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    BS en 196 Part 21 1992

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    Zahoor Ahmed Mohsan

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    of 22
    BRITISH STANDARD Methods of testing cement Part 21. Determination of the chloride, carbon dioxide and alkali content of cement ‘The European Standard EN 196-21 ; 1989 has the status of a + British Standard AN ETS BS EN 196-21 : 1992 i Cooperating organizations anudardization (CEN), under whose supervision onal standards Austria esterreichisehes Nonny Belgium Institut belge de Denmark Dansk Standardiseringsrad an Standanlissinistite, Association f Hellenic Organization for Starkarliza fecland Thehmological Institute of Teeland Ireland National Standirds Authority of Ireland hal Ente Nazionale Italiane di Unifiezione Lusembouns Inspeetion du Travail et des Mines Netherlands Nederlands Nornatlsatie-institunt Norw Norges Standardiseringstorburnic Port Institutes Portugués dt Quaid Spiny Asociavidn Espaivola de Normalizaeiin y Certitiva Sweden, Stanvlarviseringskonmissionen 1 Sver Switzerland Asset ian sist dee ormalisation: Chited Kingelom —Hritish Standards lastinution Ps Hrs Stars at eae An las Hoel sos ae Amd. No | Date Test afferted | | | | BS EN 196-21 : 1992 —— Contents Page Cooperating organizations Inside front ewer National forewort Brief history Foreword Text of EN 196 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 conercte 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’, pul lished by the European Committee for Standardization (CEN). EN 196-21 was drawn up by ‘Technical Committee 51, 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 19411 revisions of British Standards for cement BS 12, BS 146, BS 4027, BS 4246, BS (588 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 purpese of ithe “react content of concrete, In consequence, the BS 4550 : Part 2 : 1970 test method is retained as national annex NA to he used only for the determination of the alkali content of cement for the purpose of calculations to cheek compliance with the maximun value af 3.0 kg/m? of Na Hi content of a concrete mis, alkali reactive constituent, of wseresate combination, isin use (see 4.2.4 of BS EN 196-21 : 1992 However, the European test method is called up tn 8.3 of BS 4027 : 19011) Which specifies the maximum pe ment of sulfate-resisting Portiand cement, type Low Alkali ional 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 im from legal obligations. BS 4027 + 1991 Spe on for sulfate-resstinys Martanel ewment EUROPEAN STANDARD EN 196 NORME EUROPEENNE Part 21 EUROPAISCHE NORM December 1980 UDC G8 Nt 620.L EL Descriptors: Cements tests elemical analysis nent, eaarides, cath ioe, allt Engl version Methods of testing cement; Determination of the chloride, carbon dioxide and alkali content of cement Méthodes d’essais des ciments; Détermination — Priifverfahren far Zement; Bestimmung des de la teneur en chlorures, en dioxide de Chlorid-, Koblenstoffdioxid- und Alkalianteils, bone et en alcalis dans les ciments von Zement, ly with the CEN/CENELBC Int 1¢ the conditions for giving ional standard without any a Up-to-date lists and bibliographical references co wlarls may be wbtained on applic N mo, het cerning n to the Central Secte bodies of Austria, Belgium, Iceland, “Ireland, Maly, Sweden, Switzerland and CEN mittee for Standardization option de Nori lies: Kenn European ¢ fir Normung de Staxsart :16, B-1050 Brussels © CEN 1989 Copyright reserved to ¢ bers Ref No, EN IGE: 1980 E tics Page 2 EN 196-21 : 1989 Brief history Foreword ‘This European Standard was prepared by Technical ‘The standard EN 196 on methods of testing cement Committee CEN/TC 51 ‘Cement’, the Secretariat of consists of the following parts: which is held by 1B It is intended, in a revision of European Standard Part 1. Determination of strength EN 196 : Part 2, to adopt the methods of test in Part 2. Chemical analysis of cement this standard into EN 196 : Part 2, so that this: standard will then contain all methods of test required for the chemical analysi In accontance with the Common CEN/CENE Rules, the followi are bound to implement this European Standard Part 5. Pazzolanicity test for pozzolanic cements Part 3. Determination of setting time and soundness Part 4. Quantitative determination of constituents, Austria, Belgium, Denm Part 6. Determination of fineness Part 7, Methods of taking and preparing samples of cement Deter ination of the chloride, carbon Contents 1 Object and field of appli 2 References 3° General requirements for LL Number of tests 3.2 Repeatability and reproducibility. 