1、October 2013 Translation by DIN-Sprachendienst.English price group 25No part of this translation 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).IC
2、S 91.100.10!%)?$“2062801www.din.deDDIN EN 196-2Method of testing cement Part 2: Chemical analysis of cement;English version EN 196-2:2013,English translation of DIN EN 196-2:2013-10Prfverfahren fr Zement Teil 2: Chemische Analyse von Zement;Englische Fassung EN 196-2:2013,Englische bersetzung von DI
3、N EN 196-2:2013-10Mthodes dessais des ciments Partie 2: Analyse chimique des ciments;Version anglaise EN 196-2:2013,Traduction anglaise de DIN EN 196-2:2013-10SupersedesDIN EN 196-2:2005-05www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises
4、 75 pages 08.13 DIN EN 196-2:2013-10 2 A comma is used as the decimal marker. National foreword This document (EN 196-2:2013) has been prepared by Technical Committee CEN/TC 51 “Cement and building limes” (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the No
5、rmenausschuss Bauwesen (Building and Civil Engineering Standards Committee), Working Committee NA 005-07-13 AA Zement (SpA zu Teil-bereichen von CEN/TC 51 und ISO/TC 74). Amendments This standard differs from DIN EN 196-2:2005-05 as follows: a) Clause 1 “Scope” has been supplemented; b) Clause 5 “Ch
6、emical analysis by X-ray fluorescence” has been added; c) Annexes A to C and the Bibliography have been added. Previous editions DIN 1164-3: 1970-06, 1978-11 DIN EN 196-2: 1990-03, 1995-05, 2005-05 DIN EN 196-21: 1990-03 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 196-2 June 2013 ICS 91.100
7、.10 Supersedes EN 196-2:2005English Version Method of testing cement - Part 2: Chemical analysis of cement Mthodes dessais des ciments - Partie 2: Analyse chimique des ciments Prfverfa en fr Zement - Teil 2: Chemische Analyse von Zement This European Standard was approved by CEN on 5 April 2013. CEN
8、 members are bound 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 appl
9、ication to the CEN-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 Ma
10、nagement Centre 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, Lat
11、via, Lithuania, 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-10
12、00 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 196-2:2013: EhrEN 196-2:2013 (E) 2 Contents Page Foreword . 3 1 Scope 4 2 Normative references . 4 3 General requirements for testing 4 3.1 Number of tests 4 3.2 Repe
13、atability and reproducibility 5 3.3 Expression of masses, volumes, factors and results . 5 4 Analysis by wet chemistry . 5 4.1 General . 5 4.2 Reagents . 6 4.3 Apparatus . 18 4.4 Analysis procedure 22 4.5 Determination of major elements 28 5 Chemical analysis by X-ray fluorescence . 49 5.1 Reagents
14、and reference materials . 49 5.2 Apparatus . 50 5.3 Flux . 51 5.4 Determination of loss on ignition and the change in mass on fusion of the cement 53 5.5 Factoring test results and correcting total analyses for presence of sulfides and halides 54 5.6 Preparation of fused beads and pressed pellets 56
15、 5.7 Calibration and validation 59 5.8 Calculation and expression of results 68 5.9 Performance criteria (repeatability, accuracy and reproducibility limits) . 69 Annex A (informative) Examples of fluxes . 70 Annex B (informative) Sources of certified reference materials . 71 Annex C (informative) E
16、xamples of calibration standards and monitor beads and pellets . 72 Bibliography 73 DIN EN 196-2:2013-10 EN 196-2:2013 (E) 3 Foreword This document (EN 196-2:2013) has been prepared by Technical Committee CEN/TC 51 “Cement and building limes”, the secretariat of which is held by NBN. This European S
17、tandard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2013, and conflicting national standards shall be withdrawn at the latest by December 2013. Attention is drawn to the possibility that some of the element
18、s 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. This document supersedes EN 196-2:2005. This edition adds, to the previous version EN 196-2:2005, provisions for the use of X-ray fluorescence (XRF)
19、 analysis as an alternative method. In relation to correctly calibrating the method, specified procedures, reference materials and performance criteria are included in order to attain and maintain suitable accuracy and precision for equivalence. The method has not been validated for use yet as a ref
20、erence procedure for conformity or dispute purposes. This European Standard on the methods of testing cement is comprised of the following parts: Part 1: Determination of strength Part 2: Chemical analysis of cement Part 3: Determination of setting times and soundness Part 5: Pozzolanicity test for
21、pozzolanic cement Part 6: Determination of fineness Part 7: Methods of taking and preparing samples of cement Part 8: Heat of hydration Solution method Part 9: Heat of hydration Semi-adiabatic method Part 10: Determination of the water-soluble chromium (VI) content of cement NOTE Another document, C
22、EN/TR 196-4 Methods of testing cement Part 4: Quantitative determination of constituents, has been published as a CEN Technical Report. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Au
23、stria, 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, Slovakia, Slovenia, Spain, Swe
24、den, Switzerland, Turkey and the United Kingdom. DIN EN 196-2:2013-10 EN 196-2:2013 (E) 4 1 Scope This European Standard specifies the methods for the chemical analysis of cement. This document describes the reference methods and, in certain cases, an alternative method which can be considered to be
25、 equivalent. In the case of a dispute, only the reference methods are used. An alternative performance-based method using X-ray fluorescence (XRF) is described for SiO2, Al2O3, Fe2O3, CaO, MgO, SO3, K2O, Na2O, TiO2, P2O5, Mn2O3,SrO, Cl and Br. When correctly calibrated according to the specified pro
26、cedures and reference materials, it provides a method equivalent to the reference methods but has not been validated for use yet as a reference procedure for conformity and dispute purposes. It can be applied to other relevant elements when adequate calibrations have been established. This method is
27、 based on beads of fused sample and analytical validation using certified reference materials, together with performance criteria. A method based on pressed pellets of un-fused sample can be considered as equivalent, providing that the analytical performance satisfies the same criteria. Any other me
