1、BSI Standards PublicationBS ISO 17942:2014Fine ceramics (advancedceramics, advanced technicalceramics) Methods forchemical analysis of boronnitride powdersBS ISO 17942:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 17942:2014.The UK participation in its p
2、reparation 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 its co
3、rrectapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 78551 1ICS 81.060.30Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strate
4、gy Committee on 31 August 2014.Amendments issued since publicationDate Text affectedBS ISO 17942:2014 ISO 2014Fine ceramics (advanced ceramics, advanced technical ceramics) Methods for chemical analysis of boron nitride powdersCramiques techniques Mthodes pour lanalyse chimique de poudres de nitrure
5、 de boreINTERNATIONAL STANDARDISO17942First edition2014-08-15Reference numberISO 17942:2014(E)BS ISO 17942:2014ISO 17942:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utiliz
6、ed 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 requester.ISO copyright
7、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 17942:2014ISO 17942:2014(E) ISO 2014 All rights reserved iiiContents PageForeword vIntroduction vi1 Scope . 12 Normative references 13 General rules
8、in chemical analysis 14 Analysis items 15 Sampling, weighing, and drying of sample 25.1 Sampling . 25.2 Weighing . 25.3 Drying . 26 Reporting analytical values . 36.1 Number of analyses. 36.2 Blank test . 36.3 Evaluation of analytical values 36.4 Expression of analytical values . 37 Determination me
9、thods of total boron . 37.1 Classification of determination methods . 37.2 Fusion-acidimetric titration method . 47.3 Fusion-ICP-OES . 68 Determination methods of free boron . 88.1 Classification of determination methods . 88.2 Sulfuric acid digestion-ICP-OES and spectrophotometry 98.3 Nitric acid d
10、igestion-ICP-OES 118.4 Methanol extraction-borate separation-ICP-OES and spectrophotometry .129 Determination methods of total nitrogen .169.1 Classification of determination methods 169.2 Acid pressure decomposition-distillation separation-acidimetric titration method 179.3 Fusion-ammonia separatio
11、n-acidimetric titration method 229.4 Inert gas fusion-thermal conductivity method 2210 Determination method of silicon .2610.1 Determination method2610.2 Principle .2610.3 Reagents.2610.4 Apparatus and instrument . 2710.5 Amount of sample . 2710.6 Operation 2710.7 Blank test 2710.8 Drawing calibrati
12、on curves . 2710.9 Calculation . 2811 Determination methods of aluminium, cadmium, calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, nickel, titanium, vanadium, and zinc .2811.1 Classification of determination methods 2811.2 Acid pressure decomposition-ICP-OES . 2811.3 Fusion-ICP-
13、OES 3112 Determination methods of sodium and potassium .3412.1 Classification of determination methods 3412.2 Acid pressure decomposition-AAS 3512.3 Acid pressure decomposition-FES 3712.4 Acid pressure decomposition-ICP-OES . 39BS ISO 17942:2014ISO 17942:2014(E)iv ISO 2014 All rights reserved13 Dete
14、rmination methods of carbon .4113.1 Classification of determination methods 4113.2 Combustion (resistance furnace)-IR absorption spectrometry 4213.3 Combustion (RF furnace)-conductometry . 4513.4 Combustion (RF furnace)-IR absorption spectrometry .4713.5 Combustion (resistance furnace)-coulometry .4
15、913.6 Combustion (resistance furnace)-gravimetry 4913.7 Combustion (resistance furnace)-conductometry 4914 Determination method of Oxygen .4914.1 Determination method 4914.2 Inert gas fusion-IR absorption spectrometry 4915 Test report 52Annex A (informative) List of commercial certified reference ma
16、terials .53Annex B (informative) Analytical results obtained from a round robin test .54Annex C (informative) Spectral lines for ICP-OES .58Bibliography .59BS ISO 17942:2014ISO 17942:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standar
17、ds 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 organi
18、zations, 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 fu
19、rther 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/direct
