1、BSI Standards PublicationBS ISO 17947:2014Fine ceramics (advancedceramics, advanced technicalceramics) Methods forchemical analysis of fine siliconnitride powdersBS ISO 17947:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 17947:2014.The UK participation i
2、n its preparation was entrusted to TechnicalCommittee RPI/13, Advanced technical ceramics.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for
3、 its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 78553 5ICS 81.060.30Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and
4、 Strategy Committee on 31 August 2014.Amendments issued since publicationDate Text affectedBS ISO 17947:2014 ISO 2014Fine ceramics (advanced ceramics, advanced technical ceramics) Methods for chemical analysis of fine silicon nitride powdersCramiques techniques Mthodes pour lanalyse chimique de poud
5、res de nitrure de siliciumINTERNATIONAL STANDARDISO17947First edition2014-09-01Reference numberISO 17947:2014(E)BS ISO 17947:2014ISO 17947:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be re
6、produced 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 ISOs member body in the country of the reques
7、ter.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 17947:2014ISO 17947:2014(E) ISO 2014 All rights reserved iiiContents PageForeword vIntroduction vi1 Scope . 12 Normative references
8、 13 Analytes and ranges 24 Preparation of test sample . 24.1 Sampling . 24.2 Drying . 24.3 Weighing . 25 Apparatus and reagents 26 Blank test 27 Determination of total silicon . 37.1 Classification of determination methods . 37.2 Fusion-dehydration/insolubilization separation-gravimetry and ICP-OES
9、. 37.3 XRF using fused cast-bead method . 58 Determination of total nitrogen . 58.1 Classification of determination methods . 58.2 Acid pressure decomposition-distillation separation-acidimetric titration method .58.3 Inert gas fusion-thermal conductivity method 108.4 Fusion-ammonia separation-acidi
10、metric titration method 139 Determination of aluminium, iron, and calcium 139.1 Principle . 139.2 Reagents. 139.3 Apparatus and instrument . 149.4 Procedure . 149.5 Blank test 159.6 Drawing calibration curve 159.7 Calculation .1510 Determination of oxygen 1610.1 Principle .1610.2 Reagents.1610.3 App
11、aratus .1610.4 Instrument .1610.5 Procedure .1610.6 Blank test 1610.7 Calculation of calibration coefficient 1610.8 Calculation . 1711 Determination of carbon .1711.1 Classification of determination methods 1711.2 Combustion (RF furnace)-IR absorption spectrometry .1711.3 Combustion (resistance furn
12、ace)-coulometry .2011.4 Combustion (resistance furnace)-gravimetry 2011.5 Combustion (resistance furnace)-conductometry 2012 Determination of fluorine and chlorine 2012.1 Principle . 2012.2 Reagents. 2012.3 Apparatus and instruments 2112.4 Procedure . 2112.5 Blank test 22BS ISO 17947:2014ISO 17947:2
13、014(E)iv ISO 2014 All rights reserved12.6 Drawing calibration curve 2212.7 Calculation . 2213 Reporting analytical values 2313.1 Number of analyses 2313.2 Evaluation of analytical values . 2313.3 Expression of analytical values 2314 Test report 24Annex A (informative) List of commercial certified re
14、ference materials .25Annex B (informative) Analytical results obtained from a round robin test .26Annex C (informative) Spectral lines for ICP-OES .31Bibliography .32BS ISO 17947:2014ISO 17947:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of nation
15、al 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. Internatio
16、nal 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
17、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.
