1、PUBLISHED DOCUMENTPD CEN/TR 196-4:2007Methods of testing cement Part 4: Quantitative determination of constituentsICS 91.100.10g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g6
2、0g53g44g42g43g55g3g47g36g58PD CEN/TR 196-4:2007This Published Document was published under the authority of the Standards Policy and Strategy Committee on 30 November 2007 BSI 2007ISBN 978 0 580 61119 3National forewordThis Published Document is the UK implementation of CEN/TR 196-4:2007.The UK part
3、icipation in its preparation was entrusted by Technical Committee B/516, Cement and lime, to Subcommittee B/516/12, Sampling and testing.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 pr
4、ovisions of a contract. Users are responsible for its correct application. Amendments issued since publicationAmd. No. Date CommentsTECHNICAL REPORTRAPPORT TECHNIQUETECHNISCHER BERICHTCEN/TR 196-4September 2007ICS 91.100.30 Supersedes ENV 196-4:1993 English VersionMethods of testing cement - Part 4:
5、 Quantitative determinationof constituentsMthodes dessais des ciments - Partie 4 : Dterminationquantitative des constituantsPrfverfahren fr Zement - Teil 4: Quantitative Bestimmungder BestandteileThis Technical Report was approved by CEN on 14 April 2007. It has been drawn up by the Technical Commit
6、tee CEN/TC 51.CEN members are the national 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, Slove
7、nia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN natio
8、nal Members.Ref. No. CEN/TR 196-4:2007: E2 Contents Page Foreword 3 1 Scope. 5 2 Normative references 6 3 General requirements for testing . 7 3.1 Number of tests 7 3.2 Determination of constant mass 7 3.3 Expression of masses and results. 8 3.4 Repeatability and reproducibility . 8 4 Preparation of
9、 a cement sample. 8 5 Reagents . 8 6 Determination of the contents of cement constituents . 8 6.1 General 8 6.2 Selective dissolution method . 9 7 Determination of the contents of constituents for cements with three constituents16 7.1 General 16 7.2 Determination of the slag content 16 7.3 Determina
10、tion of the siliceous fly ash content . 26 7.4 Determination of the natural pozzolana content 28 CEN/TR 196-4:20073 Foreword This document (CEN/TR 196-4:2007) has been prepared by Technical Committee CEN/TC 51 “Cement and building limes”, the secretariat of which is held by NBN. Attention is drawn t
11、o 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. This document supersedes ENV 196-4:1993. This European Technical Report was drawn up by Technical Committe
12、e CEN/TC 51 “Cement and building limes“ the Secretariat of which is held by NBN. It is based on a revision of the European Pre-standard ENV 196-4 of July 1993. The main aim of this document is to quantitatively verify the compositions (analysis of the constituents) of all the cements included in EN
13、197-1:2000 (Cements Part1: composition, specifications and conformity criteria for common cements) as set out in Table 1 “The 27 products in the family of common cements”. Further to this objective, original methods of analysis were devised, firstly, for cements with 3 constituents and then a refere
14、nce method for cements with more constituents. Following the progress of work on EN 197-1, cements with blastfurnace slag, siliceous fly ash and natural pozzolans have been successively studied. As a result the first draft of ENV 196-4 was published in December 1989, followed by the ENV 196-4 in Jul
15、y 1993. The main aim of the revision of the Pre-standard was to adapt the reference method in such a way that it would be qualitative and quantitative whatever the constituent materials, including blastfurnace slag (which had not been included in the 1989 draft ENV 196-4). This entailed revising the
16、 analytical procedure and the calculation of the constituents. The opportunity was taken at the same time to unify the presentation of the different methods, reference and alternative, endeavoring to standardize the notational symbols to eliminate all ambiguities in the interpretation of the formula
17、e for calculations. Table 1 of ENV 197-1:1992 introduced further new constituent materials. One of them, silica fume, could be routinely determined by the reference method, while calcareous fly ash and burnt shale, being composites of several minerals, react partially like other constituents capable
18、 of being determined by the reference method. Where these materials are constituents it has proved not to be possible to determine the mass composition of the cement but only to obtain an overall bulk analysis. Almost all of the cements manufactured in Europe can be correctly characterized and quant
