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[email protected] • Web: http://infostore.saiglobal.com/store/ In Asia Pacific Contact:- Licensed to Mr George Calvar on 26 May 2015. 1 user personal license only. Copying, copy/pasting, storage & distribution or use on network prohibited. (10530313). Get permission to copy from or network this publication www.saiglobal.com/licensing BRITISH STANDARD Tests for chemical properties of aggregates Part 1: Chemical analysis ICS 91.100.15 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BS EN 1744-1:2009 +A1:2012 BS EN 1744-1:2009+A1:2012 Licensed to Mr George Calvar on 26 May 2015. 1 user personal license only. Copying, copy/pasting, storage & distribution or use on network prohibited. (10530313). Get permission to copy from or network this publication www.saiglobal.com/licensing National foreword This British Standard is the UK implementation of EN 1744-1:2009+A1:2012. It supersedes BS EN 1744-1:2009, which is withdrawn. The start and finish of text introduced or altered by amendment is indicated in the text by tags. Tags indicating changes to CEN text carry the number of the CEN amendment. For example, text altered by CEN amendment A1 is indicated by !". The UK participation in its preparation was entrusted by Technical Committee B/502, Aggregates to Subcommittee B/502/6, Test methods. A list of organizations represented on this subcommittee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May 2010. © The British Standards Institution 2013. Published by BSI Standards Limited 2013 ISBN 978 0 580 76567 4 Amendments/corrigenda issued since publication Date Comments 31 January 2013 Implementation of CEN amendment A1:2012 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 the official versions. Croatia. Hungary. Greece. Latvia. Estonia. Germany. Romania.Part 1: Chemical analysis Essais visant à déterminer les propriétés chimiques des granulats .EUROPEAN STANDARD EN 1744-1:2009+A1 NORME EUROPÉENNE Licensed to Mr George Calvar on 26 May 2015. German). CEN members are the national standards bodies of Austria.100. Ireland. Poland. (10530313). B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Lithuania. Switzerland. France. French. Sweden. Italy. Malta. No. Get permission to copy from or network this publication www. Former Yugoslav Republic of Macedonia. Iceland. Cyprus. Slovakia. Slovenia. This European Standard exists in three official versions (English. Belgium.saiglobal. Spain. storage & distribution or use on network prohibited. Netherlands. Portugal. Norway.Teil 1: Chemische Analyse This European Standard was approved by CEN on 17 October 2009 and includes Amendment 1 approved by CEN on 15 October 2012. Denmark. Bulgaria. Ref. EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: Avenue Marnix 17.15 Supersedes EN 1744-1:2009 English Version Tests for chemical properties of aggregates . Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. Turkey and United Kingdom. CEN 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. EN 1744-1:2009+A1:2012: E . copy/pasting.com/licensing EUROPÄISCHE NORM November 2012 ICS 91. 1 user personal license only.Partie 1: Analyse chimique Prüfverfahren für chemische Eigenschaften von Gesteinskörnungen . Finland. Czech Republic. Luxembourg. Copying. ................... 19 ......... 17 Additional apparatus required for determination of lightweight contaminators (see 14....................................................6 5................................................................................................................. 17 Additional apparatus required for determination of sulfide content (see Clause 13) ..... 13 4........ 11 4.................................................... 15 Apparatus for general purposes ........................................Licensed to Mr George Calvar on 26 May 2015............... 15 Additional apparatus required for determination of water-soluble chloride salts following Volhard (see Clause 7) .................................................... 15 4................................... 15 General requirements .................1 Silicone oil......... 10 4....................................................... 19 Additional apparatus required for determination of free lime by complexometry (see 18....... 7 1 Scope...................... 17 Additional apparatus required for the determination of total sulfur content (see Clause 11) .....2) .......................................... (10530313)............................................................................................... ... copy/pasting....................1 5............. 19 Additional apparatus required for determination of free lime by conductometry (see 18.................................2) ................ 11 4.................................................................10 Reagents for determination of fulvo acid content (see 15................ 14 4............. 1 user personal license only..............................2) ....................... 16 Additional apparatus required for potentiometric determination of water-soluble chloride salts (see Clause 8) ...................................... 13 4..... 11 4............................................................................13 Reagents for determination of free lime by acidimetry (see 18........... 15 4........................................2 Reagents ........................14 Reagent for the determination of the expansion of steel slag (see 19..................5 5...9 Reagents for determination of potential presence of humus (see 15............ 8 2 Normative references ..................9 5.................................3 Reagents for determination of water-soluble chloride salts by potentiometry (Clause 8) ..............................................................3 5............................................................................................................................7 Reagents for determination of acid soluble sulfide content (Clause 13) ...................................................................................... 13 4.............3) ............................................................................................................................. storage & distribution or use on network prohibited...3) .....4 5.............................................................................................1 4..........1) ............... 18 Additional apparatus required for determination of fulvo acid content (see 15....... 9 Reagents for determination of water-soluble chloride salts using the Volhard method (Clause 7) .... 19 Additional apparatus required for determination of organic contaminators by mortar method (see 15...............................................8 5..............................................................2) .............................................................................................2 Hydrochloric acid diluted (1 + 5)......... 11 4.............. 15 5 5............................................................................10 5......................................2 5...... 8 3 Terms and definitions .........................4) ....8 Reagents for determination of lightweight contaminators (see 14...............................11 Reagents for determination of free lime by complexometry (see 18.........1) .................. 9 4 4.......................14............................................................................................2) ...................................................................................................................................................2) ............................... .. 14 4...........................................12 Reagent for determination of free lime by conductometry (see 18............12 5....................................................................................................... Get permission to copy from or network this publication www...............................saiglobal....................................................................14 2 Apparatus .........................................................................................................................................................11 5......................3) ................... 9 General ....7 5...........................14.........................................com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Contents Page Foreword .................................6 Reagents for determination of total sulfur content (Clause 11) ........................................4 Reagent for factory production control determination of water-soluble chloride salts using the Mohr method (Clause 9) ...........................................................13 5......................... 11 4....... Copying...................................5 Reagents for determination of water-soluble sulfates (Clause 10) ............................................................................. 18 Additional apparatus required for determination of the potential presence of humus (see 15..... 17 Additional apparatus required for determination of water-soluble sulfates (see Clause 10) .......................................................................... 16 Additional apparatus required for factory production control determination of water soluble chloride salts following Mohr (see Clause 9) .......................................... 14 4.......3) ............................................................................................................................................................................................. ................. 33 Principle ................................................5 7... 31 Principle ........................ 34 Preparation of extracts ..........1 7... 26 Drying of materials......................................................................1 10........................................................................................... 35 Determination of total sulfur content by acid digestion (Reference method) ........................................................................................3) .... 31 Determination of water soluble sulfates in natural and manufactured aggregates ............................................. 30 Sampling ..........................................2 8.....................................................................................6 10...................... 31 Preparation of extracts .........BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 5.............1 8.......... 26 Ignitions of precipitates..... 22 Additional apparatus required for the determination of dicalcium silicate disintegration of air-cooled blast-furnace slag (see 19...............5 9.................................................................4 9 9............................................................................saiglobal..................................................................................................4 6.........................6 9.................................................. 1 user personal license only..................................................................................................................... 37 3 ..........................2 Determination of total sulfur content .............................................................................................5 6............16 Licensed to Mr George Calvar on 26 May 2015...................................... 27 Check for the absence of chloride ions (silver nitrate test) ....................................................1 10.............................................................. 32 Procedure for the determination of the sulfate content of the extracts ............................................ 31 10 10.........4 9........................7 Determination of water-soluble chloride salts by potentiometry (Alternative method) .1 11.............................................................3 9...1) .............................................15 5.....................................................1 6.. 23 6 6......2 10.................................................. copy/pasting..... 34 Procedure for the determination of the sulfate content of the extracts.......................................................................................................................................................................5 Determination of water-soluble sulfates............. 27 Preparation of test specimens ...........................2.................................................................................3 7.........2 7......... 29 Procedure for the determination of the chloride content of the extracts ..............................1.......... 32 Calculation and expression of results .......................17 5...............................4 10.......................................................................................................................................................................................................... 33 Preparation of test specimen ..............4) ................................................................................................................................................com/licensing 5..................................4 10.......................................................................................................5 10......6 General requirements for testing ............ 26 Number of tests ............. 28 Calculation and expression of results . 30 Preparation of test portion ............. 33 Determination of water soluble sulfates in recycled aggregates ........5).3 6..............................................................................1.......................................................... 29 7...............................................................2....................................................................... 27 7 Determination of water-soluble chloride salts using the Volhard method (Reference method) ............................................................................. 26 Repeatability and reproducibility .......... 29 Sampling..................................................................1. 31 Procedure for the determination of the chloride content of the extracts ............2....2............ storage & distribution or use on network prohibited.......................................................6 8 8....................................................................................... Get permission to copy from or network this publication www................................. 34 11 11............................ factors and results .. ........................................................................................... 30 General ..................... (10530313)......3 8..................................... 31 Calculation and expression of results .............................2 10..........................................................................................................1......................................................................................................................... 32 Preparation of test portion ... using a spectrophotometer .. 29 Calculation and expression of results ...................................................................................................................................2 10.............................................. 32 Preparation of extracts ..................................................................................................................... 30 Principle . 35 Determination of total sulfur content by high temperature combustion (Alternative method) .................. 29 Principle .....................3 10.......................................... 31 Sampling ............................ 28 Procedure for the determination of the chloride content of the extracts ....................... 30 Determination of water-soluble chloride salts using the Mohr method (Alternative method) ...........................................................................................................................................1 10.................................................................................................. 23 Additional apparatus required for determination of the volume expansion of steel slag (see 19.2 6........2 9.................................................... 27 Sampling ............................2............................................ Copying..................................... 26 Expression of mass.............. 27 Preparation of extracts .................................................................4 7.... preparation of test specimens and extracts ...............1..1.......................................................................... 22 Additional apparatus required for the determination of CaO in steel slag by X-ray diffraction (see 18.............................................................................................. volume........................... 33 Sampling ........18 Additional apparatus required for acidimetric determination of free lime (see 18.... 27 Principle ..................................................................................................1 9..................................................................................3 10.............................................................. Licensed to Mr George Calvar on 26 May 2015. 1 user personal license only. Copying, copy/pasting, storage & distribution or use on network prohibited. (10530313). Get permission to copy from or network this publication www.saiglobal.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 11.2.1 11.2.2 11.2.3 11.2.4 11.2.5 Principle ............................................................................................................................................... 37 Sampling .............................................................................................................................................. 37 Preparation of test portion ................................................................................................................. 37 Procedure ............................................................................................................................................ 37 Calculation and expression of results .............................................................................................. 37 12 12.1 12.2 12.3 12.4 12.5 Determination of acid soluble sulfates ............................................................................................. 37 Principle ............................................................................................................................................... 37 Sampling .............................................................................................................................................. 38 Preparation of test portion ................................................................................................................. 38 Procedure ............................................................................................................................................ 38 Calculation and expression of results .............................................................................................. 38 13 13.1 13.2 13.3 13.4 13.5 Determination of acid soluble sulfides ............................................................................................. 39 Principle ............................................................................................................................................... 39 Sampling .............................................................................................................................................. 39 Preparation of test portion ................................................................................................................. 39 Procedure ............................................................................................................................................ 39 Calculation and expression of results .............................................................................................. 40 14 14.1 14.1.1 14.1.2 14.1.3 14.2 14.2.1 14.2.2 14.2.3 14.2.4 Determination of components affecting the surface finish of concrete ....................................... 40 Examination for the presence of reactive iron sulfide particles .................................................... 40 General ................................................................................................................................................. 40 Sampling .............................................................................................................................................. 40 Procedure ............................................................................................................................................ 41 Determination of lightweight contaminators ................................................................................... 