3.3 Expression of masses, volumes and results 3.4 Determination of constant mass 3.5. Preparation of the cement sample 3.6 Reagents 3.7 Volumetric glassware 4 Determination of the chloride content 4.1. Principle 4.2 Reagents 4.3 Apparatus 4.4 Procedure 4.5 Expression of results 4.6 Repeatability and reproducibility 5 Determination of the carbon dioxide content (reference method) * 5.1 Principle 5.2 Reagents 5.3 Apparatus 5.4 Procedure 5.5. Expression of results 5.6 Repeatability and reproducibility 6 Determination of carbon dioxide ‘content (alternative method) 6.1 Principle 6.2 Reagents 6.3 Apparatus 6.4 Procedure 6.5. Expression of ssults 6.6 Repeatability and reproducibility 7 Determination of the alkali content (reference method) Principle Reagents Apparatus Preparation of Page 9 10 18 78 BL 82 8.3 84 85 8.6 8.7 Page 3 EN 196-21 : 1989 Procedure pression of results Repeatability and reproducibility Determination of the alkali content (alternative method) Principle Reagents Apparatus Plotting the calibration curve Procedure Expression of results Repeatability and reproduci Page 10 ut " 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 w alkali content of eement. The standard describes the reference methods and, in certain cases, an alternative method which €: be considered as giving equivalent results, other methods are used, thei results shall b shown to be equivalent to the reealts given by the reference methads. In the case of a dispute, only the reference methods are applicable This standard applies to cements and aso to their constituent materials, such as clinker and Diastrumace slag. 2 References EN 196-2 Methods of testing cement — ‘Chemical analysis of cement Methods of testing cement — Methods of taking and preparin samples of coment Statisties — Vocal symbols EN 196-7 Iso. 8534-177 3 General requirements for testing 3.1 Number of tests ‘The number of tests for the vurious determinations (clauses 4 to 8) shall be tw (see ale 3.3) 3.2 Repeatability and reproduc ‘Toe standard deviation of repeatability sives the CGoseness of agreement between sitecessive Pestlts obtained with the same methed on identical test inaterial, under the same conditions (ssune to, same aboraory al short time inter The standard deviation of reproducibility wives the closeness of agreement benseen individual results obtained with the same method on identical test material but under different conditions (different operators, different apparatus, different Jaboratories andl o different times!) ‘The standard deviations of req reproducibility a dility at ‘expressed in alsalule: percent 3.3 Expression of masses, volumes and results State mayses in grams te the nearest 0.0001 x saul vooluanes fren Duurettes in mnlitees te Ui nearest 0,05 As tefinat ISD EL prow the results, given by the mean of two determinations, as a percentage generally to two decimal places. If the results of two det than twice the st repeat the test an closest values us the result 1-4 Determination of constant mass Determine constant mass by making successive 15 min ignitions followed exch time by cooling and then weighing, Constant mass is reached when the difference between two successive weighing is less than 0,0005 3.5 Preparation of the cemen Before starting the determinat ws differ by mone mn for repeatability, can of the 19H sampl ns, treat the Follows to obtain a sample for testing. sximately 100 g of the sample usin i. Sieve this portion m sieve until the residue emove the metallic iron from material retained on the sieve by means of a wgnet. Then grind the iron free fraction of the mater asses pm sieve. If this sample contains particles of metallic iron such as these that may be introduced accidentally during grinding, remove these iron particles completely {Using maxetic stiryer in a suspension, for nple in evelobexane, Transfer the sample tot van dry flask with an autight elostere and shake oh jons ats quickly as possible 1 entre tl imple is exposed te ambi only for the minimum time. 3.6 Reagents Use only reagents of anatytival quality and distilled water, oF Water of equal purity, during the :nalysis Chiles athersvise stated Take app el means percent by mass. The concenteated liquid reagents tise ty this ant have the following densities (p) (a x em aC) hydrochloric acid haste Lio haa Hato te 12 160 10 67 17h 175 Lat hydrofluoric acid nitrie avid perehlorie acid phusphorie acid sulphuric acid Thi degree of dilation is as volumetric acid Ps hydrochto ample, dilute hydiachlorie 2 means that T volume of concentrated ic aid is to be nixed with 2 volumes of 3.7 Volumetric glassware The volumetric glassware shall be of a i.e, elas A as defined in th tory glassware 4 Determination of the chloride content 4.1 Principle This method gives the total halogen content exce} for fluoride and expresses the result as C1. Thi cement sample is decomposed with boiling dilute ulphides are oxidized into sulphates erfere. The dissolved chloride is, precipitated using a known we silver nitrate solution, After boiling, 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 (IID) salt as indicator, 4.2 Reagents 4.2.1 Concentrated nitric acid (UNO3). 