Water quality - Determination of organochlorine pesticides (OCP) in whole water samples using solid phase extraction (SPE) with SPE-disks combined with gas chromatography mass spectrometry (GC-MS)

This European Standard specifies a method for the determination of selected organochlorine pesticides (OCP, see Table 1), in water samples. The method uses solid-phase extraction with SPE-disks followed by gas chromatography-mass spectrometry (GC-MS). It is applicable to the analysis of OCPs in surface water containing suspended particulate matter (SPM) up to 500 mg/l (whole water samples), drinking water and groundwater. The lower limit of the working range depends on the matrix, on the specific compound to be analyzed and on the sensitivity of the mass spectrometric detection unit. For compounds listed in Table 1 the limit of determination (LOQ) it is at least 30 % of the corresponding AA-EQS value (0,000 15 µg/l to 0,1 µg/l) according to the requirements of the European EQS Directive 2008/105/EC for both inland surface waters and other surface waters.
This method may be used for the analysis of other OCPs not listed in Table 1 or other types of water. However, it is necessary to verify its applicability before use.
(...)

Wasserbeschaffenheit - Bestimmung von Organochlorpestiziden (OCP) in Gesamtwasserproben mittels Festphasenextraktion (SPE) mit SPE-Scheiben in Verbindung mit Gaschromatographie-Massenspektrometrie (GC-MS)

Diese Europäische Norm legt ein Verfahren für die Bestimmung von ausgewählten Organochlorpestiziden (OCP, siehe Tabelle 1) in Wasserproben fest. Das Verfahren nutzt die Festphasenextraktion mit SPE Scheiben, gefolgt von Gaschromatographie-Massenspektroskopie (GC MS). Die Norm gilt für die Analyse von OCP in Oberflächenwasser, mit einem Schwebstoffanteil bis zu 500 mg/l (Gesamtwasserproben), Trinkwasser und Grundwasser. Der untere Grenzwert des Arbeitsbereiches hängt von der Matrix, der jeweils zu untersuchenden Verbindung und der Empfindlichkeit der Detektoreinheit des Massenspektrometers ab. Für die in Tabelle 1 angeführten Verbindungen beträgt die Bestimmungsgrenze mindestens 30 % des jeweiligen JD UQN-Werts (0,000 15 µg/l bis 0,1 µg/l) entsprechend den Anforderungen der Europäischen Richtlinie über Umweltqualitätsnormen im Bereich der Wasserpolitik (2008/105/EG).
Dieses Verfahren kann für die Analyse weiterer OCP, die nicht in Tabelle 1 angeführt sind, oder andere Arten von Wasser angewendet werden, dies muss jedoch vorher verifiziert werden.
(...)

Qualité de l'eau - Dosage des pesticides organochlorés (POC) dans la totalité de l'échantillon d'eau par extraction en phase solide (EPS) avec disques EPS, avec couplage chromatographie en phase gazeuse-spectrométrie de masse (CG-SM)

La présente Norme européenne spécifie une méthode pour le dosage d'une sélection de pesticides organochlorés (POC, voir Tableau 1) dans des échantillons d'eau. Cette méthode utilise une extraction en phase solide avec disques SPE suivie d'une chromatographie en phase gazeuse-spectrométrie de masse (CG-SM). Elle s'applique à l'analyse des POC dans les eaux de surface contenant jusqu'à 500 mg/l (totalité des échantillons d'eau) de matières en suspension (MES), dans l'eau potable et dans les eaux souterraines. La limite inférieure du domaine de travail dépend de la matrice, du composé à analyser et de la sensibilité du détecteur par spectrométrie de masse. Pour les composés répertoriés dans le Tableau 1, la limite de quantification (LQ) correspond à au moins 30 % de la valeur MA-NQE correspondante (0,000 15 µg/l à 0,1 µg/l) conformément aux exigences de la Directive 2008/105/CE sur les NQE européenne pour les eaux de surface intérieures et autres eaux de surface.
Cette méthode peut être utilisée pour analyser d'autres POC non mentionnés dans le Tableau 1 ou d'autres types d'eau. Cependant, il est important de vérifier son applicabilité avant de l'employer.
(...)

