~ BSI BS¥EN*L9b-2) 92 MM 1624669 0292373 9 a BRITISH STANDARD BS EN | 1992 Methods of testing cement Part 21. Determination of the chloride, carbon dioxide and alkali content of cement Copie de Travail a BOUYGUES OFFSHORE Centre de Documentation ‘The European Standard EN 196-21 ; 1989 has the status of a British Standard Méthodes d'essais des cients Profverfahren f0r Zement Partie 2: Determination de la teneur en ‘Til 21, Bestimmung des Chlorid-, hlorures, en dioxide de carbone et en alcalis _Kohlenstoffdioxid: und Altahasteils won dans les ciments Zement OETABS EN 196-21 : 1992 BST BS*ENKDSb-22 92 MM 1b24669 0292374 0 mm Cooperating organizations ‘The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national standards ‘organizations of the following countries. Austria Belgium Denmark Finland France Germany Greece Iceland Ireland e- Tealy Laxenibouty Netherlands Norway Portugal Spain Sweden Switzerland United Kingdom ‘This British Standard, having been prepared under the direction ofthe Technical Sector Board for Building and Civil Engineering, was published under the authority of the ‘Standards Board and comes into Oesterreichisches Normungsinstitut Institut belge de normalisation Dansk Standardiseringsraad ‘Suomen Standardisoimislito, ry. Association francaise de normalisation Deutsches Institut far Normung e. V. Hellenic Organization for Standardization ‘Technological Institute of Iceland National Standards Authority of Ireland Ente Nazionale Italiano di Unificazione Inspection Gi Travail et des Mines Nederlands Normalisatie-instituut Norges Standardiseringsforbund Instituto Portugués da Qualidade Asociacién Espaiiola de Normalizacién y Certificacién Standardiseringskommissionen i Sverige Association suisse de normalisation British Standards Institution Amendments issued since publication ‘effect on 16 June 1002 Amd. No. [Date ‘Text affected © BsI 1992 ‘The following BSI references relate to the work on this, standard: Commitee reference 1Y516 Draft for comment 87/10353 DC ISBN 0 580206807 154 STANDARDS INSTITUT TERTBSI BS¥EN*19b-21 92 MH LG24bb9. 0292375 2 am Contents Page Cooperating organizations Inside front cover National foreword * i Brief history 2 Foreword 2 ‘Text of EN 196-21 National annexes NA (informative) Test method for the alkali content of cement to be used. for the purpose of calculating the reactive alkali content of concrete 16 NB (informative) Committees responsible Inside back cover NC (informative) Cross-references Inside back cover National foreword ‘This British Standard has been prepared under the direction of the Technical Sector Board for Building and Civil Engineering. It is the English language version of EN 196-21 : 1989 ‘Methods of testing cement; Determination of the chloride, carbon dioxide and alkali content of cement’, published by the European Committee for Standardization (CEN). EN 196-21 was drawn up by ‘Technical Committee 61, Cement and building limes, as Part 21 of a series on testing cement which was accepted by CEN on 3 October 1989. The UK gave a negative vote at the final voting stage, but under the CEN Rules now in force, is bound to abide by the majority decision and to implement this Part, Thus, the European test procedures have been introduced, where relevant, into the 1991 revisions of British Standards for cement BS 12,'BS 146, BS 4027, BS 4246, 'BS 6588 and BS 6610. This British Standard supersedes clauses 16 and 17 of BS 4550 : Part 2 which are withdrawn, ‘The UK negative vote on this Part was due to the fact that the European methods for alkalis give values for NazO equivalent of cement higher by approximately 0.025 % absolute than those obtained using either the current BS or the ASTM methods which have been used in the UK for the purpose of calculating the ‘reactive’ alkali content of concrete. In consequence, the BS 4560 : Part 2 : 1970 test method is retained as national annex NA to be used only for the determination of the alkali content of coment for the purpose of calculations to check compliance with the maximum value of 3.0 kg/m? of NagO equivalent for the reactive alkali content of a concrete mix, recommended when aggregate containing an alkali reactive constituent, or when an unfamiliar cement/aggregate combination, is in use (see 4.2.4 of BS 5328 : Part 1: 1991), "BS 5328 Concrete, Part I : 1991 Guide to specifying concrete cprriahe by ene GRITESH staNDAROS ENSTETUTION (8st)‘BST BS¥ENX}96-2) 92 MM LL24669 0292376 4 mm «BS EN 196-21: 1992 However, the European test method is called up in 8.3 of BS 4027 : 1991!) which specifies the maximum permitted alkali content of sulfate-resisting Portland cement, type Low Alkali, National annex NB gives the committees responsible for the UK participation in the preparation of this standard, National annex NC gives details of corresponding British Standards for international standards referred to in the European Standard. Compliance with a British Standard does not of itself confer immunity from legal obligations. BS 4027 : 1991 Specitication for sulfate-resisting Portland cementBSI BS*EN*}9b-21 92 MM Lb24bb4 0292377 & mm! 3 EUROPEAN STANDARD EN 196 NORME EUROPEENNE oe EUROPAISCHE NORM December 1989 { UC 666.94 : 601.64 : 620.1 : $43.84 Descriptors: Cements, tests, chemical analysis, determination of content, chlorides, carbon dioxide, alll English version Methods of testing cement; Determination of the chloride, : carbon dioxide and alkali content of cement | Méthodes d’essais des ciments; Détermination _Priifverfahren fir Zement; Bestimmung des de la teneur en chlorures, en dioxide de Chlorid-, Kohlenstoffdioxid- und Alkalianteils carbone et en alcalis dans les ciments ‘von Zement ‘This European Standard was approved by CEN on 1989-06-16. CEN members are bound to comply with the CEN/CENBLBC Internal Regulations which } stipulate the conditions for giving this Buropean Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the e Central Secretariat has the same status as the official versions, CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom, CEN Buropean Committee for Standardization Comité Européen de Normalisation Buropaisches Komitee fir Normung Central Secretariat: ruc de Stassart 36, B-1050 Brussels : © CEN 1989 Copyright reserved to CEN members Ref. No, EN 196-21 : 1989 EBSI BS*EN*196-2) 92 MM UL246b9 0292378 6 me Page 2 EN 196-21 : 1989 Brief history ‘This European Standard was prepared by Technical Committee CEN/TC 61 ‘Cement’, the Secretariat of which is held by IBN. Ibis intended, in a revision of European Standard EN 196 : Part 2, to adopt the methods of test in this standard into EN 196 : Part 2, so that this standard will then contain all methods of test required for the chemical analysis of cement. In accordance with the Corumon CEN/CENELEC Rules, the following countries are bound to implement this European Standard: @Pestri2, Belgium, Denmark, Finland, France, many, Greece, tceland, ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. orglonyby its aeien staonsos srrTuTZO4 (as!) Foreword ‘The standard EN 196 on methods of testing cement consists of the following parts: Part 1. Part 2. Part 3. Part 4. Part 6. Part 6. Part 7. Part 21. Determination of strength Chemical analysis of cement Determination of setting ti soundness Quantitative determination of constituents Pozzolanicity test for pozzolanic cements Determination of fineness Methods of taking and preparing samples of cement Determination of the chloride, carbon dioxide and alkali content of cement. e andBSI BS*EN19b-21 92 MM LE24G69 0292375 T am! Contents 3.2. 