4.2.2 Dilute nitvie acid 1 + 2. Dilute nitric acid V+ 100. Silver witrate (AgNO), ried at 150 °C. her nitrate solution 0.05 mol}. Dissolve 840 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 thiveyanate (SIYSCN). 4.2.7 Ammonium thiveyanate solution, appravimately 0.05 moll, Dissolve 3,8 of ammonium thioeyanate in water and make up to 1000 ml. 4.2.8 Ammoninmn iron (MY) sulphate (SH E80). 12110), 4.2.9 Indicator sulation, Md 10 snl of diate nitsie acid L 2 to 100 ml of a enld saturated solution of nunonivum inn (IL) sulphate in water, 3 Apparatus 4.3.1 Balance, capable of weighing (0001 the 4.3.2 10 ml burctic, graduated to 0,1 ml ye anhydrones magsnesin BA Filter paper reximately 20 un coarse (pore di Fr pipette Page 5 EN 196-21 : 1989 4.4 Procedure Weigh (5 £ 0,05) g of cement and place in a 250 ml beaker, adel 50 ml of water and, while stirring with a glass rod, 50 ml of dilute nitric acid 1 + 2 (4.2.2). Heat the mixture to boiling, stirring occasionally, and boil for L min, Add 5 ml of silver nitrate solution (4.2.5) by pipette (4.3.5) into the boiling solution. Then boil for a maximum of 1 min ‘and filter through a filter paper (4.3.4) washed before use with dilute nitric acid T+ 100 (4.2.3) into a 500 ml flask. Wash the beaker, glass rod ard filter paper with dilute nitric acid 1 +100 until the volume of the filtrate and the washings is 04 ml. Cool the filtrate and washings to below °C, Add 5 inl indicator son the ammonium thioe om (4.2.7) shaking, ly until a drop of this solution produces t-brown colouration which no longer disappears on shaking. Record the volume V} If the chloride content of cement exceeds 0.17 "%, it will be necessary to start the test again with & smaller quantity of coment Carry out the same procedure with no cement sample and record the volume, V2, of ammonium thiocyanate solution used in the blank titration, 4.5 Expression of results aleulate the chloride content (in fortnula: ) from ‘The mean of the two results shall be rounded to the nearest 0,01“ 4.6 Repeatability and reproducibility ability is 0,005 ol on of rep : of rep Page 6 EN 196-21 : 1989 5 Determination of the carbon dioxide content (reference method) 3.1 Principle The cement sumple is treated with phosphe to decompose the carbonate present, T al is entrained ina current of ir Hhrough a series of mn tubes. The fist two remove (er and the following then alors ‘bon dioxide, Two absorption tubes, each cont absorbent for earbe and weighed to determi reased. dosti liber dlioxide-fnve jaws oF absorp invite retain the reaction an e the mass of carbon dioxide 5.2 Reagents B.A Copptr"sulphate (Cur0y-5M20). Copper sulphate solution, saturated. Absorbent fin Inydregen sulphide, Place a Weighed quantity of dried pumice stone with a xznain size between 1.2 mm and 2.4 mm inte a Mat 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 t0 di While stirring frequently with a lass real, Pry the nits of the dish for at least 5h inv an aven ata nperature of (155 £5) °C, Allow the solid mixture to col ina desiceator and store in an Might bottle, Alsortent bur water, anlydrons mayeaesin ) with a particle si perchlorate (M(CIOy botwe Anwortent fir avian dinvide, synthetic a particle siz between 0.5 1 ignated with sedi hydride te 12 mn (Nat Comentrated plassphorie weil MPO) 5.2.7 Comerntrated sulphuric acid WSO) Apparatus BARI Apparatus tor te determination of the carbon divide content, Fire piece of a 2 ested T shuts t pies aratus which ean be fitted with eter small electrical suitable suction pump whieh will nL even Tow of gs oF air Th as ( Compressor apparatus hies by first psorbent tube or tower pected to at dropping. fan necting tube and neck C te condenser. The funnel onto H ¢ free flow cither Hhrough the connecting tube ar the funnel by ‘of a Mobr clip (N). After the: ‘condenser (1). the goes is passed Throat concentrated sulphuric acid (1), then through absorption tubes containing the absorbent for hydrogen sulphide (5.2.3) (E) and for water (3.2.4) (F) and subsequently through two absorption tubes (GAD which ¢ three-quarters filled with the dioxide (5.2 for w dioxide ( for W 1 be weighed and which aze absorb nt tor carbon dhsorbent isorbent for carbon 5) is placed upstream of the absorbent A} with respeet to the sets flow he (H) is followed by: an additional be (1). which abo contains the rho dioxide and water, which is to protect abs against penetration by «a from the air The absorption