20、ives).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 I
21、ntroduction 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 expressions related t
22、o 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 information.The committee responsible for this document is ISO/TC 206, Fine ceramics. ISO 2014 All rights reserved vBS I
23、SO 17942:2014ISO 17942:2014(E)IntroductionThis International Standard describes the chemical analysis of boron nitride powders for use in fine ceramics applications. Determination methods of both main and trace constituents of interest are fully covered.vi ISO 2014 All rights reservedBS ISO 17942:20
24、14Fine ceramics (advanced ceramics, advanced technical ceramics) Methods for chemical analysis of boron nitride powders1 ScopeThis International Standard specifies the methods for the chemical analysis of fine boron nitride powders used as the raw material for fine ceramics.This International Standa
25、rd stipulates the analysis methods of total boron, free boron, total nitrogen, aluminium, cadmium, calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, nickel, potassium, silicon, sodium, titanium, vanadium, zinc, carbon, and oxygen in boron nitride powders for fine ceramics. Total b
26、oron is determined by using either a fusiontitration method or a fusioninductively coupled plasma-optical emission spectrometry (ICP-OES). Free boron is determined by using either an acid digestionICP-OES or a methanol extractionICP-OES. If necessary, the boron amount which arises from the hydrolysi
27、s of boron nitride during sample treatment is corrected using spectrophotometry. Total nitrogen is determined by using either an acid pressure decompositiondistillation separationtitration method or an inert gas fusionthermal conductivity method. Silicon is determined by using a fusionICP-OES. Alumi
28、nium, cadmium, calcium, chromium, cobalt, copper, iron, lead, magnesium, manganese, nickel, titanium, vanadium, zinc are determined by using an acid pressure decompositionICP-OES or a fusionICP-OES. Sodium and potassium are determined by using atomic absorption spectrometry (AAS), flame emission spe
29、ctrometry (FES), or ICP-OES following acid pressure decomposition. Carbon is determined by using a combustionIR absorption spectrometry or a combustionthermal conductivity method. Oxygen is determined by using an inert gas fusionIR absorption spectrometry.2 Normative referencesThe following document
30、s, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.EN 12698-1:2007, Chemical anal
31、ysis of nitride bonded silicon carbide refractories - Part 1: Chemical methodsISO 3696, Water for analytical laboratory use Specification and test methodsISO 6353-3, Reagents for chemical analysis Part 3: Specifications Second seriesISO 9138, Abrasive grains Sampling and splittingISO 21068-2:2008, C
32、hemical 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 silica and total and free silicon3 General rules in chemical analysisChemical analysis shall be performed in a
33、ccordance with general rules regulated as standards, if available.4 Analysis itemsAnalysis items specified in this International Standard shall be as follows:a) Total boron (T.B)INTERNATIONAL STANDARD ISO 17942:2014(E) ISO 2014 All rights reserved 1BS ISO 17942:2014ISO 17942:2014(E)b) Free boron (F.
34、B)c) Total nitrogen (T.N)d) Silicon (Si)e) Aluminium (Al)f) Cadmium (Cd)g) Calcium (Ca)h) Chromium (Cr)i) Cobalt (Co)j) Copper (Cu)k) Iron (Fe)l) Lead (Pb)m) Magnesium (Mg)n) Manganese (Mn)o) Nickel (Ni)p) Titanium (Ti)q) Vanadium (V)r) Zinc (Zn)s) Sodium (Na)t) Potassium (K)u) Carbon (C)v) Oxygen (
35、O)5 Sampling, weighing, and drying of sampleThe method of preparing samples shall be in accordance with ISO 9138 unless otherwise mutually agreed upon between the analyser and customer.5.1 SamplingTake the sample in accordance with ISO 9138.5.2 WeighingWeigh the sample of the required quantity to th
36、e nearest 0,1 mg using an electric balance.5.3 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 (120 5) C for 2 h without a lid, and then cool in a desiccator (desiccant: magne
