BS ISO BRITISH STANDARD 17858:2007 Water quality Determination of dioxin-like polychlorinated biphenyls Method using gas chromatography/mass spectrometry ICS 13.060.50 BSi NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW British Standards BSIS017858:2007 National foreword This British Standard was published by BSI. It is the UK implementation of ISO 17858:2007. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality,to Subcommittee EH/3/2,Physical chemical and biochemical methods. A list of organizations represented on EH/3/2 can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was Amendmentsissuedsincepublication published underthe authority of the Standards Policy and Amd. No. Date Comments Strategy Committee on 30 March 2007 BSI 2007 ISBN 9780580503207 BSISO17858:2007 ISO INTERNATIONAL STANDARD 17858 First edition 2007-02-15 Water quality Determination of dioxin- like polychlorinated biphenyls Method using gas chromatography/mass spectrometry Qualite de I'eau-Dosage des biphenyls polychlorés de type dioxineMethodeparchromatographieenphase gazeuse/spectrometrie de masse Reference number ISO17858:2007(E) ii BS ISO 17858:2007 Contents Page Foreword vi Introduction vii 1 Scope... 2 Normativereferences. 3 Terms,definitionsandabbreviatedterms 3.1 Terms and definitions.... 3.2 Abbreviated terms.... 4 Principle......... 4.1 Spiking and extraction... 4.2 Clean-up.... 4.3 Concentration... 4.4 Identification.... 4.5 Quantification.... 4.6 Analytical quality .... 5 Contaminationand interferences... 5 6 Reagents and standards... 6 7 Apparatus and materials.. 10 7.1 Sampling equipment for discrete sampling .... 7.2 Equipment for sample preparation.... 7.3 Extraction apparatus .... 7.4 Filtration apparatus ... 7.5 Clean-up apparatus .. 7.6 Concentrationapparatus. 7.7 Other equipment.... 8 Sample collection, preservation, storage and holding times .... 4 9 Quality assurance (QA)/quality control (QC)... 9.1 Genera...... 9.2 Initial precision and recovery (IPR). 15 9.3 Spiking..... 15 9.4 Recovery of labelled compounds assessment.... 9.5 Method blanks.... 16 9.6 Qc check sample.... 16 9.7 Method precision ... 10 Calibration... 10.1 Operating conditions... 10.2 Mass spectrometer(MS)resolution. 10.3 lonabundanceratios,minimum levels,signal-to-noise ratios,andabsoluteretention times... 10.4 Retention time . 10.5 18 10.6 Calibration by isotope dilution... 18 10.7 Calibration by internal standard.. 19 10.8 Combined calibration.. 11 Sample preparation 20 11.1 General.. 20 ili BSISO17858:2007 11.2 Determination of percentsuspended solids. .20 11.3 Preparation ofaqueous samplescontaining1%of suspended solidsor less ... 21 12 Extractionandconcentration... 22 12.1 Separatoryfunnel extraction offiltratesand of aqueous samples that are visiblyabsent of particles... 12.2 Solid-phase extraction (SPE)of samples containing less than 1%suspended solids 12.3 Soxhlet extraction of filters and/or disks ..... 12.4 Back.extraction with acid and base.... 12.5 Macro-concentration..... .24 12.6 Micro-concentration and solvent exchange.... 26 13 Extract clean-up... .26 13.1 General....... 13.2 Gel permeation chromatography (GPC.... 13.3 Silica clean-up...... 13.4 Alumina clean-up ... .28 13.5 Carbon column.... 29 13.6 High performance liquid chromatography (HPLC).... ..29 13.7 Florisil clean.up....... 13.8 Silver nitrate/silica column..... 14 HRGC/HRMS analysis..... ..31 15 System and laboratory performance .... .31 15.1 General 31 15.2 MS resolution... 31 15.3 Calibration verification ... ..31 15.4 Gc resolution.... 15.5 16 Qualitative determination.... .32 17 Quantitative determination... .32 17.1 Isotope dilutionquantification... 17.2 Internal standard quantificatio