Kakovost vode - Določevanje organoklornih pesticidov (OCP) v celotnem vzorcu vode z ekstrakcijo na trdni fazi (SPE) s SPE-diski v kombinaciji s plinsko kromatografijo/masno spektrometrijo (GC/MS)

Razvoj metode za kvantitativno določevanje organoklornih pesticidov v celotnih vzorcih vode z uporabo plinske kromatografije/masne spektrometrije (GC-MS).
Ta analitska metoda določa določevanje organoklornih pesticidov, ki izpolnjujejo naslednje zahteve:
– analiza celotnih vzorcev vode, ki vsebujejo do 0,5 g/l trdnih delcev;
– meja določljivosti (LOQ) mora biti enaka ali manjša od 30 % EQS;
– merilna negotovost mora biti enaka ali manjša od 50 %;
– pred medlaboratorijskim potrjevanjem morajo biti metode v celoti preverjene interno in testirane glede robustnosti;
– evropska medlaboratorijska študijska primerjava bo potekala v skladu s standardom ISO 5725.

General Information

Status
Published
Public Enquiry End Date
31-Jan-2014
Publication Date
01-Nov-2015
ICS
13.060.50 - Examination of water for chemical substances
Technical Committee
KAV - Water quality
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
12-Oct-2015
Due Date
17-Dec-2015
Completion Date
02-Nov-2015
Directive
2000/60/EC - Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 establishing a framework for Community action in the field of water policy (substitutes Directive Reference 01/991 - Common Position on WFD)
EUR-PUB - European Union - Public Standards
Mandate
M/424 - Mandate for standardisation addressed to CEN for the development or improvement standards in support of the water framework directive
Ref Project
EN 16693:2015 - Water quality - Determination of organochlorine pesticides (OCP) in whole water samples - Method using solid phase extraction (SPE) with SPE-disks combined with gas chromatography mass spectrometry (GC-MS)

Overview

EN 16693:2015 (CEN) is a European Standard for the determination of selected organochlorine pesticides (OCP) in whole water samples using solid‑phase extraction (SPE) with SPE‑disks followed by gas chromatography–mass spectrometry (GC‑MS). The method is designed to analyse OCPs in surface water (including suspended particulate matter up to 500 mg/L), drinking water and groundwater without prior filtration, and supports compliance monitoring under EU water legislation.

Key topics and requirements

  • Analytes covered: The method targets a list of OCPs (Table 1) including DDT (and metabolites), HCH isomers (alpha, beta, gamma, delta), hexachlorobenzene (HCB), cyclodiene pesticides (aldrin, dieldrin, endrin, isodrin), alachlor, pentachlorobenzene, trichlorobenzenes and endosulfan isomers. It can be extended to other OCPs after verification.
  • Sampling & sample type: Whole water samples must not be filtered to retain particle‑bound pesticide fractions (handles SPM up to 500 mg/L).
  • Extraction: Solid‑phase extraction using SPE‑disks extracts dissolved and particle‑bound OCPs; an internal standard mixture is added prior to extraction.
  • Concentration & solvent: Extracts are concentrated by evaporation (nitrogen); acetone is recommended for extraction/elution. Avoid solvent drying steps on acetone and ensure effective disk drying to minimize residual water.
  • Chromatography & detection: Separation and quantification by capillary GC‑MS with electron‑impact (EI) ionization. Large volume injection or increased enrichment may be necessary for some compounds (e.g., endosulfan).
  • Performance criteria: Limits of quantification (LOQ) are compound- and matrix-dependent; for Table 1 compounds LOQ is at least 30% of the AA‑EQS, corresponding to approx. 0.00015 µg/L to 0.1 µg/L, meeting requirements for WFD monitoring.
  • Quality control: Pay attention to SPE‑disk batch variability, chromatographic interferences, blank controls, procedural recoveries and calibration (GC and total procedure).

