EN ISO 20565-1-2008 en Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) - Part 1 Apparatus re.pdf

1、BS EN ISO20565-1:2008ICS 81.080NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDChemical analysisof chrome-bearingrefractory productsand chrome-bearingraw materials(alternative to theX-ray fluorescencemethod)Part 1: Apparatus, reagents,dissolution and determinati

2、on ofgravimetric silica (ISO 20565-1:2008)Incorporating corrigendum September 2010National forewordThis British Standard is the UK implementation of EN ISO 20565-1:2008. Together with BS EN ISO 20565-2:2008 and BS EN ISO 20565-3:2008, it supersedes BS 1902-2.2:1974 which is withdrawn.The UK particip

3、ation in its preparation was entrusted to Technical Committee RPI/1, Refractory products and materials.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are

4、responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.BS EN ISO 20565-1:2008This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2009 BSI 2010Amendments/corrigenda issued

5、since publicationDate Comments 30 September 2010 Addition of supersession detailsISBN 978 0 580 72652 1EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 20565-1December 2008ICS 81.080English VersionChemical analysis of chrome-bearing refractory products andchrome-bearing raw materials (alternati

6、ve to the X-rayfluorescence method) - Part 1: Apparatus, reagents, dissolutionand determination of gravimetric silica (ISO 20565-1:2008)Analyse chimique des produits rfractaires contenant duchrome et des matires premires contenant du chrome(mthode alternative la mthode par fluorescence derayons X) -

7、 Partie 1: Appareillage, ractifs, mise en solutionet dtermination de la teneur en silice par gravimtrie (ISO20565-1:2008)Chemische Analyse von chromhaltigen feuerfestenErzeugnissen und chromhaltigen Rohstoffen (Alternativezum Rntgenfluoreszenzverfahren) - Teil 1: Gerte,Reagenzien, Aufschluss und gra

8、vimetrische Bestimmungvon Silicium(IV)-oxid (ISO 20565-1:2008)This European Standard was approved by CEN on 8 November 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard with

9、out any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language m

10、ade by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France

11、, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMU

12、NGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 20565-1:2008: E3 Foreword This document (EN ISO 20565-1:2008) has been prepared by Technical Committee ISO/TC 33 “Refra

13、ctories“ in collaboration 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 June 2009

14、, and conflicting national standards shall be withdrawn at the latest by June 2009. 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. Ac

15、cording to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, La

16、tvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 20565-1:2008 has been approved by CEN as a EN ISO 20565-1:2008 without any modification. BS EN ISO 20565-1:200

17、8EN ISO 20565-1:2008 (E) ISO 20 0 All rights reserved iiiContents Page Foreword iv 1 Scope 1 2 Normative references 2 3 Terms and definitions .2 4 Apparatus .2 5 Reagents.3 5.1 Stock reagents .3 5.2 Indicators5 5.3 Standard solutions 6 6 Sample preparation .11 7 Basic procedure.12 8 Determination of

18、 loss on ignition (gravimetric)12 9 Decomposition of the sample and preparation of solutions used in the analysis .12 9.1 General decomposition techniques.12 9.2 Dissolution methods by fusion 12 9.3 Dissolution methods by hydrofluoric acid attack 14 9.4 Separation methods by ion-exchange.16 10 Calcu

19、lation and expression of test results .19 11 Examination and adoption of test results .19 12 Test report 19 Annex A (informative) References for stock solutions and blank solutions in ISO 20565-1:2008 .20 1BS EN ISO 20565-1:2008EN ISO 20565-1:2008 (E)iv ISO 2010 All rights reservedForeword ISO (the

20、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 for which a technical committee

21、 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 all matters of electrotechnic

22、al 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 circulated to the member bo

23、dies 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 responsible for identifying an

24、y or all such patent rights. ISO 20565-1 was prepared by Technical Committee ISO/TC 33, Refractories, in collaboration with Technical Committee CEN/TC 187, Refractory products and materials. ISO 20565 consists of the following parts, under the general title Chemical analysis of chrome-bearing refrac