41 General ................................................................................................................................................. 41 Principle ............................................................................................................................................... 41 Procedure ............................................................................................................................................ 41 Calculation and expression of results .............................................................................................. 42 15 Determination of organic components affecting the setting and the hardening of cement .................................................................................................................................................. 42 15.1 Determination of potential presence of humus ............................................................................... 42 15.1.1 Principle ............................................................................................................................................... 42 15.1.2 Sampling .............................................................................................................................................. 42 15.1.3 Preparation of test portion ................................................................................................................. 42 15.1.4 Procedure ............................................................................................................................................ 43 15.1.5 Expression of results.......................................................................................................................... 43 15.2 Determination of fulvo acid content .................................................................................................. 43 15.2.1 Principle ............................................................................................................................................... 43 15.2.2 Sampling .............................................................................................................................................. 43 15.2.3 Preparation of test portion ................................................................................................................. 43 15.2.4 Procedure ............................................................................................................................................ 43 15.2.5 Expression of results.......................................................................................................................... 44 15.3 Determination of organic contaminators by mortar method .......................................................... 44 15.3.1 Principle ............................................................................................................................................... 44 15.3.2 Sampling .............................................................................................................................................. 44 15.3.3 Preparation of test portions ............................................................................................................... 44 15.3.4 Preliminary treatment of test portions .............................................................................................. 44 15.3.5 Constituents ........................................................................................................................................ 45 15.3.6 Mix quantities ...................................................................................................................................... 45 15.3.7 Mixing procedure ................................................................................................................................ 45 15.3.8 Measurement of stiffening time ......................................................................................................... 46 15.3.9 Compressive strength of hardened mortar ...................................................................................... 46 15.3.10 Calculation and expression of results .............................................................................................. 46 16 16.1 16.1.1 16.1.2 16.1.3 4 Determination of water solubility ...................................................................................................... 47 Determination of water solubility of aggregate, excluding filler .................................................... 47 Principle ............................................................................................................................................... 47 Sampling .............................................................................................................................................. 47 Preparation of test portion ................................................................................................................. 47 Licensed to Mr George Calvar on 26 May 2015. 1 user personal license only. Copying, copy/pasting, storage & distribution or use on network prohibited. (10530313). Get permission to copy from or network this publication www.saiglobal.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 16.1.4 16.1.5 16.2 16.2.1 16.2.2 16.2.3 16.2.4 16.2.5 Extraction of soluble components .................................................................................................... 47 Calculation and expression of results .............................................................................................. 47 Determination of water solubility of filler ......................................................................................... 48 Principle ............................................................................................................................................... 48 Sampling .............................................................................................................................................. 48 Preparation of test portion ................................................................................................................. 48 Extraction of soluble component ...................................................................................................... 48 Calculation and expression of results .............................................................................................. 48 17 17.1 17.2 17.3 17.4 Determination of loss on ignition ...................................................................................................... 49 Principle ............................................................................................................................................... 49 Sampling and preparation of test portion ........................................................................................ 49 Procedure for the determination of loss on ignition ....................................................................... 49 Calculation and expression of results .............................................................................................. 49 18 18.1 18.2 18.2.1 18.2.2 18.2.3 18.2.4 18.3 18.3.1 18.3.2 18.3.3 18.3.4 18.4 18.4.1 18.4.2 18.4.3 18.4.4 18.5 18.5.1 18.5.2 18.5.3 18.5.4 Determination of free lime in steel slag ............................................................................................ 50 General ................................................................................................................................................. 50 Determination of free lime by complexometry (Reference method) .............................................. 50 Principle ............................................................................................................................................... 50 Sampling and preparation of test portion ........................................................................................ 50 Procedure ............................................................................................................................................ 50 Calculation and expression of results .............................................................................................. 51 Determination of free lime by conductometry (Alternative method) ............................................. 51 Principle ............................................................................................................................................... 51 Sampling and preparation of test portion ........................................................................................ 51 Procedure ............................................................................................................................................ 51 Evaluation and expression of results ............................................................................................... 51 Determination of free lime by acidimetry (Alternative method) ..................................................... 51 Principle ............................................................................................................................................... 51 Sampling and preparation of test portion ........................................................................................ 52 Procedure ............................................................................................................................................ 52 Calculation and expression of results .............................................................................................. 52 Determination of CaO in steel slag by X-ray diffraction ................................................................. 52 Principle ............................................................................................................................................... 52 Procedure of analysis ......................................................................................................................... 53 Calibration procedure ......................................................................................................................... 54 Analytical results ................................................................................................................................ 55 19 19.1 19.1.1 19.1.2 19.1.3 19.1.4 19.1.5 19.1.6 19.2 19.2.1 19.2.2 19.2.3 19.2.4 19.2.5 19.3 19.3.1 19.3.2 19.3.3 19.3.4 19.3.5 19.3.6 Determination of unsoundness of blast-furnace and steel slags .................................................. 55 Determination of dicalcium silicate disintegration of air-cooled blast-furnace slag ................... 55 General ................................................................................................................................................. 55 Principle ............................................................................................................................................... 55 Sampling .............................................................................................................................................. 55 Preparation of test portion ................................................................................................................. 55 Procedure ............................................................................................................................................ 55 Expression of results.......................................................................................................................... 55 Determination of iron disintegration of air-cooled blast-furnace slag .......................................... 56 General ................................................................................................................................................. 56 Principle ............................................................................................................................................... 56 Sampling .............................................................................................................................................. 56 Procedure ............................................................................................................................................ 56 Expression of results.......................................................................................................................... 56 Determination of the expansion of steel slag .................................................................................. 56 General ................................................................................................................................................. 56 Principle ............................................................................................................................................... 56 Sampling .............................................................................................................................................. 56 Preparation and compaction of the specimens ............................................................................... 56 Steam test procedure ......................................................................................................................... 58 Calculation and expression of results .............................................................................................. 58 Annex A (informative) Precision ..................................................................................................................... 60 5 BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) A.1 A.2 Licensed to Mr George Calvar on 26 May 2015. 1 user personal license only. Copying, copy/pasting, storage & distribution or use on network prohibited. (10530313). Get permission to copy from or network this publication www.saiglobal.com/licensing A.3 A.4 A.5 A.6 Symbols ............................................................................................................................................... 60 Determination of water-soluble chloride salts using the Volhard method (Reference method) (See Clause 7)................................................................................................... 60 Determination of water-soluble chloride salts by potentiometry (Alternative method) (See Clause 8) ...................................................................................................................... 60 Determination of water-soluble sulfates in recycled aggregate (See 10.2) .................................. 60 Determination of total sulfur content by acid digestion (Reference method) (See 11.1) ...................................................................................................................................................... 60 Determination of acid soluble sulfates (See Clause 12) ................................................................. 61 Bibliography ..................................................................................................................................................... 62 6 Norway. the national standards organisations of the following countries are bound to implement this European Standard: Austria. This document supersedes !EN 1744-1:2009". Romania. Netherlands. Czech Republic. Portugal. Iceland. Luxembourg. Sweden. and conflicting national standards shall be withdrawn at the latest by May 2012. Spain. Slovakia. Tests for chemical properties of aggregates. Greece. Tests for thermal and weathering properties of aggregates The other parts of EN 1744. The start and finish of text introduced or altered by amendment is indicated in the text by tags ! ". Slovenia. (10530313). copy/pasting.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Foreword This document (EN 1744-1:2009+A1:2012) has been prepared by Technical Committee CEN/TC 154 “Aggregates”. Ireland. Cyprus. Finland. Tests for general properties of aggregates EN 933 (all parts). This standard forms part of a series of tests for chemical properties of aggregates. Bulgaria. Estonia. at the latest by May 2012. Belgium. Croatia. France. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This European Standard shall be given the status of a national standard. Latvia. Tests for mechanical and physical properties of aggregates EN 1367 (all parts). either by publication of an identical text or by endorsement.Licensed to Mr George Calvar on 26 May 2015. Get permission to copy from or network this publication www. Denmark. are: Part 3: Preparation of eluates by leaching of aggregates Part 4: Determination of water susceptibility of fillers for bituminous mixtures Part 5: Determination of acid soluble chloride salts Part 6: Determination of the influence of recycled aggregate extract on the initial setting time of cement According to the CEN/CENELEC Internal Regulations. Switzerland. Copying. Hungary. Poland. Italy. storage & distribution or use on network prohibited.saiglobal. Former Yugoslav Republic of Macedonia. Turkey and the United Kingdom. 7 . Lithuania. Malta. Tests for geometrical properties of aggregates EN 1097 (all parts). This document includes Amendment 1. Germany. the secretariat of which is held by BSI. approved by CEN on 2012-10-15. Test methods for other properties of aggregates are covered by the following European Standards: EN 932 (all parts). Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. 1 user personal license only. 1 user personal license only. Get permission to copy from or network this publication www.com/licensing 1 Scope This European Standard specifies procedures for the chemical analysis of aggregates. Tests for mechanical and physical properties of aggregates — Part 6: Determination of particle density and water absorption ISO 384:1978. only the edition cited applies. For the purpose of type testing and in cases of dispute only the reference method should be used. Laboratory glassware — Burettes 8 . Tests for general properties of aggregates — Part 5: Common equipment and calibration EN 932-6. Tests for general properties of aggregates — Part 2: Methods for reducing laboratory samples EN 932-5. Methods of testing cement — Part 2: Chemical analysis of cement EN 459-2. in certain cases. For other purposes. an alternative method which can be considered as giving equivalent results. Methods of testing cement — Part 1: Determination of strength EN 196-2:2005.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. Methods of test for mortar for masonry — Part 9: Determination of workable life and correction time of fresh mortar EN 1015-11. the test methods specified in this standard may be used for factory production control. Copying. Tests for general properties of aggregates — Part 1: Methods for sampling EN 932-2. Tests for general properties of aggregates — Part 6: Definitions of repeatability and reproducibility EN 933-2. Methods of test for mortar for masonry — Part 11: Determination of flexural and compressive strength of hardened mortar EN 1097-6. EN 196-1. It specifies the reference procedures and. Unless otherwise stated. For dated references. in particular factory production control. copy/pasting. This standard describes the reference methods used for type testing and in cases of dispute (and alternatives methods) for chemical analyses of aggregates. nominal size of apertures EN 1015-4. 2 Normative references The following referenced documents are indispensable for the application of this document. storage & distribution or use on network prohibited.saiglobal. the latest edition of the referenced document (including any amendments) applies. Laboratory glassware — Principles of design and construction of volumetric glassware ISO 385. (10530313). Tests for geometrical properties of aggregates — Part 2: Determination of particle size distribution — Test sieves. For undated references. for audit tests or for type tests. Methods of test for mortar for masonry — Part 4: Determination of consistence of fresh mortar (by plunger penetration) EN 1015-9. Building lime — Part 2: Test methods EN 932-1. other methods may be used provided that an appropriate working relationship with the reference method has been established. 5 are considered sufficiently accurate for the purposes of this European Standard. Laboratory glassware — One-mark volumetric flasks ISO 4788. NOTE 2 Where no tolerances are given for reagent volumes or masses.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) ISO 648.2. 