ISO/TR TECHNICAL REPORT 19716 First edition 2016-05-01 Nanotechnologies Characterization of cellulose nanocrvstals Nanotechnologies - Caractérisation des nanocristaux de cellulose Reference number IS0/TR 19716:2016(E) ISO International Organization for Standardization See=ZHEJIANG INST OF STANDARDIZATION C1 5956617 @IS02016 vided by IHS under I No reproduction or networking permitted without license from IHS IS0/TR 19716:2016(E) COPYRIGHT PROTECTEDDOCUMENT 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 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 [email protected] www.iso.org Licensee-ZHEJIANG INST OF STANDARDIZAISQ 0d6 - All rights reserved Not for Resale, 2016/7/20 08:20:05 networking permited without license from IHS IS0/TR 19716:2016(E) Contents Page Foreword ..iv Introduction. ..V 1 Scope. ..1 2 Terms and definitions 3 Symbols and abbreviated terms 4 Production of cellulose nanocrystals (CNCs) 5 Composition ..6 5.1 Chemical composition .6 5.2 Surface functional groups. ..7 5.2.1 Determination of sulfate half-esters .7 5.2.2 Determination of carboxylic acids 11 5.3 Degree of polymerization. .12 5.4 Crystallinity .13 5.4.1 General. .13 5.4.2 X-ray diffraction. .14 5.4.3 Nuciear magnetic resonance .16 5.4.4 Vibrational spectroscopy ..18 5.4.5 Crystallinity measurements for CNCs .18 5.5 Moisture content. 20 5.6 Contaminants. 20 5.6.1 General. 20 5.6.2 Residual impurities derived from cellulosic biomass 21 5.6.3 Metalions 21 5.6.4 Detection of contaminants by X-ray photoelectron spectroscopy 21 6 CNC Morphology. .22 6.1 Distributions of length and cross-section from microscopy 22 6.1.1 General 22 6.1.2 Electron microscopy 23 6.1.3 Atomic force microscopy 25 6.1.4 Image analysis considerations. 27 6.1.5 Microscopy size distributions for CNCs 27 6.2 Size measurement by dynamic light scattering (DLS) 31 7 CNC Surface characteristics .33 7.1 Specific surface area. 33 7.2 Surface charge .34 8 Miscellaneous ..35 8.1 Thermal properties. 35 8.2 Viscosity. ..38 9 Concluding comments. ..38 Bibliography .40 ii icensee=ZHEJIANG INST OF STANDARDIZATION C1 5956617 ed without license from IHS IS0/TR 19716:2016(E) Foreword Iso (the International Organization for Standardization) is a worldwide federation of national standards bodies (IsO member bodies). The work of preparing International Standards is normally carried out through IsO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with Iso, also take part in the work ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. The procedures used to develop this document and those intended for its further maintenance are described in the Iso/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of IsO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives). Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. IsO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the Iso list of patent declarations received (see www.iso.org