SIST-TS ISO/TS 16780:2018
Water quality - Determination of polychlorinated naphthalenes (PCN) - Method using gas chromatography (GC) and mass spectrometry (MS)
Water quality - Determination of polychlorinated naphthalenes (PCN) - Method using gas chromatography (GC) and mass spectrometry (MS)
ISO/TS 16780:2015 specifies a method for the determination of polychlorinated naphthalenes (PCNs), where "poly" means "mono" to "octa", in waters and waste waters [containing less than 2 g/l solid particulate material (SPM)] using high resolution gas chromatography?high resolution mass spectrometry (HRGC?HRMS).
NOTE 1 The congeners analysed by this method are listed in Table 1.
The working range of the method is 20 pg/l to 8 ng/l. The method is optimized for PCNs, but can be modified to include other coplanar compounds such as polychlorinated dioxins and furans (PCDDs/PCDFs) and dioxin-like tetra- to heptachlorinated biphenyls (dlPCBs). This method can be used to determine PCNs in other matrices (e.g. biota, sediments, air); however, additional clean-up steps and techniques can be necessary for samples with high organic loadings. Low resolution mass spectrometry (LRMS) and mass spectrometry?mass spectrometry (MS?MS) can be used.
NOTE 2 LRMS and MS?MS conditions are summarized in Annex A.
Both LRMS and MS?MS can be less selective than HRMS and there is a possibility of bias due to interfering compounds if these techniques are used.
The detection limits and quantification levels in this method are dependent on the level of interferences as well as instrumental limitations.
NOTE 3 The minimum levels (ML) in Table 4 are the levels at which the PCNs can typically be determined with no interferences present.
This method is performance based. The analyst is permitted to modify the method, e.g. to overcome interferences, provided that all performance criteria in this method are met.
NOTE 4 The requirements for establishing method validation or equivalency are given in Clause 9.
Qualité de l'eau - Détermination des naphtalènes polychlorés (PCN) - Méthode par chromatographie en phase gazeuse (CG) et spectrométrie de masse (SM)
Kakovost vode - Določevanje polikloriranih naftalenov (PCN) - Metoda plinske kromatografije (GC) in masne spektrometrije (MS)
Ta tehnična specifikacija določa metodo za določevanje polikloriranih naftalenov (PCN), pri čemer beseda »poli« pomeni vse od »mono« do »okta«, v vodah in odpadnih vodah [z vsebnostjo manj kot 2 g/l trdnih snovi z delci (SPM)] z uporabo visokoločljivostne plinske kromatografije – visokoločljivostne masne spektrometrije (HRGC – HRMS).
OPOMBA 1: Analogi, analizirani s to metodo, so navedeni v Tabeli 1.
Delovni razpon metode je od 20 pg/l do 8 ng/l. Metoda je optimizirana za poliklorirane naftalene, vendar jo je mogoče prilagoditi tako, da vključuje še druge koplanarne spojine, kot so poliklorirani dioksini in furani (PCDD/PCDF) ter dioksinom podobni tetra- do heptaklorirani bifenili (dIPCB). To metodo je mogoče uporabiti za določevanje polikloriranih naftalenov v drugih matricah (npr. živih organizmih, usedlinah, zraku); vendar so za vzorce z visoko organsko sestavo morda potrebni dodatni koraki in tehnike čiščenja. Uporabiti je mogoče nizkoločljivostno masno spektrometrijo (LRMS) in masno spektrometrijo – masno spektrometrijo (MS – MS).
OPOMBA 2: Pogoji nizkoločljivostne masne spektrometrije in masne spektrometrije – masne spektrometrije so povzeti v Dodatku A.
Postopka nizkoločljivostne masne spektrometrije in masne spektrometrije – masne spektrometrije sta lahko manj selektivna od postopka visokoločljivostne masne spektrometrije ter pri uporabi teh tehnik obstaja možnost pristranskosti zaradi motilnih spojin.