1 user personal license only.1 test portion subsample used as a whole in a single test 3. NOTE 4 All chemicals should be treated as potential poisons with toxic properties and appropriate precautions taken before their use. Laboratory glassware. the following terms and definitions apply.com/licensing ISO 649-1. NOTE 3 Unless otherwise stated reagent solutions may be assumed to have long-term stability. dimensions. In such cases volumes delivered from measuring cylinders and indicated masses using the ordinary balances specified in 5. Get permission to copy from or network this publication www. Laboratory glassware — Density hydrometers for general purposes — Part 1: Specification ISO 1042.3 laboratory sample sample intended for laboratory testing 3. or water of equivalent purity. NOTE 1 Unless otherwise stated "%" means "% by mass". use only analytical grade reagents and demineralized water. (10530313).4 and 5. Copying. Test laboratories can determine the time required to achieve constant mass for specific types and sizes of sample dependent upon the drying capacity of the oven used.1 % NOTE In many cases constant mass can be achieved after a test portion has been dried for a predetermined period in a specified oven at (110 ± 5) °C. Always take time to assess possible hazards before starting any procedures and constant attention should be maintained.4 constant mass successive weighings after drying at least 1 h apart not differing by more than 0. interchangeable conical ground joints. Laboratory glassware — Graduated measuring cylinders DIN 12242-1:1980. tolerances 3 Terms and definitions For the purposes of this document. 3.1 Reagents General 4. 9 . Laboratory glassware — Single-volume pipettes Licensed to Mr George Calvar on 26 May 2015. the values quoted are approximate.2 test specimen sample used in a single determination when a test method requires more than one determination of a property 3.1 Unless otherwise stated. storage & distribution or use on network prohibited. copy/pasting.saiglobal.1. 4 4.2. 2.42 Sulfuric acid : 1. prepared by drying about 20 g of silver nitrate for at least 1 h at a temperature of (110 ± 5) °C.com/licensing 4.5 Ammonium iron (III) sulfate NH4Fe(SO4)2.2. "hydrochloric acid (1+1)" means that 1 volume of concentrated hydrochloric acid is to be mixed with 1 volume of water.987 ± 0.3.3.2. Standardize the solution at weekly intervals.14) and protect from prolonged exposure to sunlight.2. 1 user personal license only. boiling the diluted acid in a fume cupboard (5.6). (10530313). (in mol/l). 4.2. Store the solution in the amber-coloured glass reagent bottle (5.2. Get permission to copy from or network this publication www. approximately 6 mol/l. NOTE 1 For example in 4.1 mol/l. 4.2.91 The degree of dilution shall be indicated as a volumetric sum.18 to 1.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.5-trimethylhexan-1-ol.3) and 1 ml of ammonium iron (III) sulfate indicator solution (4.saiglobal.1. prepared by dissolving 9.15). prepared by adding 100 ml of nitric acid (4. Add the thiocyanate solution from a burette (5. storage & distribution or use on network prohibited. 4. from the following equation: cT = 2.3 Nitric acid (HNO3).13) until the first permanent colour change occurs. and adding 10 ml nitric acid (4.5). that is from white opalescence to pale brown.12H2O indicator solution. or before use if the tests are less frequent.2.17) until it is colourless and leave to cool to room temperature. prepared by adding 60 g of water to 50 g ammonium iron (III) sulfate.84 Ammonium hydroxide : 0. NOTE 2 Ready for use solutions may be used as an alternative.39 to 1.11.88 to 0.6 g ammonium thiocyanate in water and diluting to 1 l in a volumetric flask.4 Chloride free technical grade 3.1) to 150 ml water.001) g of the dried silver nitrate.2 Reagents for determination of water-soluble chloride salts using the Volhard method (Clause 7) 4.2. 4. warming to dissolve.1) into a conical flask (5. left to cool in a desiccator and then weighing (16.2 Concentrated liquid reagents shall have the following densities in g/cm³ at 20 °C: Hydrochloric acid : 1. Copying. Calculate the concentration of the thiocyanate solution cT.2.2.2.1 Silver nitrate (AgNO3) solution. Leave the solution to cool to room temperature and store in a glass bottle (5.4. 4.2.100 mol/l. approximately 0.5/V1 (1) where V1 is the volume of thiocyanate added (in ml). copy/pasting.5) and add 5 ml of nitric acid (4.3). 10 . Pipette 25 ml of silver nitrate solution (4. 0.7 g of potassium thiocyanate or 7.19 Nitric acid : 1. Note the volume of thiocyanate solution added. dissolving in water and diluting to 1 l in a volumetric flask (5.2 Thiocyanate (KSCN or NH4SCN) solution. Leave to stand for at least 24 h and filter through a medium grade filter paper.3 Tin (II) chloride (SnCl2.5.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.2H2O) in 1 l of water. made by dissolving approximately 0. storage & distribution or use on network prohibited. Make up to the mark with freshly boiled and cooled water. and filtered through a medium grade filter paper before use.5 Reagents for determination of water-soluble sulfates (Clause 10) 4.3.7.1) g to the nearest 0.1 mg (6.5. 4.1.2 Ammoniacal zinc sulfate solution.7H2O) in 150 ml water and add 350 ml of concentrated ammonium hydroxide (NH4OH). 4.699 g of dried silver nitrate in a 1 l volumetric flask (5. in powder form.566 8 (2) 11 . two pellets (about 0. 4.4 g) of sodium hydroxide (NaOH) and 25 g of potassium iodide (KI). made by dissolving 50 g of zinc sulfate (ZnSO4.2H2O). NOTE 1 A trace of sodium hydroxide will help to stabilize this solution. 4.7.02 mol/l.7. (10530313).6). but dissolving 1. made by adding 200 ml concentrated hydrochloric acid (4.7. Copying. 4.2 g of lead acetate (Pb(CH3COO)2. Get permission to copy from or network this publication www. then add 50 ml of water).6. leaving to cool and then weighing (1.2 Indicator methyl red (dissolve 20 mg methyl red powder in 50 ml of ethanol. 4.6).1 Hydrogen peroxide (H2O2). prepared by drying about 2 g of sodium chloride at a temperature of (110 ± 5) °C for 1 h to 2 h. prepared by dissolving 10 g of potassium chromate in 100 ml water.6.169 ± 0. 4.1) to 800 ml water.6 ± 0. copy/pasting. 4. made by dissolving successively in freshly boiled and cooled water in a 1 l volumetric flask.saiglobal. 4.3 Reagents for determination of water-soluble chloride salts by potentiometry (Clause 8) 4.01 mol/l.001) g of the dried sodium chloride.016 7 mol/l.1 Silver nitrate (AgNO3) solution.2 Sodium chloride (NaCl) solution. The solution should be discarded when it becomes discoloured.3H2O) in water and making up to 100 ml. The factor F of this solution is calculated from the following equation: F= m1 3. (3. dissolving in water and diluting to 1 l in a volumetric flask (5. 4.2.5 Standard potassium iodate solution containing 0. made by dissolving 100 g of barium chloride (BaCl2.7.3.com/licensing 4. 1 user personal license only.3) of potassium iodate (KIO3) dried at (110 ± 5) °C.1 Hydrochloric acid (HCl) solution.3. 4.4 Metallic chromium (Cr). 0. 30 % concentration.3. prepared using the same procedure as specified in 4.1 Lead acetate solution.7 Reagents for determination of acid soluble sulfide content (Clause 13) 4.6 Reagents for determination of total sulfur content (Clause 11) 4.2 Barium chloride (BaCl2) solution. 0.4 Reagent for factory production control determination of water-soluble chloride salts using the Mohr method (Clause 9) Potassium chromate (K2CrO4) solution. made by dissolving 24.01 × F F = 20 × 3. 4.5H2O) in water and making up to 1 l. (4) . Then add 2 ml of the starch solution (4.6 Sodium thiosulfate solution approximately 0. solutions ten times less concentrated should be used. Get permission to copy from or network this publication www. (10530313). copy/pasting.566 8 × V 3 V3 where m2 12 is the mass of the portion of potassium iodate in g.5) expressed in mol/l. b) Standardization in relation to a known quantity of potassium iodate. NOTE 2 The value of factor F for the solution should be calculated using the mean value of three determinations. determine the factor f of this solution using one of the two methods that follow.5 and 4.1 % by mass.7. Place (70 ± 5) mg of potassium iodate in a 500 ml conical flask and dissolve in approximately 150 ml of water. a) Standardization (preferred method) in relation to the standard potassium iodate solution (4. expressed to three decimal places.1 mol/l sodium thiosulfate solution until a pale yellow colour is obtained. NOTE 1 3.566 8 g/l of potassium iodate corresponds to a solution with exactly 0. V2 is the volume of the approximately 0.com/licensing m1 is the mass of the portion of potassium iodate in g. The factor f of this solution is calculated from the following equation: f = m 1 000 × m2 = 280.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) where Licensed to Mr George Calvar on 26 May 2015.82 g of sodium thiosulfate (Na2S2O3.7) and continue the titration until the colour changes from blue to colourless.01 is the molecular mass of KIO3.016 67 × 214. acidify with 25 ml of hydrochloric acid (1 + 1) and titrate with the approximately 0.7. NOTE 3 If the sulfide content is less than 0.1 mol/l sodium thiosulfate solution used for the titration.5). They are prepared by pipetting 100 ml of the solutions (4. Pipette 20 ml of the standard potassium iodate solution into a 500 ml conical flask and dilute with approximately 150 ml of water.016 67 mol/l of potassium iodate and 214.7.7.363 4 × 2 3.7.1 mol/l. 1 user personal license only.1 mol/l sodium thiosulfate solution to a pale yellow colour.7.566 8 × V2 V2 (3) where F is the factor of the standard potassium iodate solution (4. Add about 1 g of potassium iodide.7) and titrate until the colour changes from blue to colourless. storage & distribution or use on network prohibited. Before each test series.6) into 1 l volumetric flasks and making up to the mark with water. Acidify with 25 ml of hydrochloric acid (1 + 1) and titrate with the approximately 0.7. Copying.saiglobal. Then add 2 ml of the starch solution (4. The factor f of this solution is calculated from the following equation: f = 20 × 0. nl or
[email protected]. storage & distribution or use on network prohibited. 4. shall be checked using a suitable hydrometer (5. made by dissolving 22.02) g/cm at (20 ± 3) °C.6H2O and 5. Fax: +31 (0)76 503 31 81.50 g of CoCl2. UK Tel: +44.9 Reagents for determination of potential presence of humus (see 15.1980.1). shall be checked using a suitable hydrometer (5.4870 AJ Etten-Leur Phone: +31 (0)76 501 53 51. 4.8. (10530313).1). 3.10.7 Starch solution.1). Licensed to Mr George Calvar on 26 May 2015. after cooling to room temperature. 4. Copying. NOTE The solution should be stable for at least two weeks.H2O crystals in water until the density of well stirred solution containing no 3 undissolved crystals is (1. prepared by dissolving 3Na2WO4.com or Intertest Benelux v.1 mol/l sodium thiosulfate solution used for the titration. The relative density of the solution. made taking 1 g of starch (water soluble). after cooling to room temperature.664800.9. NOTE 1 The solution should be stable for at least two weeks.8.1980. SPA 7SZ. 4. 4. The relative density of the solution. Fax: +44.9W03.5 g of water with 1 ml concentrated HCl. expressed to three decimal places. obtained by dissolving 7 kg of ZnCl2 in 3 l of water to obtain a saturated 3 solution of density of (1. 1) Colour scale discs and equivalent standard solutions can be obtained from: Tintometer Ltd.f. 4. cooling to room temperature and diluting to 1 l in a volumetric flask. Wiltshire. Get permission to copy from or network this publication www.2 Standard colour solution.3).6H2O in 279. Solar Way.O. 4.intertest.10 Reagents for determination of fulvo acid content (see 15.2) 4.9.2H2O in 1 l of hydrochloric acid (4.2 Stannous chloride solution. diluted (1 + 23) (4. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of the product named. dissolving in water and making up to 100 ml.0 g of FeCl3. Amesbury.1 Hydrochloric acid.1 A 3 % solution of sodium hydroxide. website: www. Lovibond House.com.5 g of SnCl2. adding 1 g of potassium iodide KI.9. NOTE 2 The standard colour solution (tangerine-orange) is equivalent to Gardner Colour Standard Number°11 or Organic Plate Number°31).nl. copy/pasting. Email:
[email protected] 67 mol/l of potassium NOTE 3 The value of factor f for the solution should be calculated using the mean value of three determinations. 1 user personal license only.2) 4. prepared by dissolving 45.com/licensing NOTE 2 iodate.1 Zinc chloride solution.3). 13 .2 Sodium polytungstate solution (as an alternative to 4.8. NOTE Zinc chloride solution is moderately irritating to skin and mucous membranes.9. P. Store the solution in a glass bottle. Solstice Park. made by dissolving 30 g of sodium hydroxide pellets in water.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) V3 is the volume of the approximately 0.7.tintometer. Equivalent products may be used if they can be shown to lead to the same results.1) 4.625412.nl.566 8 g/l of potassium iodate corresponds to a solution with exactly 0. Box 373 NL . Email:
[email protected] ± 0.02) g/cm at (20 ± 3) °C.o.8 Reagents for determination of lightweight contaminators (see 14. website: www.98 ± 0. 13. cooling to room temperature and diluting to 1 l in a volumetric flask. 2 mol/l.1).1 Reagents for determination of free lime by acidimetry (see 18.11. dried to constant mass at 80 °C.13.acetic acid disodium salt.6).4) Ethyl acetoacetate. for example (1.2) Licensed to Mr George Calvar on 26 May 2015.3) Ethanediol (4. 4. storage & distribution or use on network prohibited.3.11.13. 1 user personal license only. 0. 4. (10530313). Get permission to copy from or network this publication www. 4.5 Solvent solution. 4.11.7 Sodium hydroxide solution.com/licensing 4.11.1 g of thymol blue indicator powder dissolved in 100 ml of 2-methylpropan-l-ol. copy/pasting.11.11.13. 4.2 2-methyl propan-l-ol.11 Reagents for determination of free lime by complexometry (see 18.10).1). 4.11.13. 4.12 Soda-lime.11.8 Indicator. cover and cool to room temperature and dilute to 1 l with water in a volumetric flask (5.785 ± 0.4 Hydrochloric acid. (3. 4. make up 17 ml of hydrochloric acid (4.11 Calcium carbonate (CaCO3) precipitated grade. To prepare this solution. dissolved in water and made up to 1 l. 14 .BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 4.11. 4. (4.13. 4.11. This solution needs to be standardized against a solution of known calcium content (4.4 Hydrochloric acid. Boil the solution to expel carbon dioxide. 4. anhydrous grade.3 ± 0. 4. 4.2 mol/l. NOTE Commercially standardized solutions are available. made by grinding together 1 g of murexide (ammonium purpurate) and 100 g NaCl using a pestle and mortar. 4. 4.10 Standard calcium solution (1 ml = 1 mg of calcium oxide).11. made by dissolving 80 g of sodium hydroxide pellets in water.6 Indicator.2 Propan-2-ol (Isopropanol). 450 ml of ethyl acetoacetate in 3 l of 2-methylpropan-l-ol.9 EDTA solution 1/112 mol/l.002) g CaO/l. Copying.1 g in 100 ml H20). granulated.11.1 Ethanediol (Ethylene glycol). anhydrous.1) to 1 l with 2-methylpropan-l-ol.7 Hydrochloric acid solution approximately 0.13 4. (isobutyl alcohol) anhydrous grade.12 Reagent for determination of free lime by conductometry (see 18.5 Triethanolamine.3 Filter paper pulp.11. 4. anhydrous. 4.13. in anhydrous ethanediol.001) g of pure calcium carbonate (4.6 m-Nitrophenol (0. 4.1).000 ± 0.11.saiglobal. volumetric standard.3 Thymol blue indicator (thymolsulfonephthalein). Dissolve (1. 4. diluted (1+1) (4.11.11) dried at (110 ± 5) °C in a slight excess of (1 + 4) hydrochloric acid. fresh.1) g of ethylenediaminetetra . 5.14. Volumetric glassware of class A accuracy shall be used for audit tests and for type tests. 15 .saiglobal. storage & distribution or use on network prohibited. Apparatus for general purposes 5. (10530313). readable to the nearest 1 g.1 Silicone oil.2 Electric muffle furnace capable of being controlled to maintain a constant temperature in the range of 800 °C to 1 100 °C with an accuracy of ± 25 °C. Get permission to copy from or network this publication www.3 Crushing and grinding equipment to reduce aggregates to sizes that pass through sieves suitable for particular tests while producing a minimum of fines. readable to the nearest 0. capable of weighing up to 1 kg.2. 1 user personal license only.2.1 Well ventilated oven. capable of weighing up to 100 g.1) mg of calcium carbonate (4. 5.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) To standardize this solution.1 General requirements All apparatus shall comply with the general requirements of EN 932-5. capable of being controlled to maintain a constant temperature in the range of 40 °C to 150 °C with an accuracy of ± 5 °C.8 mm to 1. copy/pasting.4. k represents the number of mg of free CaO per ml of standardized hydrochloric acid solution.2. 4. weigh (100 ± 0. 4.2 Hydrochloric acid diluted (1 + 5).6 mm for elementary analysis.13.3) 4. Extract the free lime and titrate in accordance with 18. 5 Apparatus 5.09 × V 4 (5) where V4 is the volume of hydrochloric acid added (in ml). Copying. 5.2.5 Balance.1 mg. readable to the nearest 0.11. expressed to three decimal places.2.6. NOTE 5. Licensed to Mr George Calvar on 26 May 2015. 5.14.01 g.com/licensing Determine the k factor from the following equation: k= 56. 5.2) and calcine for 1 h at 1000 °C.2.4 Balance. NOTE The value of factor k for the solution should be calculated using the mean value of three determinations.11) in a crucible (5. Unless otherwise stated.14 Reagent for the determination of the expansion of steel slag (see 19. equipped with a heat resistant tray made of noncorrodible material.3. capable of weighing up to 10 kg.8 Sodium hydroxide on support granulated about 0.2 Where no tolerances are specified for dimensions. all volumetric glassware shall be of class B accuracy as defined in ISO 384:1978.08 × 100 100. 4. the values quoted are approximate.6 Analytical balance. 14 Amber-coloured glass reagent bottles.2.10 Pipettes. and 300 ml Erlenmeyer flasks for testing filler.selective electrode.2. 5. readable to 0.16 Desiccators.2.3.1 Test sieve.2. 5.2. complying with the requirements of ISO 385.2 Two glass. containing demineralized water.Licensed to Mr George Calvar on 26 May 2015. 5. graduated to 0.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 5. 5.12 Wash bottles. 5.fitted with either a silver electrode (preferably chloridized) or a chloride ion . complying with the requirements of ISO 648.1 A potentiometric titrator suitable for the determination of chloride ion concentration with an electrode system consisting of: a) Measuring electrode . copy/pasting.3. 1 user personal license only.15 Plain glass reagent bottles. storage & distribution or use on network prohibited. 5.3 Additional apparatus required for determination of water-soluble chloride salts following Volhard (see Clause 7) 5.5 Stoppered conical flasks.3. approximately 2 l capacity when testing fine aggregates. 50 ml and 100 ml.3. 250 ml and 500 ml. 5.4.either mercurous sulfate or a double junction silver/silver chloride with chloride free electrolyte in the outer chamber.3. 100 ml and 250 ml capacity. conical flasks.2. plastic or metal bottles. Copying. complying with the requirements of ISO 4788.saiglobal.3. b) Reference electrode . to take the extraction bottles (5. 25 ml.2.7 Hot plate with magnetic stirrer.2.2. complying with the requirements of ISO 1042.18 Watch glass. 5. Get permission to copy from or network this publication www. 5. 16 mm square hole perforated plate complying with the requirements of EN 933-2.4 Two filter funnels. funnels and filter paper. 5.2.4 Additional apparatus required for potentiometric determination of water-soluble chloride salts (see Clause 8) 5.13 Burettes. capacity 10 ml. 50 ml size.2).8 pH meter. (10530313). NOTE The bottles should be approximately 5 l capacity when testing coarse aggregates or lightweight aggregates.3 Mechanical shaker or roller. 5.2.17 Fume cupboard.1 ml.6 Two volumetric flasks. of approximately 100 mm diameter with medium and fine grade filter papers of a diameter appropriate to the size of the funnel.3.9 Beakers. 5. 5. or wide-mouthed Erlenmeyer flasks.1 pH units. 5. 5. capacity of 1 l. 5. with well fitting stoppers. 5. 16 . 5.2.11 Graduated measuring cylinders. 6.6 Additional apparatus required for determination of water-soluble sulfates (see Clause 10) 5. Blanks should be run and if any sulfur is detected the machine should be cleaned until no sulfur is detected in the blanks. silica or platinum are suitable materials for ignition crucibles.7 Additional apparatus required for the determination of total sulfur content (see Clause 11) High temperature combustion apparatus.5 Additional apparatus required for factory production control determination of water soluble chloride salts following Mohr (see Clause 9) Licensed to Mr George Calvar on 26 May 2015. Copying. An appropriate accelerator should be used (for example. as alternative to 5.6. approximately 35 mm in diameter and 40 mm in height and capable of maintaining a constant mass when heated to 1 100 °C. 5. 5. 1 user personal license only. the machine should be recalibrated with appropriate standards and the test repeated. an induction furnace capable of reaching a temperature of at least 2 000 ºC within a 40-second analysis period. with stoppers. Any evolved water vapour should be efficiently trapped. tungsten trioxide or vanadium pentoxide).saiglobal.8 Additional apparatus required for determination of sulfide content (see Clause 13) Typical apparatus for the determination of sulfide content is shown in Figure 1. For this. including aggregates of the type to be tested and pyrite.