BS EN ISO 14720-1-2013 Testing of ceramic raw and basic materials Determination of sulfur in powders and granules of non-oxidic ceramic raw and basic materials Infrared measurement.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 14720-1:2013Testing of ceramic rawand basic materials Determination of sulfur inpowders and granules of non-oxidic ceramic raw and basicmaterialsPart 1: Infrared measur

2、ement methods (ISO14720-1:2013)BS EN ISO 14720-1:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO14720-1:2013.The UK participation in its preparation was entrusted to TechnicalCommittee RPI/1, Refractory products and materials.A list of organizations rep

3、resented 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 correctapplication. The British Standards Institution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580

4、 71493 1ICS 81.060.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 April 2013.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUR

5、OPENNE EUROPISCHE NORM EN ISO 14720-1 March 2013 ICS 81.060.10 English Version Testing of ceramic raw and basic materials - Determination of sulfur in powders and granules of non-oxidic ceramic raw and basic materials - Part 1: Infrared measurement methods (ISO 14720-1:2013) Essais des matires premi

6、res pour produits rfractaires - Dosage du soufre dans les matires premires non oxydantes sous forme de poudre et de granuls - Partie 1: Mthodes dessai par infrarouge (ISO 14720-1:2013) Prfung keramischer Roh- und Werkstoffe - Bestimmung des Schwefelgehaltes in pulver- und kornfrmigen nichtoxidischen

7、 keramischen Roh- und Werkstoffen - Teil 1: Infrarotmessverfahren (ISO 14720-1:2013) This European Standard was approved by CEN on 16 February 2013. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status o

8、f a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German

9、). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia,

10、Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United

11、 Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14720-1:20

12、13: EBS EN ISO 14720-1:2013EN ISO 14720-1:2013 (E) 3 Foreword This document (EN ISO 14720-1:2013) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration with Technical Committee CEN/TC 187 “Refractory products and materials” the secretariat of which is held by BSI. This E

13、uropean Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by September 2013, and conflicting national standards shall be withdrawn at the latest by September 2013. Attention is drawn to the possibility that some of

14、the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement

15、 this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slo

16、vakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 14720-1:2013 has been approved by CEN as EN ISO 14720-1:2013 without any modification. BS EN ISO 14720-1:2013ISO 14720-1:2013(E) ISO 2013 All rights reserved iiiContents PageForeword iv1 Sc

17、ope . 12 Principle 13 Apparatus . 14 Reagents 25 Sampling and sample preparation 26 Calibration 27 Performance 27.1 Preparation of analysis 27.2 Determination of blank value . 37.3 Determination of sulfur content 38 Calculation and report of the results. 39 Precision . 39.1 Repeatability . 39.2 Repr

18、oducibility . 310 Test report . 3Annex A (informative) Results of the round-robin test . 5Annex B (informative) Information regarding the validation of the uncertainty of the mean value 7Annex C (informative) Commercial Certified Reference Materials (CRM) 8Bibliography 9BS EN ISO 14720-1:2013ISO 147

19、20-1:2013(E)ForewordISO (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 fo

20、r 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

21、all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are

22、circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.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 resp

23、onsible for identifying any or all such patent rights.ISO 14720-1 was prepared by Technical Committee ISO/TC 33, Refractories.ISO 14720 consists of the following parts, under the general title Testing of ceramic raw and basic materials Determination of sulfur in powders and granules of non-oxidic ce

24、ramic raw and basic materials: Part 1: Infrared measurement methods Part 2: Inductively coupled plasma optical emission spectrometry (ICP/OES) or ion chromatography after burning in an oxygen flowiv ISO 2013 All rights reservedBS EN ISO 14720-1:2013INTERNATIONAL STANDARD ISO 14720-1:2013(E)Testing o

25、f ceramic raw and basic materials Determination of sulfur in powders and granules of non-oxidic ceramic raw and basic materials Part 1: Infrared measurement methods1 ScopeThis part of ISO 14720 defines a method for the determination of sulfur in powdered and granular non-oxidic ceramic raw materials

26、 and materials, such as silicon carbides, silicon nitrides, graphites, carbon blacks, cokes, carbon powders. If proved by the recovery rate, this method can also be applied for other non-metallic powdered and granular materials, e.g. silicon dioxide.This part of ISO 14720 is applicable for materials

27、 with mass fractions of sulfur from 0,005 % to 2 %.This part of ISO 14720 can also be applied for materials with higher mass fractions of sulfur after verification of the particular case.2 PrincipleThe sample and added combustion accelerators (mostly tungsten- or iron-granules) are heated in an indu

28、ctive furnace under oxygen atmosphere. The high-frequency field of the furnace couples with electrically conductive components of sample and combustion accelerators. The sample is heated to temperatures above 1 800 C and the total sulfur content of the sample is released as sulfur dioxide. The react

29、ion gas is transferred to the infrared absorption cell of the analyser. The molecular absorption of sulfur dioxide is measured by using a narrow-band optical filter which is translucent for the wavelength of the characteristic infrared absorption of sulfur dioxide. The mass fraction of sulfur dioxid

30、e in the reaction gas is proportional to peak-height and peak-area, respectively, of the transient absorption signal. The mass fraction of sulfur in the sample is calculated by using a calibration function established by suitable calibration standards measured under comparable conditions.3 Apparatus