18、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
19、be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents). Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressio
20、ns related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 206, Fine ceramics. ISO 2014 All rights res
21、erved vBS ISO 17947:2014ISO 17947:2014(E)IntroductionThis International Standard has been developed from Japanese Industrial Standard JIS R 1603:2007 with reference to CEN ENV 14226:2002 and ASTM C1494-01:2007, and is applicable to the chemical analysis of silicon nitride raw powders for fine cerami
22、cs use. This International Standard covers both major and minor constituents such as total silicon, total nitrogen, and some of trace metallic and non-metallic elements.vi ISO 2014 All rights reservedBS ISO 17947:2014Fine ceramics (advanced ceramics, advanced technical ceramics) Methods for chemical
23、 analysis of fine silicon nitride powders1 ScopeThis International Standard specifies the methods for the chemical analysis of fine silicon nitride powders used as the raw material for fine ceramics.This International Standard stipulates the determination methods of total silicon, total nitrogen, al
24、uminium, iron, calcium, oxygen, carbon, fluorine, and chlorine in fine silicon nitride powders.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited appli
25、es. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 2828, Aluminium oxide primarily used for the production of aluminium Determination of fluorine content Alizarin complexone and lanthanum chloride spectrophotometric methodISO 3696, Water
26、for analytical laboratory use Specification and test methodsISO 6353-1, Reagents for chemical analysis Part 1: General test methodsISO 6353-2, Reagents for chemical analysis Part 2: Specifications First seriesISO 6353-3, Reagents for chemical analysis Part 3: Specifications Second seriesISO 8656-1,
27、Refractory products Sampling of raw materials and unshaped products Part 1: Sampling schemeISO 21068-2, Chemical analysis of silicon-carbide-containing raw materials and refractory products Part 2: Determination of loss on ignition, total carbon, free carbon and silicon carbide, total and free silic
28、a and total and free siliconISO 21068-3, Chemical analysis of silicon-carbide-containing raw materials and refractory products Part 3: Determination of nitrogen, oxygen and metallic and oxidic constituentsISO 21438-2, Workplace atmospheres Determination of inorganic acids by ion chromatography Part
29、2: Volatile acids, except hydrofluoric acid (hydrochloric acid, hydrobromic acid and nitric acid)ISO 21438-3, Workplace atmospheres Determination of inorganic acids by ion chromatography Part 3: Hydrofluoric acid and particulate fluoridesISO 26845, Chemical analysis of refractories General requireme
30、nts for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methodsEN 12698-1, Chemical analysis of nitride bonded silicon carbide refractories - Part 1: Chemical methodsEN 12698-2, Chemical analysis of nitride bonded sili
31、con carbide refractories - Part 2: XRD methodsINTERNATIONAL STANDARD ISO 17947:2014(E) ISO 2014 All rights reserved 1BS ISO 17947:2014ISO 17947:2014(E)3 Analytes and rangesAnalytes and ranges specified in this International Standard shall be as follows.a) Total silicon (T. Si), range of 30 % to 70 %
32、 (mass fraction)b) Total nitrogen (T. N), range of 30 % to 45 % (mass fraction)c) Aluminium (Al), range of 0,001 % to 0,6 % (mass fraction)d) Iron (Fe), range of 0,001 % to 0,6 % (mass fraction)e) Calcium (Ca), range of 0,001 % to 0,03 % (mass fraction)f) Oxygen (O), range of 0,05 % to 5 % (mass fra
33、ction)g) Carbon (C), range of 0,01 % to 6 % (mass fraction)h) Fluorine (F), range of 0,001 % to 0,2 % (mass fraction)i) Chlorine (Cl), range of 0,001 % to 0,2 % (mass fraction)4 Preparation of test sampleThe method of preparing samples shall be in accordance with ISO 8656-1 unless otherwise mutually
34、 agreed upon between the analyser and the customer.4.1 SamplingTake the sample in accordance with ISO 8656-1.4.2 DryingTake about 10 g of the sample into a flat-type weighing bottle (60 mm 30 mm) and spread it uniformly over the bottom of the bottle. Place the bottle in an air bath at 110 C 5 C for
35、2 h without a lid, and then cool in a desiccator (desiccant: magnesium perchlorate for drying) with a lid for 1 h.4.3 WeighingWeigh the sample of the required quantity to the nearest 0,1 mg using a balance.5 Apparatus and reagentsUnless otherwise specified in each determination, use ordinary laborat