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 5.3 % sulfate should be determined. This is established by dissolving known quantities of calcium sulfate in hot water and measuring the absorbance of the test solutions.3 Porcelain. NOTE The apparatus should be calibrated regularly using standard materials. Get permission to copy from or network this publication www. 5. The absorbance of the blank solution should always be established and deducted from the test solution.com/licensing Two wide-mouthed plastic bottles of 1 l. If results outside this range are obtained. storage & distribution or use on network prohibited. porosity grade 4.2 Ignition crucibles. 17 . (10530313). copy/pasting. the absorbance of at least five different solutions within the range 0 % to 1.6. Spectrophotometer NOTE The water-soluble sulfate content is obtained from the measured absorbance using a calibration graph. 5.1 Sintered silica filtering crucibles.6. NOTE 5. The standards should cover the range of sulfur content expected.1. approximately 35 mm in diameter and 40 mm in height. 10 Additional apparatus required for determination of the potential presence of humus (see 15. complying with the requirements of ISO 649-1. 18 . 5.1 300 µm and 250 µm sieves complying with EN 933-2.2) 2 Nitrogen or argon 4 Reaction flask Figure 1 — Example of apparatus for the determination of sulfide 5.9.saiglobal. 5. copy/pasting.1) 5.2 Porcelain evaporating basin.000. Get permission to copy from or network this publication www. range 1. Copying.1 4 mm sieve. 1 user personal license only. complying with EN 933-2.950 to 2.3 Hydrometer.10. storage & distribution or use on network prohibited.Licensed to Mr George Calvar on 26 May 2015.9.9. (10530313).2) 5. 5.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Key 1 Lead acetate solution (4.7.1) 3 Ammoniacal solution of zinc sulfate (4.9 Additional apparatus required for determination of lightweight contaminators (see 14.7. 2 Refractory porcelain or silica basins of size suitable for placing inside the muffle furnace.12. with ground glass stopper. 5. with a capacity of approximately 450 ml and an external diameter of approximately 70 mm. 5. capable of maintaining a temperature of (480 ± 25) °C.4 Sintered glass filter.13. 5.1 Stopwatch or a timer.3) 5. with a capacity large enough for calcination of a 2 kg aggregate portion. copy/pasting. 5.11.2 Conductive electrode with ground cone NS 14.10.12.com/licensing 5.2 Volumetric flask.3) 5. Get permission to copy from or network this publication www. Copying. 5. A bottle of a different size can affect the comparison with the standard colour.1 Glass stirring rod.12. complying with the requirements of ISO 1042.4 Hot plate.3 Plunger test apparatus conforming with the requirements of EN 1015-4. 5. 500 ml capacity. 63 µm woven wire cloth complying with the requirements of EN 933-2.3 Magnetic stirrer with temperature controlled water bath. storage & distribution or use on network prohibited.12. 5. 5. 5. 5.12.12 Additional apparatus required for determination of organic contaminators by mortar method (see 15.5 Stiffening rate apparatus conforming with EN 1015-9.2 Clear.11 Additional apparatus required for determination of fulvo acid content (see 15.5 Titration equipment with galvanometer for photoelectric end point determination. NOTE The approximate dimensions are intended to match a bottle that is commercially available. 5.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.11.7 Electric muffle furnace.12. 5.11.11.14 Additional apparatus required for determination of free lime by conductometry (see 18. 1 user personal license only.2) 5.14.12.2) 5.13. 5.4 Mixer complying with the requirements of EN 196-1.1 Measuring vessel (volume approximately 160 ml) with a thermoplastic casing and screw cap with two apertures with ground cone NS 14 as defined in DIN 12242-1:1980. (see Figure 2). 5. 5.6 Flexural and compressive strength apparatus conforming to the requirements of EN 1015-11.13. 5. (10530313). 19 .1 Erlenmeyer flask. 5.13. 250 ml capacity.13. cylindrical glass bottle with stopper. readable to 1 s.14. 5. 10 µm to 16 µm diameter of pores.13.13 Additional apparatus required for determination of free lime by complexometry (see 18.saiglobal. 5.2 Glass filter funnel.6 Test sieve.3 180 mm diameter medium grade filter paper. storage & distribution or use on network prohibited. 20 . Get permission to copy from or network this publication www.saiglobal.4 Conductance meter. Copying. This is established by dissolving known quantities of calcined CaO in ethanediol and measuring the conductance of their solutions. In this case. in each case with three individual measurements.6 Magnetic stirrer with temperature controlled water bath.11) at 1 000 °C until it reaches a constant mass and then cooling in a desiccator which contains absorption materials for water and carbon dioxide.1 °C graduated.8 % (by mass) for the content of free lime.14.1) should be determined. a measured conductance of 100 µS yields a value of 4. 1 user personal license only.14. Licensed to Mr George Calvar on 26 May 2015.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 5.14. NOTE 4 Figure 3 shows the calibration of an ethanediol solution containing calcium oxide at 80 °C and an -1 electrode constant of 0.11. copy/pasting. NOTE 2 The CaO used is produced by calcining CaCO3 (4.3 Thermometer (50 °C to 100 °C): 0.5 Water bath controllable to (80 ± 0. NOTE 3 The value of conductance of the blank solution of ethanediol should be established for each determination and deducted from the test solution. For this. NOTE 1 The free lime content is obtained from the measured conductance using a calibration graph. the conductance of at least five different solutions within the range from 0 mg to 10 mg CaO/100 ml ethanediol (4.com/licensing 5.11. (10530313). with ground cone NS 14. 5.573 cm .1) °C. 5. for example soda-lime.14. 14. storage & distribution or use on network prohibited.2) 3 Polypropylene cap 4 Vessel made of borosilicate glass 5 Plastic casing 6 Water inlet 7 Magnetic stirrer (5.14.6) Figure 2 — Vertical section of a measuring vessel for determination of free lime by conductometry (5. copy/pasting. 1 user personal license only.14. Copying.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Key 1 Thermometer (5. Get permission to copy from or network this publication www.3) 21 .14 and 18.saiglobal.Licensed to Mr George Calvar on 26 May 2015.3) 2 Electrode (5. (10530313). 63 µm woven wire cloth complying with the requirements of EN 933-2. fitted with water-cooled condensers by means of standard-taper inner joints.16 Additional apparatus required for the determination of CaO in steel slag by Xray diffraction (see 18.2 63 µm sieve complying with EN 932-2.4 Glass microfibre filters of 1.15. 5. X = Calcium oxide content of ethanediol solution in mg CaO/100 ml. 5. 63 µm woven wire cloth complying with the requirements of EN 933-2.6 Test sieve. 250 ml or 300 ml capacity. 5.3 nm beads about 2 mm diameter. 5.3).15 Additional apparatus required for acidimetric determination of free lime (see 18. Copying.14. copy/pasting.Licensed to Mr George Calvar on 26 May 2015.15.5 Equipment for vacuum filtration.16.15.15.16. 1 user personal license only.15.1 X-ray diffractometer.15.1) °C. 200 ml.1 Erlenmeyer flasks.8) and the molecular sieve (5. 5. 5.15. (10530313). Figure 3 — Example of a calibration graph 5. Y = Conductance in µS. storage & distribution or use on network prohibited. 5.3 Molecular sieve 0.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Key 1 = 0 mg to 10 mg weighed in 100 ml ethanediol. 5. Measuring temperature (80 ± 0. 5.573 cm .saiglobal.13. Get permission to copy from or network this publication www.7 Test sieve. Electrode -1 constant 0.2 Absorption tubes to fit to the upper part of the condensers and containing the sodium hydroxide (4. 22 .5).4) 5.2 mm retention. Above the heating chamber is the compressed slag specimen in a cylinder with a perforated base. copy/pasting.3) 5.01) mm as shown in Figures 4. storage & distribution or use on network prohibited. 5 and 6. (10530313).17 Additional apparatus required for the determination of dicalcium silicate disintegration of air-cooled blast-furnace slag (see 19.18 Additional apparatus required for determination of the volume expansion of steel slag (see 19.1 Steam unit with test cylinder and displacement indicator with a measuring range of (10 ± 0.6) l/h.18. The water usage should be (1. 5. 1 user personal license only.saiglobal. in which water is heated up to boiling point over heating elements during the test. Key 1 Test cylinder 2 Water gauge 3 Displacement indicator 4 Slag specimen 5 Heating jacket 6 Perforated base 7 Steam 8 Water 9 Heating coil Figure 4 — Vertical section of a typical steam test equipment with two chambers 23 .1) 5.1 Ultra-violet lighting equipment. of wavelength 300 nm to 400 nm with a maximum wavelength intensity at 366 nm. The holes in the base allow steam to rise through the specimen evenly. NOTE The steam equipment consists of one or more chambers.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. Get permission to copy from or network this publication www. Copying. the cylinder is heated to (120 ± 10) °C by a circular heating jacket fitted to the outside wall.1 ± 0.com/licensing 5.17. an internal diameter of about 210 mm and a height of about 120 mm. To prevent condensation building up on the inside of the cylinder due to the heat loss. 49 holes. copy/pasting. Copying.Licensed to Mr George Calvar on 26 May 2015. distributed as given in Figure 6 2 Fabric mat 3 Compacted slag specimen 4 Glass beads. 1 user personal license only. (10530313). Get permission to copy from or network this publication www. allowing steam to pass 8 Perforated plate. (30 ± 5) % open area Figure 5 — Cylinder with sample and loading/measuring equipment 24 . 5 mm diameter 5 Surcharge 6 Displacement indicator 7 Surcharge support.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Key 1 Cylinder with perforated base. 3 mm diameter. storage & distribution or use on network prohibited.saiglobal. 18. 1 user personal license only. with a total scale length of 200 mm of more.5 mm.2 mm.18.6 mm. (10530313). with an approximate frequency of (48 ± 3) Hz and an amplitude of ± 1. 65 mm diameter: 8 holes nd 16 holes rd 24 holes 2 circle. Copying. a Proctor hammer or a hand-held vibrating hammer may be suitable.0 mm and 22.2 Sieves.4 mm.com/licensing Dimensions in millimetres Key Central point: 1 hole st 1 circle. diameter 5 mm. 2.18.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.5 Vibrating table. 11. 16.18. 5.6 Sounding rod graduated to the nearest mm.18. copy/pasting.saiglobal. or another compacting devise which allows a final compaction of the test portion to a void content of (25 ± 3) % (by volume). with mesh sizes 0.0 mm.5 mm. NOTE Other types of vibrating table. 5. complying with EN 933-2. 8. 5. 185 mm diameter: Figure 6 — Drill diagram of the cylinder base 5.3 Glass beads. 125 mm diameter: 3 circle. diameter 210 mm. 5. 5. Get permission to copy from or network this publication www.0 mm.4 Medium grade filter paper. storage & distribution or use on network prohibited. 25 . 05 ml.1). different apparatus. repeat the test and take the mean of the two closest values. The total combined mass of the surcharge. storage & distribution or use on network prohibited. Copying. 6. to three decimal places.13) in ml to the nearest 0.18.4 in g to the nearest 1 g or from the balance specified in 5.7. If the difference between two determinations is more than twice the repeatability standard deviation.2.2. 6. 1 user personal license only.1 mg and volume from the burettes (5.01 %. Express the results of the tests. copy/pasting.saiglobal. given by the mean of three determinations.7 Surcharge with an exterior diameter less than 210 mm (180 mm is typical) with a central hole about 15 mm diameter to allow the stem of the displacement indicator to sit on top of the surcharge support.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. the results for the two determinations shall be reviewed. same apparatus.com/licensing 5.7. 6 6. Get permission to copy from or network this publication www.2.5 to the nearest 0. same laboratory and short time interval).3 Expression of mass. The standard deviations of repeatability and reproducibility are expressed in absolute percentage.3). surcharge support and perforated plate shall be (6 ± 0. The standard deviation of reproducibility gives the closeness of agreement between individual results obtained with the same method on identical material but tested under different conditions (different operators.5. Express the factors of solutions (4. NOTE The values of precision are taken from previous national standards or from cross-testing exercises recognised by CEN. If an accepted value of repeatability is available (Annex A). 4. unless otherwise stated. and to allow steam to escape.2.1 General requirements for testing Number of tests Unless otherwise stated the number of single determinations of the various test methods (see Clauses 7 to 19) is fixed at two (see also 6.2 Repeatability and reproducibility The standard deviation of repeatability gives the closeness of agreement between successive results obtained with the same method on identical material tested under the same conditions (same operator. volume. Record the mass from the ordinary balance specified in 5. 26 . given by the mean of two determinations.01) kg.6 and 4.01 g.2. Recognised values for some of the test methods are given in Annex A (informative). at a temperature of (110 ± 5) °C.6) in g to the nearest 0. factors and results Record the mass from an analytical balance (5.4 Drying of materials Unless otherwise stated in a test method. (10530313).7). as a percentage. different laboratories and/or different times) (see EN 932-6).13. 6. to the nearest 0. materials shall be dried in a well-ventilated oven (5. The method of analysis of the extract is based on that of Volhard titration where an excess of silver nitrate solution is added to the chloride solution and the unreacted portion is back titrated with a standardized solution of thiocyanate.com/licensing Ignite precipitates as follows: Place the filter paper and its contents into a crucible. 7.2. whilst ensuring complete combustion. Allow the crucible and its contents to cool to the room temperature in a desiccator. 27 . Copying.g.4). Get permission to copy from or network this publication www.1 Principle This test is suitable for aggregates where the chloride content derives directly from contact with. Wash the filter and its contents with several ml of water and collect this in a test tube. NOTE batch. Ignite the precipitate for at least 1 h at the stated temperature.6 Check for the absence of chloride ions (silver nitrate test) After five or six washes of a precipitate.5 Ignitions of precipitates Licensed to Mr George Calvar on 26 May 2015. copy/pasting. e. Check for the absence of turbidity or precipitate in the solution. Weigh the crucible and its contents. Add several drops of concentrated nitric acid (4.saiglobal. e.1). Dry the sub-sample at a temperature of (110 ± 5) °C to constant mass (3.3 For marine aggregates the laboratory sample should be representative of the moisture content of the Preparation of test specimens Reduce the laboratory sample by the procedures specified in EN 932-2 to an amount not less than the mass given in Table 1. If necessary. rinse the base of the filter stem with a few drops of water. which has been previously ignited and tarred. appropriate to the upper (D) sieve size of the aggregate. 7. using ammonium iron (III) sulfate solution as an indicator. continue washing. saline water. Dry and then incinerate the filter paper slowly in an oxidizing atmosphere without flaming. The absence of turbidity in the silver nitrate test confirms that the washings are free from chloride ions. typical sea-dredged aggregates.1) and of silver nitrate solution (4. 6. testing a nitric acid extract of the finely ground aggregate can show significantly higher levels of chloride than the water extraction method specified in this clause. storage & distribution or use on network prohibited. The chlorides are expressed in terms of. 1 user personal license only. or immersion in.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 6. (10530313). and reported as.g. from some desert areas. 7 Determination of water-soluble chloride salts using the Volhard method (Reference method) 7. NOTE With some aggregates.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1. the chloride ion content as a percentage by mass of the aggregate. An aggregate test specimen is extracted with water to remove chloride ions. 3) to the bottles. Weigh each bottle and record its mass to the nearest 1 g.13) until all the chloride has been precipitated and then add excess.4) using a 100 ml pipette (5. avoiding excessive grinding.2.com/licensing Sieve the sub-sample through a 16 mm sieve (see 5. medium grade filter papers (5. Get permission to copy from or network this publication www. Add to each bottle a mass of water equal to the mass of the test specimen.3. avoiding loss of solution and rinse the stopper with water. kg 63 50 45 35 31. Agitate the bottles continuously for 60 min by means of the shaker or the roller (5. 7. storage & distribution or use on network prohibited. Add 2 ml of 3. In the case of lightweight aggregates.2.2.3) to the flask followed by silver nitrate solution (4. mix thoroughly and using the procedures specified in EN 932-2 produce two test specimens each with a mass of about (2 ± 0.2.1) and crush any oversize samples to pass the sieve. 1 user personal license only.2. Combine.9).5 15 22. but it is not necessary to filter this off. Then filter the extracts through dry.saiglobal.5. When aggregates containing sulfides (e.4 Minimum mass of sub-sample. allow the solution to digest for 5 min at a temperature just below boiling. Add sufficient silver nitrate to ensure a titre of at least 3 ml of thiocyanate solution.g.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. 28 . Calculate the mass of aggregate in each bottle by difference.3. For lightweight aggregates add 1 l water. Weigh the bottles and contents and record their mass to the nearest 1 g. Record the total volume V5 of silver nitrate solution added. Copying. Cool and add the silver nitrate solution. copy/pasting. mm 7.5).4) until at least 100 ml of clear or slightly opalescent filtrate has been collected in clean dry beakers (5. and shake the flask vigorously to coagulate the precipitate. the two test portions shall each have a volume of about 1 l. Add 5 ml of nitric acid (4.1) from a burette (5.3) kg for coarse aggregates or each with a mass of about (500 ± 75) g for fine aggregates.4 or less 5 Preparation of extracts For coarse aggregates and lightweight aggregates.3. A white precipitate of sulfur may form. Table 1 — Minimum mass of preliminary sub-sample Upper (D) sieve size of the aggregate. collecting the washings in the solution.3).2).2). stopper. (10530313).10) and transfer to a 250 ml capacity flask (5.2.4). use two wide-mouthed bottles of 5 l capacity (5.5 Procedure for the determination of the chloride content of the extracts Take 100 ml of the filtered extract (7. For fine aggregates use two bottles of 2 l capacity (5. slags) are being analysed.5-trimethylhexan-1-ol (4.3. Transfer the test specimens (7.3.3. Carefully loosen the stopper. copy/pasting.003 546 W {V5 .2.4. using a suitable electrode as indicator.2.001 %. NOTE A statement on the precision of the determination of water-soluble chlorides is given in Annex A. Get permission to copy from or network this publication www.2.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.2. Sampling.2 Chloride ion selective electrodes and Gran's plot can also be used.10) and transfer to a 250 ml beaker.4.saiglobal. Record the volume V6 of the thiocyanate solution added.2. W is 1 000 g/mass of the aggregate in g. 8 Determination of water-soluble chloride salts by potentiometry (Alternative method) 8.2) from a burette until the first permanent colour change occurs (from white opalescence to pale brown) and the solution has the same depth of colour as was used for the standardization specified in 4. preparation of test specimens and extracts Follow the procedures specified in 7. W is the water aggregate ratio (in g/g) .3 and 7. V6 is the volume of standardized thiocyanate solution added (in ml). The chloride ions are precipitated from the extracts by means of a standard silver nitrate solution.2).5) followed by the standardized thiocyanate solution (4. The result is given as the mean of the determination on the two extracts as a percentage. Repeat the procedure with the extract from the second test specimen. 1 user personal license only.for lightweight aggregates. The number of determinations on each extract is fixed at one. storage & distribution or use on network prohibited. 29 .1 Principle The aggregate test specimen is extracted in the same way as in 7.3.2.2. 7.3) to a pH value of 2 to 3. Copying. Add by pipette 5 ml of sodium chloride solution (4. 