19、ified by the reference method. However, for cements containing burnt shale (CEM II/A-T and B-T) or calcareous fly ash (CEM II/A-W and B-W) it would be necessary to undertake further research in order to obtain an acceptable reference method. For cements having constituents that can be analyzed by th
20、e current reference method as defined in section 1 “Scope” the method will be adequate. Where other constituents are known, or suspected, to be included it will be necessary to develop additional methods for the quantitative determination of those particular constituents. The European Standard on th
21、e methods of testing cement comprises the following Parts: EN 196-1 Methods of testing cement Part 1: Determination of strength CEN/TR 196-4:20074 EN 196-2 Methods of testing cement Part 2: Chemical analysis of cement EN 196-3 Methods of testing cement Part 3: Determination of setting times and soun
22、dness EN 196-5 Methods of testing cement Part 5: Pozzolanicity test for pozzolanic cement EN 196-6 Methods of testing cement Part 6: Determination of fineness EN 196-7 Methods of testing cement Part 7: Methods of taking and preparing samples of cement EN 196-8 Methods of testing cement Part 8: Heat
23、of hydration Solution method EN 196-9 Methods of testing cement Part 9: Heat of hydration Semi-adiabatic method. NOTE A previous Part, EN 196- 21: Methods of testing cement Part 21: Determination of the chloride, carbon dioxide and alkali content of cement, has been revised and incorporated into EN
24、196-2 CEN/TR 196-4:20075 1 Scope This European Technical Report describes procedures for determining the contents of most of the constituents of the cements that fall within the scope of EN 197-1. In principle, the method described in Clause 6 applies to all cements, whatever the number and nature o
25、f their constituents, but in practice is limited to the cements identified in Table 1. The method in clause 6 should be considered to be the method of choice and is based on a sequential selective dissolution of the cements constituents, generally of an unknown number, where they are not available s
26、eparately for analysis at the same time as the cement. The method of choice enables the quantitative determination (by mass) of: Portland cement clinker, blastfurnace slag, siliceous fly ash, natural pozzolans, limestone, silica fume and set regulators in cements of the types identified in Table 1.
27、Table 1 is derived from Table 1 of EN 197-1. Table 1 Common cement types specified in EN 197-1 Type of cement Designation Notation Excluding (1)CEM I Portland cement I Portland-slag cement (with blastfurnace slag) II/A-S II/B-S Portland-silica fume cement II/A-D Portland pozzolana cement (with natur
28、al pozzolana) II/A-P II/B-P Portland-fly ash cement (with siliceous fly ash) II/A-V II/B-V Portland-limestone cement II/A-L or LL* II/B-L or LL* CEM II Portland-composite cement II/A-M II/B-M limestone Burnt shale CEM III Blastfurnace cement III/A III/B III/C CEM IV Pozzolanic cement IV/A IV/B CEM V
29、 Composite cement V/A V/B *The method is incapable of distinguishing between limestones of type L and LL NOTE 1 Where cements contain calcareous fly ash, burnt shale and/or constituents that partly contain mineral phases, similar to those of clinker, further investigation into the characteristics of
30、 those constituents will be necessary before the method can be applied. CEN/TR 196-4:20076 The method of choice has limitations, as indicated earlier, and cannot be considered to be a means by which clinker content can simply be determined in isolation from any other constituent. Clinker content is
31、determined by difference and other constituents contain, in part, mineral phases similar to those present in clinker and can cause interferences that lead to difficulties in interpretation of the results. Where apparently anomalous results are obtained, it is recommended that further investigations
32、are undertaken in accordance with the procedure given in Section 6.2.5.4. Any other method with the same objectives, and intended for use where the constituents are unavailable for separate analysis, can be considered to be an alternative to the method of choice when it is shown that, with appropria
33、te statistical validity, it gives equivalent results. In individual cases, where the laboratory has been formally advised that: the cement contains only two constituents, the method is greatly simplified because it is sufficient to determine the set regulator content (R) in order to be able to calcu
