
6.2 Equipment for extraction
6.2.1 Temperature-controlled ultrasonic bath, 35 Hz, effective HF-power of at least 140 W.
Water bath capable of maintaining the temperature at (30 ± 5) °C or at (50 ± 5) °C during ultrasonic
extraction.
6.2.2 Horizontal mechanical shaker.
The shaker shall maintain a frequency of 100 cycles/min and offer a shaking width of about 10 cm.
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6.3 Liquid chromatograph-tandem mass spectrometer (LC-MS/MS)
6.3.1 LC system, consisting of a pump that supports a pressure of at least 40 MPa (400 bar) and an
injection system with an appropriate loop capacity depending on injection volume.
6.3.1.1 Stationary phase
Temperature-controlled columns packed with reversed phasematerial. The column should be selected
from those made by filling 25 cm long stainless tubes with inner diameters within the range of 2,1mm
to 4,6 mm with silica gel (particle diameter 5 m) chemically bonded with octadecylsilyl (ODS) group or
those with an equivalent separating ability. If the applicability is verified, other types of column can be
used.
NOTE For verification purposes, where applicable, repeat the chromatographic separation using a
column of different selectivity; CN reversed-phase column or phenyl-hexyl reversed-phase column are
recommended.
6.3.1.2 Mobile phase
A solution made by mixing 2,5 mmol/l ammonium acetate in water (5.2.4) with 2,5 mmol/l ammonium
acetate in methanol (5.2.5) can be used as a mobile phase.
6.3.2 Tandem mass spectrometer
The LC-MS/MS system should be capable of negative ion atmospheric pressure chemical Ionization
(APCI). Use a triple quadrupole tandem mass analyzer (MS/MS) consisting of two successive
quadrupole mass analyzer or a system with at least equivalent performance as a mass spectrometer.
Also, multiple reaction monitoring (MRM) mode should be available for mass analysis.
7 Procedure
7.1 Sample pretreatment, sample storage and determination of water content
While taking a field-moist sample, remove coarse impurities, e.g. plant residues and stones. Put the
sample in an amber glass flask and store immediately in a cool, dark transport container.
Soil samples shall be analyzed as soon as possible. Before analyzing the sample, homogenize the sample
through a sieve with an aperture of 2 mm.
Soil samples shall be stored in a dark place at (4 ± 2) °C. Samples thatare stored for longer periods (i.e. >
than 1 week) prior to analysis, shall be stored at −20 °C.
In order to calculate the dry matter based content of explosive compounds, determine the dry matter
content of the field-moist soil in accordance with ISO 11465. Be aware of potential evaporation of
volatile toxic contaminants.
7.2 Extraction
7.2.1 General
For extraction, the following two methods may be applied:
— extraction using ultrasonic waves;
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— extraction using mechanical shaking.
The use of a method-checking standard is recommended. Method-checking standards have to be added
prior to extraction. For the selection of suitable method-checking standards, refer to 5.3.1.2. When
comparing with acetonitrile, methanol has showed serious problem in the recovery test for HMX, RDX
and tetryl with LC-MS/MS detection (refer to Annex D). Also, it should be avoided to extract tetryl at the
temperatures above room temperature.
7.2.2 Extraction using ultrasonic waves
Take approximately 20 g of the field-moist sample and weighit into the extraction container (6.1.1) with
a precision of ± 0,1 g and add the method-checking standard (5.3.1.2), if used, with a concentration
range of 0,04 mg/l to 0,1 mg/l in the final extract. Add 40 ml ± 0,1 ml of acetonitrile (5.2.2) and seal
with a cap containing a PTFE coated lining. Shake the vial briefly by hand, and then apply ultrasonic
extraction in the bath (6.2.1) for 16 h at (30 ± 5) °C or 4 h at (50 ± 5) °C. During extraction, the water
level in the bath should be at least 1 cm above the level of the solvent inside the extraction flasks. This
extraction method might not be proper for tetryl.
After applying ultrasonic extraction, allow the soil particles to settle for 30 min. Do not open the vial
before it has cooled down to room temperature. If necessary, filter an aliquot of the supernatant using a
0,45 µm PTFE or polyamide filter (6.1.7) into the vial (6.1.2) or centrifuge at 1 000 G for 20 min.
It is recommended to li
...
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