7. NOTE 8.com/licensing Add 5 ml of the ammonium iron (III) sulfate indicator solution (4. (10530313). cT is the concentration of the standardized thiocyanate solution (in mol/l). The titration is executed by potentiometry.3 Procedure for the determination of the chloride content of the extracts Take 50 ml of the filtered extract (7. Acidify with nitric acid (HNO3) (4.(10 cT V6)} (in %) (6) where V5 is the volume of silver nitrate solution (in ml). 8. to the nearest 0.6 Calculation and expression of results Calculate the chloride content C of aggregate from the following equation: C = 0.4) by means of the 50 ml pipette (5. 9. Copying. The extract is then analysed by the method based on Mohr.4 Calculation and expression of results Calculate the chloride content C of aggregate from the following equation: C = 0. copy/pasting.1 General The chloride ion concentration of the aqueous extract of natural aggregate may be determined using instrumental techniques based on conductivity measurement. It is strongly recommended that this procedure is used as a preliminary check before using the test specified in Clause 7 to confirm compliance with a specification. titrate with the silver nitrate solution (4. in ml. 30 . NOTE A statement on the precision of the determination of water-soluble chlorides by potentiometry is given in Annex A. allow the solution to digest for 5 min at a temperature just below boiling. The chloride is titrated with silver nitrate using potassium chromate as an indicator. slags) are being analysed. The amount of sodium chloride added shall be confirmed by a blank test. storage & distribution or use on network prohibited. A white precipitate of sulfur may form.2) added to improve end point recognition having been deducted. Get permission to copy from or network this publication www. 1 user personal license only. if necessary. 8. W is the water aggregate ratio (in g/g) . This test method gives a more rapid method of extraction than the one specified in Clause 7. subtracting 10 ml for the added chloride solution.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.2 Principle An aggregate test portion is rapidly extracted with water at room temperature to remove chloride ions. The result is given as the mean of the determination on the two extracts as a percentage of the nearest 0.3.com/licensing When aggregates containing sulfides (e.saiglobal. 9 Determination of water-soluble chloride salts using the Mohr method (Alternative method) 9.3 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1. the quantity of sodium chloride (4.000 709 V7 W (in %) (7) where V7 is the consumption of silver nitrate solution. (10530313).001 %.3.g.for lightweight aggregates. The chloride ion concentration may also be determined using instrumental methods based on conductivity. Cool the contents of the beaker. The chloride content of the solution is indicated by the consumption of silver nitrate solution relative to the point of inflection of the potential curve.1). This procedure shall only be used for factory production control. W is 1 000 g/mass of the aggregate in g. but it is not necessary to filter this off.4. Repeat the procedure with the extract from the second test specimen. By means of the potentiometric device (5. 9.1). saiglobal.3. at the boiling point.3.4 Preparation of test portion Licensed to Mr George Calvar on 26 May 2015.1 Determination of water soluble sulfates in natural and manufactured aggregates 10. Fasten the watertight bottle closures and mix the contents by shaking at least 20 times.01 mol/l silver nitrate solution (4. Calculate the mass of aggregate in each bottle by difference. (10530313).1.1 Principle An aggregate test specimen is extracted with water to remove water-soluble sulfate ions.2).01 mol/l silver nitrate solution.5 Preparation of extracts For coarse and fine aggregates use two wide-mouthed plastic bottles of 1 l capacity (5.5). Take 25 ml of the supernatant water (9.1) until light red. 10 Determination of water-soluble sulfates 10. Note the volume V8 of the silver nitrate solution used.01 0. 1 user personal license only. For lightweight aggregate add 1 l of water. 31 . 9. Weigh each bottle and record its mass to the nearest 1 g.4) and mix. storage & distribution or use on network prohibited. W is the water aggregate ratio (in g/g) . decant approximately 100 ml into a 250 ml beaker and measure the concentration.2.6 Procedure for the determination of the chloride content of the extracts NOTE If conductivity measurement is being used. use a volume of 1 l. Transfer the test portion into the bottles. The watersoluble sulfate content is determined by precipitation at pH between 1 and 1. Copying.10) and transfer to a 100 ml capacity flask (5. For lightweight aggregate use two bottles of 5 l capacity (5.5) using a 25 ml pipette (5. W is 1 000 g/mass of the aggregate in g.5 by a solution of barium chloride. For lightweight aggregates.7 Calculation and expression of results Calculate the chloride content C of the aggregate from the following equation: C = 0. 9. Allow to settle until the supernatant water is more or less clear. Get permission to copy from or network this publication www. Titrate by means of the 0. Add 4 ml to 6 ml of the potassium chromate solution (4.5).for lightweight aggregates.3.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 9. Add to each bottle a mass of water equal to the mass of aggregate. 9. copy/pasting. Weigh each bottle with its contents and record the mass to the nearest 1 g.com/licensing Reduce the laboratory sample to a test portion with a mass of 250 g using the procedures specified in EN 932-2.0354 5 V8 W 4 (in %) (8) where V8 is the used volume of 0. 2. Get permission to copy from or network this publication www.9). Copying. slags.5 Procedure for the determination of the sulfate content of the extracts With a pipette (5. Dry the sub-sample at a temperature of (110 ± 5) °C to constant mass (3. Combine. For lightweight aggregate. stand the solution in a warm place for 30 min.5. Continue boiling for 15 min so that a precipitate is properly formed. 10.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1.4) until at least 100 ml of clear filtrates have been collected in clean dry beakers (5. Crush any oversize particles to pass the sieve.3 to the bottles. Sieve the sub-sample through a 16 mm sieve (see 5. Weigh each bottle and record its mass to the nearest 1 g. Weigh each bottle and contents and record the mass to the nearest 1 g.1. for example.1. 32 .1).3 Preparation of test portion Reduce the laboratory sample by the procedures specified in EN 932-2 to an amount not less than the mass given in Table 1 (7. are being analysed.3.3.4 Preparation of extracts For coarse or lightweight aggregates use two plastic or metal bottles of 5 l capacity and for fine aggregate use two bottles of 2 l capacity (5. e.3) appropriate to the upper (D) sieve size of the aggregate. Dilute to 300 ml with water and add 10 ml of hydrochloric acid solution (4.2) heated to just below boiling.5. mix thoroughly and using the procedures specified in EN 932-2 produce two test specimens each with a mass of about (2 ± 0.g. slags. While stirring vigorously and maintaining the solution at boiling point.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) The determination is then completed gravimetrically and the sulfate ion content is expressed as a percentage by mass of the aggregate. Calculate the mass of aggregate in each bottle by difference. 10.3) continuously for a minimum of 24 h.3.3) kg for coarse aggregates or each with a mass of about (500 ± 75) g for fine aggregates. Add to each bottle a mass of water equal to twice the mass of the test specimen. NOTE 1 If the aggregate contains sulfides. 1 user personal license only.4).1. copy/pasting.com/licensing This method is applicable when aggregates containing sulfides. storage & distribution or use on network prohibited. 10. add drop-by-drop 5 ml of the barium chloride solution (4. filter through a medium grade filter paper and wash thoroughly with hot distilled water. (10530313).10).1. large crystals of gypsum) that all of the soluble sulfate will not be extracted in 24 h. Filter the extracts through dry. medium-grade filter papers (5. the two test specimens shall have a volume of about 1 l.saiglobal. Bring to the boil and boil for 5 min. Discard the residue and continue as below.2). add 1 l of water.3. avoiding excessive grinding. If a white precipitate forms. transfer 50 ml of filtered extract to a 500 ml beaker. e. Fasten the watertight bottle closures and mix the contents by shaking or rolling (5. Transfer the test specimens obtained as specified in 10.2.1.1).g. 10. NOTE If mechanical agitation equipment is not used and the aggregate and water are merely left in contact with occasional shaking there is a possibility (particularly if the source of sulfate is. In the case of lightweight aggregates. after boiling for 5 min. Licensed to Mr George Calvar on 26 May 2015. 343 m3 (in %) (9) where m3 is the mass of the precipitate of barium sulfate in g. The extraction with hot water removes active sulfates (e. 33 .2.16) and weigh to the nearest 0. storage & distribution or use on network prohibited.6. Cool the crucible in a desiccator (5. (10530313).2) following the procedure specified in 6. If a sintered silica filter crucible is used.saiglobal. Transfer the precipitate of barium sulfate with care to a previously ignited and weighed sintered silica filter crucible (5.g. The water-soluble sulfate content is then determined by spectrophotomery. so that sulfate ions precipitate as barium sulfate. 10.2. Calculate the mass of the precipitate m3 from the increase in mass of the crucible.6).1 mg. Copying.2. W is 1 000 g/mass of the aggregate in g.4116 m3 (in %) 10.1 mg. Alternatively transfer the precipitate with care to a fine filter paper in a glass funnel and filter.1) using suction. copy/pasting.for lightweight aggregates.6 Calculation and expression of results Calculate the soluble sulfate content of the aggregate. Cool the crucible in a desiccator (5. 10.2. Calculate the mass of the precipitate m3 from the increase in mass of the crucible.2. NOTE Results can be expressed in SO4 using the following equation: Soluble SO4 = 2 W 0. Barium chloride is then added to the extract. from the following equation: Soluble SO3 = 2 W 0.2 10.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1. Get permission to copy from or network this publication www. expressed as SO3.16) and weigh to the nearest 0.1 Determination of water soluble sulfates in recycled aggregates Principle An aggregate test specimen is mixed with hot water to extract water-soluble sulfate ions. In either case wash the precipitate several times with hot water until the washings are free from chloride (6. W is the water aggregate ratio (in g/g) . NOTE 2 15 min at the higher temperature should suffice.5.6.com/licensing Stand just below boiling for 30 min then leave in a warm place overnight. Place the crucible and contents in the electric muffle furnace (5. It shall have a mass of at least 3 000 g.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. If the precipitate is filtered through a filter paper. buffered at neutral pH.2).1.2) until no further loss in mass occurs. transfer the filter paper and precipitate to a previously ignited and weighed crucible (5. remove it from the filter flask and dry at (110 ± 5) °C for approximately 30 min and gradually raise the temperature to (925 ± 25) °C in an electric muffle furnace (5.2. gypsum plaster) which are potential sources of unsoundness in the aggregate. 1 user personal license only. whilst maintaining a temperature of (60 ± 5) °C.2 Blank test on the solution Before each determination carry out a blank test using the procedure in 10.2. record the result as CH2O.5. Filter the remainder of the solution and retain it in a third beaker marked as "C". 10. Weigh the test specimen to the nearest 0.9). NOTE The contents of beaker C may be used later for a dilution (10.3.18). If necessary.1 g in a 2 l beaker marked as "A" (5.2. storage & distribution or use on network prohibited.5. After the indicated resting time for the apparatus.3 Preparation of test specimen Licensed to Mr George Calvar on 26 May 2015.2. copy/pasting.5.5. Buffer the filtered solution in beaker B with tartaric acid or nitric acid to obtain a pH value of 7 ± 1. Get permission to copy from or network this publication www.4 Preparation of extracts Weigh (1 000 ± 5) g distilled or demineralized water previously heated at (60 ± 5) °C in a 1 l or 2 l beaker (5.2. Check the pH value of the solution using pH meter (5.2. check the sulfate content of the distilled or demineralized water.2. Take the indicated quantity of buffered solution from beaker B using a pipette and pour it into a suitable test tube.2. The result should normally be 0 mg/l. Follow the procedures outlined for the determination specified in 10.2) and let it stand for the indicated resting time.saiglobal.3. Copying. but without adding barium chloride. allow them to cool.1 Blank test on the water Before each series of determinations. record the result as C0.2.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 10. Add the specified amount of barium chloride solution (4. If the pH value becomes too acid (below 6).5. 34 . Reduce to a test specimen of about (25 ± 0. Immediately add the heated water to the test portion in beaker "A" (10. Cover the beaker with a watch glass (5. 1 user personal license only.2.5.5 Procedure for the determination of the sulfate content of the extracts.3). (10530313). add a little of the retained extract from beaker C to return it to neutrality.2.8). Immediately filter (200 ± 50) ml of the extract solution through a rapid filter into a 500 ml beaker marked as "B".1) g.3). 10. 10. Vigorously shake the test tube for 10 s and read the spectrophotometer result.2. If it is not. using a spectrophotometer 10.9).2. Cover the buffered solution in beaker B and the retained solution in beaker C with a watch glass. Stir content of beaker for (15 ± 1) min with a magnetic stirrer. Take the indicated quantity of distilled or demineralized water using a pipette and pour it into a test tube.2.com/licensing Sieve the laboratory sample through a 4 mm sieve and crush any oversize to pass 4 mm sieve. 5. in grams (g) of the test portion (10.2).5. 10.3).2. as indicated by the manufacturer.5.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 10.2).2.1. If the result exceeds 200 mg/l. Use a pipette to transfer 50 ml of buffered solution from beaker B to another beaker marked as "D".2. Use another pipette to add 50 ml of distilled or demineralized water to beaker D.com/licensing Take the quantity of buffered solution indicated by the manufacturer from beaker B using a pipette and pour it into a test tube or apparatus tank. 1 user personal license only.2.3 Procedure for the determination of sulfate content Licensed to Mr George Calvar on 26 May 2015.4 Calculation and expression of results Calculate the soluble sulfate SO4 content of the recycled aggregate from the following equation: T SO4 = [((CSO4 – C0)/10 000) P/P’] – CH2O ≅ (CSO4 – C0)/250 (10) where T SO4 is the water-soluble sulfate content of the sample.1 Determination of total sulfur content Determination of total sulfur content by acid digestion (Reference method) ! 11. The sulfur content is expressed as a percentage by mass of the aggregate.5.4). P’ is the mass. CH2O is the spectrophotometer result for the water test (10. Add the specified amount of barium chloride solution (4. C0 is the spectrophotometer result for the blank test (10. Vigorously shake the test tube again for 10 s to put any crystals of BaSO4 deposited on the base of the test tube into suspension.3 using the diluted solution and make appropriate adjustments when calculating the results.2.2. copy/pasting.3).5. storage & distribution or use on network prohibited.saiglobal. Stir for 1 min with a magnetic stirrer.2. P is the mass of water in grams (g) used for leaching the sample (10. 11 11.1). Any sulfates are precipitated as barium sulfate (BaSO4) and weighed.5.2. Copying. repeat the operation with a diluted test portion. 35 . Allow to stand for 15 s to allow any air bubbles to disperse and record the spectrophotometer result as CSO4 in mg/l.5. in %. (10530313).1 Principle An aggregate test specimen is treated with hydrogen peroxide and hydrochloric acid to convert any sulfur compounds present to sulfates. Get permission to copy from or network this publication www. CSO4 is the spectrophotometer result (10. Repeat the determination described in 10. Vigorously shake the test tube for 30 s and leave it during for the resting time recommended in the manufacturer’s instructions (usually 5 min to 10 min). 2. Acidify the combined filtrates and washings (which should be about 220 ml in all) with 1 ml concentrated hydrochloric acid and bring it to the boil. Add a small amount of filter paper pulp and warm up the content of the beaker to below the boiling point.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.1) and leave the test specimen in a heat bath for 30 min.4 Procedure Weigh the test portion to the nearest 0.8).1.com/licensing 11.5. 11. copy/pasting.1). While maintaining the solution at boiling point and stirring vigorously.74 (in %) where 36 (11) . Mature. The laboratory sample should be representative of the moisture content of the batch. Wash the contents of the filter once with a little hot. Take approximately 1 g of this material as the test portion. dry the sample at a temperature of (110 ± 5) °C.1. Boil for (5 ± 0. After the dissolution. expressed as S to the nearest 0. Repeat the procedure above (boil. Stepwise crush and reduce the sub-sample to a mass of approximately 20 g and then grind the particles until they all pass the 125 µm sieve. If necessary. precipitate. Add 20 ml distilled water to elutriate. add 10 ml of hydrogen peroxide (4. 11.2).6.1.5 Calculation and expression of results Calculate the total sulfur content of the aggregate.5. Get permission to copy from or network this publication www. Transfer the paper filter and the particles retained on it into the beaker and dissolve in 5 ml concentrated hydrochloric acid (4. NOTE Drying at a higher temperature will oxidise any sulfides.1. Simmer for 30 s and then filter under gentle suction using a medium porosity filter paper. 1 user personal license only. filter and wash) and reject the precipitate if any. Weigh to the nearest 0.1.1 mg and calculate the mass of precipitate m5.1) to which has been added 70 ml hot water. (10530313).saiglobal.5) min.2. filter and ignite the barium sulfate precipitate as specified in 10. using a glass rod and watch glass.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1. In the fume cupboard.1%. Make the solution alkaline by adding ammonium hydroxide (4. storage & distribution or use on network prohibited. Check the alkalinity by using methyl red as an indicator (4.6.1) and warm for 30 min below the boiling point.3 Preparation of test portion Reduce the laboratory sample by the procedures specified in EN 932-2 to an amount not less than the mass specified in Table 1 appropriate to the upper (D) sieve size of the aggregate.2) heated to just below boiling. demineralized water and reserve the filtrates. add drop-by-drop 10 ml of the barium chloride solution (4. from the following formula: S = m5/m4 × 13. add 20 ml hydrochloric acid (1+1) (4. or by using a pH-meter (5.1 mg (m4) into a 400 ml high form beaker (5.9). Copying. 11. 3 The laboratory sample should be representative of the moisture content of the batch. 12 Determination of acid soluble sulfates ! 12. This converts any sulfur compounds present into sulfur dioxide which is quantified by infrared detectors.5 Calculation and expression of results The results should be presented as S.2. The total sulfur content is obtained directly from the readout of the apparatus. Copying. Preparation of test portion Reduce the laboratory sample by the procedures specified in EN 932-2 to an amount not less than the mass specified in Table 1 (7." 11. Stepwise crush and reduce the sub-sample to a mass of approximately 20 g and then grind the particles until they all pass the 125 µm sieve.7) in accordance with the manufacturer's instructions.saiglobal.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) NOTE m5 is the mass of precipitate in grams. dry the sample at a temperature of (110 ± 5) °C.1 Principle An aggregate test portion is ignited at high temperature in an atmosphere of pure oxygen. NOTE 11. The sulfur content is expressed as a percentage by mass of the aggregate. 1 user personal license only.4 Procedure The test portion shall be tested using an appropriate high temperature combustion apparatus (5. Take approximately 1 g of this material as the test specimen. NOTE Drying at a higher temperature will oxidise any sulfides. 11.1 Principle Sulfates are extracted from a test portion of the aggregate by dilute hydrochloric acid.3) appropriate to the upper (D) sieve size of the aggregate. m4 is the mass of the test portion in grams. If necessary. Get permission to copy from or network this publication www. (10530313).2 Determination of total sulfur content by high temperature combustion (Alternative method) 11. to the nearest 0. A statement on the precision of the determination of total sulfur content is given in Annex A.1 %.2. 