EN 196-5-2011 en Methods of testing cement - Part 5 Pozzolanicity test for pozzolanic cement《测试水泥的方法 火山灰水泥的火山灰性试验》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 196-5:2011Methods of testing cementPart 5: Pozzolanicity test for pozzolaniccementBS EN 196-5:2011 BRITISH STANDARDNational forewordThis British Standard is the UK implemen

2、tation of EN 196-5:2011. Itsupersedes BS EN 196-5:2005 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee B/516/12, Sampling and testing.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does

3、not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 71441 2ICS 91.100.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of th

4、eStandards Policy and Strategy Committee on 30 April 2011.Amendments issued since publicationDate Text affectedBS EN 196-5:2011EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 196-5 March 2011 ICS 91.100.10 Supersedes EN 196-5:2005English Version Methods of testing cement - Part 5: Pozzolanicity

5、 test for pozzolanic cement Mthodes dessais des ciments - Partie 5: Essai de pouzzolanicit des ciments pouzzolaniques Prfverfahren fr Zement - Teil 5: Prfung der Puzzolanitt von Puzzolanzementen This European Standard was approved by CEN on 20 February 2011. CEN members are bound to comply with the

6、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 application to the CEN-CENELEC Management

7、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 Management Centre has the same status as

8、 the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Rom

9、ania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved

10、 worldwide for CEN national Members. Ref. No. EN 196-5:2011: EBS EN 196-5:2011EN 196-5:2011 (E) 2 Contents Page Foreword . 31 Scope 52 Normative references . 53 Principle . 54 General requirements for testing 54.1 Number of tests . 54.2 Repeatability and reproducibility 54.3 Expression of masses, vo

11、lumes and factors . 64.4 Determination of constant mass . 65 Preparation of a test sample of cement 66 Reagents 67 Apparatus 78 Standardization of solutions 88.1 Standardization of the EDTA solution 88.2 Standardization of the 0,1 mol/l solution of hydrochloric acid 99 Procedure 99.1 Storage and fil

12、tration 99.2 Determination of the hydroxyl ion concentration 99.3 Determination of the calcium oxide concentration . 1010 Results . 1010.1 Calculation and expression of results 1010.2 Assessment of pozzolanicity . 1010.3 Repeatability and reproducibility 1111 Reporting of results 11Bibliography . 12

13、BS EN 196-5:2011EN 196-5:2011 (E) 3 Foreword This document (EN 196-5:2011) has been prepared by Technical Committee CEN/TC 51 “Cement and building limes”, the secretariat of which is held by NBN. This European Standard shall be given the status of a national standard, either by publication of an ide

14、ntical text or by endorsement, at the latest by September 2011, and conflicting national standards shall be withdrawn at the latest by September 2011. 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

15、 held responsible for identifying any or all such patent rights. This document supersedes EN 196-5:2005. This European Standard on the methods of testing cement comprises the following Parts: EN 196-1, Methods of testing cement Part 1: Determination of strength; EN 196-2, Methods of testing cement P

16、art 2: Chemical analysis of cement; EN 196-3, Methods of testing cement Part 3: Determination of setting times and soundness; CEN/TR 196-4, Methods of testing cement Part 4: Quantitative determination of constituents; EN 196-5, Methods of testing cement Part 5: Pozzolanicity test for pozzolanic ceme

17、nt; 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 of hydration Solution method; EN 196-9, Methods of testing cement Part 9: Heat of

18、 hydration Semi-adiabatic method; EN 196-10, Methods of testing cement Part 10: Determination of the water-soluble chromium (VI) content of cement. 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

19、 revised and incorporated into EN 196-2. This edition introduces the following technical changes based on comments received by the secretariat: a) the procedure, reagents and layout of the standard have been aligned with the relevant clauses of EN 196-2; b) the procedure for preparation of a test sa

20、mple has been clarified; BS EN 196-5:2011EN 196-5:2011 (E) 4 c) Patton and Reeders reagent has been included as an additional, optional indicator for visual determination of EDTA titrations; d) the specification for apparatus has been extended to include a balance of specified accuracy; apparatus fo

21、r measuring the absorbance of a solution whilst being stirred and a pH meter of specified accuracy. 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, Croatia, C