28、thods may be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence. This document describes methods which apply principally to cements, but which can also be applied to their constitu
29、ent materials. They can also be applied to other materials, the standards for which call up these methods. Standard specifications state which methods are to be used. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensabl
30、e for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 196-7, Methods of testing cement Part 7: Methods of taking and preparing samples of cement ISO 385, Laboratory gla
31、ssware Burettes ISO 835, Laboratory glassware Graduated pipettes ISO Guide 30, Terms and definitions used in connection with reference materials ISO Guide 31, Reference materials Contents of certificates and labels 3 General requirements for testing 3.1 Number of tests Analysis of a cement may requi
32、re the determination of a number of its chemical properties. For each determination, one or more tests shall be carried out in which the number of measurements to be taken shall be as specified in the relevant clause of this document. Where the analysis is one of a series subject to statistical cont
33、rol, the determination of each chemical property by a single test shall be the minimum required. Where the analysis is not part of a series subject to statistical control, the number of tests for determination of each chemical property shall be two (see also 3.3 and 5.8). In the case of a dispute, t
34、he number of tests for determination of each chemical property shall be two (see also 3.3). DIN EN 196-2:2013-10 EN 196-2:2013 (E) 5 3.2 Repeatability and reproducibility Repeatability: Precision under repeatability conditions where independent test results are obtained with the same method on ident
35、ical test items (material) in the same laboratory by the same operator using the same equipment within short intervals of time. Reproducibility: Precision under reproducibility conditions where test results are obtained with the same method on identical test items (material) in different laboratorie
36、s with different operators using different equipment. Repeatability and reproducibility in this document are expressed as repeatability standard deviation(s) and reproducibility standard deviation(s) in e.g. absolute percent, grams, etc., according to the property tested. 3.3 Expression of masses, v
37、olumes, factors and results Express masses in grams to the nearest 0,000 1 g and volumes from burettes in millilitres to the nearest 0,05 ml. Express the factors of solutions, given by the mean of three measurements, to three decimal places. Express the results, where a single test result has been o
38、btained, as a percentage generally to two decimal places. Express the results, where two test results have been obtained, as the mean of the results, as a percentage generally to two decimal places. If the two test results differ by more than twice the standard deviation of repeatability, repeat the
39、 test and take the mean of the two closest test results. The results of all individual tests shall be recorded. 4 Analysis by wet chemistry 4.1 General 4.1.1 Ignitions Carry out ignitions as follows. Place the filter paper and its contents into a crucible which has been previously ignited and tared.
40、 Dry it, then incinerate slowly in an oxidising atmosphere in order to avoid immediate flaming, while ensuring complete combustion. Ignite the crucible and its contents at the stated temperature then allow to cool to the laboratory temperature in a desiccator. Weigh the crucible and its contents. 4.
41、1.2 Determination of constant mass Determine constant mass by making successive 15 min ignitions followed each time by cooling and then weighing. Constant mass is reached when the difference between two successive weighings is less than 0,000 5 g. 4.1.3 Check for absence of chloride ions (silver nit
42、rate test) After generally five to six washes of a precipitate, rinse the base of the filter stem with a few drops of water. Wash the filter paper and its contents with several millilitres of water and collect this in a test tube. Add several drops of silver nitrate solution (4.2.44). Check the abse
43、nce of turbidity or precipitate in the solution. If present, continue washing while carrying out periodic checks until the silver nitrate test is negative. DIN EN 196-2:2013-10 EN 196-2:2013 (E) 6 4.1.4 Blank determinations Carry out a blank determination without a sample, where relevant, following
44、the same procedure and using the same amounts of reagents. Correct the results obtained for the analytical determination accordingly. 4.1.5 Preparation of a test sample of cement Before chemical analysis, treat the laboratory sample, taken in accordance with EN 196-7, as follows to obtain a homogene
45、ous test sample. Take approximately 100 g of the laboratory sample by means of a sample divider or by quartering. Sieve this portion on a 150 m or 125 m sieve until the residue remains constant. Remove metallic iron from the material retained on the sieve by means of a magnet (see Note 1). Then grin
46、d the iron-free fraction of the retained material so that it completely passes the 150 m or 125 m sieve. Transfer the sample to a clean dry container with an airtight closure and shake vigorously to mix it thoroughly. Carry out all operations as quickly as possible to ensure that the test sample is
47、exposed to ambient air only for the minimum time. NOTE 1 Where the analysis is one of a series subject to statistical control and the level of the metallic iron content has been shown to be insignificant in relation to the chemical properties to be determined then it is not necessary to remove metal
48、lic iron. NOTE 2 Where the sample is to be used for XRF analysis and it contains quartz, it might be necessary to grind the sample to pass a 90 m sieve in order to obtain a satisfactory fusion (see 5.6). The time and temperature required to obtain a satisfactory fusion is affected by the fineness of the sample. NOTE 3 Where the sample is to be used for XRF analysis using pressed pellets, accuracy can be improved by grinding the sample more finely. 4.2 Reagents 4.2.1 General Use only reagents of analytical quality.
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