3.3 a4 @ 3.6 3.7 41 4.2 43 44 45 4.6 5.1 5.2 e= 54 5.5 5.6 61 6.2 63 64 6.5 66 TW 12 7.3 TA 7.5 Preparation of th: Object and field of application References General requirements for testing Number of tests Repeatability and reproducibility Expression of masses, volumes and results Determination of constant mass Reagents Volumetric glassware Determination of the chloride content Principle Reagents Apparatus Procedure Expression of results Repeatability and reproducibility Determination of the carbon dioxide content (reference method) Principle Reagents Apparatus Procedure Expression of results Repeatability and reproducibility Determination of carbon dioxide content (alternative method) Principle Reagents Apparatus Procedure Expression of results Repeatability and reproducibility Determination of the alkali content (reference method) Principle Reagents Apparatus Preparation of calibration solutions and calibration graphs Dissolution of the test portion eee eee eens 10 10 10 76 1 18 81 82 83 Be 8.6 a6 a7 Page 3 EN 196-21: 1989 Procedure Expression of results Repeatability and reproducibility Determination of the alkali content (alternative method) Principle Reagents Apparatus Plotting tne Calibration Curve Procedure Expression of results Repeatability and reproducibility 10 u ll 12 32 12 12 1 13 13 13Page 4 EN 196-21 : 1989 1 Object and field of application ‘This European Standard lays down the methods for the determination of the chloride, carbon dioxide and alkali content of cement. ‘The standard describes the reference methods and, {in certain cases, an alternative method which can be considered as giving equivalent results, If other methods are used, their results shall be shown to be equivalent to the results given by the reference methods, In the case of a dispute, only the reference methods are applicable. ‘This standard applies to cements and also to their @onstituent materials, such as clinker and tfarnece slags ~~" — 2 References ‘Methods of testing cement — Chemical analysis of cement ‘Methods of testing cement — Methods of taking and preparing samples of cement ISO 3634-1977 Statistics — Vocabulary and symbols EN 196-2 EN 196-7 3 General requirements for testing 8.1 Number of tests ‘The number of tests for the various determinations (clauses 4 to 8) shall be two (see also 3.3). @ 2 Repeatability and reproducibility ‘The standard deviation of repeatability gives the closeness of agreement between successive results obtained with the same method on identical test material, under the same conditions (same operator, same apparatus, same laboratory and short time interval?)), The standard deviation of reproducibility gives the closeness of agreement between individual results obtained with the same method on identical test material but under different conditions (different operators, different apparatus, different laboratories and/or different times) ‘The standard deviations of repeatability and reproducibility are expressed in absolute percent. 3.8 Expression of masses, volumes and results State masses in grams to the nearest 0,0001 g and volumes from burettes in millilitres to the nearest.0,05 ml. BSI BS*EN*}9b-2) 92 MMH UG24EE9 0292380 6 a Express the results, given by the mean of two determinations, as a percentage generally to two decimal places. If the results of two determinations differ by more than twice the standard deviation for repeatability, repeat the test and take the mean of the two closest values as the result. 3.4 Determination of constant mass Determine constant mass by making successive 16 min ignitions followed each time by cooling and then weighing. Constant mass is reached when the difference between two successive weighings is less than 0,0005 g. paracin Ox GI CeiERE Bape Before starting the determinations, treat the laboratory sample, taken in accordance with EN 196-7, as follows to obtain a sample for testing. ‘Take approximately 100 g of the sample using a sample divider or by quartering. Sieve this portion on a 150 um or 125 yum sieve until the residue remains constant. Remove the metallic iron from the material retained on the sieve by means of a magnet. ‘Then grind the iron free fraction of the retained material so that it completely passes the 160 um or 125 um sieve, If this sample contains particles of metallic iron such as those that may be introduced accidentally during grinding, remove these iron particles completely using a magnetic stirrer in a suspension, for ‘example in cyclohexane, Transfer the sample to a clean dry flask with an airtight closure and shake vigorously to mix it thoroughly Carry out all operations as quickly as possible to ‘ensure that the sample is exposed to ambient air only for the minimum time. 3.6 Reagents Use only reagents of analytical quality and distilled water, or water of equal purity, during the analysis. Unless otherwise stated % means percent by mass. ‘The concentrated liquid reagents used in this Standard have the following densities (p) (in g/m? at 20 °C) hydrochloric acid 1,18 to 1,19 hydrofluoric acid 113 nitric acid 1,40 to 1,42 perchloric acid 1,60 to 1,67 phosphoric acid 1,71 to 1,75 sulphuric acid 1,84 ‘The degree of dilution is always given as a volumetric sum, for example, dilute hydrochloric acid I + 2 means that 1 volume of concentrated hydrochloric acid is to be mixed with 2 volumes of water.BSI BS*EN*L9b-2) 92 MM L249 029298) 8 mm! 3.7 Volumetric glassware ‘The volumetric glassware shall be of analytical accuracy, i.e. class A as defined in the ISO standards on laboratory glassware. 4 Determination of the chloride content 4.1 Principle ‘This method gives the total halogen content except for fluoride and expresses the result as Cl-. The cement sample is decomposed with boiling dilute nitric acid. Sulphides are oxidized into sulphates and do not interfere. The dissolved chloride is precipitated using a known volume of a standard_ “silver nitrate solution. Atte é precipitate is washed with dilute nitric acid and discarded. ‘The filtrate and washings are cooled to less than 25 °C and the residual silver nitrate is titrated with a standard ammonium thiocyanate solution using an iron (IM) salt as indicator. 4.2 Reagents 4.2.1 Concentrated nitric acid (HNO). 4.2.2 Dilute nitric acid 1 + 2. 4.2.8 Dilute nitric acid 1 + 100, 4.2.4 Silver nitrate (AgNOs), dried at 160 °C. 4.2.5 Silver nitrate solution 0,05 mol/l. Dissolve 8,494 g of silver nitrate in water in a 1000 ml volumetric flask and make up to the mark. Store the solution in a brown glass flask and protect it, from the light. 4.2.6 Ammonium thiocyanate (NH4SCN). 4.2.7 Ammonium thiocyanate solution, approximately 0,05 mol. Dissolve 3,8 g of ammonium thiocyanate in water and make up to 1000 ml 4.2.8 Ammonium iron (II) sulphate (NH,Fe($04)2.12H 20). 4.2.9 Indicator solution. Add 10 ml of dilute nitric acid 1 + 2 to 100 ml of a cold saturated solution of ammonium iron (If) sulphate in water, 4.3 Apparatus 4.8.1 Balance, capable of weighing to the nearest 0,001 g. 4.3.2 10 mi burette, graduated to 0,1 ml. 4.3.3 Desiccator, containing anhydrous magnesium, perchlorate (Mg(C104)p) 4.3.4 Filter paper, coarse (pore diameter approximately 20 jim). 