DIN EN ISO 26845-2008 Chemical analysis of refractories - General requirements for wet chemical analysis atomic absorption spectrometry (AAS) and inductively coupled plasma atomic 4.pdf

1、June 2008DEUTSCHE NORM English price group 11No 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!$O+R“14

2、40847www.din.deDDIN EN ISO 26845Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorptionspectrometry (AAS) and inductively coupled plasma atomic emissionspectrometry (ICP-AES) methods (ISO 26845:2008)English version of DIN EN ISO 26845:2008-06Chemische Anal

3、yse feuerfester Erzeugnisse Allgemeine Anforderungen an die nasschemische Analyse, Atomabsorptionsspektrometrie(AAS)-Verfahren, Atomemissionsspektrometrie mit Anregung durch ein induktivgekoppeltes Plasma (ICP-AES) (ISO 26845:2008)Englische Fassung DIN EN ISO 26845:2008-06DIN EN ISO 21587-3:2007-12s

4、upersedesDIN V ENV 955-4:1997-07,withdrawn 2007-12www.beuth.deTogether with DIN EN ISO 21587-1:2007-12 andDocument comprises 20 pagesDIN EN ISO 26845:2008-06 2 National foreword This standard has been published in accordance with a decision taken by Technical Committee CEN/TC 187 “Refractory product

5、s and materials” (Secretariat: BSI, United Kingdom) to adopt, without alteration, International Standard ISO 26845:2008 as a European Standard. ISO 26845 was prepared by Technical Committee ISO/TC 33 “Refractories”. The responsible German body involved in its preparation was the Normenausschuss Mate

6、rialprfung (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 referred to in the EN are as follows: ISO 31-0 DIN 1313 and DIN 1338 ISO 3310-1 DIN ISO 3310-1

7、 Amendments This standard differs from DIN V ENV 955-4:1997-07 as follows: a) Specifications for reagents concentrations have been modified. b) Clause 9 “Procedure”, Clause 10 “Multi-element calibration” and Clause 11 “Analytical parameters” have been deleted (see DIN EN ISO 21587-1 and DIN EN ISO 2

8、1587-3). c) Permissible differences in test values have been specified. d) Specifications relating to the expression of test results and the preparation of the test report have been modified. e) The standard has been editorially revised. Previous editions DIN V ENV 955-4: 1997-07 National Annex NA (

9、informative) Bibliography DIN 1313, Quantities DIN 1338, Writing and typesetting of formulae DIN ISO 3310-1, Test sieves Technical requirements and testing Part 1: Test sieves of metal wire cloth EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 26845 March 2008 ICS 81.080 Supersedes ENV 955-

10、4:1997 English Version Chemical analysis of refractories - General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods (ISO 26845:2008) Analyse chimique des matriaux rfractaires - Exigences gnrales

11、 pour les mthodes danalyse chimique par voie humide, par spectromtrie dabsorption atomique (AAS) et par spectromtrie dmission atomique avec plasma induit par haute frquence (ICP-AES) (ISO 26845:2008) Chemische Analyse feuerfester Erzeugnisse - Allgemeine Anforderungen an die nasschemische Analyse, A

12、tomabsorptionsspektrometrie (AAS)-Verfahren, Atomemissionsspektrometrie mit Anregung durch ein induktiv gekoppeltes Plasma (ICP-AES) (ISO 26845:2008)This European Standard was approved by CEN on 16 February 2008. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipula

13、te 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 CEN Management Centre or to any CEN member. This European Standard ex

14、ists 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 Management Centre has the same status as the official versions. CEN members are the national standards

15、 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 Kingdom

16、. 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 26845:2008: ECon

17、tents Page 2 EN ISO 26845:2008 (E) :DIN EN ISO 26845:2008-06 Foreword 3 Introduction 4 1 Scope .5 2 Normative references .5 3 Terms and definitions 6 4 Apparatus 6 5 Reagents .10 6 Sampling .15 7 Sample mass .16 8 Basic procedure .16 9 Determination of loss an ignition (gravimetric) 16 10 Expression

18、 of test results .17 11 Examination and adoption of test results 17 12 Test report .18 3 DIN EN ISO 26845:2008-06 EN ISO 26845:2008 (E) Foreword collaboration with Technical Committee CEN/TC 187 “Refractory products and materials” the secretariat of which is held by BSI. This European Standard shall