31、3.1 Device with induction furnace or alternatively resistance furnace and infrared cell.NOTE The correctness of the analysis result can be proved by using matrix-analogous reference materials or by comparing with an independent alternative test method. If determining mass fractions below 100 mg/kg,

32、it has to be considered that some analytical devices may deliver incorrect results.3.2 Analytical balance, capable of reading to the nearest 0,01 mg.3.3 Ceramic crucible, e.g. mullite or alumina.3.4 Crucible lid with hole, e.g. mullite or alumina. ISO 2013 All rights reserved 1BS EN ISO 14720-1:2013

33、ISO 14720-1:2013(E)4 Reagents4.1 GeneralReagents of known analytical grade shall be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.4.2 Tungsten granulesNOTE Depending on the material, the de

34、composition of the sample in the furnace may be improved by partially replacing tungsten granules by tin granules. Tungsten/tin-mixtures are commercially available.4.3 Iron granules4.4 Calibration standards, preferably certified reference materials with composition and sulfur content similar to the

35、analysed material.NOTE See Annex C. Also suitable are primary substances, preferably sulfates.4.5 Oxygen, purity 99,998 % V/V.5 Sampling and sample preparationSampling shall be performed in a way such that the sample to be analysed is representative for the total amount of material, for example acco

36、rding to ISO 8656-1.1In an unknown drying state, the sample shall be dried at (110 5) C to constant mass. The sample shall be cooled to ambient temperature in a desiccator and stored therein.The sample material shall have a particle size of 160 m. If necessary, it shall be crushed and homogenized.6

37、CalibrationThe calibration shall be performed according to the manufacturers manual. It shall be ensured that the mass of sulfur in the calibration sample and test sample are within the same order of magnitude.NOTE This is achieved by choosing a suitable calibration substance (4.4) and adapted masse

38、s.For a mass fraction below 100 mg/kg, the trueness of the result shall be verified using a suitable reference material, preferably a certified reference material.The calibration shall be carried out according to the procedure in 7.3.7 Performance7.1 Preparation of analysisCeramic crucibles (3.3) an

39、d lids (3.4) have to be pre-cleaned by heating to 1 200 C for 1 h prior to analysis, preferably using a muffle furnace. The sulfur content of the iron granules (4.3) shall be determined batch-wise. In the case of a too high and irreproducible sulfur content of the iron granules in relation to the ex

40、pected sulfur content in the sample, they shall be pre-cleaned by the following procedure: weigh 1 g of iron granules into each ceramic crucible used for analysis. Cover with a lid and melt the iron granules under oxygen atmosphere in the inductive furnace of the analytical device. If the sulfur con

41、tent of the sample is less than 100 mg/kg, the iron granules can be alternatively purified by heating in hydrogen atmosphere at approximately 800 C for 1 h.2 ISO 2013 All rights reservedBS EN ISO 14720-1:2013ISO 14720-1:2013(E)7.2 Determination of blank valueUse the procedure in 7.3 but without any

42、sample.7.3 Determination of sulfur contentAccording to the expected sulfur content, a sub-sample of 20 mg to 200 mg is weighed to the nearest 0,01 mg into the crucibles prepared according to 7.1.The sub-sample is covered with approximately 1 g and 2 g of iron and tungsten granules (4.2 and 4.3), res

43、pectively. If the crucible already contains pre-cleaned iron (see 7.1), no further iron has to be added. For mixing, the crucible has to be shaken carefully. Afterwards, the crucible is closed with the lid, placed in the analysis device and the combustion cycle is started.Each sample has to be analy

44、sed at least two times. If the single values of the double-test deviate more than a given degree, depending on the repeatability of the method, then the analysis has to be repeated according to this Clause. If necessary, the sample has to be homogenized according to Clause 5.8 Calculation and report

45、 of the resultsThe sulfur content of the sample shall be calculated under consideration of sample mass and blank values. The sulfur content as the mean of the corrected single values of the multiple determinations shall be expressed as a mass fraction and rounded off in accordance with the uncertain

46、ty of measurement (Annex B).NOTE Most state-of-the-art analysers automatically calculate the mass fraction of sulfur for each measurement after input of blank values and sample masses.9 Precision9.1 RepeatabilityThe repeatability limit r will not be exceeded in more than 5 % of cases by the absolute

47、 difference between two single test results, determined in rapid succession by the same analyst with the same sample material using the same analytical procedure and the same equipment in the same laboratory.NOTE The repeatability limit r depends on the examined material type and the determined mass

48、 of sulfur.The precision data determined within a round robin test are listed in Annex A.9.2 ReproducibilityThe reproducibility limit R will not be exceeded in more than 5 % of cases by the absolute difference between two single test results, determined by different analysts with the same sample mat

49、erial using the same analytical procedure and different equipments in different laboratories.The reproducibility R depends on the examined material type and the determined mass of sulfur.The precision data determined within a round-robin test are listed in Annex A.10 Test reportTest reports shall include the following informationa) sample identification;b) a reference to this part of ISO 14720; ISO 2013 All rights reserved 3BS EN ISO 14720-1:2013ISO 14720-1:2013(E)c) test results for the sulfur content, expressed as the mean of the s