22、yprus, 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 the United Kingdom. BS EN 196-5:2011EN 196-5:2011 (E)

23、5 1 Scope This European Standard specifies the method of measuring the pozzolanicity of pozzolanic cements conforming to 1 EN 197-1. This standard does not apply to Portland pozzolana cements or to pozzolanas. This method constitutes the reference procedure. 2 Normative references The following refe

24、renced 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. EN 196-7, Methods of testing cement Part 7: Methods of taking and p

25、reparing samples of cement EN ISO 385:2005, Laboratory glassware Burettes (ISO 385:2005) EN ISO 835:2007, Laboratory glassware Graduated pipettes (ISO 835:2007) 3 Principle The pozzolanicity is assessed by comparing the concentration of calcium ion, expressed as calcium oxide, present in the aqueous

26、 solution in contact with the hydrated cement, after a fixed period of time, with the quantity of calcium ion capable of saturating a solution of the same alkalinity. The cement is considered to satisfy the test, i.e. gives a positive result, if the concentration of calcium ion in the solution is lo

27、wer than the saturation concentration. NOTE Experiment has shown that a mixture of 20 g of cement and 100 ml of water at 40 C achieves equilibrium after a period of between 8 d and 15 d. If the cement satisfies the test at 8 d (see 10.2) it is not necessary to continue to 15 d. 4 General requirement

28、s for testing 4.1 Number of tests Where the determination is one of a series subject to statistical control, determination by a single test shall be the minimum required. Where the determination is not part of a series subject to statistical control, the number of tests shall be two (see also 10.1).

29、 In the case of dispute, the number of tests shall be two. 4.2 Repeatability and reproducibility Repeatability and reproducibility in this document are expressed as repeatability standard deviation(s) and reproducibility standard deviation(s). BS EN 196-5:2011EN 196-5:2011 (E) 6 4.3 Expression of ma

30、sses, volumes and factors Express masses in grams to the nearest 0,000 1 g and volumes from the burette in millilitres to the nearest 0,05 ml. Express the factors of solutions, given by the mean of three determinations, to three decimal places. 4.4 Determination of constant mass Determine constant m

31、ass by drying for successive periods at the stated temperature, or 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. 5 Preparation of a test sample of cement Befor

32、e starting the determinations, treat the laboratory sample, taken in accordance with EN 196-7, as follows to obtain a homogenous test sample. Take approximately 100 g of the sample using a sample divider or by quartering. Sieve this portion on a 150 m or 125 m sieve until the residue remains constan

33、t. Grind 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 sample is exposed to ambient air o

34、nly for the minimum time. 6 Reagents Use only reagents of analytical quality. References to water mean distilled or de-ionised water having an electrical conductivity 0,5 mS/m. The quantities of reagents listed are to indicate concentrations; actual quantities to be prepared shall be adjusted accord

35、ing to the amounts required. Unless otherwise stated (%) means percent by mass. 6.1 Concentrated hydrochloric acid (HCl), ( = 1,18 g/cm3to 1,19 g/cm3). 6.2 Hydrochloric acid, about 0,1 mol/l, prepared by measuring with a graduated cylinder (7.16) 8,5 ml of concentrated hydrochloric acid (6.1) to a l

36、itre volumetric flask (7.10) containing about 500 ml of water and make up to 1 000ml with water. Determine the factor of normality of the solution as indicated in 8.2. 6.3 Dilute hydrochloric acid (1 + 2), prepared by adding 250 ml of concentrated hydrochloric acid (6.1) to 500 ml water. 6.4 Methyl

37、orange, (dimethylaminoazobenzene p-sodium sulfonate). 6.5 Methyl orange indicator, prepared by dissolving (0,020 0,002) g of methyl orange (6.4) in water and making up to 1 000 ml. 6.6 Sodium hydroxide, (NaOH). 6.7 Sodium hydroxide solution, prepared by dissolving (100 1) g of sodium hydroxide (6.6)

38、 in water and making up to 1 000 ml. 6.8 Calcium carbonate, (CaCO3), dried to constant mass at (200 10) C (purity greater than 99,9 %). BS EN 196-5:2011EN 196-5:2011 (E) 7 6.9 Sodium chloride, (NaCl), dried to constant mass at (110 5) C. 6.10 Murexide, (ammonium purpurate). 6.11 Murexide indicator,