25、tory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method): Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emis

26、sion spectrometry (ICP-AES) BS EN ISO 20565-1:2008EN ISO 20565-1:2008 (E)INTERNATIONAL STANDARD ISO 2010 All rights reserved 1Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissoluti

27、on and determination of gravimetric silica 1 Scope This part of ISO 20565 specifies methods for the chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials, using traditional (“wet”) methods, ICP-AES spectrometry and FAAS spectrometry. It covers apparatus, reagents,

28、dissolution and determination of gravimetric silica. It is applicable in the ranges of determination given in Table 1. ISO 20565 provides alternatives to the X-ray fluorescence (XRF) method given in ISO 12677. Table 1 Range of determination (% by mass) Component Range SiO20,5 to 10 Al2O32 to 30 Fe2O

29、30,5 to 25 TiO20,01 to 1 MnO 0,01 to 1 CaO 0,01 to 3 MgO 15 to 85 Na2O 0,01 to 1 K2O 0,01 to 1 Cr2O32 to 60 ZrO20,01 to 0,5 P2O50,01 to 5 LOI 0,5 to 5 NOTE These values are after the loss on ignition (LOI) has been taken into account. BS EN ISO 20565-1:2008EN ISO 20565-1:2008 (E)2 ISO 2010 All right

30、s reserved2 Normative references The following referenced 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 6353-1, Reag

31、ents for chemical analysis Part 1: General test methods ISO 6353-2, Reagents for chemical analysis Part 2: Specifications First series ISO 6353-3, Reagents for chemical analysis Part 3: Specifications Second series ISO 26845:2008, Chemical analysis of refractories General requirements for wet chemic

32、al analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 26845 apply. 4 Apparatus Use normal laboratory apparatus and the following

33、. NOTE Other apparatus is defined in ISO 26845. 4.1 Polyethylene tetrafluoride beaker, 200 ml. Heat in nitric acid for at least 2 h and wash in water. Instead of a polyethylene tetrafluoride beaker, a 150 ml platinum dish may be used. 4.2 Volumetric flasks, 100 ml each, made of plastics material as

34、appropriate for each solution, calibrated as follows. Wash the plastic flask and stand it to dry naturally, or wash it with water, ethanol and diethylether and dry it by sending air into it. Cut the 20 graduations off a sheet of section paper (1 mm2) into a strip and attach it on the marked line of

35、the plastic flask with the central line of the paper. Weigh the flask to the nearest milligram. Pour water (at a temperature approximately equal to the room temperature) up to the lower end (B) of the strip and weigh the flask. Then add water up to the upper end (A) of the strip and weigh the flask.

36、 Separately, measure the water temperature (C), the room temperature (C) and the atmospheric pressure (kPa). Obtain the correct marked line i.e. the number of graduations counted from bottom edge (B) of graduation paper, S, by using Equation (1). BAB1000 000 ( )20mmmfSmm+=(1) where mAis the mass of

37、water up to the top edge (A) of the graduation paper, in milligrams (mg), i.e. (mass obtained by second weighing) (mass of Erlenmeyer flask): mA= mA+ (mass of water from A to B); BS EN ISO 20565-1:2008EN ISO 20565-1:2008 (E) ISO 2010 All rights reserved 3mBis the mass of water up to bottom edge (B)

38、of the graduation paper, in milligrams (mg), i.e. (mass obtained by first weighing) (mass of Erlenmeyer flask); m is the correction value, in milligrams (mg), at 20 C room temperature, and 101,325 kPa atmospheric pressure; m is the correction value, in milligrams (mg), due to the deviation from room

39、 temperature of 20 C, and an atmospheric pressure 101,325 kPa; it is 4,0 mg per 1 C room temperature, and 1,3 mg per 0,133 kPa atmospheric pressure; f is 100 ml (nominal capacity of plastic flask to be calibrated). Change the paper strip for a fresh paper strip marked with the correct marked line ma

40、de on the plastic flask. When using this flask, employ the marked line newly obtained above. 5 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. Reagents shall conform to the requirements of

41、 ISO 6353-1, ISO 6353-2 and ISO 6353-3 as appropriate. Specific requirements for reagents are given in the appropriate clause. Reagents that are listed in ISO 26845 and the following. NOTE Where solutions are referred to as (1+1), etc., this implies v/v unless otherwise stated. 5.1 Stock reagents 5.