Mejne vrednosti zaznavanja in stopnje kvantifikacije v tej metodi so odvisne tako od ravni motenj
kot od instrumentalnih omejitev.
OPOMBA 3: Minimalne ravni (ML) v Tabeli 4 so ravni, pri katerih je poliklorirane naftalene običajno mogoče določiti brez prisotnosti motenj.
Ta metoda temelji na učinkovitosti. Analitik lahko prilagodi metodo, npr. za premagovanje motenj, če so izpolnjeni vsi kriteriji učinkovitosti v tej metodi.
OPOMBA 4: Zahteve za vzpostavitev preverjanja metode ali enakovrednosti so podane v točki 9.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2018
.DNRYRVWYRGH'RORþHYDQMHSROLNORULUDQLKQDIWDOHQRY 3&1 0HWRGDSOLQVNH
NURPDWRJUDILMH *& LQPDVQHVSHNWURPHWULMH 06
Water quality - Determination of polychlorinated naphthalenes (PCN) - Method using gas
chromatography (GC) and mass spectrometry (MS)
Qualité de l'eau - Détermination des naphtalènes polychlorés (PCN) - Méthode par
chromatographie en phase gazeuse (CG) et spectrométrie de masse (SM)
Ta slovenski standard je istoveten z: ISO/TS 16780:2015
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
TECHNICAL ISO/TS
SPECIFICATION 16780
First edition
2015-08-15
Water quality — Determination of
polychlorinated naphthalenes (PCN)
— Method using gas chromatography
(GC) and mass spectrometry (MS)
Qualité de l’eau — Détermination des naphtalènes polychlorés
(PCN) — Méthode par chromatographie en phase gazeuse (CG) et
spectrométrie de masse (SM)
Reference number
©
ISO 2015
© ISO 2015, Published in Switzerland
All rights reserved. Unless otherwise specified, 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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2015 – All rights reserved
Contents Page
Foreword .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions, and abbreviated terms . 2