37 .Licensed to Mr George Calvar on 26 May 2015.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1.2. storage & distribution or use on network prohibited.2. 11. The sulfate ion content is determined by gravimetry and expressed as a percentage by mass of the aggregate. 11. copy/pasting.2. Wash the contents of the filter at least 3 times with a little hot.2).9) and heat to boiling point.1 mg (m6). While maintaining the solution at boiling point and stirring vigorously. Break up the solids with the flattened end of a glass-stirring rod.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1.6. Remove from the source of heat and. The laboratory sample should be representative of the moisture content of the batch.2.2) heated to just below boiling. expressed as SO3 to the nearest 0.5. Simmer for 30 s and then filter under gentle suction using a medium porosity filter paper. dry the sample at a temperature of (110 ± 5) °C.30 (in %) 38 (12) . start the test again using a new test portion. Weigh to the nearest 0. filter and ignite the barium sulfate precipitate as specified in 10. Place 360 ml water and 40 ml of concentrated hydrochloric acid (4. copy/pasting. Check the alkalinity by using methyl red as an indicator (4. or by using a pH-meter (5. from the following formula: Sulfate content (SO3) = m7/m6 × 34.saiglobal. Check the washings to ensure the absence of chloride ions using the silver nitrate test (6. 12. Make the solution alkaline by adding ammonium hydroxide solution (4. demineralised water. 12.6). If it is not clear. Bring to the boil and boil for (5 ± 0.1 mg and calculate the mass of precipitate (m7). sprinkle the test portion on to the acid solution.1) in a 1000 ml conical flask (5. NOTE Drying at a higher temperature will oxidise any sulfides. Get permission to copy from or network this publication www. Allow the solution to digest for (15 ±1) min at a temperature just below boiling.2). 12. Acidify the filtrates and washings by means of hydrochloric acid (1+11) to red coloration of methyl red indicator (4.5) min and then check that the solution is clear.5.4 Procedure Weigh the test portion to the nearest 0.6.3 Preparation of test portion Reduce the laboratory sample by the procedures specified in EN 932-2 to an amount not less than the mass specified in Table 1 appropriate to the upper (D) sieve size of the aggregate.1. Mature.8). Stepwise crush and reduce the sub-sample to a mass of approximately 20 g and then grind the particles until they all pass the 125 µm sieve. storage & distribution or use on network prohibited.1%. while stirring.1. 1 user personal license only.2.2). Copying.5 Calculation and expression of results Calculate the acid soluble sulfate content of the aggregate. (10530313).BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. If necessary. Thoroughly wash the contents of the filter with hot demineralized water. reserve the filtrates and reject the precipitate if any. Take approximately 8 g of this material as the test portion. Adjust the volume to about 600 ml with demineralized water and warm up the content of the beaker to below the boiling point.com/licensing 12. slowly add 40 ml of the barium chloride solution (4. Filter the residue through a medium filter paper into a 1000 ml beaker. 5 g of tin (II) chloride (4. Stepwise crush and reduce the sub-sample to a mass of approximately 20 g and then grind the particles until they all pass the 125 µm sieve. NOTE 2 Chromium contributes to the dissolution of any pyrites (FeS2) that may be present in the aggregate.com/licensing where m7 is the mass of precipitate in grams.1 mg (m8) and transfer into a 250 ml stoppered round bottom flask with a ground glass joint. 1 user personal license only.saiglobal. Disperse the mixture in 50 ml of demineralized water. The precipitated zinc sulfide is determined by iodometry. The sulfides are converted into hydrogen sulfide. Add about 2.1 Principle The test portion is decomposed by hydrochloric acid under reducing conditions. (10530313).2) and 285 ml of demineralized water. Copying. Weigh the test portion to the nearest 0.16 (in %) NOTE 2 A statement on the precision of the determination of the acid soluble sulfate content is given in Annex A.7. NOTE 13. 13. copy/pasting. If necessary. dry the sample at a temperature of (110 ± 5) °C.3) appropriate to the upper (D) sieve size of the aggregate.5 and 4. NOTE Drying at a higher temperature will oxidise any sulfides." 13 Determination of acid soluble sulfides 13.7. 39 . which is carried over by a gaseous stream into an ammoniacal solution of zinc sulfate. reagent solutions ten times more dilute should be used (4.7. Take approximately 1 g of this material as the test specimen.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.7.4 Procedure Use the apparatus shown in 5.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1. storage & distribution or use on network prohibited. m6 is the mass of the test portion in grams. 13.4).8 and Figure 1.1 g of chromium (4.7. NOTE 1 Results can be expressed in SO4 using the following formula: Sulfate content(SO4) = m7/m6 × 41. Fix to the flask the ground neck supporting the separating funnel and connect this neck to the inlet of the condenser.6). Preparation of test portion Reduce the laboratory sample by the procedures specified in EN 932-2 to an amount not less than the mass specified in Table 1 (7. NOTE 1 If the sulfide content is low (< 0.1 %).3) and 0.3 the laboratory sample should be representative of the moisture content of the batch. connect the outlet of the condenser to the glass tube which dips into the beaker containing 15 ml of ammoniacal zinc sulfate solution (4. Get permission to copy from or network this publication www. If no precipitate appears. 14 14. expressed in S. which will serve as a stirrer during the titration. Cool the receiver to 20 °C and add by pipette 10 ml of the 0. f is the factor of the sodium thiosulfate solution as specified in 4.160 3 × {(V9 × F ) − (V10 × f )}(in %) 1 000 × ms ms (13) where V9 is the volume of the potassium iodate solution in ml. V10 is the volume of sodium thiosulfate solution used for the titration in ml. when present at or near the surface of concrete. can cause the formation of brown stains that are very difficult to remove. 40 .016 6 mol/l potassium iodate solution (4. Get permission to copy from or network this publication www. Reconnect the gas supply.1.7.6.1 Determination of components affecting the surface finish of concrete Examination for the presence of reactive iron sulfide particles General This clause specifies methods for detection of iron sulfide particles which.7) and titrate until the colour changes from blue to colourless. (10530313).6) until pale yellow. m8 is the mass of the test portion in g. Copying. Disconnect the outlet tube.7. Check that the extraction is complete by bubbling the outlet into fresh ammoniacal zinc sulfate solution.5) and 25 ml concentrated hydrochloric acid (4.com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Connect the gas supply (nitrogen or argon) and adjust the flow to about 10 ml per min.7.7. Titrate with sodium thiosulfate solution (4.5 Calculation and expression of results Calculate the sulfide content of the aggregate. Aggregates of higher sulfide content will require more than 10 min reaction time for complete transformation of all sulfides to precipitated zinc sulfide.1 14. representative of those suspected to contain iron sulfide.1) from the separating funnel taking care that a small amount of acid remains in the separating funnel to prevent leakage. 14.Licensed to Mr George Calvar on 26 May 2015.2 Sampling The stockpile shall be inspected and approximately 50 particles. Stop the flow of gas. the extraction is complete. 13. F is the factor of the potassium iodate solution as specified in 4. storage & distribution or use on network prohibited.603 ×100 = 0. heat the contents of the flask to boiling and boil for 10 min.7. from the following equation: S= {(V9 × F ) − (V10 × f )}×1. Release 50 ml of hydrochloric acid (1 + 1) (4.1.5.saiglobal. 1 user personal license only. copy/pasting. Then add 2 ml of starch solution (4. shall be taken for testing.1). allowing the floating particles to be retained on the sieve. 14. When a test portion of the fine aggregate is immersed in a liquid with a density just below 2. Gently agitate the floating particles with the glass rod to dislodge any air bubbles that may have caused heavier aggregate particles to float.2. the method can be adapted for use on coarse aggregates by examining larger test portions (see Table 1).9.1) or sodium polytungstate (4. NOTE 2 Where a particular quarry has a history of occasionally producing aggregate containing iron sulfide. lower density particles will float on the surface. store for 28 days in a moist condition and then examine the cement paste for staining. Copying.8. NOTE 1 A blue-green gelatinous precipitate of ferrous sulfate should form within 5 min. When presence of slowly reacting particles is suspected.0.1 Determination of lightweight contaminators General This test is a method for estimating the mass percentage of lightweight particles in fine aggregate.2. This allows them to be removed for examination and quantification. they may be slowly reacting particles. Decant the supernatant solution into a second 2 l beaker through a 250 µm sieve (5.0.8.3 The flotation process cannot be used with lightweight aggregates.9. decant through the sieve again.1 g. The method estimates substances such as lignite and coal which may cause staining or pop-outs on concrete or mortar surfaces. In other cases. Separate the aggregate on the 300 µm sieve (5.2 14. If no brown gelatinous precipitate is formed when the particles are placed in saturated limewater. Spread the test portion over a tray and dry it to constant mass (6.2.1).BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 14.saiglobal. storage & distribution or use on network prohibited.4) at (110 ± 5) °C. (10530313). embed the recovered particles in Portland cement paste.2 Principle Most normal weight fine aggregates for concrete and mortar have a particle density greater than 2. If further particles float on the solution. NOTE 14. Return the solution to the first beaker and agitate the bed of aggregate again.1). This shall be reduced to produce a test portion of mass (350 ± 50) g. Record the mass of the dried test portion (m9) to the nearest 0. Get permission to copy from or network this publication www. If necessary. discarding the finer fraction.1. 41 . copy/pasting. This precipitate changes rapidly to brown ferric hydroxide on exposure to air and light.com/licensing Determine the reactivity of the particles by placing them in a saturated limewater solution. Pour about 1 l of the solution of zinc chloride (4. 14. 1 user personal license only. examine the particles visually to assess as well as possible their propensity to cause staining in mortar or concrete.2) into a 2 l beaker and then pour the aggregate into the solution. Gently agitate the bed of aggregate with a glass rod to assist lightweight particles to leave the bed and rise to the surface of the solution. examination with a low power microscope by a technologist with experience of the quarry may be sufficient to determine whether or not the material is deleterious.3 Procedure Licensed to Mr George Calvar on 26 May 2015. Ensure that none of the heavier aggregate particles pass into the sieve. This reaction should be complete within 30 min and indicates the presence of rapidly reacting iron sulfide. Procedure The minimum quantity of fine aggregate in the laboratory sample shall be 5 kg. Repeat the procedure until all of the floating particles have been collected in the sieve. storage & distribution or use on network prohibited.4 Calculation and expression of results Calculate the percentage of lightweight particles in the aggregate. expressed as mLPC. 15. Sieve the dried particles on a 4 mm sieve (5.25) h.1 g. Dry the sub-sample in a drying oven (5.2.1 %. Preparation of test portion Reduce the laboratory sample by the procedures specified in EN 932-2 to an amount not less than the mass specified in Table 1 (7. NOTE 15. the method does not give a definitive conclusion. NOTE The method is based on the principle that humus develops a dark colour when it reacts sodium hydroxide (NaOH). (10530313).2. the aggregate does not contain an amount of humus that is considered to be significant. Get permission to copy from or network this publication www. 1 user personal license only. 15 Determination of organic components affecting the setting and the hardening of cement 15.2). Cool the basin and then weigh the lightweight particles (m10). copy/pasting.9.1.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. Dry the sieve and contents for (20 ± 4) h at (40 ± 5) °C and then tip the contents into an evaporating basin (5. Copying.10.3 The laboratory sample should be representative of the moisture content of the batch. The humus content of aggregate is estimated from the colour formed when a test portion is shaken in a sodium hydroxide solution. 14. If the solution is clear or only slightly coloured. to the nearest 0. In this case.1.1 15.1. The result shall be recorded to the nearest 0. The intensity of the colour depends on the humus content. A strong colour reaction will usually reflect high humus content.1 Determination of potential presence of humus Principle Humus is an organic substance which forms in the ground by the decomposition of animal and plant residues.4). 42 . m10 is the mass of oven dried lightweight particles separated from the test portion in g.1) and retain the fraction that passes.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1.1) at (40 ± 5) °C (6.com/licensing Wash the sieve and the particles on it with water until the zinc chloride or sodium polytungstate has been removed. from the following equation: mLPC = (m10/m9)) 100 (in %) (14) where m9 is the mass of the oven dried test portion in g.saiglobal.3) appropriate to the upper (D) sieve size of the aggregate. but can be due to other factors. Complete the drying at (110 ± 5) °C for (4 ± 0. 1. Filter 75 ml of the solution from the flask into a clear glass 250 ml graduated cylinder (5. Get permission to copy from or network this publication www. 15.4 Procedure Carry out the test at a room temperature of (20 ± 2) °C. Stopper the bottle and shake it vigorously for 1 min. (10530313). Add 100 ml of hydrochloric acid (1 + 23) (4. NOTE 15. sulfides are present. If after adding the stannous chloride the solution becomes turbid.3 The laboratory sample should be representative of the moisture content of the batch.9.1 Determination of fulvo acid content Principle This clause specifies a method for the determination of the fulvo acid content of fine aggregates. Fulvo acids are components of the humic acids which have a retarding effect on the hydration of cements. Record whether the colour of the solution is lighter or darker than the standard colour.2). If this happens. Compare the colour of the solution to the standard colour solution (4.2.1).10. using the procedures specified in EN 932-2.10. Use a 10 ml graduated cylinder (5.9.2. The moisture content of the test portion shall not be greater than 10 % by mass of the sample. Fulvo acids dissolve in hydrochloric acid producing a yellow colour.5) g.1. Copying. 15.4) before adding the stannous chloride. Compounds of Fe(III) produce a brown colour in hydrochloric acid.com/licensing 15. 15.2). Allow the flask and its contents to stand for 4 h. 43 .2.11.10. storage & distribution or use on network prohibited.4 Procedure Pour a 3 % sodium hydroxide (NaOH) solution (4.2.2.9). Preparation of test portion Reduce the laboratory sample to a test portion of (100 ± 0.1) into the glass bottle (5.1 and 4.2) to a height of about 80 mm. Shake the bottle to enable air bubbles to escape.2.2 15. contained in a similar clear cylindrical glass bottle.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1. Leave it to stand for 24 h. 15.2.9. Weight the test portion into a 250 ml or 300 ml flask (5.5 Expression of results The test result shall state whether the colour of the solution is Negative Test (lighter than the standard colour) or Positive Test (darker than the standard colour) (4.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. This colour is eliminated by converting Fe(III) compounds to colourless Fe(II) compounds using stannous chloride solution.2). copy/pasting. shaking it occasionally. Then pour some of the test portion into the glass bottle until the height of aggregate and solution is 120 mm. The intensity of the colour increases as the concentration of fulvo acids increases. Test portions with moisture contents greater than 10 % shall be dried at a temperature of (40 ± 5) °C until the moisture content is reduced to 10 % or less.11).11) to add 10 ml of clear stannous chloride solution (4.saiglobal. 1 user personal license only. repeat the test by boiling the solution for 5 min on a hot plate (5. storage & distribution or use on network prohibited.3.12.9. The heated aggregate acts as a control alongside which the original aggregate is compared. Compare the colour of the resulting solution to the standard colour solution (4. NOTE If only a small furnace is available. while the 28-day strength indicates any longer term effect. Mix the contents of the cylinder using a glass stirring rod (5.2).2).4.12.7) at ambient temperature. The laboratory sample shall have a mass of at least 15 kg. each test portion can be divided into two or more parts.5 Expression of results The test result shall state whether the colour of the solution is Negative Test (lighter than the standard colour) or Positive Test (darker than the standard colour) (4.25) h.3 Preparation of test portions Dry the laboratory sample by spreading it onto trays and allowing it to dry naturally in the laboratory at ambient temperature.2 Pour a test portion into a weighed porcelain or silica basin (5. contained in a similar clear glass graduated cylinder (5.1 Retain of the two test portions (15. 15.com/licensing Let the 250 ml graduated cylinder and its contents stand for a further 1 h then fill to the 100 ml graduation mark with hydrochloric acid (1 + 23) (4. Using the procedures specified in EN 932-2. 15. without further treatment. Heat the other two test specimens using the procedure in 15.3) in sealed containers. further reduce the dried laboratory sample to produce four test portions each of (1 900 ± 100) g. (10530313).1 Determination of organic contaminators by mortar method Principle The mortar method is a performance test intended to demonstrate and quantify any effects which organic contaminators in aggregate can have on the stiffening and hardening of mortar.2. 15. or if necessary three times to yield a sub-sample which when added to the first produces a combined mass of no more than 2 kg.4. Preliminary treatment of test portions 15. Copying.3.11. 15.3 15. When reducing the dried laboratory sample to produce test portions for the mortar method.11). NOTE 15. The principle of the method is to prepare two nominally identical mortars and test them for stiffening rate and compressive strength. 15. Get permission to copy from or network this publication www.4. 1 user personal license only. then one test portion shall be split once.1).4 For lightweight aggregate. or twice.2. weigh and place in the muffle furnace (5.10. should a splitting operation produce two test portions each of mass less than 1.2).3. Record whether the colour of the solution is lighter or darker than the standard colour. One mortar contains the test aggregate as received while the other mix is prepared from a duplicate test portion which has been heated to destroy organic matter. and recombined when cool.9. heated and reweighed separately. The parts should be weighed.2.1). Raise the temperature of the furnace to (480 ± 25) °C over a period of (4 ± 0.3. 44 .3. copy/pasting. The stiffening test assesses acceleration or retardation of the setting of the mortar.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. the volume of each test portion shall be 1 l.3.saiglobal.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1.3.8 kg.3. Bring all the materials to a temperature of (20 ± 2) °C before starting the mixing procedure and mix in a room or other controlled environment with a temperature of (20 ± 2) °C and a relative humidity of not less than 50 %.3.3. one for each test portion.4.6.6. Get permission to copy from or network this publication www. 15. Then add to each calculated mass of water.saiglobal.3) penetration of (23 ± 0. The water content of the mortars containing the unheated aggregate shall be chosen to produce a standard consistence. calculate the mass of water required for each mix and weigh to ± 0.3.6 15.2.3) is started for the control aggregate. To establish the required water contents.2.1 Four mixes are required. NOTE 2 Control mixes will usually be prepared a day after the test mixes.1.3.12.1 Mix quantities General requirements and trial mixes Each mortar mix shall contain either a test portion of the unheated aggregate.5) mm.5 Constituents The cement shall be stored in an airtight container. Licensed to Mr George Calvar on 26 May 2015. Prepare each mix using the procedure in 15.3.4. Laboratory conditions should be as similar as practicable on the two mixing days.2 Test mixes Calculated the required mass of cement for each unheated test portion (15.2.6. 