36、ory apparatus for chemical analysis listed in ISO 26845, Clause 4, as necessary. Reagents should conform to the requirements of ISO 6353-1, ISO 6353-2, and ISO 6353-3, as appropriate. Unless otherwise specified in each determination, use corresponding reagents of analytical grade listed in ISO 26845
37、, Clause 5, as necessary.6 Blank testBlank test shall be carried out by using identical quantities of reagents, conditions, and procedures throughout each determination to correct the analytical values obtained.2 ISO 2014 All rights reservedBS ISO 17947:2014ISO 17947:2014(E)7 Determination of total
38、silicon7.1 Classification of determination methodsTotal silicon shall be determined by either of the following methods. If analytical results with four figures are required, use the method A. If analytical results with two or three figures are required, the method B can be used. Method A: Fusiondehy
39、dration/insolubilization separationgravimetry and ICP-OES Method B: XRF using fused cast-bead method7.2 Fusion-dehydration/insolubilization separation-gravimetry and ICP-OES7.2.1 PrincipleA sample is fused with alkaline carbonate and the melt is treated with an acid to separate into two parts of sil
40、icon, insoluble silicon and soluble silicon, by filtration. Insoluble silicon is determined using gravimetry as silicon dioxide converted after ignition, whereas soluble silicon in the filtrate is determined using ICP-OES. The sum of them represents the total silicon.7.2.2 ReagentsReagents of analyt
41、ical grade shall be used. Reagent solutions shall be preserved in plastic bottles.7.2.2.1 Water, of grade 1 or superior specified in ISO 3696.7.2.2.2 Sodium carbonate, anhydrous, specified in ISO 6353-3 or that of higher grade.7.2.2.3 Hydrochloric acid (1+1), (1+4), (1+50), prepared by diluting hydr
42、ochloric acid with water, respectively.7.2.2.4 Sulfuric acid (1+1), (1+4), prepared by diluting sulfuric acid with water, respectively.7.2.2.5 Cellulose powder.7.2.2.6 Polyethylene oxide solution 0,05 % (m/V), prepared by dissolving polyethylene oxide with water.7.2.2.7 Hydrofluoric acid, concentrat
43、ion of 48 %.7.2.3 Apparatus and instrumentsUse ordinary laboratory apparatus and instruments for chemical analysis in accordance with ISO 26845, Clause 4.7.2.3.1 Platinum dish.7.2.3.2 Platinum crucible.7.2.3.3 Burner, capable of heating at 1 100 C.7.2.3.4 Muffle furnace, capable of being operated at
44、 1 100 C. ISO 2014 All rights reserved 3BS ISO 17947:2014ISO 17947:2014(E)7.2.3.5 Balance, readable to 0,1 mg.7.2.3.6 Inductively coupled plasma optical emission spectrometer (ICP-OES).7.2.4 ProcedureThe procedure shall be as follows. The procedure described in ISO 21068-2, Clause 8 can be alternati
45、vely used.7.2.4.1 Fusion of sampleWeigh 0,30 g of the sample and 2,0 g of sodium carbonate, anhydrous into a platinum dish and mix well. Start to heat carefully and increase the temperature gradually to 1 000 C to completely fuse the sample using a burner or in a muffle furnace.7.2.4.2 Separation of
46、 siliconAdd 20 ml of hydrochloric acid (1+1) to dissolve the melt on a hot plate. Silicon dioxide will appear to be jellified and precipitated at this stage. There are two methods to separate the precipitated silicon dioxide.a) Dehydrate carefully the precipitate to dryness in order to prevent it fr
47、om spattering and add 5 ml of hydrochloric acid and 20 ml of water to dissolve any salt mixed with the precipitate. Filtrate the precipitate with a filter paper and wash with hot hydrochloric acid (1+50) several times and then with hot water sufficiently until it contains no salt. Receive the filtra
48、te and washings together in a volumetric flask and make constant volume. Preserve this precipitate for gravimetry of insoluble silicon and the solution for the ICP-OES determination of soluble silicon, respectively.b) After eduction of jellified silicon dioxide, add 0,05 g of cellulose powder and 10
49、 ml of polyethylene oxide solution to agglomerate silicon dioxide for easy filtration. Filtrate and wash in the same procedure, and then preserve this precipitate for gravimetry of insoluble silicon and the solution for the ICP-OES determination of soluble silicon, respectively.7.2.4.3 Gravimetry for insoluble siliconTransfer the precipitate embedded in the filter paper together into a platinum crucible and ignite at 1 100 C after charring and ashing the paper. Weigh the crucible. Moisten the preci