19、 be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by September 2008, and conflicting national standards shall be withdrawn at the latest by September 2008. Attention is drawn to the possibility that some of the elements of this d

20、ocument may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes ENV 955-4:1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are

21、 bound to implement this European Standard: 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, Swede

22、n, Switzerland and the United Kingdom. Endorsement notice The text of ISO 26845:2008 has been approved by CEN as a EN ISO 26845:2008 without any modification. This document (EN ISO 26845:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories” in Introduction This International Standa

23、rd gives the general requirements common to the standards used for the chemical analysis of refractories and refractory products, i.e.: ISO 10058, Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method): Part 1: Apparatus, reagents, dissolution

24、and gravimetric silica Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) ISO 20565 Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluores

25、cence method) Part 1: Apparatus, reagents, dissolution and gravimetric silica Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) ISO 21079 Chemical analysis of refractories containing alumina, zirconia and

26、silica Refractories containing 5 % to 45 % of ZrO2 (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents and dissolution Part 2: Wet chemical analysis Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) ISO 21587 Che

27、mical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) Part 1: Apparatus, reagents, dissolution and gravimetric silica Part 2: Wet chemical analysis Part 3: Inductively coupled plasma and atomic absorption spectrometry methods These International Standar

28、ds give wet chemical, AAS and ICP methods for the analysis of refractory materials and products. They are to be used as an alternative to ISO 12677, when the laboratory does not have an XRF instrument or its instrument does not meet the requirements of ISO 12677: Chemical analysis of refractory prod

29、ucts by XRF Fused cast bead method. 4 EN ISO 26845:2008 (E) DIN EN ISO 26845:2008-06 1 Scope This International Standard specifies apparatus, reagents, sampling, sample preparation, terms and definitions, basic procedures, loss on ignition and reporting of results applicable to the following standar

30、ds, which are used for the chemical analysis of refractory products and raw materials by wet chemical, AAS and ICP-AES: ISO 10058-1, ISO 10058-2 and ISO 10058-3; ISO 20565-1, ISO 20565-2 and ISO 20565-3; ISO 21079-1, ISO 21079-2 and ISO 21079-3; ISO 21587-1, ISO 21587-2 and ISO 21587-3. 2 Normative

31、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 31-0, Quantities and units Part 0:

32、 General principles ISO 836, Terminology for refractories ISO 3310-1, Test sieves Technical requirements and testing Part 1: Test sieves of metal wire cloth ISO 5022, Shaped refractory products Sampling and acceptance testing ISO 6286, Molecular absorption spectrometry Vocabulary General Apparatus I

33、SO 6353-1:1982, Reagents 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 6955, Analytical spectroscopic methods Flame emission, atomi

34、c absorption, and atomic fluorescence Vocabulary ISO 8656-1, Refractory products Sampling of raw materials and unshaped products Part 1: Sampling scheme 5 EN ISO 26845:2008 (E) DIN EN ISO 26845:2008-06 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO

35、836 and the following apply. 3.1 dry unshaped refractories particles and/or powder of unshaped refractories without liquid (mortar and mixture of refractory aggregate and pitch or resin) 3.2 wet unshaped refractories particles and/or powder of unshaped refractories with liquid (mortar and mixture of

36、 refractory aggregate and pitch or resin) 3.3 alumina-zirconia-silica refractories refractories in which aluminium oxide (1 % to 80 % by mass), zirconium oxide (including hafnium oxide) (5 % to 50 % by mass) and silicon(IV) oxide (0,1 % to 45 % by mass) are used as chemical components 4 Apparatus St

37、andard laboratory apparatus and the following. 4.1 Spectrometers 4.1.1 Atomic absorption (AA) spectrometer, conforming to the requirements of ISO 6955. An instrument which can be operated using a dinitrogen oxide/acetylene flame for the determinations of aluminium oxide and calcium oxide is appropri

38、ate. 4.1.2 Flame emission spectrophotometer, comprising a stand-alone flame emission instrument or an AA spectrometer used in emission mode. 4.1.3 Inductively coupled plasma atomic emission (ICP-AE) spectrometer. 4.1.4 Molecular absorption spectrometer, conforming to the requirements of ISO 6286. 4.

