EN ISO 14720-2-2013 en Testing of ceramic raw and basic materials - Determination of sulfur in powders and granules of non-oxidic ceramic raw and basic materials - Part 2 Inductive.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 14720-2:2013T e s t i n g o f c e r a m i c r a w and basic materials Determination of sulfur in powders and granules of non-oxidic ceramic raw and basic materialsPart

2、2: Inductively coupled plasma optical emission spectrometry (ICP/OES) or ion chromatography after burning in an oxygen flowBS EN ISO 14720-2:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO14720-2:2013.The UK participation in its preparation was entruste

3、d to TechnicalCommittee RPI/1, Refractory products and materials.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 correctapplication.

4、The British Standards Institution 2013. Published by BSI StandardsLimited 2013 ISBN 978 0 580 71494 8 ICS 81.060.10 Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on

5、 30 April 2013. Amendments issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14720-2 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

6、raw and basic materials - Part 2: Inductively coupled plasma optical emission spectrometry (ICP/OES) or ion chromatography after burning in an oxygen flow (ISO 14720-2:2013) Essais des matires premires pour produits rfractaires - Dosage du soufre dans les matires premires non oxydantes sous forme de

7、 poudre et de granuls - Partie 2: Spectromtrie dmission optique avec plasma induit par haute frquence (ICP/OES) ou chromatographie ionique aprs combustion dans un courant doxygne (ISO 14720-2:2013) Prfung keramischer Roh- und Werkstoffe - Bestimmung des Schwefelgehaltes in pulver- und kornfrmigen ni

8、chtoxidischen keramischen Roh- und Werkstoffen - Teil 2: Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES) oder Ionenchromatographie (IC) nach Verbrennung im Sauerstoffstrom (ISO 14720-2:2013) This European Standard was approved by CEN on 16 February 2013. CEN members are bou

9、nd to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the C

10、EN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). 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

11、has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

12、Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2013

13、 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14720-2:2013: EBS EN ISO 14720-2:2013EN ISO 14720-2:2013 (E) 3 Foreword This document (EN ISO 14720-2:2013) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in c

14、ollaboration with Technical Committee CEN/TC 187 “Refractory products and materials” the secretariat of which is held by BSI. This European 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 co

15、nflicting national standards shall be withdrawn at the latest by September 2013. Attention is drawn to the possibility that some of 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. Accor

16、ding to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,

17、 Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 14720-2:2013 has been approved by CEN as EN ISO 14720-2:2

18、013 without any modification. BS EN ISO 14720-2:2013ISO 14720-2:2013(E) ISO 2013 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Interferences 25.1 ICP/OES . 25.2 Ion chromatography . 26 Apparatus . 37 Reagents 38 Sampling a

19、nd sample preparation 49 Preparation 49.1 Combustion device 49.2 Oxygen (7.10) . 49.3 Inductively coupled plasma optical emission spectrometer (6.7) . 49.4 Ion chromatograph (6.8) 410 Calibration 410.1 Inductively coupled plasma optical emission spectrometer . 410.2 Ion chromatograph 411 Performance

20、 511.1 Determination of the blank value . 511.2 Determination of the sulfur content . 512 Calculation and report of the results. 513 Precision . 613.1 Repeatability . 613.2 Reproducibility . 614 Test report . 6Annex A (informative) Example of a combustion device . 7Annex B (informative) Example for

21、suitable operating parameters for the determination of sulfur by ion chromatography 8Annex C (informative) Example for suitable operating parameters for the determination of sulfur by inductively coupled plasma optical emission spectroscopy . 9Annex D (informative) Results of the round-robin test10A

22、nnex E (informative) Information regarding the validation of the uncertainty of the mean value .13Annex F (informative) Commercial Certified Reference Materials (CRM) .14Bibliography .15BS EN ISO 14720-2:2013ISO 14720-2:2013(E)ForewordISO (the International Organization for Standardization) is a wor

23、ldwide 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

24、 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.International Standards are drafted i

25、n 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 circulated to the member bodies for voting. Publication as an International Standard

26、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 responsible for identifying any or all such patent rights.ISO 14720-2 was prepared by Tec

27、hnical 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 ceramic raw and basic materials: Part 1: Infrared measurement methods Part 2: Inductive

28、ly coupled plasma optical emission spectrometry (ICP/OES) or ion chromatography after burning in an oxygen flowiv ISO 2013 All rights reservedBS EN ISO 14720-2:2013INTERNATIONAL STANDARD ISO 14720-2:2013(E)Testing of ceramic raw and basic materials Determination of sulfur in powders and granules of

29、non-oxidic ceramic raw and basic materials Part 2: Inductively coupled plasma optical emission spectrometry (ICP/OES) or ion chromatography after burning in an oxygen flow1 ScopeThis part of ISO 14720 defines a method for the determination of sulfur in powdered and granular non-oxidic ceramic raw ma

30、terials and materials, which are completely oxidized at a higher temperature in an oxygen atmosphere, e.g. carbon and graphite materials.For materials which are not completely oxidizable under these conditions, it is possible to determine sulfur that can be released under these conditions, e.g. the