15.25) h and then allow the furnace to cool down to ambient temperature (usually overnight). use 300 g of cement for each mortar mix and 30 g for each preliminary test.1).4. defined as a mean plunger (5.3.5 g. (10530313).3.3.5 g. 15. Note the mass of water contained in this last mix and calculate the water-cement ratio. the mass lost by the corresponding portion of aggregate during the heating detailed in 15.6. Using the water-cement ratio obtained using the trial mixes in 15. storage & distribution or use on network prohibited.7. Copying. 15. 45 .3. Weigh the required mass of water to ± 0.3.6. or a test portion of the aggregate previously heated as in 15. 15. For lightweight aggregate.3 Control mixes Ensure that the water-cement ratio of the heated aggregate control mortars is the same as that of unheated aggregate test mortars by first calculating the required mass of cement and water for each mix as in 15.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Maintain the temperature of (480 ± 25) °C for (4 ± 0.com/licensing Repeat this procedure with the second test portion. Weigh the basin and aggregate and record the loss in mass.7 Mixing procedure 15. Reject the trial mixes.6. copy/pasting. This means that the trial mixes and mortar test specimens made with the test aggregate should be prepared on the same day as the heating procedure (15.3. 1 user personal license only. NOTE 1 The unheated test aggregate should have similar moisture content to the heated (control) aggregate when it was weighed before heating. Each mortar mix shall also contain CEM I cement of mass one quarter that of the aggregate mass in the mix.3. Vary the water content successively and measure the consistence of each trial mix until the correct value of consistence is attained. The test portions and the cement shall be weighed to ± 1 g.3. when determined using by the plunger test method given in EN 1015-4. prepare a series of trial mixes using the unheated aggregate.7. (10530313). Get permission to copy from or network this publication www.3.4) and mix for 30 s. 15. Test the prisms for compressive strength after 28-days in accordance with EN 1015-11. 15.3.10. Cover the bowl with a damp cloth and allow to stand for 5 min. Replace the bowl in the mixer and mix the mortar for a further 60 s.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. NOTE Organic contaminators can entrain air in mortar mixes.3.com/licensing 15. 1 user personal license only.10. taking particular care to ensure that no unmixed materials remain at the bottom of the bowl. NOTE A negative result indicates that organic contaminators accelerated the setting of the mortar. Complete this part of the procedure within 60 s.2 Place the test portion and then the cement in the dry mixing bowl (5. Record the 12 compressive strengths for the duplicate test portions of unheated and heated (control) aggregates. 46 . in N/mm². 15.2 Compressive strength Calculate to the nearest 1 % the relative compressive strength S % of the unheated aggregate mortar by the following equation: S = (A/B) 100 ( in %) (15) where A is the mean compressive strength of the six unheated aggregate prisms.10 Calculation and expression of results 15. copy/pasting. Determine the density of each prism on demoulding. Record the stiffening times of the duplicate test portions of unheated and heated (control) aggregates.12.7. storage & distribution or use on network prohibited. in N/mm². 15.1 Stiffening time Calculate the change in stiffening time by subtracting the mean stiffening time of the heated aggregate mortars from the mean stiffening time of the unheated aggregate mortars. Stop the mixer and clean any adhering material from the paddle and sides into the bowl using a scraper.saiglobal.3. using the procedure specified in EN 1015-11. Continue mixing for a further 60 s after all the water has been added.9 Compressive strength of hardened mortar Prepare three 160 mm × 40 mm × 40 mm prisms from each mortar mix. Copying.3. The presence of entrained air can be assessed by comparing the mean mass and density of the two sets of prisms. Entrained air can also affect compressive strength. Express the result to the nearest 15 min.8 Measurement of stiffening time Immediately after completion of mixing of each mortar. determine the stiffening rate in accordance with EN 1015-9.3. Continue mixing and add the water during the next 30 s. B is the mean compressive strength of the six heated (control) aggregate prisms. Filter as much of the supernatant liquid as is practical on a pre-weighed medium-grade filter paper (5. Preparation of test portion Reduce the laboratory sample by the procedures specified in EN 932-2 to an amount not less than the mass specified in Table 1 (7. After extraction. 16. Weigh the dried test portion to the nearest 0.4 Extraction of soluble components Extract the soluble components from the aggregate using the procedure specified in 10. Calculate the mass of dried aggregate by subtracting the masses of the basin and the mass of the filter paper (m12).1.1.1 Determination of water solubility of aggregate. NOTE 16.1 g (m11). 1 user personal license only. to a pre-weighed porcelain evaporating basin (5.com/licensing 16.saiglobal. m12 is the mass of aggregate after extraction in g. Record the result to 0. Copying. from the following equation: WS = m11 − m12 × 100 (in %) m11 (16) where m11 is the mass of aggregate before extraction in g. the recovered aggregate is dried and weighed. excluding filler Principle The aggregate test portion is extracted with twice its own mass of water in accordance with the procedure specified in 10. with the aid of a minimum amount of water. 16.1. Add the filter paper and the retained particles to the aggregate in the basin.9.1.3.4) and weigh to the nearest 0. Get permission to copy from or network this publication www.2. Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1. storage & distribution or use on network prohibited.1. Transfer the settled aggregate from the extraction bottle.1 16.4). Dry the sample at a temperature of (110 ± 5) °C.4 and then allow most of the solids to settle. copy/pasting. Dry and then cool the contents of the basin to constant mass (3.2).1.2 The water solubility of filler is determined using the procedures in 16.1 g. (10530313). 47 .3) appropriate to the upper (D) sieve size of the aggregate.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 16 Determination of water solubility Licensed to Mr George Calvar on 26 May 2015.4 and 6.4.5 Calculation and expression of results Calculate the water solubility of the aggregate. NOTE 16.1 %. expressed as WS.3 The laboratory sample should be representative of the moisture content of the batch.1. each of (5 ± 0. Calculate the mass of filler in each flask by difference (m11). 16. 48 (17) .1 g. determine the calcium hydroxide content (Ka) according to EN 459-2.2.4) and weigh to the nearest 0. expressed as WS. Calculate the mass of dried filler by subtracting the masses of the basin and the mass of the flasks. weigh the two flasks and contents and record their mass to the nearest 0. Dry and then cool the Erlenmeyer flasks. the recovered filler is dried and weighed. Get permission to copy from or network this publication www.com/licensing 16. Stopper the flasks and mix the contents by shaking (5. Take two test specimens. leaving the remaining residue in the Erlenmeyer flasks. filter papers. from the following equation: WS = m11 − m12 × 100 − K a (in %) m11 where m11 is the mass of filler before extraction in g. 16.4 %. with a maximum of 8. Dry the sub sample at a temperature of (110 ± 5) °C to constant mass (6. storage & distribution or use on network prohibited.4 Extraction of soluble component If the filler contains added calcium hydroxide.4). m12 is the mass of filler after extraction in g. 16. add a mass of water equal fifty times the mass of the test specimen. to an amount not less than 25 g.3.2. Copying. After extraction. 1 user personal license only.01 g. To each flask. Weigh two 500 ml Erlenmeyer flasks (5. copy/pasting.2) to the nearest 0.2. funnels and filter papers (m12).3.5 Calculation and expression of results Calculate the water solubility of the filler or the mixed filler. filter funnels.4 and 6.01 g.3 The laboratory sample should be representative of the moisture content of the batch.4).2. Ka is the determined calcium hydroxide content of a mixed filler. (10530313).1 Principle The filler test portion is extracted with fifty times its own mass of water.2.3) continuously with sufficient agitation to avoid any sedimentation for a minimum of 24 h. Filter as much of the supernatant liquid as is practical on a pre-weighed filter funnels fitted with mediumgrade filter paper (5.2 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1.3. NOTE 16. Preparation of test portion Reduce the laboratory sample by the procedures specified in EN 932-2.2) g.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 16. and their contents to constant mass (3.saiglobal. Transfer the test specimens to the flasks.2 Determination of water solubility of filler Licensed to Mr George Calvar on 26 May 2015. Get permission to copy from or network this publication www. By igniting the aggregate in air at (950 ± 25) °C the carbon dioxide and the water not evaporated during drying are driven off. copy/pasting. NOTE 2 17 For fillers that do not contain added calcium hydroxide. Leave the crucible in the furnace for at least 60 min. For other mixed fillers a value of 8. the loss on ignition should be corrected in accordance with EN 196-2:2005. Licensed to Mr George Calvar on 26 May 2015. If the calcium hydroxide value is less than 8. 17. Stepwise crush and reduce the sub-sample to a mass of approximately 20 g and then grind the particles until they all pass the 125 µm sieve. Take (1 ± 0.3 Procedure for the determination of loss on ignition Weigh the test portion to the nearest 0.com/licensing NOTE 1 Mixed filler contains added calcium hydroxide.05) g of this material as the test specimen.4 Calculation and expression of results Calculate the loss on ignition of the aggregate from the following formula: 49 . 17. NOTE 3 This test may be used as an alternative test for humus content.4. the ignition temperature should be (480 ± 25) °C. Determination of loss on ignition ! 17. NOTE 1 If the aggregate contains non-volatile oxidizable constituents.2) which has been previously ignited and tarred. Ka = 0. dry the sample at a temperature of (110 ± 5) °C. In that case temperature should be (480 ± 25) °C.6.2) controlled at (950 ± 25) °C. Copying. NOTE Drying at a higher temperature will oxidise any sulfides.2.1 %. as are any oxidizable volatile elements present. Reduce the laboratory sample by the procedures specified in EN 932-2 to an amount not less than the mass specified in Table 1 (7. 7. NOTE 2 For aggregates produced from incinerator residues.1 Principle The loss on ignition is determined in an oxidizing atmosphere.2 Sampling and preparation of test portion The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1.saiglobal. as in the case of blast-furnace slags.2.16) and then re-weigh (m14).4 % is used.1 mg (m13) into a crucible (5. Place the crucible in the electric furnace (5. The laboratory sample should be representative of the moisture content of the batch. 17.3) appropriate to the upper (D) sieve size of the aggregate. storage & distribution or use on network prohibited.4 % the determined value is used. In the case of calcareous aggregates. If necessary. (10530313).BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Record the result to 0. heating to 950 °C should proceed slowly to minimize the risk of violent decrepitation. Cool the crucible to room temperature in a desiccator (5. 1 user personal license only. 11. Acidify the clear filtrate.11. Coarse iron fragments remaining on the sieve shall be removed.2. copy/pasting.3 but crushing the last 20 g until they all pass a 63 µm sieve and take approximately 0.8) and titrate with EDTA solution (4.1.1) and transfer into the flask. and hydrated lime (Ca(OH)2) which is not expansive. which is potentially expansive.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.4). A blank value shall always be determined from the ethanediol and the reagents. The temperature of ignition used shall be reported.2. extra tests are necessary. Add ten drops of m-nitrophenol solution (4. To distinguish between these two forms of lime.6) and ten drops of triethanolamine (4. which has a layer (approximately 4 mm to 5 mm) of firmly rammed filter paper pulp in ethanediol.11. Seal the flask with the glass stopper and stir in a 70 °C water bath for 30 min after reaching the temperature.5) (to sequester the Mn and Fe ions). and then neutralize with the 2 mol/l NaOH solution (4. Copying.3 Procedure Weigh the test portion to the nearest 0.5 g of this material as the test portion. 1 user personal license only. transfer 50 ml or 100 ml to a glass beaker using a pipette.11.saiglobal. Fill up to the mark and homogenize by shaking.2 18.1 Determination of free lime in steel slag General Each of the methods specified in this clause determine the presence of free lime (CaO).2).11. Add indicator (4. with 10 ml of hydrochloric acid (1 + 1) (4.1 Determination of free lime by complexometry (Reference method) Principle Free lime is extracted from a ground sample of aggregate by hot ethanediol. Measure 50 ml of anhydrous ethanediol (4.9) until the reddish mauve changes to blueish mauve.1 mg (m15) and transfer into the conical flask (5.2.13. 18. Wash out the flask three times with a total of 50 ml propan-2-ol (4.13. Determine the end point of titration by using the photoelectric titration equipment (5.11.13.2 Sampling and preparation of test portion Proceed as specified in 11. Then filter immediately through the sintered glass filter (5. The content of calcium ions in the extract is subsequently determined by complexometric titration. In accordance with the presumed content. Get permission to copy from or network this publication www. 18.com/licensing Loss on ignition = m13 − m14 × 100 (in %) m13 (18) where m13 m14 is the mass of the initial test portion in grams.4) and rinse through with water into the measuring flask (5.5). dilute with water to approximately 500 ml and bring the pH-value to greater than 13 by adding about 10 ml of 2 mol/l NaOH solution. is the mass of ignited test portion in grams. containing the dissolved free lime. 18." 18 18.11. such as thermo gravimetric or X-ray diffraction analysis.7). 50 . (10530313).13.1) already containing a PTFE stirrer.2 and 11.2).2.11. using the magnetic stirrer at 300 rpm to 400 rpm. storage & distribution or use on network prohibited. Express the mass percentage of free lime to the nearest 0. (10530313). 18.4 Calculation and expression of results Licensed to Mr George Calvar on 26 May 2015. stirring with a magnetic stirrer.3. storage & distribution or use on network prohibited.4.3.1 Determination of free lime by acidimetry (Alternative method) Principle Free lime is extracted from a ground sample of aggregate by boiling in ethyl acetoacetate (Franke method). Copying. 18. copy/pasting. The amount of free lime is rounded to the nearest 0.1 %.5 in the case of pipetting 100 ml out of the flask (5. 18. Get permission to copy from or network this publication www.com/licensing Calculate the free lime content of the aggregate from the following equation: Free Lime = (V11 − V12 )× F ×100 (in % ) m15 (19) where V11 is the volume of EDTA solution added (in ml).2 and take (100 ± 0.1) mg of the passing 63 µm material as the test portion. After an extraction time of at least 10 min and when no further change in conductance occurs. 18. V12 is the volume of EDTA solution added for the blank (in ml). 51 .2).1 %.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 18.3. 1 user personal license only.11.2 Sampling and preparation of test portion Proceed as specified in 18.1 Determination of free lime by conductometry (Alternative method) Principle Free lime is extracted from a ground sample of aggregate by hot ethanediol.saiglobal.1) to (80 ± 0. The content of calcium ions in the extract is subsequently determined by conductance measurements. the extract is titrated with a standard 0.2. the extraction process is completed.4 18.4 Evaluation and expression of results Convert the measured conductivity into free lime content using a calibration graph (see Figure 3).3 Procedure Preheat 100 ml of ethanediol (4. F is the EDTA solution factor in mg of CaO per ml. 18.3 18.13.3. NOTE By measuring the conductance during extraction time. the dissolution of the free lime can be monitored directly. Then read off the final conductance value. Add the test portion to this solvent and introduce the measuring electrode. m15 is the mass of the test portion (in g). multiply by 0.1) °C in the measuring vessel (see Figure 2) with the aid of a connected thermostat.2.2 mol/l hydrochloric acid solution. 13. “free lime”. periodic framework of atoms. NOTE If the titration is conducted by means of a recording pH meter. By X-ray diffraction both minerals (free lime = CaO and Portlandite = Ca(OH)2) can be distinguished due to their different crystal structure.2 mol/l hydrochloric acid solution (4.1 Principle In wet chemical analyses “free lime” is determined by selective extraction of the minerals CaO (free lime. 1 user personal license only. reflux at boiling temperature. copy/pasting.7) for 3 h.13.4). 18.1 mg (m16) and transfer into the flask.13.e. (10530313). the hydration 2+ product of CaO).2 and take approximately 1 g of the passing 63 µm material as the test portion. Wash the first flask and residue with 50 ml of 2-methylpropan-l-ol (4. k is the factor defined in 4. NOTE The crystal structure of each mineral is a three-dimensional.saiglobal. Copying. using a stirring rod fitted with a rubber policeman to guide the flow. stirring on the hot plate (5.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 18.2.5) containing ethyl acetoacetate and 2methylpropan-1-ol in the proportion of 3 to 20.13.3). Adjust the flask in position to the water-cooled condenser. 18.7) to a distinct reddish tinge.5 Determination of CaO in steel slag by X-ray diffraction 18. Add 10 to 12 drops of the indicator solution (4. i. 52 . storage & distribution or use on network prohibited.6) to the filtrate and titrate with the standard 0. then filter under vacuum through the glass microfibre filter (5.1).com/licensing Proceed as specified in 18.4 Calculation and expression of results Calculate the free lime content of the aggregate from the following equation: Free lime = k/1 000 V12/m16 100 (in %) (20) where V12 is the volume of hydrochloric acid added (in ml). representing the number of mg of free CaO per ml of standardized hydrochloric acid solution.2). This framework can be described by different sets of parallel lattice planes. in its narrower sense as detrimental slag constituent) and Ca(OH)2 (Portlandite.2 Sampling and preparation of test portion Licensed to Mr George Calvar on 26 May 2015. Each single set of parallel lattice planes has a constant spacing “d”. Remove the hot plate.8) and the molecular sieve (5.4. m16 is the mass of the test portion (in g). fitted with the upper adapter tube containing the sodium hydroxide (4. receiving the filtrate in a second flask. X-ray diffraction can be understood as reflection of X-rays by the different sets of lattice planes.5.13.15.15.7.4. Get permission to copy from or network this publication www.4. Weigh the test portion to the nearest 0. allow to cool. 18. The intensities of the measuring signals are proportional to the concentrations of CaO and Ca(OH)2.13. the filtration of the extract is not necessary.3 Procedure Measure 70 ml of the prepared solvent solution (4.15. The concentration of Ca ions is analysed and expressed as CaO.2. and transfer into the Erlenmeyer flask (5. Then this sub-sample shall be prepared in accordance with the requirements of the X-ray device. 18.2.saiglobal. θ or 2 θ is linked to the d-values of a mineral by Bragg’s law and depends on the wavelength of the used Xrays. 53 . i. 1 user personal license only.1 Procedure of analysis Starting and stopping the X-ray powder diffraction device Follow up the procedure in the instruction manual of the X-ray powder diffraction device used. The laboratory sample taken shall be dried immediately in the laboratory at (110 ± 5) °C until a constant mass (3. 18.895 Å for Portlandite (Ca(OH)2).5. = lattice spacing. = diffraction angle of the reflected X-radiation. = wave length of the used X-radiation. Make sure that there is no serious interference with other minerals of the slag or of impurities in the steel slag.e.2 18.5.3 Analysis Before any operation.389 Å for free lime (CaO) and dCHpeak = 4. commercially available data files. (10530313). Contact with water shall be avoided. 