42、1.1 Acetic acid (ISO 6353-2, R 1), concentrated, minimum 99,7 % by mass. 5.1.2 Aluminum chloride solution, Al (25 mg/ml). Dissolve 123,5 g of aluminum chloride into water and dilute to 1 l with water. 5.1.3 Ammonium chloride. 5.1.4 Ammonia solution (concentrated) (ISO 6353-2, R 3), minimum 25 % by m

43、ass. 5.1.5 Ammonia solution (1+1). Add 1 volume of ammonia solution (concentrated) (5.1.4) to 1 volume of water. 5.1.6 Ammonia solution (1+9). Add 1 volume of ammonia solution (concentrated) (5.1.4) to 9 volumes of water. 5.1.7 Ammonium acetate solution, 200 g/l. Dissolve 200 g of ammonium acetate w

44、ith water and dilute to 1 l. 5.1.8 Ammonium molybdate solution, 20 g/l. Dissolve 2 g of ammonium molybdate tetrahydrate in 20 ml of hot water, filter if necessary, and dilute to 100 ml with the addition of 60 ml of sulfuric acid (1+1) and water. BS EN ISO 20565-1:2008EN ISO 20565-1:2008 (E)4 ISO 201

45、0 All rights reserved5.1.9 L (+)-ascorbic acid solution, 100 g/l. Dissolve 10 g of L (+)-ascorbic acid in water and dilute to 100 ml. This solution shall be kept in the dark and at low temperature. Discard after 2 weeks. 5.1.10 Boric acid solution, 40 g/l. Dissolve 40 g of boric acid with water and

46、dilute to 1 l. 5.1.11 Chloroform. 5.1.12 Cupferron solution, 60 g/l. Dissolve 6 g of cupferron in 100 ml of water; filter if necessary. Prepare this solution freshly, as required. Store the solid reagent in a tightly stoppered bottle in the presence of a piece of ammonium carbonate to prevent decomp

47、osition. 5.1.13 Diantipyrylmethane (DAM) solution, 10 g/l. Dissolve 1 g of diantipyrylmethane monohydrate in 30 ml of hydrochloric acid (1+50), and dilute to 100 ml with water. 5.1.14 Fusion mixture, an equimolecular mixture of sodium and potassium carbonates. 5.1.15 Hydrazinium dichloride solution,

48、 150 g/l. Dissolve 15 g of hydrazinium dichloride in water and dilute to 100 ml. 5.1.16 Hydrochloric acid (concentrated), (ISO 6353-2, R 13), 35 % by mass. 5.1.17 Hydrochloric acid (1+1). Add 1 volume of hydrochloric acid (concentrated) (5.1.16) to 1 volume of water. 5.1.18 Hydrochloric acid (1+50).

49、 Add 1 volume of hydrochloric acid (concentrated) (5.1.16) to 50 volumes of water. 5.1.19 Hydrofluoric acid (concentrated), (ISO 6353-3, R 67), 40 % to 42 % by mass. 5.1.20 Hydrofluoric acid (1+9). Add 1 volume of hydrofluoric acid (concentrated) (5.1.19) to 9 volumes of water. Store in a plastic container. 5.1.21 Hydroxyammonium chloride solution, 100 g/l. Dissolve 10 g of hydroxyammonium chloride in warm water, filter if necessary, cool and dilute to 100 ml. 5.1.22 Liquid cation-exchange resi