39、prepared by grinding (1,0 0,1) g of murexide with (100 1) g of dry sodium chloride (NaCl). 6.12 EDTA, (dihydrated disodium salt of ethylenediaminetetra-acetic acid). 6.13 EDTA solution, about 0,03 mol/l, prepared by dissolving (11,17 0,01) g of EDTA in water and making up to 1 000 ml. Store in an ai

40、r-tight polyethylene container. Determine the factor of molarity of the solution as indicated in 8.1. 6.14 Sodium carbonate, (Na2CO3), dried to constant mass at (250 10) C. 6.15 Mixed calcein and methylthymol blue indicator, prepared by grinding (0,20 0,02) g calcein (bis bis (carboxymethyl)-amino-m

41、ethyl) 2, 7-fluorescein (fluorescein, Flurorescein di-(methylimino diacetic acid) sodium salt) and (0,10 0,01) g methylthymol blue, sodium salt of 3, 3-bis- bis (carboxy-methyl)-aminomethyl-thymolsulfophthalein, (C37H41N2O13SNa3) with (100 1) g of potassium nitrate (KNO3). 6.16 Calcon indicator, pre

42、pared by grinding (1,0 0,1) g of calcon, sodium 2-hydroxy-4-(2-hydroxy-1-napthylazo) napthalene-1-sulfonate, (Eriochrome Blue-Black R) with (100 1) g of anhydrous sodium sulfate (Na2SO4). 6.17 Patton and Reeders reagent, prepared by mixing (1,0 0,1) g of Calcon carboxylic acid, (2-hydroxy-1-(2-hydro

43、xy-4-sulfo-1-napthylazo)-3-napthoic acid, (C21H14N2O7S), with (100 1) g of anhydrous sodium sulfate (Na2SO4). 7 Apparatus 7.1 500 ml cylindrical polyethylene container, of about 70 mm diameter with a pressure seal-plug locked by a screw plug, capable of preventing evaporation during storage. 7.2 Wid

44、e stem funnel. 7.3 Porcelain Bchner funnel, of 60 mm inner diameter. 7.4 Filter paper, with low porosity (mean pore diameter of about 2 m). 7.5 250 ml vacuum flask. 7.6 250 ml and 400 ml beakers. 7.7 50 ml and 100 ml pipettes, class A of EN ISO 835:2007. 7.8 50 ml burette, class A of EN ISO 385:2005

45、. 7.9 Uniform temperature enclosure, controlled thermostatically at (40 1) C. 7.10 500 ml and 1 000 ml volumetric flasks. 7.11 250 ml conical flask. 7.12 Balance, capable of weighing to an accuracy of 0,000 5 g. BS EN 196-5:2011EN 196-5:2011 (E) 8 7.13 Apparatus for measuring the absorbance, at 520

46、nm and 620 nm of a solution contained in a titration beaker, while stirring. 7.14 Stirrer, e.g. magnetic stirrer, with inert, e.g. PTFE, covered bar. 7.15 pH meter, capable of measuring to an accuracy of 0,05. 7.16 Graduated cylinder of 10ml or 20 ml. 8 Standardization of solutions 8.1 Standardizati

47、on of the EDTA solution Weigh to an accuracy of 0,000 5 g (1,00 0,01) g of calcium carbonate (6.8), m1, and place it in a 400 ml beaker (7.6) with approximately 100 ml of water. Cover the beaker with a watch glass and carefully introduce approximately 10 ml of hydrochloric acid (1 + 2) (6.3). Stir w

48、ith a glass rod and ensure that dissolution is complete, bring to the boil in order to expel the dissolved carbon dioxide. Cool to room temperature, transfer to a volumetric flask (7.10), wash the beaker and watch glass carefully with water, adding the washings to the solution and make up to 1 000 m

49、l with water. Pipette 50 ml of the calcium solution into a beaker suitable for the measuring apparatus (7.13). Then dilute with water to a volume suitable for the operation of the apparatus. Using a pH meter (7.15), adjust the pH of this solution to (12,5 0,2) with the sodium hydroxide solution (6.7). Determine the end-point using one of the following two methods.