Applications and users

Who uses EN 16693:2015:

  • Environmental and water analysis laboratories performing trace pesticide monitoring
  • Water utilities and public health labs testing drinking water and groundwater
  • Regulatory agencies and consultants implementing Water Framework Directive (WFD) monitoring programs
  • Research groups studying pesticide fate and particle‑bound contaminants

Practical applications:

  • Compliance testing against EQS values (Directive 2008/105/EC)
  • Whole water monitoring to capture both dissolved and particle‑associated OCP fractions
  • Method standardization for inter‑laboratory comparability in surveillance programs

Related standards and references

  • EN ISO 3696 - Water for analytical laboratory use
  • EN ISO 5667‑3 - Water sampling: preservation and handling
  • EU legislation referenced: Water Framework Directive (2000/60/EC), EQS Directive (2008/105/EC) and related monitoring requirements (Directive 2009/90/EC)

Keywords: EN 16693:2015, organochlorine pesticides, OCP, SPE‑disks, solid‑phase extraction, GC‑MS, whole water samples, water quality, EQS, WFD monitoring.

Frequently Asked Questions

SIST EN 16693:2015 is a standard published by the Slovenian Institute for Standardization (SIST). Its full title is "Water quality - Determination of organochlorine pesticides (OCP) in whole water samples using solid phase extraction (SPE) with SPE-disks combined with gas chromatography mass spectrometry (GC-MS)". This standard covers: This European Standard specifies a method for the determination of selected organochlorine pesticides (OCP, see Table 1), in water samples. The method uses solid-phase extraction with SPE-disks followed by gas chromatography-mass spectrometry (GC-MS). It is applicable to the analysis of OCPs in surface water containing suspended particulate matter (SPM) up to 500 mg/l (whole water samples), drinking water and groundwater. The lower limit of the working range depends on the matrix, on the specific compound to be analyzed and on the sensitivity of the mass spectrometric detection unit. For compounds listed in Table 1 the limit of determination (LOQ) it is at least 30 % of the corresponding AA-EQS value (0,000 15 µg/l to 0,1 µg/l) according to the requirements of the European EQS Directive 2008/105/EC for both inland surface waters and other surface waters. This method may be used for the analysis of other OCPs not listed in Table 1 or other types of water. However, it is necessary to verify its applicability before use. (...)

This European Standard specifies a method for the determination of selected organochlorine pesticides (OCP, see Table 1), in water samples. The method uses solid-phase extraction with SPE-disks followed by gas chromatography-mass spectrometry (GC-MS). It is applicable to the analysis of OCPs in surface water containing suspended particulate matter (SPM) up to 500 mg/l (whole water samples), drinking water and groundwater. The lower limit of the working range depends on the matrix, on the specific compound to be analyzed and on the sensitivity of the mass spectrometric detection unit. For compounds listed in Table 1 the limit of determination (LOQ) it is at least 30 % of the corresponding AA-EQS value (0,000 15 µg/l to 0,1 µg/l) according to the requirements of the European EQS Directive 2008/105/EC for both inland surface waters and other surface waters. This method may be used for the analysis of other OCPs not listed in Table 1 or other types of water. However, it is necessary to verify its applicability before use. (...)

SIST EN 16693:2015 is classified under the following ICS (International Classification for Standards) categories: 13.060.50 - Examination of water for chemical substances. The ICS classification helps identify the subject area and facilitates finding related standards.

SIST EN 16693:2015 is associated with the following European legislation: EU Directives/Regulations: 2000/60/EC, EUR-PUB; Standardization Mandates: M/424. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.

You can purchase SIST EN 16693:2015 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of SIST standards.

