EN 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 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.

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

• Status: Published
• Publication Date: 05-Oct-2021
• Withdrawal Date: 29-Apr-2022
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: CEN/TC 444 - Environmental characterization
• Drafting Committee: CEN/TC 444/WG 2 - Organic analysis
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 06-Oct-2021
• Completion Date: 06-Oct-2021
• Ref Project: SIST EN ISO 11916-3:2022 - 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)

Standards Content (Sample)

SLOVENSKI STANDARD
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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.

Contents Page
European foreword . 3

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.
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
ISO 11916-3:2021(E)
© 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: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved

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 11916-3:2021(E)
Foreword
ISO (the International O
...

SLOVENSKI STANDARD
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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.

Contents Page
European foreword . 3

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.
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
ISO 11916-3:2021(E)
© 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: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved

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 11916-3:2021(E)
Foreword
ISO (the Internatio
...