4.3.5 5 ml pipette pyetane by the ORITISH STANDARDS INSTHTUT EON (B51) Page 5 EN 196-21 : 1989 4.4 Procedure Weigh (6 0,06) g of cement and place in 250 mi beaker, add 60 ml of water and, while stirring with a glass rod, 60 ml of dilute nitric acid 1 + 2 (4.2.2). Heat the mixture to boiling, stirring occasionally, and boil for 1 min, Add 6 ml of silver nitrate solution (4.2.6) by pipette (4.3.5) into the bolling solution. Then boil for a maximum of 1 min and filter through a filter paper (4.8.4) washed before use with dilute nitric acid 1 + 100 (4.2.8) into a 600 mi flask. Wash the beaker, glass rod and filter paper with dilute nitric acid 1 ‘+ 100 until the volume of the filtrate and the washings is 200 mal. Cool the filtrate and washings to below _ Add 6 ml indicator solution (4.2.9) and titrate with the ammonium thiocyanate solution (4.2.7) shaking vigorously until a drop of this solution produces a faint reddish-brown colouration which no longer disappears on shaking. Record the volume Vj. If the chloride content of cement exceeds 0,17 %, it will be necessary to start the test again with a smaller quantity of cement. Carry out the same procedure with no cement sample and record the volume, Vz, of ammonium thiocyanate solution used in the blank titration. 4.5 Expression of results Calculate the chloride content (in %) from the formula: ar = 0,173 x C2— Vo) a ‘m,_ is the mass of the cement test portion; Vj; _ is the volume of the ammonium thiocyanate solution used for the titration of the test solution; Vp is the volume of the ammonium thiocyanate solution used for the titration of the blank solution, ‘The mean of the two results shall be rounded to the nearest 0,01 %, 4.6 Repeatability and reproducibility The standard deviation of repeatability is 0,005 %. ‘The standard deviation of reproducibility is 0,010 %.‘BSI BS*EN4}9b-24 52 MH Lb24bb9 O292a82 T A Page 6 EN 196-21 : 1989 5 Determination of the carbon dioxide content (reference method) 5.1 Principle ‘The cement sample is treated with phosphoric acid to decompose the carbonate present. The carbon dioxide liberated is entrained in a current of carbon dioxide-free gas or air through a series of absorption tubes. The first two remove hydrogen sulphide and water and the following then absorb carbon dioxide. Two absorption tubes, each containing a granular absorbent for carbon dioxide and anhydrous magnesium perchlorate to retain the water formed during the absorption reaction are tordetenaine-the mass-of-earton dioxide released. 6.2 Reagents 8.2.1 Copper sulphate (CuSO4-5H20). 5.2.2 Copper sulphate solution, saturated. 6.2.8 Absorbent for hydrogen sulphide. Place a weighed quantity of dried pumice stone with a grain size between 1,2 mm and 2,4 mm into a flat, dish and cover with a volume of saturated copper sulphate solution so the mass of the copper sulphate solution is approximately half that of the pumice stone. Evaporate the mixture to dryness, while stirring frequently with a glass rod, Dry the contents of the dish for at least 5 h in an oven at a temperature of (165 + 6) °C. Allow the solid mixture to cool in @ desiceator and store in an airtight bottle. G24 Absorbent for water, anhydrous magnesium Perchlorate (Mg{(CI04)2) with a particle size between 0,6 mm and 1,2 mm. 5.2.6 Absorbent for carbon dioxide, synthetic silicates with a particle size between 0,6 mm to 1,2 mm®) impregnated with sodium hydroxide (NaOH). 5.2.6 Concentrated phosphoric acid (HgPO4) 6.2.7 Concentrated sulphuric acid (Hy804). 5.3 Apparatus 5.3.1 Apparatus for the determination of the carbon dioride content. Figure 1 shows a typical piece of apparatus which can be fitted with cither a cylindrical pressure container, a small electrical compressor or a suitable suction pump which will ensure an even flow of gas or air ‘The gas (air or nitrogen) entering the apparatus has previously had its carbon dioxide removed by first being passed through an absorbent tube or tower containing the carbon dioxide absorbent (5.2.5). The apparatus consists of a 100 mal reaction flask (A) fitted with a three neck adaptor. Neck By is ‘connected to a dropping funnel (0), neck Bg to a ‘connecting tube and neck C to a water cooled condenser. The funnel onto B; and the connecting tube onto By are joined together by means of a ‘¥-piece (P), so that the carbon dioxide-free air can flow either through the connecting tube or the funnel by means of a Mohr clip (N). After the condenser (L), the gas is passed through ‘concentrated sulphuric acid (D), then through absorption tubes containing the absorbent for hydrogen sulphide (6.2.3) (E) and for water (5.2.4) (F) and subsequently through two absorption tubes (G,H) which can be weighed and which are ‘three-quarters filled with the absorbent, for carbon lonide (6.2.5) and e-quarter-witi the absorbent ——— for water (6.2.4). The absorbent for carbon dioxide (6.2.6) is placed upstream of the absorbent for water (6.2.4) with respect to the gas flow. Absorption tube (H) is followed by an additional absorption tube (1), which also contains the absorbent for carbon dioxide and water, which is fitted in order to protect absorption tube (If) against penetration by carbon dioxide and water from the ait. ‘The absorption tubes (G) and (#H) which are to be weighed may have, for example, the following sizes. External distance between branches 45 mm Internal diameter 20 mm Distance between the lower part of 75 mm. the tube and the upper part of the ground section ‘Tube wall thickness 1,5 mm 6.3.2 Balance, capable of weighing to the nearest 0,0001 g. 5.3.3 Electric oven, which can be set at (105 + 5) °C and at (165 + 6) °C. 6.8.4 Desiccator, containing anhydrous magnesium perchlorate (Mg(CI04)). 5.4 Procedure Weigh (1 # 0,05) g of cement and place it ina dry 100 mi distillation flask. Connect the flask to the apparatus (6.3.1) as shown in figure 1, but without the two absorption tubes (G) and (H). Pass a current of carbon dioxide-free gas through the apparatus for 15 min at approximately 3 bubbles per second (bubble counter) via the connecting tube onto By (branch onto By, Mohr clip closed). Release the Mohr clip and remove the gas supply from the funnel (0). Add 30 ml concentrated phosphoric acid into the dropping funnel and reconnect the gas supply to fill the funnel (0).BSI BS*EN*19b-21 92 Ml Lb24b69 0292383 1 a Page 7 EN 196-21 : 1989 Key 100 mi distlation fase Dropping funnel connector Connecting tube connector Condenser connector Wiash bottle with concentrated sulphuric acid (6.2.7) Absorption tube with absorbent for hydrogen sulphide (6.2.8) Absorption tube with magnesium perchlorate absorbent for water (6.24) ‘Absorption tubes with absorbents for carbon dioxide (6.2.6) and for water (6.2.4) Absorption tower containing carbon dioxide absorbent (6.2.6) “Three-armed still head, Condenser Mohe clip Dropping funne! ¥piece womens an mcoge> Figure 1. Apparatus for the determination of the carbon dioxide content (reference method) Condition the closed absorption tubes (G) and (H) for 15 min in the balance case in order to achieve temperature equilibrium. Then weigh each tube separately. Shut off the flow of gas and attach the ‘tubes to the apparatus as shown in figure 1, Wear protective gloves when carrying out this operation. Then reopen the gas flow. After 10 min close absorption tubes (G) and (H), remove them, place them in the balance case for 15 min and then. weigh them separately. Repeat the passage of gas, removal and weighing of absorption tubes (G) and (H) for as long as is required for the