ISO INTERNATIONAL STANDARD 17947 First edition 2014-09-01 Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of fine silicon nitride powders Céramiques techniques - Methodes pour I'analyse chimique de poudres de nitrure de silicium Reference number ISO 17947:2014(E) LSO @ IS0 2014 I without license from IHS Not for Resale IS0 17947:2014(E) COPYRIGHTPROTECTEDDOCUMENT @ ISO 2014 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 Case postale 56:CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyright@iso.org Web www.iso.org Published in Switzerland @ IS0 2014 - All rights reserved No reproductic networking permited without license from IHS Not for Resale IS0 17947:2014(E) Contents Page Foreword ..V Introduction. ...vi 1 Scope 2 Normative references 3 Analytes and ranges. 4 Preparation of test sample ..2 4.1 Sampling. .2 4.2 Drying.... 4.3 Weighing. ..2 5 Apparatus and reagents .2 6 Blanktest .2 7 Determination of total silicon .3 7.1 Classification of determination methods .3 7.2 Fusion-dehydration/insolubilization separation-gravimetry and ICP-OES .3 7.3 XRF using fused cast-bead method 8 Determination of total nitrogen .5 8.1 Classification of determination methods. .5 8.2 Acid pressure decomposition-distillation separation-acidimetric titration method 8.3 Inert gas fusion-thermal conductivity method .10 8.4 Fusion-ammonia separation-acidimetric titration method .13 9 Determination of aluminium, iron, and calcium .13 9.1 Principle ..13 9.2 Reagents. ..13 9.3 Apparatus and instrument. ..14 9.4 Procedure ..14 9.5 Blank test .15 9.6 Drawing calibration curve .15 9.7 Calculation .15 10 Determination of oxygen .16 10.1 Principle. .16 10.2 Reagents... .16 10.3 Apparatus .16 10.4 Instrument. .16 10.5 Procedure .16 10.6 Blanktest .16 10.7 Calculation of calibration coefficient ..16 10.8 Calculation ..17 11 Determination of carbon. ..17 11.1 Classification of determination methods. ..17 11.2 Combustion (RF furnace)-IR absorption spectrometry .17 11.3 Combustion (resistance furnace)-coulometry 20 11.4 Combustion (resistance furnace)-gravimetry 20 11.5 Combustion (resistance furnace)-conductometry 20 12 Determination of fluorine and chlorine .20 12.1 Principle. 20 12.2 Reagents. 20 12.3 Apparatus and instruments. .21 12.4 Procedure 21 12.5 Blank test. .22 iii ted without license from IHS Not for Resale