31、adherent sulfur.This part of ISO 14720 is applicable for materials with mass fractions of sulfur 10 % and mass fractions of ash 20 %, The defined method is limited for materials with mass fractions of barium 10 mg/kg, because the sulfur bonded in barium sulfate is not detectable with this method.For

32、 the lower detection limit of this method, a mass fraction of sulfur of 0,5 mg/kg in the case of inductively coupled plasma optical emission spectrometry (ICP/OES) and 5 mg/kg in the case of ion chromatography (IC) has to be considered as a recommended value.2 Normative referencesThe following refer

33、enced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 11885, Water quality Determination of selected elements by induct

34、ively coupled plasma optical emission spectrometry (ICP-OES)ISO 10304-1, Water quality Determination of dissolved anions by liquid chromatography of ions Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate3 Terms and definitionsFor the purposes of this docum

35、ent, the following terms and definitions apply.3.1sulfur contentmass fraction of inorganic and organic bound sulfur4 PrincipleThe dried sample is oxidized in a flow of oxygen at a temperature of 1 100 C using a porcelain crucible. The resulting sulfur oxides are absorbed in a solution of sodium hydr

36、oxide and hydrogen peroxide. The ISO 2013 All rights reserved 1BS EN ISO 14720-2:2013ISO 14720-2:2013(E)remaining material (ash) is dissolved and combined with the absorption liquid in the case of calcium-sulfate-containing sample material. The concentration of sulfur in the sample solution is deter

37、mined by inductively coupled plasma optical emission spectrometry (ICP/OES) according to ISO 11885 or by ion chromatography (IC) as sulfate according to ISO 10304-1 .5 Interferences5.1 ICP/OES5.1.1 Spectral interferencesThe compensation of spectral interferences is performed according to the manual

38、of the manufacturer of the spectrometer.NOTE 1 Spectral interferences can be caused by:a) Overlapping with the emission line of another element;b) Overlapping with molecular bands;c) Unspecific background (e.g. scattering, recombinations).Overlapping of lines can be compensated for by arithmetical c

39、orrection of the raw data if applicable.Correction factors are determined by measuring at least one undisturbed additional emission line of the interfering element and considering the relation of the intensity of this emission line to the emission line which interferes with the analyte element.In th

40、e case of overlapping with molecular bands, an alternative emission line has to be chosen.NOTE 2 Unspecific background is usually compensated for by measuring the background signal in the surroundings of the analyte emission line.5.1.2 Physical interferencesTo compensate physical interferences, suit

41、able measures shall be taken.NOTE Physical interferences occur as plasma interferences or as transport interferences. Both are caused by a different behaviour of the calibration solution compared to the sample solution based on a different chemical composition. Plasma interferences are caused by cha

42、nges in plasma conditions, e.g. temperature distribution and electron density, leading to a changed excitation of emission lines. Transport interferences are caused by differences in physical characteristics of the calibration solution and sample solution, mainly density, viscosity and surface tensi

43、on.Some of the transport interferences can be reduced by using appropriate (peristaltic) pumps. Plasma interferences as well as transport interferences can be reduced significantly by using suitable reference lines of a reference element with the same concentration in both the calibration and analyt

44、e solution (internal standard). Other possibilities are to equalize the chemical composition of the calibration and sample solution as much as possible (matrix matching) or to use a standard addition procedure or a standard addition calibration procedure instead of the standard calibration procedure

45、.5.2 Ion chromatographyTo avoid cross-interferences by additional anions, suitable measures shall be taken.NOTE Anions like chloride, bromide, fluoride, nitrite, nitrate, formiate and acetate in the absorption liquid may lead to cross-interferences. By using the chromatographic parameters given in A

46、nnex B, the sulfate signal usually can be separated completely from the signals of the other anions.2 ISO 2013 All rights reservedBS EN ISO 14720-2:2013ISO 14720-2:2013(E)6 Apparatus6.1 Combustion device, adjustable to (1 100 20) C, suitable for oxidizing the sample in an oxygen flow and suitable to

47、 absorb the reaction gases completely.NOTE For an example of a suitable device see Annex A.6.2 Porcelain boat, unglazed.6.3 Gas-washing bottles, standard type, nominal volume 100 ml, filled with 25 ml of absorption solution (7.6 and Annex A).6.4 Filtration adaptor, with a membrane filter with a pore

48、 width of 0,45 m, connectable to the outlet of the disposable syringe (6.5).6.5 Disposable syringe, nominal volume 5 ml.6.6 Ultrasonic bath, preferably with a volume of 1 l and an ultrasonic power of 150 W.6.7 Inductively coupled plasma optical emission spectrometer, sequential or simultaneous spect

49、rometer with a lower wavelength limit of at least 180 nm.6.8 Ion chromatograph with a column for anions and conductivity detector, if available with suppressor technique.7 Reagents7.1 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.7.2 Hydrogen peroxide solution, H2O2, w(H2O2) = 30 %.7.3 Sodium hydroxide solution, NaOH, c(NaOH) = 0,001 mol/l.7.4 Hydrochloric acid, HCl