results of two Successive weighings of a tube not to differ by more than 0,005 g If the change in mass of the absorption tubes (G) and (H) remains greater than 0,0005 g, renew the absorbents in tubes (B) and (F). lah by ee SRITISH STMOAROS INSTITUTION (B51) Attach the weighed absorption tubes (G) and (H) to the apparatus, as shown in figure 1, Open the funnel tap and allow the phosphoric acid to drop into the distillation flask (A), After the reaction has ceased, heat the contents of the flask to boiling and boil gently for 6 min. Maintain the gas flow through the apparatus until the flask has cooled to room temperature. Close absorption tubes (G) and (H), remove them and place them in the balance case for 15 min and then weigh them separately. The increase in mass of each tube is used for the calculation of the carbon dioxide content (see 6.6). The carbon dioxide is practically completely absorbed by tube (@). If the increase in mass of tube (H) exceeds 0,0005 g, renew the absorbent in tube (@) and start the test again,BSI BS¥EN*}96-2) 92 MH Jb24b69 Gede3684 3 Page 8 EN 196-21 : 1989 5.5 Expression of results Calculate the carbon dioxide content (in %) of the cement from the formula: COp = “8+ 74 x 100 where ‘tmz is the mass of cement test portion; ‘mg_is the increase in mass of tube G after absorption; @ ._is the incre: absorption. ‘The mean of the two results shall be rounded to the nearest 0,01 %. If the carbon dioxide content calculated from equation (2) is less than 0,6 %, repeat the determination with a cement sample weighing 2 g, 6.6 Repeatability and reproducibility The standard deviation of repeatability is 0,07 %. ‘The standard deviation of reproducibility is 0,10 % in,mass.of tube,H.after. 6 Determination of the carbon dioxide content (alternative method) 6.1 Principle ‘The carbon dioxide is driven off by means of sulphutic acid, absorbed by sodium hydroxide and gietermined gravimetrically. Any hydrogen sulphide sent which may distort the results is absorbed ‘by mercuric (I) chloride. 6.2 Reagents 6.2.1 Mercuric (I) chloride (HgCl.). 6.2.2 Absorbent for carbon dicside, synthetic silicates with a particle size between 0,6 mm and 1,2 mm® impregnated with sodium hydroxide, (Na08). 6.2.8 Concentrated sulphuric acid (H2S0¢). 6.2.4 Dilute sulphuric acid 1 + 4. 6.2.6 Absorbent for water, anhydrous magnesium perchlorate (Mg(Cl0,)g) with a particle size Between 06 wovang 2 min 6.3 Apparatus 6.8.1 Apparatus for the determination of the carbon dioride content. The apparatus is shown in figure 2. A small vacuum pump is used to generate reduced pressure in the apparatus. 6.8.2 Balance, capable of weighing to the nearest 0,001 g. Sulphuric. acid. (6.2.4) from the ror 6.4 Procedure Place (1 + 0,05) g of cement into the 100 ml distillation flask A of the apparatus (6.8.1). Mix this cement with a small (about. 60 mg) amount of ‘mercuric (1) chloride (6.2.1) using a spatula and (2) then add enough water to form a slurry. Connect the flask to the ground joint of the dropping funnel (0). Then draw air for 15 min through the apparatus, passing the air through an absorption tower (J) filled with absorbent (6.2.2) to remove the carbon dioxide before the air passes into the flask. After stopping the flow of air add 26 mi to 30 ml of ing frnnel (0). wnerenn into the flask, Take care to ensure that some of the acid remains in the dropping funnel as a seal. ‘Tum the vacuum pump on again, so that the current of air carries the liberated carbon dioxide through the condenser (L) and the first two absorption tubes (F), filled with magnesium perchlorate (6.2.6) for the purposes of drying the air, to the two previously weighed absorption tubes (6) filled with absorbent (6.2.2). An absorption tube (1) filled with magnesium perchlorate (6.2.6) and absorbent (6.2.2) is fitted after these tubes in order to prevent penetration by the ambient air. A gas washing bottle (D) filled with sulphuric acid (6.2.3) is connected to this as a bubble counter. After about 10 min heat the contents of the flask to boiling and boil gently for 5 min. Maintain the air flow through the apparatus until the flask has cooled to room temperature. Close the taps and remove the absorption tubes (), place them in the balance case for 15 min in order to achieve temperature equilibrium and then weigh them. 6.5 Expression of results Calculate the carbon dioxide content (in %) from the formula: mg x 100 moe 3) COz 7 @) where ‘ms, is the mass of the cement test portion; ‘mg is the increase in mass of the absorption tubes G after absorption, ‘The mean of the two results shall be rounded to the nearest 0,01 %. 6.6 Repeatability and reproducibility ‘The standard deviation of repeatability is 0,07 %. ‘The standard deviation of reproduciblity is 0,10 %.~ BSI BSEN*}96-21 52 MM Le24eb9 O292385 5 me Page 9 EN 196-21 : 1989 ‘A100 mi distlation flask 1D Washing bottle containing concentrated sulphuric acd (6.2.3) Absorption tubes containing magnesium perchlorate (6.2.6) Absorption tubes containing absorbent for earbon dioxide (0.2.2) Absorption tube containing carbon dioxide absorbent (6.2.2) and magnesium perchlorate (6.2.6) ‘Absorption tower containing carbon dioxide absorbent (6.2.2) ‘To the vacuum pump F a t J L Condenser M © Dropping funnel for sulphuric acd (6.2.3) Fi igure 2. Apparatus for the determination of the carbon dioxide content (alternative method) 7 Determination of the alkali content (reference method) 7.1 Principle A butane or propane flame is used to excite the alkalis to emit their characteristic spectrum in the visible range. The emission is proportional to the alkali content at low concentrations. The influence of large quantities of calcium on the sodium determination is suppressed by means of phosphoric acid, 7.2 Reagents 7.2.1 General requirements References to water mean distilled water or water of the same degree of purity with an electrical conductivity of approximately 2 S/em. Use reagents of analytical quality (see also 3.6); their alkali content shall be tested by means of this method, If the alkali content of a reagent exceeds 0,01 %, the batch concerned is unsuitable and shall therefore be replaced by another which shall be tested in the same way. fpyctane by the QRITISM STAXOAROS INSTITUTION (B31) 7.2.2 Concentrated hydrochloric acid (HC). 7.2.3 Dilute hydrochloric acid 1 + 19. ‘7.2.4 Concentrated phosphoric acid (HsP04). 7.2.6 Dilute phosphoric acid 1 + 19; store this solution in a polyethylene flask, 7.2.6 Concentrated nitric acid (HNO3). 7.2.7 Concentrated perchloric acid (HC104). 7.2.8 Concentrated hydrofluoric acid (HF). 7.2.9 Sodium chloride (NaCl), dried at 10 °C to constant mass. 7.2.10 Potassium chloride (KCl), dried at 105 °C to constant mass. 7.2.11 Alkali stock solution, Weigh about 0,566 g of sodium chloride and about: 0,476 g of potassium chloride, transfer them to a 1000 ml volumetric flask, add 100 ml each of dilute hydrochloric acid. 1 + 19 and dilute phosphoric acid 1 + 19, dissolve and make up to the mark with water. This solution= BSI BS*EN*196-2) 42 MM LL24b69 0292386 7 mm” Page 10 EN 196-21 : 1989 contains approximately 0,00 g each of NazO and Kg0. The actual contents can be determined from the original quantities from the following formulae: 20 (in g/l) = 0,6138 x actual mass of potassium chloride ing (4) 'Nag0 (in g/l) = 0,5303 x actual mass of sodium chloride in g ©) 7.8 Apparatus 7.8.1 Balance, capable of weighing to the nearest, 01 g. 7.88 Calibrated buretias. ~~ 7,8.8 Flame photometer, with which the intensities of the sodium line at 689 nm and the potassium line at 768 nm can be measured: a sufficiently stable apparatus shall be used. 7.8.4 Platinum dish, 1,8.6 Filter paper, medium pore size (pore diameter approximately 7 um). 