34、late the clinker content by difference; the cement contains only three constituents, i.e. a set regulator, clinker and one of the following three: slag, pozzolana or siliceous fIy ash. Some of the methods in clause 7 are variations on the method of choice whereas others are based on physical separat
35、ion of constituents and different analytical principles. NOTE 2 This European Technical Report adopts the following use of terms for major constituents: Portland cement clinker as defined in EN 197-1 is referred to as clinker; granulated blastfurnace slag as defined in EN 197-1 is referred to as sla
36、g; natural pozzolans as defined in EN 197-1 is referred to as pozzolans; siliceous fly ash as defined in EN 197-1 is referred to as fly ash; calcium sulfate as defined in EN 197-1 is referred to as set regulator. 2 Normative references This European Technical Report incorporates by dated or undated
37、reference provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Technical Report only wh
38、en incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. EN 196-2, Methods of testing cement Part 2: Chemical analysis of cements EN 196-7, Methods of testing cement Part 7: Methods of taking and preparing samples of cement EN
39、197-1, Cement Part 1: Composition, specifications and conformity criteria for common cements ISO 3534, Statistics Vocabulary and symbols CEN/TR 196-4:20077 3 General requirements for testing 3.1 Number of tests To carry out the calculation for the contents of the cement constituents, two tests shall
40、 be made for each. The following analytes are determined: for the method of choice by selective dissolution (clause 6): sulfuric anhydride and carbon dioxide contents, residues after EDTA and nitric acid dissolution and sulfide contents in the cement and in the EDTA residue; for the methods of analy
41、sis for cements with three constituents (clause 7): sulfuric anhydride and carbon dioxide contents, loss on ignition, calcium oxide, magnesium oxide and manganese oxide contents, sulfide contents and insoluble residues. Depending on the method used, only some of these analytes can be determined. If,
42、 for each analyte, the difference between the two values obtained is less than twice the standard deviation for repeatability for this analyte, the value to take for further calculations is the arithmetic mean of the two values. If the difference between the two values is greater than twice the stan
43、dard deviation for repeatability, a third test shall be carried out and the value to be taken for further calculations shall be the arithmetic mean of the two closest values. Hence, for the method of choice by selective dissolution, only one calculation will need to be carried out for the quantitati
44、ve determination of constituents, in particular for clinker. Likewise, for the methods of analysis for cements with three constituents, a single calculation will enable the content of hydraulic or pozzolanic constituent to be determined. The standard deviations for repeatability of the various analy
45、tes to be considered, most of which can be found in EN 196-2: 2005, are as follows: Analyte Standard deviation for repeatability (srin % by mass) SO30,07 CO2a (EDTA residue) 0,50 b (HNO3residue) 0,11 S2-0,02 CaO 0,18 MgO 0,15 MnO 0,003 insoluble residue 0,10 loss on ignition 0,04 3.2 Determination o
46、f constant mass Constant mass shall be determined by making successive 15 min ignitions, followed each time by cooling and then by weighing. Constant mass is reached when the difference between two successive weighing is less than 0,0005 g. CEN/TR 196-4:20078 3.3 Expression of masses and results Exp
47、ress masses in grams to the nearest 0,0001 g. Express the values for the analytes, given by the mean of two determinations (see 3.1) as the contents of constituents calculated in percentages, to one decimal place. 3.4 Repeatability and reproducibility Repeatability - Precision under repeatability co
48、nditions where independent test results are obtained with the same method on identical 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 obtain
49、ed with the same method on identical test items (material) in different laboratories 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 absolute percent and relate to clinker contents for the general method of determination of the constituents by selective dissolution and to hydraulic and pozzolanic contents for the methods of analysis of cement with thre
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