3.1 Terms and definitions . 2
3.2 Abbreviated terms . 6
4 Principle . 6
4.1 Extraction . 6
4.2 Clean-up . 7
4.3 Identification and quantification . 7
4.4 Quality . 8
5 Contamination and interferences . 8
6 Reagents and standards .10
7 Apparatus and materials.16
8 Sample collection, preservation, storage and holding times .19
8.1 General .19
8.2 Storage times .19
9 Quality assurance and quality control .20
9.1 General .20
9.2 Spiking .20
9.3 Recovery of labelled compounds assessment .21
9.4 Method blanks .21
9.5 QC check sample .21
10 Calibration .21
10.1 Operating conditions .21
10.2 Mass spectrometer resolution .22
10.3 Ion abundance ratios, minimum levels, signal-to-noise ratios, and absolute
retention times .22
10.4 Retention time .22
10.5 Column resolution performance check .23
10.6 Calibration by isotope dilution .23
10.7 Calibration by internal standard .23
10.8 Combined calibration .24
10.8.1 General.24
10.8.2 Data storage .24
10.8.3 Data acquisition .24
10.8.4 Response factors and multipoint calibrations . .24
11 Sample preparation .25
11.1 General .25
11.2 Determination of solid particulate material .25
11.3 Preparation of aqueous samples containing 2 g/l of solid particulate material or less .25
11.3.1 General.25
11.3.2 Preparation of sample and QC aliquots .26
11.3.3 Filtration of particles . .26
12 Extraction .26
12.1 Separating funnel extraction of filtrates and of aqueous samples that are visibly
absent of particles .26
12.2 Solid phase extraction (SPE) of samples containing less than 2 g/l suspended
particlulate matter .27
12.2.1 Disk/cartridge preparation .27
12.2.2 Sample extraction .27
12.3 Soxhlet or PLE extraction of filters or disks .28
12.4 Macro-concentration .28
12.4.1 General.28
12.4.2 Rotary evaporation .28
12.4.3 Heating mantle .29
12.4.4 Kuderna-Danish (K-D) .29
12.5 Micro-concentration and solvent exchange .31
13 Extract clean-up.31
13.1 General .31
13.2 Back-extraction with acid and base .32
13.3 Gel permeation chromatography (GPC) .32
13.3.1 Column packing .32
13.3.2 Column calibration .32
13.3.3 Extract clean-up .33
13.4 Silica clean-up .33
13.5 Carbon column .34
13.6 Florisil clean-up .
...
TECHNICAL ISO/TS
SPECIFICATION 16780
First edition
2015-08-15
Water quality — Determination of
polychlorinated naphthalenes (PCN)
— Method using gas chromatography
(GC) and mass spectrometry (MS)
Qualité de l’eau — Détermination des naphtalènes polychlorés
(PCN) — Méthode par chromatographie en phase gazeuse (CG) et
spectrométrie de masse (SM)
Reference number
©
ISO 2015
© ISO 2015, Published in Switzerland
All rights reserved. Unless otherwise specified, 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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2015 – All rights reserved
Contents Page
Foreword .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions, and abbreviated terms . 2
3.1 Terms and definitions . 2
3.2 Abbreviated terms . 6
4 Principle . 6
4.1 Extraction . 6
4.2 Clean-up . 7
4.3 Identification and quantification . 7
4.4 Quality . 8
5 Contamination and interferences . 8
6 Reagents and standards .10
7 Apparatus and materials.16
8 Sample collection, preservation, storage and holding times .19
8.1 General .19
8.2 Storage times .19
9 Quality assurance and quality control .20
9.1 General .20
9.2 Spiking .20
9.3 Recovery of labelled compounds assessment .21
9.4 Method blanks .21
9.5 QC check sample .21
10 Calibration .21
10.1 Operating conditions .21
10.2 Mass spectrometer resolution .22
10.3 Ion abundance ratios, minimum levels, signal-to-noise ratios, and absolute
retention times .22
10.4 Retention time .22
10.5 Column resolution performance check .23
10.6 Calibration by isotope dilution .23
10.7 Calibration by internal standard .23
10.8 Combined calibration .24
10.8.1 General.24
10.8.2 Data storage .24
10.8.3 Data acquisition .24
10.8.4 Response factors and multipoint calibrations . .24
11 Sample preparation .25
11.1 General .25
11.2 Determination of solid particulate material .25
11.3 Preparation of aqueous samples containing 2 g/l of solid particulate material or less .25
11.3.1 General.25
11.3.2 Preparation of sample and QC aliquots .26
11.3.3 Filtration of particles . .26
12 Extraction .26
12.1 Separating funnel extraction of filtrates and of aqueous samples that are visibly
absent of particles .26
12.2 Solid phase extraction (SPE) of samples containing less than 2 g/l suspended
particlulate matter .27
12.2.1 Disk/cartridge preparation .27
12.2.2 Sample extraction .27
12.3 Soxhlet or PLE extraction of filters or disks .28
12.4 Macro-concentration .28
12.4.1 General.28
12.4.2 Rotary evaporation .28
12.4.3 Heating mantle .29
12.4.4 Kuderna-Danish (K-D) .29
12.5 Micro-concentration and solvent exchange .31
13 Extract clean-up.31
13.1 General .31
13.2 Back-extraction with acid and base .32
13.3 Gel permeation chromatography (GPC) .32
13.3.1 Column packing .32
13.3.2 Column calibration .32
13.3.3 Extract clean-up .33
13.4 Silica clean-up .33
13.5 Carbon column .34
13.6 Florisil clean-up .34
13.7 Silver nitrate–silica column .34
14 HRGC–HRMS analysis .35
14.1 General .35
14.2 MS resolution .35
14.3 Calibration verification .
...
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