1、June 2009DEUTSCHE NORM English price group 13No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 71.040.40; 81.080!$X5w“15
2、31884www.din.deDDIN EN ISO 20565-1Chemical analysis of chrome-bearing refractory products andchrome-bearing raw materials (alternative to the X-ray fluorescencemethod) Part 1: Apparatus, reagents, dissolution and determination ofgravimetric silica (ISO 20565-1:2008)English version of DIN EN ISO 2056
3、5-1:2009-06Chemische Analyse von chromhaltigen feuerfesten Erzeugnissen und chromhaltigenRohstoffen (Alternative zum Rntgenfluoreszenzverfahren) Teil 1: Gerte, Reagenzien, Aufschluss und gravimetrische Bestimmung vonSilicium(IV)-oxid (ISO 20565-1:2008)Englische Fassung DIN EN ISO 20565-1:2009-06Toge
4、ther with DIN EN ISO 20565-2:2009-06 and DIN EN ISO 20565-3:2009-06 supersedesDIN 51074-1:1971-08, DIN 51074-2:1971-08, DIN 51074-3:1971-08 and DIN 51074-4:1971-08Supersedes: see belowwww.beuth.deDocument comprises pages28DIN EN ISO 20565-1:2009-06 2 National foreword This standard has been publishe
5、d in accordance with a decision taken by Technical Committee CEN/TC 187 “Refractory products and materials” (Secretariat: BSI, United Kingdom) to adopt, without alteration, International Standard ISO 20565-1:2008 as a European Standard. ISO 20565-1 was prepared by Technical Committee ISO/TC 33 “Refr
6、actories”. The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Technical Committee NA 062-02-61 AA Chemische Analyse von oxidischen Roh- und Werkstoffen. The DIN Standards corresponding to the International Standards
7、 referred to in this document are as follows: ISO 12677 DIN EN ISO 12677 ISO 26845 DIN EN ISO 26845 Amendments This standard differs from DIN 51074-1:1971-08, DIN 51074-2:1971-08, DIN 51074-3:1971-08 and DIN 51074-4:1971-08 as follows: a) The standard has been completely revised taking into account
8、the current chemical analysis aspects. Previous editions DIN 51074-1: 1971-08 DIN 51074-2: 1971-08 DIN 51074-3: 1971-08 DIN 51074-4: 1971-08 DIN EN ISO 20565-1:2009-06 3 National Annex NA (informative) Bibliography DIN EN ISO 12677, Chemical analysis of refractory products by XRF Fused cast bead met
9、hod DIN EN ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, AAS and ICP methods DIN EN ISO 20565-1:2009-06 4 This page is intentionally blank. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 20565-1 December 2008 ICS 81.080 English Version Chemica
10、l analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica (ISO 20565-1:2008) Analyse chimique des produits rfractaires contenant du chrome et des ma
11、tires premires contenant du chrome (mthode alternative la mthode par fluorescence de rayons X) Partie 1: Appareillage, ractifs, mise en solution et dtermination de la teneur en silice par gravimtrie (ISO 20565-1:2008) Chemische Analyse von chromhaltigen feuerfesten Erzeugnissen und chromhaltigen Roh
12、stoffen (Alternative zum Rntgenfluoreszenzverfahren) Teil 1: Gerte, Reagenzien, Aufschluss und gravimetrische Bestimmung von 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 w
13、hich stipulate the conditions for giving this EuropeanStandard 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 CEN Management Centre or to any CEN member. This European
14、Standard exists in three official versions (English, French, German). A version in any other language made 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
15、standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United
16、Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 20565-1:2
17、008: EContents Page Foreword 3 1 Scope 4 2 Normative references 5 3 Terms and definitions .5 4 Apparatus .5 5 Reagents.6 5.1 Stock reagents .6 5.2 Indicators8 5.3 Standard solutions 9 6 Sample preparation .14 7 Basic procedure.15 8 Determination of loss on ignition (gravimetric)15 9 Decomposition of
18、 the sample and preparation of solutions used in the analysis .15 9.1 General decomposition techniques.15 9.2 Dissolution methods by fusion 15 9.3 Dissolution methods by hydrofluoric acid attack 17 9.4 Separation methods by ion-exchange.19 10 Calculation and expression of test results .22 11 Examina
