ISO INTERNATIONAL STANDARD 18635 Firstedition 2016-04-01 Water quality Determination of short-chain polychlorinated alkanes (SCCPs) in sediment, sewage sludge and suspended (particulate) matter Method using gas chromatography-mass spectrometry (GC-MS) and electron capture negative ionization (ECNI) Qualité deI'eau-Déterminationdes alcanes polychlorés a chaine courte dans les sédiments et matieres en supsension (particules) Méthode par chromatographie en phase gazeuse-spectrométrie de masse (CPG-SM) et ionisation chimique négative (ICN) Reference number IS0 18635:2016(E) ISO International Organization for Standardization @ IS0 2016 STANDARDIZATIONC15956617 sefrom IHS IS0 18635:2016(E) COPYRIGHTPROTECTEDDOCUMENT IS0 2016, 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 copyrightoffice Ch. de Blandonnet 8 . CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 [email protected] www.iso.org Internatinair PrganizationforStandardization ensee-ZHEJIANG INST.OF STANDARDIzARoISQ16- All rights reserved etworking permitted without license from IHS IS0 18635:2016(E) Contents Page Foreword ..iv Introduction ..V 1 Scope. .1 2 Normative references 3 Principle ..1 4 Interferences ..2 5 Reagents ..3 6 Apparatus .6 7 Sampling and sample pretreatment .7 8 Procedure .7 8.1 Extraction .7 8.2 Extract clean-up .7 8.3 Measurement and integration of the chromatogram .8 8.4 Calibration .8 8.4.1 General. .8 8.4.2 Basic calibration .9 8.4.3 Identification and quantification with mass fragment combinations .10 8.4.4 Calculation of the results .10 8.4.5 Quality checks for internal standardization. 11 9 Expression of results ..11 10 Test report ..11 Annex A (normative) Programme for pressurized liquid extraction ..12 Annex B (informative) Explanation of the calibration of the sum of ScCPs with multiple linearregression ..13 Annex C (informative) Examples of typical GC-MS conditions ..18 Annex D (normative) Alternative clean-up with column chromatography ..22 Annex E (informative) Alternative clean-up with gel chromatography .24 Annex F (informative) Typical chromatograms of standard solutions 1 μg/ml .25 Annex G (informative) Presentation of goodness of fit of the calibration ..26 Annex H (informative) Example for recoveries of quality assurance solutions ..27 Annex I (informative) Chromatograms of real samples ..29 Annex J (informative) Performance data .31 Annex K (informative) Quality control check solutions .32 Bibliography ..33 iii HEJIANG INST OF STANDARDIZATION C15956617 thout license from IHS