ISO INTERNATIONAL STANDARD 17280 First edition 2015-05-15 Surface active agents Determination of 1,4-dioxan residues in surfactants obtained from epoxyethane by gas chromatography Agents de surface-Détermination de la teneur en residus de 1,4-dioxane dans les agents tensioactifs obtenus a partir d'epoxyethane par chromatographie en phase gazeuse Reference number IS0 17280:2015(E) SO International Organization for Standardization @ IS0 2015 ed without license from IHS IS0 17280:2015(E) COPYRIGHTPROTECTEDDOCUMENT IS0 2015, Published in Switzerland All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form written permission. Permission can be requested from either ISO at the address below or ISO's member body in the country of the requester. IsOcopyrightoffice Ch. de Blandonnet 8 . CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +4122 749 09 47 [email protected] www.iso.org Not for Resale, 2015/8/7 03:29:43 networking permitted without license from IHS IS0 17280:2015(E) Contents Page Foreword ..iv 1 Scope 2 Normative references ..1 3 Principle. 4 Reagents 4.1 1,4-Dioxane, purity 99,5 % minimum. ..1 4.2 4-Methyl-1,3-dioxane, purity 98 % minimum. 4.3 N, N-dimethylformamide (DMF) .1 4.4 Carrier gas: nitrogen or helium, purity 99,99 % minimum. 2 Apparatus ..2 5.1 Analytical balance, O,1 mg readability. 2 5.2 Gas chromatography system, attached with temperature programmed device and flame ionization detector (FID). ..2 5.3 Head space sampling unit. ..2 5.4 20 ml crimped top glass vials, sealing pliers and sealing clamp suitable for head space unit. .2 5.5 Septum and crimped tops, lined with aluminium or PTFE, for closing the vials. .2 5.6 .2 Sealing pliers, for the vials. 5.7 Capillary column, capable of the separation characteristics shown in Figure 2 5.8 Volumetric flasks, 50 ml and 100 ml capacity. 2 5.9 Gas tight syringes or glass pipettes, 1 ml ± 0,01 ml capacity. .2 Preparation of calibration solutions .2 6 6.1 Calibration solution A 2 6.2 Calibration solution B 3 7 Procedure .3 7.1 Preparation of the test sample 3 7.2 Standard addition procedure ..3 7.2.1 Preparation of test sample solutions 3 7.2.2 Determination. .4 7.2.3 Expression of results. .4 7.3 Relative response factor procedure 4 7.3.1 Determination of relative response factor .4 7.3.2 Preparation of test sample solutions. .5 7.3.3 Determination. 7.3.4 Expression of results. .5 8 Chromatographic conditions. ..5 9 Evaluation ..6 9.1 General ..6 9.2 Identification 7 9.3 Calculation 7 10 Precision 10.1 Repeatability limit. 7 10.2 Reproducibility limit 7 11 Test report. .1 Annex A (informative) Statistical data from the ring carried out. iii Isee=Zhejang Insttute of Standardization 5956617 ed without license from IHS Not for Resale, 2015/8/7 03:29:43