37、sium perchlorate for drying) with a lid for 1 h.2 ISO 2014 All rights reservedBS ISO 17942:2014ISO 17942:2014(E)6 Reporting analytical values6.1 Number of analysesAnalyse the sample twice on different days.6.2 Blank testUpon analysis, perform a blank test to correct the measured values.6.3 Evaluatio
38、n of analytical valuesa) When the difference between two analytical values does not exceed the tolerance shown in Table 1, the average value shall be reported.b) When the difference between two analytical values exceeds the tolerance shown in Table 1, perform additional two analyses. When the differ
39、ence does not exceed the tolerance, the average value thereof shall be reported. If the difference also exceeds the tolerance, the median of four analytical values shall be reported.6.4 Expression of analytical valuesThe analytical values shall be given in % (mass fraction) in dryness.a) Total boron
40、 and total nitrogen express the results with two to four figures according to the method used.b) Free boron express the results with two to four figures according to the method used.c) Others express the results to the third decimal place.Table 1 Tolerance on analytical valuesUnit: % (mass fraction)
41、Component total-B free-B total-N Si, Al, Cd, Ca, Cr, Co, Cu, Fe, Pb, Mg, Mn, Ni, Ti, V, Zn,K, NaC OTolerance 0,30 0,30a0,40b0,001c0,005d0.005 0,01e0,05faAcid pressure decompositiondistillation separationacidimetric titration method.bInert gas fusionthermal conductivity method.cApplicable to the cont
42、ent of less than 0,01 % (mass fraction).dApplicable to the content of not less than 0,01 % (mass fraction).eApplicable to the content of less than 1,0 % (mass fraction).fApplicable to the content of not less than 1,0 % (mass fraction).7 Determination methods of total boron7.1 Classification of deter
43、mination methodsTotal boron shall be determined by either of the following methods. If analytical results with three or four figures are required, use method A; whereas if two figures are required, method B can be used. Method A, fusionacidimetric titration method ISO 2014 All rights reserved 3BS IS
44、O 17942:2014ISO 17942:2014(E) Method B, fusionICP-OES7.2 Fusion-acidimetric titration method7.2.1 PrincipleFuse the sample with sodium carbonate and dissolve the melt in hydrochloric acid. Adjust the solution to pH 6,4 after removal of carbon dioxide. Add mannitol, and then titrate with sodium hydro
45、xide solution to pH 6,4.This method shall be used to obtain the results of three or four figures.7.2.2 ReagentsReagents of analytical grade shall be used. Reagent solutions shall be preserved in plastic bottles (products made of polyethylene, polypropylene, and tetrafluoroethylene resin are availabl
46、e.). The standard solutions being SI traceable shall be used.7.2.2.1 Water, Grade 1 or superior as specified in ISO 3696.7.2.2.2 Sodium carbonate, anhydrous, as specified in ISO 6353-3 or that of higher grade.7.2.2.3 Hydrochloric acid (1+1), (1+50), prepare from hydrochloric acid, respectively.7.2.2
47、.4 Sodium hydroxide, more than 97,0 % (mass fraction) of purity.7.2.2.5 Sodium hydroxide solution (200 g/l), (40 g/l), (20 g/l), prepare from sodium hydroxide, respectively.7.2.2.6 Ethanol (95).7.2.2.7 EthanolSodium hydroxide (1+1) mixed solution, prepare by mixing the same volume of ethanol (95) an
48、d a sodium hydroxide solution (200 g/l).7.2.2.8 Mannitol.7.2.2.9 Boric acid, more than 99,5 % (mass fraction) of purity.7.2.2.10 Standard boron solution, weigh 1 g of boric acid (7.2.2.9) in a platinum crucible (for example, 30 ml) and heat it initially at a low temperature and finally at about 1 10
49、0 C. After cooling in a desiccator, weigh the mass of boric oxide as B2O3. Take the product into a 200 ml beaker together with the crucible and add 100 ml of hot water. Heat and dissolve it. After cooling, transfer the solution into a 200 ml volumetric flask and dilute with water to the mark.7.2.2.11 Methyl-red indicator solution, prepare by dissolving 0,10 g of methyl-red with 50 ml of ethanol (95) (7.2.2.6) to make up to 100 ml by adding water.7.2.2.12 0.2 mol/ l Sodium hydroxide solution, weigh 50 g