7.8.6 Platinum stirrer, 7A Preparation of calibration solutions and calibration graphs Prepare the calibration solutions using the volumes of alkali stock solution, dilute hydrochloric acid 1 + 19 and dilute phosphoric acid 1 + 19 listed in table 1. The volumes listed in lines 1 to 8 shall be made up to 1000 ml with water. Store these ration solutions in polyethylene bottles. ‘Say the calibration solutions into the flame of the flame photometer (7.3.3). Spray the blank solution (table 1, line 1) first and set the indication on the apparatus to 0. ‘Then spray the other calibration solutions in the order of increasing concentration (ines 2 to 8). Measure the intensities for NagO at 689 mm and for Ky0 at 768 nm. Plot graphs of the measured intensities against the corresponding concentrations of sodium oxide and potassium oxide in the calibration solutions. 7.8 Dissolution of the test portion 7.6.1 Cements completely soluble in acid (content of insoluble residue < 3%) ‘Weigh 0,1 g cement into a 60 ml beaker, make into a slurry ‘with 10 ml of water and add 10 ml of dilute hydrochloric acid 1 + 19, Warm the mixture until the cement has dissolved, breaking any lumps down with a glass rod. Filter the suspension through the filter paper (7.3.6) into a 100 ml volumetric flask washing through with boiling water. Wash the filter paper and residue with boiling water until there is a quantity of approximately 80 ml in the 100 ml volumetric flask. Then allow the filtrate and washing water to cool to ambient temperature. Add 10 mi of dilute phosphoric acid 1 + 19 to the solution, make up to the mark and mix thoroughly. 7.6.2 Cements not completely soluble in acid se. the method Aeserihed below, shora.tho content of insoluble residue, determined in accordance with clause 9 of EN 196-2, exceeds 3 %. Weigh 0,2 g of cement into a platinum dish and add 5 ml of concentrated nitric acid (7.2.6). Heat the mixture, for example, on a hot-piate, and evaporate to dryness. Disperse the residue from evaporation in 5 ml of water, add 2 ml of concentrated perchloric acid®) (7.2.7) and then add 10 ml of concentrated hydrofluoric acid (7.2.8). Heat the mixture and evaporate to dryness. Prevent overheating by frequent agitation by means of the platinum stirrer (7.3.6). Add 40 ml of water and 20 ml of dilute hydrochloric acid 1 + 19 to the residue from evaporation and heat until the residue has dissolved. Filter the suspension through the filter paper (7.3.6) into a 200 mi volumetric flask washing through with hot water. Wash the filter paper and residue with hot water until the 200 ml volumetric flask contains a volume of approximately 150 ml. Then allow the filtrate and washing water to cool to ambient temperature. Add 20 ml of dilute phosphoric acid 1 + 19 to the solution, make up to the mark with water and mix thoroughly. 7.6 Procedure Spray the measuring solution produced as described in 7.6.1 or 7.5.2 into the flame of the flame photometer (7.3.8). Measure the intensity of the sodium line at 689 nm and the potassium line at 768 nm, Obtain the sodium oxide or potassium oxide concentration in the solution respectively by means of a linear interpolation from the intensities and the associated concentrations of the calibration solutions measured as described in 7.4. Use the graphs plotted as in 7.4 to obtain the sodium oxide and potassium oxide concentrations of the solution in mg/l or use the intensities and the associated concentrations of the calibration solutions with the next higher and the next lower intensity for the calculation as follows ® Perchlorte acid vapours form explosive mixtures with organic materials. I ls therefore necessary to take special precautionary Ieasures when working with perchloric acid: the use of furne cupboards Nushed with water and a general ban on the use of oprsahes ty tne eats Simones sr TUriOn es) | |a Ub24bb9 0252387 9 Page 11 EN 196-21 : 1989 ‘Table 1. Volumes of solutions for the preparation of calibration solutions and thelr sodium oxide and potassium oxide concentrations Tine ‘Allall stock solution | Dilute hydrochloric acld | Dilute phosphoric acid | NagO andl KjO (2a 1419 +10 concentrations nt ni ml melt 1 = 100,0 100,0. Blank solution 2 38 99,6 99,6 1,0 3 83 99,1 99,1 2,5 4 16,7 98,3 98,3 5,0 5 25,0 97,5 97,6 76 6 33,3 96,6 10,0 7 a 3s 26 8 50,0 95,0 15,0 Calculate the sodium oxide (Cys,0) oF potassium oxide (C,0) concentration of the sample from the intensities Tye,0 OF Ix,o respectively using the following formula Inyo - Ibn Grazo = Can + (Gon - Can) x “HO "EP (6) . - 40 = Ton x0 = Con + (Con ~ Opn) x HO fon (7) where Con is the concentration of the sodium oxide or potassium oxide respectively in the calibration solution having a lower concentration than the measuring solution in mg/l; Con is the concentration of the sodium oxide or potassium oxide respectively in the calibration solution having a higher concentration than the measuring solution in mg/l; Ju is the intensity of the calibration solution having a lower concentration than the measured solution; Ign _is the intensity of the calibration solution having a higher concentration than the measuring solution, 7.7 Expression of results Calculate the contents of sodium oxide or potassium oxide as percentages in the cement from the following equations using the corresponding concentrations as determined in accordance with 7.6, NagO = 0,1 Cya,o (8) X20 = 0,1 go o where ‘Nao _ is the sodium oxide concentration of the measuring solution as calculated by formula (6) (in mg/l); Ck,0 _is the potassium oxide concentration of the measuring solution as calculated by formula (7) (in mg/l). ‘The mean of the two results for each oxide shall be rounded to the nearest 0,01 %. The total alkali content, A, is obtained by converting the potassium oxide content to equivalent sodium oxide from the formula: A = Naz + 0,658 Kz0 (lo) 7.8 Repeatability and reproducibility ‘The standard deviation of repeatability is: 0,01 % for the determination of Naz0; 0,02 % for the determination of Kz0. ‘The standard deviation of reproducibility is: 0,02 % for the determination of NazO; 0,03 % for the determination of Kz0.BSI BSXENXD9b-21 92 MM 1624bb5 0292388 0 a J Page 12 EN 196-21 : 1989 8 Determination of the alkali content {alternative method) 8.1 Principle Cements which are completely soluble are treated with hydrochloric acid. Cements which are incompletely soluble are first evaporated with hydrofluoric acid/sulphuric acid. The alkali contents of the solutions are determined by means of flame photometry. 8.2 Reagents 8.2.1 Concentrated hydrochloric acid (HCl). 9. Dilste-hyrirochloniowacid-L~t~Qnm meme 8.2.8 Concentrated hydrofluoric acid (HF). 8.2.4 Concentrated sulphuric acid (H2S04). 8.2.6 Lithium chloride (LiCl); dried at 120 °C. 8.2.6 Sodéum chloride (NaC); dried at 105 °C to constant mass. 8.2.7 Potassium chloride (KCI); dried at 105 °C to constant mass. 8.2.8 Stock solution®) Dissolve 0,610 g of lithium chloride, 0,2642 g of sodium chloride and 0,1907 g of potassium chloride in water in a 1000 ml volumetric flask and make up to the mark. 8.2.9 Caesium chloride (CsCl). 