39、1.5 Photometer, with a 1 cm cell. 4.2 Heaters 4.2.1 Burner, such as a Mecker burner or a Bunsen burner. 4.2.2 Electric muffle furnace, suitable for use above 1 150 C. 4.2.3 Sand bath, comprising an electrically heated or burner-heated iron plate with sand, which can be heated to the temperature at w

40、hich white smoke of sulfuric acid occurs. 4.2.4 Steam bath, electric- or burner-type, which can be controlled at the appropriate temperature. 4.3 Devices 4.3.1 Analytical electronic balance, readable to the nearest 0,1 mg. 4.3.2 Magnetic stirrer, comprising a stirring system using a magnetic rotatin

41、g bar coated with ethylene-4-fluoride resin. 6 EN ISO 26845:2008 (E) DIN EN ISO 26845:2008-06 4.3.3 Filter paper, ashless, medium pore. 4.3.4 Cation-exchange resin column, consisting of plastic wool (10 mm) packed into a plastic tube (diameter 12 mm 200 mm) with a funnel attached to the top and an e

42、luent outlet sharp-pointed to the bottom. Pour a slurry (18 ml) of the water-expanded strongly acidic cation-exchange resin divinylbenzene 8 % (DVB), 75 m to 150 m into the column. Adjust the flow rate to 1,0 ml to 1,5 ml per minute by the packing condition of the plastic wool. Wash the column with

43、hydrochloric acid (1+2, 120 ml) and water (70 ml). An example of a normal column is shown in Figure 1. Dimensions in millimetres Key 1 polypropylene funnel 2 cation-exchange resin 3 polypropylene wool Figure 1 Example of a cation-exchange resin column 4.4 Platinum ware The platinum apparatus may be

44、of platinum or platinum alloy. 4.4.1 Platinum crucible, with a volume of 20 ml or 30 ml. 7 EN ISO 26845:2008 (E) DIN EN ISO 26845:2008-06 4.4.2 Platinum dish, with the diameters of the base and wall almost the same, and a height of approximately half the diameter. 75 ml or 150 ml volume are commonly

45、 used sizes. 4.5 Glassware 4.5.1 Burette, with a 0,1 ml scale and a maximum volume of 50 ml. 4.5.2 Conical flask, capable of holding a volume of 500 ml and 1 l. 4.5.3 Desiccator, containing dried silica gel as the drying agent. 4.5.4 Erlenmeyer flask, capable of holding a volume of 500 ml. 4.5.5 Gla

46、ss beakers, with a range of appropriate volumes (100 ml, 200 ml, 300 ml, 400 ml, 500 ml, etc.). 4.5.6 One-mark pipette, suitable for the transfer of each sample solution or standard solution. 4.5.7 Reflux steel head, comprising a funnel, with a long leg capable of being bent so that the end touches

47、the inside wall of a flask (see Figure 2). Dimensions in millimetres a) Steel head b) Steel head setting Key 1 steel head 2 erlenmeyer flask 3 head that contacts internal wall Figure 2 Steel head for reflux 8 EN ISO 26845:2008 (E) DIN EN ISO 26845:2008-06 4.5.8 Separating funnels, 250 ml and 500 ml,

48、 with stoppers. 4.5.9 Volumetric flasks, made of glassware (100 ml, 250 ml, 500 ml, 1 000 ml, etc.) as appropriate for each solution. 4.5.10 Volumetric pipette, of capacity 5 ml. 4.5.11 Watch glass, of diameter 75 mm. 4.6 Porcelain ware 4.6.1 Porcelain basin, with a diameter of 125 mm. 4.6.2 Porcela

49、in crucible, capable of holding a volume of 15 ml. 4.7 Plastic ware 4.7.1 Plastic beaker, of capacity 100 ml. 4.7.2 Polyethylene tetrafluoride beaker, of capacity 200 ml. Heat in nitric acid for at least 2 h and wash in water. NOTE Instead of a polyethylene tetrafluoride beaker, a 150 ml platinum dish can be used. 4.7.3 Volumetric flasks, made of plastic, as appropriate for each solution, and calibrated as follows. Either a) wash a plastic flask thoroughly, invert it and allow it to st