19、tion and adoption of test results .22 12 Test report 22 Annex A (informative) References for stock solutions and blank solutions in ISO 20565-1:2008 .23 DIN EN ISO 20565-1:2009-06EN ISO 20565-1:2008 (E)2Bibliography24Foreword This document (EN ISO 20565-1:2008) has been prepared by Technical Committ
20、ee 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 European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the
21、latest by June 2009, 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 suc
22、h patent rights. According 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,
23、 Ireland, Italy, Latvia, 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. 3D
24、IN EN ISO 20565-1:2009-06EN ISO 20565-1:2008 (E)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, reage
25、nts, 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
26、 Fe2O30,5 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. DIN EN ISO 20565-1:2009-06EN ISO 20565-1:2008 (E)42 Normativ
27、e 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, Reagents for chemical an
28、alysis 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 chemical analysis, atomic
29、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. NOTE Other apparat
30、us 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 appropriate for each
31、 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 the plastic flask wi
32、th 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. Separately, measure
33、 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 water up to the top
34、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); DIN EN ISO 20565-1:2009-06EN ISO 20565-1:2008 (E)5mBis the mass of water up to bottom edge (B) of the graduation paper, in milligrams (mg), i
35、.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 temperature of 20 C, and an atmospheric press
36、ure 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 made on the plastic flask. When using this flask
37、, 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 ISO 6353-1, ISO 6353-2 and ISO 6353-3 as appr
38、opriate. 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 5.1.1 Acetic acid (ISO 6353-2, R 1), concentrate
39、d, 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 mass. 5.1.5 Ammonia solution (1+1). Add 1 volum
40、e 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 with water and dilute to 1 l. 5.1.8 Ammonium mo
41、lybdate 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. DIN EN ISO 20565-1:2009-06EN ISO 20565-1:2008 (E)65.1.9 L (+)-ascorbic acid solution, 100 g/l. Disso
42、lve 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 dilute to 1 l. 5.1.11 Chloroform. 5.1.12 Cupferron solution, 60 g/l. Di
43、ssolve 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 decomposition. 5.1.13 Diantipyrylmethane (DAM) solution, 10 g/l. Dissolve 1 g
44、 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, 150 g/l. Dissolve 15 g of hydrazinium dichloride in water and dilute t
45、o 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). Add 1 volume of hydrochloric acid (concentrated) (5.1.16) to 50 volume
46、s 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
47、 g of hydroxyammonium chloride in warm water, filter if necessary, cool and dilute to 100 ml. 5.1.22 Liquid cation-exchange resin, for example, Amberlite LA-2 resin (1+4), made by adding 50 ml of the resin to 200 ml of chloroform and mixing. Transfer the mixture to a 500 ml separating funnel and sha
48、ke gently with 25 ml of H2SO4(1+9) for a few seconds, releasing the pressure frequently. Run off the organic layer into a 250 ml measuring cylinder. 5.1.23 Nitric acid (concentrated), 70 % by mass. 5.1.24 Nitric acid (1+1). Add 1 volume of nitric acid (concentrated) (5.1.23) to one volume of water.
49、DIN EN ISO 20565-1:2009-06EN ISO 20565-1:2008 (E)75.1.25 2,2, 2-Nitrilotriethanol (1+1). Add 1 volume of 2,2, 2-nitrilotriethanol to one volume of water. 5.1.26 1,10-Phenanthrolinium chloride solution, 1 g/l. Dissolve 0,1 g of 1,10-phenanthrolinium chloride monohydrate in water, dilute to 100 ml, and keep in a dark and cool place. However, discard the solution if it colours during storage. 5.1.27 Phosphoric acid (concentrated), 85 % by mass. 5.1.28 Phosphoric acid, (2+3). Add 2 volumes of phosphoric