8.2.10 Aluminium nitrate (AI(NOs)3.9H20). © 11 Buzier sotution®) Dissolve 60 g of caesium chloride and 250 g of aluminium nitrate in water and make up to 1000 ml. 8.8 Apparatus 8.8.1 Balance, capable of weighing to the nearest 0,001 g. 8.8.2 Blectric oven, which can be set at (105 £ 5) °C and at (120 £ 5) °C. 8.3.9 Flame photometer, capable of measuring the intensities of the sodium line at 689 nm and the potassium line at 768 nm, The flame photometer shall be operated with a propane-air flame at a relatively low temperature in order to avoid distortion of the determination by alkaline earths. 8.8.4 Filter paper, medium porosity (pore diameter approximately 7 um). 8.8.5 Platinum dish. 8.8.6 Heating lamp. 8.8.7 Calibrated burette. 8.4 Plotting the calibration curve In the case of cements which are completely soluble in hydrochloric acid, evaporate 20 ml of hydrochloric acid 1 + 9 to dryness, and, in the case of cements not completely soluble in acid, evaporate 16 ml of hydrofluoric acid (8.2.3) and 5 mi of sulphuric acid (8.2.4) to dryness for the ‘piirposes of preparing the calibration solutions for each calibration point. In both cases dissolve the residue from evaporation with 2 ml of hydrochloric acid 1 + 9 and 3 ml of water. Transfer the solution to a 100 ml volumetric flask and add 10 ml of buffer solution (8.2.11). Add the following quantities of the stock solution (8.2.8) to the individual volumetric flasks using the calibrated burette (8.3.7). ‘Volumetric flasks Ee Ee j ‘Stock solution (wi) Olt [3 [6 [10] 20] a0 ‘Then make up the volumetric flasks to the mark with distilled water With an original quantity of sample of 0,2000 g, the values measured for flasks 1 to 7 correspond to a K20 and Na2O content of: Volumetric flasks [i[2 [3 [4 [8 [6 |7 Naz0 content (%) [0] 0,07 | 0,20| 0,94 | 0,67 | 1.06 | 2.02 0 content (%) [00,06] 0,18 0,00 [0,60 1,20 | 1,81, Spray the calibration solutions into the flame of the flame photometer (8.3.3). Spray the blank solution 1 first and set the indication on the apparatus to 0. ‘Then spray the other calibration solutions in order of increasing concentration (2 to 7). Measure the intensities for NagO at 689 nm and for K20 at 768 nm. Plot graphs of the measured intensities against the corresponding concentrations of sodium, oxide and potassium oxide in the calibration solutions. If a sufficiently stable photometer is used, it is only necessary to establish the calibration curves from time to time. However, the values measured for flasks 1 and 7 shall be checked for each analysis.a BSI BS*EN*19b-21 92 mm 8.6 Procedure 8.5.1 Cements completely soluble in acid (content of insoluble residue < 3 %) Weigh 0,2 g cement into the platinum dish (8.3.5), rake into a slurry with 8 ml of water and evaporate to dryness after adding 20 ml of dilute hydrochloric acid 1 + 9. Add hot water and 2 ml of. dilute hydrochloric acid 1 + 9 to the residue and flter through the filter paper (8.3.4) into @ 100 ml volumetric flask which already contains 10 ml of the buffer solution (8.2.11). Wash the residue with ‘hot water until the volumetric flask is almost filled to the mark. Then cool to 20 °C and make up to @___ remark yin a Measure the solution in the flame photometer (8.3.3). The scale values read off in conjunction with the calibration curves (8.4) give the concentrations of K,0 and NazO in mg/l respectively 8.5.2 Cements not completely soluble in acid Weigh 0,2 g cement into the platinum dish (8.3.5). Make into a slurry with 3 ml of water and evaporate after adding 5 ml of concentrated sulphuric acid (8.2.4) and 15 ml of concentrated hydrofluoric acid (8.2.3). Evaporate to dryness under the heating lamp (8.3.6). Mix the residue with hot water and 2 ml of hydrochloric acid 1 + 9 and continue the procedure as described in 8.6.1, gyc1Ohe by. he GEITISE STAROAROS.INSTETUTION (BST) W624b69 0292389 2 mm | Page 13 EN 196-21 : 1989 8.6 Expression of results Calculate the content of alkali as a percentage for an original sample weight of 0,2000 g. ‘The mean of the two results for each oxide shall be rounded to the nearest 0,01 %. Convert the potassium oxide content to the equivalent sodium oxide content using formula (10). State the sum of the sodium oxide values as the total alkali content A. 8.7 Repeatability and reproducibility ‘The standard deviation of repeatability is: 0,01 % for the determination of NagO; 0,02 % TOF tie determination of Kz0. The standard deviation of reproducibility is 0,02 % for the determination of Na,O; 0,08 % for the determination of KO,BS EN 196-21 : 1992 BSI BS*EN*]9b-2) 92 MM 1b24b69 0292390 9 me! National annex NA (informative) ‘Test method for the alkali content of cement to be used for the purpose of calculating the reactive alkali content of concrete NA.1 General This method of test is intended to be used for the determination of the alkali content of cement only for the purpose of calculating the reactive alkali content of the concrete mix when aggregate containing an alkali reactive constituent, or when an unfamiliar cement/aggregate combination, is in use (see 4.2.4 of BS 6928 : Part 1), Meverscpaiees : NA.2.1 Simple flame photometers, burning natural or bottled gas and incorporating interchangeable filters which select light of the appropriate wavelengths, are generally suitable. Use in accordance with the manufacturers’ instructions, NA.3 Reagents Prepare reagents by the following methods and store in well stoppered rigid polyethylene or polypropylene bottles. NA.3.1 Sodium stock solution, (100 mg of Nag0 per litre.) Dry a quantity of analytical reagent grade, or purer, NaCl at 250 °C, weigh 0.1886 g, dissolve in water and dilute to 1000 ml. NA.3.2 Potassium stock solution, (100 mg of K_0 per litre.) Dry a quantity of analytical reagent fade, oF purer, KCl at 250 °C, weigh 0.1583 g, ssolve in water and dilute to 1000 ml NA.3.3 Aluminium sotution, (20 g of Al per litre.) Prepare this solution by dissolving super-purity aluminium metal in nitric acid. The following alternative methods have been found to be convenient. (a) From a sheet of supet-purity aluminium, between 0.5 mm and 3 mm thick, cut two pieces, one about 120 mm x 360'mm and the other about 120 mm x 200 mm. Bend the larger piece to fit inside a 2 | borosilicate glass or plastics beaker, then bend the smaller piece to fit inside the larger one. Near the middle of the top edge of each piece drill 2 hole and twist a separate piece of thick aluminium wire through each one to make electrical connections. Clean both sheets by washing successively in dilute hydrochloric acid (1 + 9), water and industrial methylated spirits. Allow the sheets to dry, ‘weigh them to + 0.05 g and place them in the beaker ensuring that they do not make contact with each other. Cover the beaker with a plastics cover and take the wire leads out through holes in the cover. Place the beaker and'contents in a fume cupboard. Connect the lead from the outer aluminium sheet to the positive terminal and the lead from the inner sheet to the negative terminal of a source of direct current which can be varied from 0 V to 12 Vi). While stirring, add 200 mi of nitric acid to 800 ml of warm water (about 60 °C) in a separate beaker and transfer this solution to the beaker containing the electrodes, Switch on the _- ~~ Donner supplycond inereaes the.applied-emltage to obtain a current of about 8 A. When it is considered that sufficient aluminium has