18. due to imperfect crystals and/or partial substitution of Ca by other elements.4) is reached. Copying. X-ray intensities of steel slag minerals usually are broadened peaks.2. Get permission to copy from or network this publication www. copy/pasting. preferably the intensities at dCpeak = 2.5. A sub-sample of at least 30 g shall be crushed until all of it passes a sieve with 63 µm woven wire cloth complying with the requirements of EN 933-2.2 Preparing the sample Sample preparation shall be done within short time to prevent further hydration of CaO by humidity.2. Each mineral is characterized by a set of specific d-values and corresponding intensity ratios. Please note that in X-ray diffraction °θ or °2 θ is frequently used as read-out of the instrument. storage & distribution or use on network prohibited. To perform an analysis of free lime (CaO) and Portlandite (Ca(OH)2) in steel slag strong intensities of these minerals shall be used. make sure that the equipment is in an optimal operational condition (refer to the manual of the X-ray diffraction device).com/licensing n λ = 2 d sin θ where n λ θ d = whole number.5. These sets are listed in literature. For this reason a d-range around the above mentioned intensities shall be scanned.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Any X-ray diffraction device records a signal – called "peak" in the following text – if Bragg’s law is fulfilled: Licensed to Mr George Calvar on 26 May 2015. 54 .3 Calibration procedure 18.2 to determine the contents of free lime. with N = counts (number of detected impulses). Calculate ICH = ICHRange – (ICH1+ICH2)/2. Make a correction for loss of intensity of the X-ray tube. NOTE Considering the temperature of the slag at the moment of the sampling (1 600 °C to 1 700 °C) it can be assumed that hydrated lime (Portlandite) is totally absent. Measure the intensity ICH2 at dCH2 = 4.3.3.01 °2 θ/sec and report the intensity ICRange. 18.01 °2 θ/sec and report the intensity ICHRange.427 Å to dCb2 = 2. (10530313).5.2 Establishing a calibration curve for free lime in steel slag Take reference samples in the converter. 18. these samples are analysed in accordance with 18. 18.saiglobal. After drying.5. ICHRange shall be at least 3 x square root ((ICH1 or ICH2)/2). Calculate IC = ICRange – (ICb1+ICb2)/2.3 Establishing a calibration curve for Portlandite in steel slag The reference samples used for establishing the calibration curve of free lime (CaO) are hydrated during 48 h in a beaker with excess water.860 Å for Portlandite (Ca(OH)2).860 Å for 160 sec.950 Å and dCHb2 = 4. the absence of free lime is confirmed by comparison between the analysis of the hydrated samples and the calibration curve of free lime. Make sure that calibration measurements and analyses are performed under identical operational conditions and same d-values for intensities and background. Use IC for all further calculations.335 Å for free lime (CaO) and dCHb1 = 4. Use ICH for all further calculations. Standard deviation in impulse statistics follows square root (N). EXAMPLE 2 An example of a measuring procedure for Portlandite (Ca(OH)2) is as follows: Measure the intensity ICHb1 at dCHb1 = 4.3 and the calibration curve for the CaO is then established. copy/pasting.860 Å in steps of 0.950 Å to dCHb2 = 4. EXAMPLE 1 An example of a measuring procedure for free lime (CaO) is as follows: Measure the background intensity ICb1 at dCb1 = 2. preferably at: Licensed to Mr George Calvar on 26 May 2015.950 Å for 160 sec.com/licensing dCb1 = 2.427 Å for 160 sec. The diffracted intensity by free lime (CaO) is measured for each of the samples in accordance with 18. Get permission to copy from or network this publication www.5. Scan the range dCb1 = 2.5. Select measuring times for each background left and right of the peaks and the d-ranges that ensure statistic save analytical results. by means of a spoon.2.1 General A calibration curve shall be established that links the intensity of the diffracted ray with the free lime contents on of reference samples with known concentrations based on one of the following methods. 1 user personal license only. After crushing.335 Å for 160 sec.5.427 Å and dCb2 = 2. Scan the range dCHb1 = 4. Copying.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Make a background correction for free lime (CaO) and Portlandite (Ca(OH)2).3.335 Å in steps of 0. Measure the background intensity ICb2 at dCb2 = 2. ICRange shall be at least 3 x square root ((ICb1 + ICb2)/2). storage & distribution or use on network prohibited. 5. (10530313).1. 19.1. bronze or a cinnamon colour on a violet background shall be recorded as suspect with respect to disintegration. shall be deemed sound.3 and the calibration curves for free lime (CaO or (Ca(OH) 2) is then established. Get permission to copy from or network this publication www.1.com/licensing 18. 19.1). 55 . 1 user personal license only. storage & distribution or use on network prohibited. copy/pasting.1 Determination of unsoundness of blast-furnace and steel slags Determination of dicalcium silicate disintegration of air-cooled blast-furnace General This clause specifies the method of determination of the susceptibility to disintegration of crushed blastfurnace lump slag resulting from the inversion of the metastable ß form of the dicalcium silicate to the γ form.2 Principle Broken slag surfaces fluoresce under ultra-violet light in the range of visible light.1. The intensity diffracted by free lime (CaO) or Portlandite (Ca(OH)2) is measured in accordance with 18.4 Analytical results Report the results to an accuracy of 1 %. Copying.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) The intensity diffracted by Portlandite (Ca(OH) 2) is measured in accordance with 18.17.saiglobal.3. 18. 19 19.1.5.5. The aspect and colour of fluorescence enable the detection of slags liable to silicate disintegration.1 slag 19.3 and the calibration curve for (Ca(OH) 2) is then established. Slags which exhibit numerous or clustered large and small bright spots of a yellow. 19. Slags with a uniform shine in various shades of violet and those exhibiting bright spots in a limited number only and uniformly distributed. 19. 19.6 Expression of results Record the observations made on the appearance of freshly broken surfaces.2. Licensed to Mr George Calvar on 26 May 2015. This phenomenon is sometimes improperly called "lime disintegration".1. then split each lump to obtain freshly broken surfaces.4 Establishing a calibration curve for free lime and Portlandite in steel slag Prepare synthetic mixtures of the relevant steel slag and reagent-grade CaO or Ca(OH)2.5 Procedure Carry out the dicalcium silicate disintegration test under ultra-violet light (5.2. then wash and dry the test portion.4 Preparation of test portion Reduce the laboratory sample to a test portion of at least 30 lumps.1.2.3 Sampling Proceed as specified in 11.5. and manganese sulfides. 19. If no pieces disintegrate or crack.2 Principle A compacted slag specimen.2.2. 4 % expansion in the test does not equate to 4 % uniform expansion in the field. Get permission to copy from or network this publication www.4 Preparation and compaction of the specimens The laboratory sample taken shall be dried immediately in the laboratory at (110 ± 5) °C until a constant mass (3. combined from known grain sizes.e. If any pieces disintegrate or crack in the second test the sample shall be regarded as having failed the test. If one or two pieces disintegrate or crack.3. the test shall be repeated with a further 30 test pieces. copy/pasting. (10530313).3 19.2. 19.com/licensing 19.3. 19.2 Licensed to Mr George Calvar on 26 May 2015.2 Principle The iron disintegration occurring by ageing in a humid atmosphere or in rain. is observed by examining the behaviour of pieces of slag which have been immersed in water. resulting from the late hydration of dead burned free lime and/or free magnesium oxide.1 Determination of iron disintegration of air-cooled blast-furnace slag General This clause specifies the method of determination of the susceptibility to disintegration of crushed blastfurnace slag. 19. The values are not directly indicative of those expected in the field.5 Expression of results Record any cracking or disintegration. The test is accelerated due to the elevated temperature and is designed to generate measurable values of expansion for the purpose of categorizing suitable slag. the necessary moisture for reaction with the free lime and free magnesium oxide is continuously conveyed to the test specimen.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) 19. resulting from the hydrolysis of iron.3.1. calculated in % volume in relation to the original volume of the compressed slag specimen. in water at (20 ± 2) °C for two days. i.saiglobal. 19.3.2. is subjected to a flow of steam at 100 °C in a steam unit at ambient pressure. 19.2.3 Sampling Proceed as specified in 11. the sample shall be regarded as having passed the test.1 Determination of the expansion of steel slag General This clause specifies the method of determination of the susceptibility to expansion of crushed steel slag. 1 user personal license only. storage & distribution or use on network prohibited. Copying. 19. but more rapidly under water. 19.2.4) is reached.4 Procedure Place 30 pieces of slag. The increase in volume is given as the result. with a nominal size between 40 mm and 150 mm.3 Sampling The laboratory sample shall be taken in accordance with the procedures specified in EN 932-1. Any change in the volume caused by this reaction is read off from a displacement indicator directly at the top of the specimen. 56 . By this means. Adjust the mass of the layer of beads so that the total mass of the surcharge.18. transfer the prepared test portion to the cylinder (5. After compaction. 1 user personal license only. Finally.2 to 16 14 16 to 22 15 Total 100 NOTE 1 if there are great differences in the particle densities of the individual grain size classes. values conforming to the practice.com/licensing For the steam test use 0 mm to 22 mm test portions of dried mineral mixtures of slag. The expansion shall be determined on at least two test specimens. The sample reduction shall be carried out in accordance with the procedures specified in EN 932-2.5 ± 0. Distribute the glass beads evenly within the test cylinder so that they give a level surface. Copying.5 kg.18. a void content of (25 ± 3) % volume remains in the slag specimen. a sample shall be combined for the determination of the pre-dried particle density. In addition. 57 . The individual grain size classes shall be taken from the crushed aggregates.saiglobal.5 15 0.5 to 2 15 2 to 5.6) and taking the average of four readings on the extremity of two at right angles crossing diameters plus at minimum four additional readings distributed over the specimen surface.5) for 6 min at a frequency of (48 ± 3) Hz (amplitude ± 1. Alternatively. Calculate VC and VA from height measurements with the sounding rod (5. in accordance with EN 1097-6.1) illustrated in Figure 5.6 to 8 10 8 to 11. If water is added to the sample to facilitate compaction.3) which have been lubricated before the test with silicone oil to reduce friction between the individual beads. Cover the perforated base of the test cylinder with a circular filter (fabric mat) and.18. Then dynamically compact the dry specimen on the vibrating table (5.2 11 11.5 kg of beads.6 20 5. The amount of material required for each individual sample is 4. storage & distribution or use on network prohibited. such as a Proctor hammer or a hand-held power hammer.035 N/mm².01) kg. The proportions of mass for the individual grain size classes are given in Table 2. Under these test conditions. Get permission to copy from or network this publication www. (10530313). the mineral mixture can be combined using proportion of volume. cover over the surface of the slag specimen with a circular filter (fabric mat) and then with a layer of glass beads (5. which have been combined in accordance with the Fuller parabola. the sample can be compacted by any other method capable of achieving the same degree of compaction. the surcharge support. Table 2 — Proportions of mass per grain size class Sizes Percentage mm in mass 0 to 0. using a laboratory scoop.18.5 mm) and a static load of 0. the perforated plate and the glass beads equals (7. copy/pasting. Each individual test portion shall be combined separately with the above-mentioned size distribution. determine the volume of the slag specimen VS. produced for example by hydraulic pressure. which is the difference between the volume of the cylinder VC and the volume of air VA between the slag specimen and the top edge of the cylinder.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015.5 g of silicone oil is sufficient for the batch of 1. NOTE 2 1. testing shall commence within 24 h of the completion of the compaction process. it is recommended that the movements be read off at intervals of 15 min. As lime is deposited on the glass beads during the steam test. Get permission to copy from or network this publication www. In the event of a reliable method being developed. Copying. it is possible to shorten the test duration by calculating the end point value using regression. asymptotic approach to a limit value). in the absence.6). If the increase in volume is taken as a function of the time. copy/pasting. Then lay the perforated plate. do not begin recording the displacement until steam is passing freely through the sample. At the end of this period the rise in the test specimen surface is read off and calculated in % volume in relation to the original volume (see 19. 19. it is useful to record the development of the increase in volume as dependent on time. MgO values declared by steel producers are acceptable for use in determining testing time for steel slag. before the steam test. attach the test cylinder to the steam equipment and fit the heating jacket to the outer wall of the test cylinder. the slag test specimen then starts heating up with an expansion of its volume.6 Calculation and expression of results Calculate the volume of the slag test portion VS. it is furthermore necessary to clean off the lime after every fourth steam test with dilute hydrochloric acid. When the MgO content determined in accordance with EN 196-2 is not greater than or equal to 5 %. As the movements at the beginning of the steam test occur sharply.3. After 4 h the interval can be extended to 60 min. The testing time in the steam test depends of the composition of slag. 1 user personal license only. from the following equation: VS = VC . Adjust the displacement indicator vertically in the centre of the perforated plate and fix it to a rigid support on the steam unit. NOTE 1 The total MgO content is used as a measure of free MgO. the testing time shall be 24 h. storage & distribution or use on network prohibited. In order not to register the lifting movements associated with this. VC is the volume of the cylinder (in mm³). a detailed interpretation of the test results can be undertaken by means of the graph (starting climb.VA (21) where VS is the volume of the slag test specimen after compaction in the test cylinder (in mm³). When the MgO content is more than 5 %. For factory production control purposes.3.com/licensing Repeat the lubrication of the glass beads after each steam test. VC and VA are calculated from the height measurements with the sounding rod and the diameter of the cylinder (210 mm).saiglobal. VA is the volume of air between the slag specimen and the top edge of the cylinder (in mm³).5 Steam test procedure After the slag test specimen has been covered with the layer of glass beads. (10530313). After switching on the heating jacket and the steam unit. care shall be taken to prevent a drop in temperature which would interrupt the production of steam.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. the types should be redefined in terms of free MgO content. 19. at present of a reliable method of determining the content of free MgO. 58 . The water container in the steam unit normally is of a size that makes it necessary to top up with water during the test.3. the testing time shall be 168 h. the surcharge support and the surcharge on top of the beads. Therefore. NOTE 2 In many cases. w is the water content of the sample (in percentage mass). VS is the volume of the slag test specimen after compaction in the test cylinder (in mm³). Record the result as the arithmetical mean of the expansion of the two test specimens.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. Copying. ρ is the pre-dried particle density of the slag. 1 user personal license only. and from the internal diameter of the test cylinder (210 mm) from the following equation: Expansion = π × h× d2 4 ×V S × 100 (24) where h is the rise of the specimen after the steam test (in mm). M is the mass of the compressed mixture (in g). (10530313). calculate the expansion in volume % from the rise of the specimen read off the displacement indicator. rounded to the nearest 0.com/licensing After compaction determine the bulk dry density and the void content of the compacted mixture as follows: ρM = 100 × M ×1 000 and V S × (100 + w) Va = (1 − ρM ) ×100 ρ (22) (23) where ρM is the bulk density of the compressed mixture (in Mg/m³). storage & distribution or use on network prohibited. After completing the test.1 % volume. d is the internal diameter of the test cylinder (210 mm). copy/pasting.saiglobal. Va is the void content of the compressed mixture (in % volume). determined as specified in EN 1097-6 (in Mg/m³). 59 . Get permission to copy from or network this publication www. as a percentage by mass of the aggregate) as: r1 = 0.1 r1 Symbols is the repeatability limit as defined in EN 932-6.2) Repeatability r1 and reproducibility R1 have been determined by a French cross testing: two repetitions in eight laboratories.000 4 + 0.124 X A.047 + 0.2 Determination of water-soluble chloride salts using the Volhard method (Reference method) (See Clause 7) The precision of the determination of water-soluble chlorides is stated (in terms of the chloride ion content.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Licensed to Mr George Calvar on 26 May 2015. Get permission to copy from or network this publication www. Copying. A.com/licensing Annex A (informative) Precision A.1) The precision of the determination of total sulfur content is stated (in terms of the sulfur content.022 + 0.081 X and R1 = 0.4 Determination of water-soluble sulfates in recycled aggregate (See 10. as a percentage by mass of the aggregate) as: r1 = 0. R1 is the reproducibility limit as defined in EN 932-6.016 X where X is the value T SO4 between 0.204 X 60 . A. X is the average of the test results. storage & distribution or use on network prohibited.062 + 0. A.029 X and R1 = 0. (10530313).003 %.3 Determination of water-soluble chloride salts by potentiometry (Alternative method) (See Clause 8) The standard deviation for repeatability r is 0.5 Determination of total sulfur content by acid digestion (Reference method) (See 11.017 + 0.000 6 + 0.018 X Reproducibility R1 = 0. copy/pasting.2 % and 1 %. The standard deviation for reproducibility R is 0.saiglobal.001 %. Repeatability r1 = 0. 1 user personal license only. saiglobal. 61 . copy/pasting. 1 user personal license only. storage & distribution or use on network prohibited. Get permission to copy from or network this publication www. Copying.BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) A.000 + 0. (10530313).200 X and R1 = 0.812 X NOTE These values were derived using a test portion of 2 g.021 + 0.6 Determination of acid soluble sulfates (See Clause 12) Licensed to Mr George Calvar on 26 May 2015.com/licensing The precision of the determination of acid soluble sulfate content is stated (as the percentage SO3 by mass of the aggregate) as: r1 = 0. Cement — Part 1: Composition. 1 user personal license only. specifications and conformity criteria for common cements . storage & distribution or use on network prohibited.Licensed to Mr George Calvar on 26 May 2015. copy/pasting. Copying. Get permission to copy from or network this publication www. (10530313).com/licensing BS EN 1744-1:2009+A1:2012 EN 1744-1:2009+A1:2012 (E) Bibliography [1] 62 EN 197-1.saiglobal. Copying. 1 user personal license only. (10530313). copy/pasting. Get permission to copy from or network this publication www.saiglobal.com/licensing .This page deliberately set blank Licensed to Mr George Calvar on 26 May 2015. storage & distribution or use on network prohibited. storage & distribution or use on network prohibited. and size. European and international standards through its Knowledge Centre. type or grade designations. or some person or entity that owns copyright in the information used (such as the international standardization bodies) has formally licensed such information to BSI for commercial publication and use. Similary for PASs. unless otherwise requested. 1 user personal license only.com Information regarding online access to British Standards and PASs via British Standards Online can be found at www. 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