Standards Content (Sample)


2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Wasserbeschaffenheit - Bestimmung von Organochlorpestiziden (OCP) in Gesamtwasserproben mittels Festphasenextraktion (SPE) mit SPE-Scheiben in Verbindung mit Gaschromatographie-Massenspektrometrie (GC-MS)Qualité de l'eau - Dosage des pesticides organochlorés (POC) dans la totalité de l'échantillon d'eau par extraction en phase solide (EPS) avec disques EPS, avec couplage chromatographie en phase gazeuse-spectrométrie de masse (CG-SM)Water quality - Determination of organochlorine pesticides (OCP) in whole water samples using solid phase extraction (SPE) with SPE-disks combined with gas chromatography mass spectrometry (GC-MS)13.060.50VQRYLExamination of water for chemical substancesICS:Ta slovenski standard je istoveten z:EN 16693:2015SIST EN 16693:2015en,fr,de01-december-2015SIST EN 16693:2015SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16693
September
t r s w ICS
s uä r x rä w r English Version
Water quality æ Determination of organochlorine Qualité de l 5eau æ Dosage des pesticides organochlorés avec couplage chromatographie en phase gazeuseæ Wasserbeschaffenheit æ Bestimmung von SPEæDisks in Verbindung mit Gaschromatographie æ This European Standard was approved by CEN on
t y June
t r s wä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
t r s w CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x x { uã t r s w ESIST EN 16693:2015

Suitable gas chromatographic conditions and example chromatograms — GC-conditions of example chromatograms in Figure A.1 . 18 Annex B (informative)
Repeatability and reproducibility data . 23 Annex C (informative)
Examples of suitable SPE-disks . 27 Annex D (informative)
Examples of internal standards . 28 Bibliography . 29
g/mol
Alachlor C14H20ClNO2 269,77 240–110–8 15972–60–8 Cyclodiene pesticides: Aldrin
Dieldrin Endrin
Isodrin
C12H8Cl6 C12H8Cl6O C12H8Cl6O C12H8Cl6
364,91 380,91 380,91 364,91
206–215–8 200–484–5 200–775–7 207–366–2
309–00–2 60–57–1 72–20–8 465–73–6 DDT-total: op´-DDT
pp´-DDT
pp´-DDD
pp´-DDE
C14H9Cl5 C14H9Cl5 C14H9Cl4 C14H9Cl4
354,49 354,49 320,04 318,03
212–332–5 200–024–3 200–783–0 200–784–6
789–02–6 50–29–3 72–54–8 72–55–9 Hexachlorobenzene (HCB) C6Cl6 284,80 204–273–9 118–74–1 Hexachlorobutadiene (HCBD) C4Cl6 260,76 201–765–5 87–68–3 Hexachlorocyclohexane c: alpha-HCH
beta-HCH
delta-HCH
gamma-HCH
C6H6Cl6
C6H6Cl6 C6H6Cl6 C6H6Cl6
290,83 290,83 290,83 290,83
206–270–8 206–271–3 206–272–9 200–401–2
319–84–6 319–85–7 319–86–8 58–89–9 Pentachlorobenzene C6HCl5 250,34 210–172–0 608–93–5 Trichlorobenzene c: 1,2,3-TCB
1,2,4-TCB
1,3,5-TCB
C6H3Cl3 C6H3Cl3 C6H3Cl3
181,45 181,45 181,45
201–757–1 204–428–0 203–608–6
87–61–6 120–82–1 108–70–3 Endosulfan c: Endosulfan-I (alpha)
Endosulfan-II (beta)
C9H6Cl6O3S C9H6Cl6O3S
406,93 406,93
– –
959–98–8 33213–65–9 a EC Number: European inventory of existing commercial substances (EINECS) or European list of notified chemical substances
(ELINCS). b CAS RN: Chemical Abstracts Service Registry Number. c Mixture of isomers. SIST EN 16693:2015
...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.

Loading comments...