dissolved), switch off and disconnect the power supply. Remove, wash, dry and reweigh the aluminium sheets together with any pieces that may have become detached: Caleulate from the loss of mass the volume the solution should occupy to contain 20.0 g of. aluminium per litre. Dilute to this volume with water. (b) Cut sufficient super-purity aluminium sheet or wire into small pieces and wash successively with dilute hydrochloric acid (1 + 9), water and industrial methylated spirits. Dry, weigh out 20.0 g and transfer a little at a time, using clean tongs, to a gently boiling solution of 100 ml of nitric ‘acid in 600 ml of water to which 2 ml of saturated mercuric chloride solution have been added. Maintain the volume at about 600 ml by adding water as necessary. When all the metal has dissolved, cool the solution and dilute to 1000 mi. NA.3.4. Calcium sotution, (6.3 g of CaO per litre.) Weigh 11.25 g of analytical reagent grade, or purer. CaCOy into a, beaker, cover with 100 ml of water and carefully add 26 ml of HINO3. When solution is complete dilute to 1000 mi with water. ‘Test for sodium and potassium contamination by the following procedure. Prepare solutions A, B and C, using the quantities given in table NA.L With the sodium light filter in place, set the flame photometer to read 0 with solution A and 100 with solution B. Spray solution C and record the reading. Replace the sodium light filter by the potassium light filter and repeat the procedure. If readings higher than 2 for NagO (0.1 mg/l) or higher than 1 for K20 (0.1 mg/l) are obtained reject the calcium solution and prepare a new solution using a purer source of CaCO3. "There should be a suitably rated fuse in the circuit to protect the power supply. with » current of 8 A approximately 20 g of aluminium is dissolved in 244 A lower current for a longer time fs permissible. |7 BSI BS*EN«19b-2 NA4 Calibration Prepare calibration solutions using the quantities given in table NA.2. With the sodium light filter in place set the flame photometer to read 0 with scale-zero solution and 100 with scale-100 solution. Record the readings obtained for each of the intermediate calibration solutions, checking and adjusting if necessary, the 0 and 100 settings between each reading. Replace the sodium light filter by the potassium light filter and repeat the calibration procedure. Construct the calibration graphs of instrument reading against milligrams per litre of NazO or Kz0. NOTE 1. For instruments using internal standardization, add the internal standard solution to the calibration solutions in accordance with the manufacturer instructions, (OTE 8. in some cases aiTereRENagO andlor KO ‘concentration ranges may be required. Should this be necessary, modify the alkali contents of the calibration solutions as appropriate but take the Al, Ca and HNO, additions from table NA.2. The concentration of the seale-100 solution should ot exceed that recommended by the instrument manufacturer eS 292 MM 1624669 0292393 0 mm | BS EN 196-21 : 1992 ————————————— eee NA.6 Procedure NA.6.1 Determination of alkalis soluble tn nitric acid NOTE, This procedure is goncrlly applicable to cements, and other materials, which are almost completely decomposed by nite weld solution, Weigh out 600 mg of sample into a beaker made from a material which will not yield sodium or potassium to the solution. Add about 50 ml of cold water, disperse the powder by swirling and add 5 mi of nitric acid. Swirl again, add hot water to about 160 ml total volume, bring to the boil and simmer for 6 min to 10 min. Cool, transfer to a 500 ml volumetric flask, add 60 ml of the aluminfum solution, dilute to the mark with satel andeionthicioughly, Allow to settle and pour off sufficient solution for the flame determinations. If necessary, centrifuge or filter the solution before spraying. ‘Table NA. 1. Solutions for checking purity of calcium solution Solution [Sodium scock | Poensslam stock | Aluminium [Gaiciam HNO, Water to make solution solution solution fotation mi mi mi ml mil mi o o 50 5 500 B 25 50 50 6 600 e o ° 50 50 5 00 | ‘Table NA.2. Solutions for calibrating flame photometer ‘calibration | Sodium ‘Aluminium [Calcium] HNO3 Water to | Equivalent solition sce folution | solution make concentrations Ne0 | iG0 ml mi ml mi mi mil ml [mi Scale-zero | 0 0 100 100 10 1000 ° ° ' Seate-100 | 50 100 100 100 10 1000 5 |10 Nominal 20 | 5 10 50 50 5 600 1 2 Nominal 40 | 10 20 50 50 5 500 2 4 Nominal 60 | 15 30 50 50 5 500 3 6 [Nominal 80 [20 40 60 50 5 500 4 8 LiBefore making Up to volume, add, where necessary, sufficient of the standard caletum solution to bring the concentration of falcum oxide in the diluted solution to approximately 630 ma/, and, for instruments using internal siardardleaton, nie eda the Internal standard solution in accordance with the manufacturer's instructions.BS EN 196-21 : 1992 With the sodium light filter in place set the flame photometer to read O with scale-zero solution and 100 with scale-100 solution. Spray the sample solution and take several readings, checking and adjusting if necessary, the 0 and 100 settings between each reading. Replace the sodium light filter by the potassium light filter and again set the flame photometer to read 0 with scale-zero solution and 100 with scale-100 solution. Spray the sample solution and take several readings, checking, and adjusting if necessary, the 0 and 100 settings between each reading. If the sample gives a reading of more than 100 for either sodium or potassium, transfer 50 ml of ample solution to a 100 mi graduated flask, dilute ¢ fhe mark with scale-nero solution and dilution may an exceptional cases a further required. NA.6.2 Determination of total alkalis ‘Weigh 600 mg of sample into a platinum basin and remove carbon or carbonaceous matter by careful ignition at 926 + 25 °C. Cool the sample and add 20 ml of water and 10 ml of perchloric acid. Sti, add 20 m) of hydrofluoric acid and evaporate the solution to strong fumes of perchloric acid in a mechanically ventilated fume cupboard, Add 20 ml of water and 5 ml of perchloric acid and again evaporate until fumes just cease to be emitted. CAUTION. Perchloric acid fumes can react explosively with some absorbent organic materials. Fume cupboards for use with perchloric acid should never be constructed in wood but polyvinyl chloride and stainless steel have been found suitable. All materials of construction should be mn-absorbent and interior surfaces should be free sm crevices and ledges that could prevent complete washing down. Guidance on the suitability of a fume cupboard for use with perchloric acid should be sought from the manufacturer 2 BS 7268 Laboratory fume cupboards. iBSI BSxENxI4) Ub24ee5 O292352 2 Recommendations on all aspects of fume cupboards are given in BS 7258), ‘Add 6 ml of nitric acid, cool and transfer to a 600 ml volumetric flask. Add 60 mL of the aluminium solution, dilute to 600 ml with water?) and mix thoroughly: Then repeat the procedure in NA.5.1 from the second paragraph onwards. Make blank determinations following the above procedure with no sample present. NA.6 Calculation From the respective calibration graphs for NagO and Kz0 (see NA.4) convert flame photometer readings to concentrations (milligrams per litre). wxfbithedetermination of totsLollntic dedzct the. blank determinations from the readings given by 'NagO and K20 respectively. Where dilution of the original solution has been made apply the dilution factor. Calculate the alkali contents as percentages by the formula: alkali oxide = 0.1D(C ~ B) where Cis the concentration of alkali (milligrams per litre); B is the blank reading (when determining alkalis soluble in nitric acid this is zero); D isthe dilution factor, ie. volume of diluted solution (ml) ‘volume of aliquot taken (ml) (where no dilution has been made this equals one). Before making up to volume, add, where necessary, sufficient of the standard calcium solution to bring the concentration of calcium oxide inthe diluted solution to appraximately 680 mg/l, and, for instruments using internal standardization, also add the internal standard solution in accordance with the manufacture instructions. ——————BST BS*EN*19b-21 92 MH 1624669 0292393 4 National annex NB (informative) Committees responsible ‘The United Kingdom participation in the preparation of this European Standard was entrusted by the ‘Technical Sector Board for Building and Civil Engineering (B/-) to Technical Committee B/516 upon which the following bodies were represented: British Aggregate Construction Materials Industries British Cement Association British Precast Concrete Federation British Ready Mixed Concrete Association Cement Admixtures Association Cementitious Slag Makers Association @ Concrete Socie ee County Surveyors’ Society Department of the Environment (Building Research Establishment) Department of the Environment (Property Services Agency) Department of Transport Federation of Civil Engineering Contractors Mortar Producers Association National Rivers Authority Quality Ash Association Society of Chemical Industry Water Services Association of England and Wales National annex NC (informative) Cross-references Publication referred to Corresponding British Standard e BS EN 196 Methods of testing cement EN 196-2 Part 2 : 1992 Chemical analysis of cement EN 196-7 Part 7 : 1992 Methods of taking and preparing samples of cement 180 3534 : 197 BS 5632 Statistical terminology Part 1 : 1978 Glossary of terms relating to probability and general terms relating to statistics ™ tn preparation.- BSEN 196-21 : 1992 BSI 2 Park Street London WIA 2BS. BSI Linford Wood Milton Keynes MK14 6LE, BSI BS*EN*19b-2) 52 MM Wb246b9 0292394 b me —_—_——_—— BSI — British Standards Institution BSI is the independent national body responsible for preparing British ‘Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Contract requirements A British Standard does not purport to include all the necessary provisions of contract. Users of British Standards are responsible for their correct application. Revisions British Standards are updated by amendment or revision. Users of British ‘Standards should make sure that they possess the latest amendments or editions. Any person who finds an inaccuracy or ambiguity while using this British Standard should notify BSI without delay so that the matter may be J investigatecrswitt = BST offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards. Buying British Standards Orders for all British Standard publications should be addressed to the Sales, Department at Milton Keynes. Information on standards BSI provides a wide range of information on national, European and international standards through its Library, the Standardline Database, the BST Information ‘Technology Service (BITS) and its Technical Help to Exporters Service. Contact Customer Information at Milton Keynes: Tel: 0908 221166. Subscribing members of BSI are kept up to date with standards developments and receive substantial discounts on the purchase price of standards. For details of these and other benefits contact the Manager, Membership Development at Milton Keynes: Tel: 0908 220022. Copyright Copyright subsists in all BSI publications and no part may be reproduced in any form without the prior permission in writing of BSI. This does not preclude the free use, in the course of implementing the standard of necessary details such as symbols and size, type or grade designations including use by incorporation into computer programs, but where these details are reproduced including without limitation in printed form, in computer programs or in any other form whatsoever, the permission in writing of BSI must be obtained and if granted will be on terms including royalty, before the product is sold, licensed or otherwise exploited for commercial gain. Enquiries about copyright should be made to the Copyright Manager, Publications at Milton Keynes.9 Pa PZT LHD IUA409 AM GALINA S¥ L44DN NOISSINUSA ISB LAOHAIM ONTAGOD ON Meme SRE ERENCE SCO HHCLIOI Fre eM. NBLETS O98y osNOH xopU) ~ JOMNaMISIG ISB IPO G>T Aa PELE one) AL ncn Map wueaNABarge aang ay seeing haat sap mca py Sapna puepueig ysnug jo smieis 242 Sey BSBT | 9-46T NT prepueg UeadoIng aU 4oneIUaUINDEg 9 P equa: AYOHS440 sanoanos Heaed, ap aido- ssououly JO uoTJeUTULII0Gq “9 118 quourasd SUTj}S9} JO Spotyey} 661 * 9-96T ——___ a a Nd S@ GUVANVLS HSILGes BRITISH STANDARD BS EN SS ——— as | 196-2: 1995 Methods of testing cement Part 2. Chemical analysis of cement pie de Travail BOUYGUES OFFSHORE Centre de Documentation ‘The European Standard EN 196-2 : 1994 has the status of a British Standard i Prints by Ol ori BS Distributor ~ IndexHouse Ascot SLS7EU UK a sa yiaue 98 900 rey [7 Ea an ORE ATHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW EEEASED EE KL ET EE ED“This British Standard, having been prepated under the direction of the Technical Committee B 516. was published under the authority Df the Standards Board and ‘mes into effect om 15 March 1995, 2 BSI 1995 ‘The following BSI references felate to the work on this Sandard Committee reference 8 516 Special announcement in ‘BSI Neus December 1982 ISBN 0 590 21489 3, Cooperating organizations ‘The European Committee for Standardization (CEN). under whose superv this European Standard was prepared. comprises the national standards organizations of the following countries: Austria Oesterreichisches Normungsinstitut Belgium Institut belge de normalisation Denmark Dansk Standard Finland ‘Suomen Standardisoimisliito, ry. France Association francaise de normalisation Germany Deutsches Institut fir Normung e.V. Greece Hellenic Organization for Standardization Iceland Technological Institute of Iceland Ireland National Standards Authority of Ireland aly Ente Nazionale Italiano di Unificazione Luxembourg Inspection du Travail et des Mines Netherlands ‘ederlands Normalisatie-instituut e Norway Norges Standardiseringsforbund Portugal Instituto Portugués da Qualidade Spain Asociacién Espanola de Normalizacién y Certifica Sweden Standardiseringskommissionen i Sverige ‘Switzerland Association suisse de normalisation United Kingdom British Standards Institution Amendments issued since publication ‘Amd, No. | Date ‘Text affected -Contents Page Cooperating organizations ” Inside front cover National foreword i Foreword 2 ‘Text of EN 196-2 3 National annexes NA (informative) Determination of total sulfur 23 NB (informative) Determination of minor constituents (TiO) and P05) and free lime 23 NC (informative) Determination of propylene glycol content 5 ND (informative) Method of analysis of cements by X-ray fluorescence spectrometry 26 NE (informative) Methylene blue test 34 NF (informative) Determination of total organic carbon 36 NG (informative) Committees responsible Inside back cover NH (informative) Cross-references Inside back cover