tubes (G) and (H) which are 1 be weighed may have, for exam fitted in ort 1 the Followine External dist ternal diameter mn ice between branches 45 mm Distance between the lower part of the tube and the upper part of the grand section ‘Tube wall thickness 13 mm 3.2 Balance, capable of weighing to the nearest 0.0001 9, ing aanhydnates magnesia 4 Procedure Weigh (1. £0.05) x of cement and plice it in a dry 100 mal distillation Mask, ¢ tes the apparatus (3.3.1) aes shown without ibsorption tabs (Gi current of carbon dioside: tte 8 IT Babies onneetint lip closed) Wont Tay, Moke Release the Mobr clip and evtnave thie funnel (€), Add 20 anf emncentrated acid into the dropping Funnel sane eet thee ages styl’ tee GL he fated (0) sal Page 7 EN 196-21 : 1989 10 dst fase Dropping funnel connector Connecting Condenser connestor Wash bette with concentrated sulphuric acid (8.2.7) iid (3.2.9) Ateorption tube wath magnesium perchlorate sorbent for water (5.2.4) Atsorption tues with abrbents for earn alate (3.2.5) andl for water (5:24) _Ateorption tlw with absorbent for hyena tubes (G) and (11) in in the balance case in onler to achiewe ure equilibrium, Then weigh each tube separately. Shut off the Mow of goes and attach the vin figure 1 ‘Then reopen the yas Now. After 10 min close ve them, p then + passKe of KAS, ion tubes (G) anil (1D reaains greater than 0,000 w the: almorbents an tubes (E) and (F). i Attach the weighed absorption tubes (@) 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 5 min, Maintain the flow through the apparatus until the flask has Hed to vom temperature Close absorption tubes (G) nl pac then of each carbon dioxide content (see 5.5) ‘The carbon dioxide is practically ¢ sorbed by: tube ( ease in mass of tue (11) exceeds 0,005 3, absorbent in tube (G) and start the test Page 8 EN 196-21 : 1989 5.5 Expression of results Calculate the carbon dioxide content (in * coment from the formula: ma + mg C02 = x 100 is the mass of cement test portion; is the increase in mass of tube G after ab. xption; is the increase in mass of tube IT after 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 0,5 ‘%, repeat the determination with a cement sample weighing 2 g. 5.6 Repeatability and reproducibility ‘The standard deviation of repeatability is 0,07 ‘The standard deviation of reproducibility is 0,10 6 Determination of the carbon dioxide content (alternative method) 6.1 Principle The carbon dioxide is driven off by means of sulphuric acid, absorbed by sodium hydroxide and determined gravimetrically. A hydrogen sulphide present which may distort the results is absorbed by mercuric (I) chloride 6.2 Reagents 6.2.1 Mercurie (II) chloride (HgCly). 6.2.2 Absorbent for curton diaride, synthetic silicates with a particle ize between 0,6 man and 1,2 mm) impregnated with sodium hydroxide, Concentrated sulphuric acid (280). 6.2.4 Dilute sulphuric acid 1 + 4. 6.2.5 Absorbent for water, anhydrous perchlorate (My(C10,)2) with a partic between 0,6 mm and 1,2 mm, 6.3 Apparatus 6.3.1 Apparatus for the determination of the carlo diaride content. The apparatus is shown in figure 2. A small vacuum pump is used to generat reduced pressure in the apparatus, 6.3.2 Balance, capable of weighing to the nearest 2,001 g eee 27a? 6.4 Procedure Place (1. £ 0,05) g of cement into the 100 mt distillation Mask A of the this cement with a small mercuric (11) chloride (6.2.1) using a spatul 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 absorp tower (J) filled with absorbent (6.2.2) to remove the carbon dioxiffe before the air passes into the flask. After stopping the flow of air add 25 ml to 30 ml of sulphuric acid (6.2.4) from the dropping funnel (0) into the Mask. 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 (6.2.5) 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 (6.2.5) 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 (6.2.8) is connected to this as bubble counter, After about 10 min heat ¢ to boil air flow through the apparatus until the flask cook e. Close the al remove the absorption tubes (@), place Ui balance ease for 15 min in order to achieve temperature equilibrium and then weigh them, 6.5 Expression of results aleulate the carbon dio from the form isthe incre: tubes G after absorption, ‘The mean of the two results sl the nearest 0.01 %. 6.6 Repeatability and reproducibility ‘The standart deviation of repeatability is 0.07 ‘The standard deviation of reprodueiblity is 0,10 ° be rouniled Page 9 EN 196-21 : 1989 a thn Maske 1D Washing bot containing concentrated Condenser “Toth vacuum pny main Fone for sulptorie acid (6.2.9) | | | 7 Determination of the alkali content (reference method) 7.1 Principle {ane o propane fla 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 ealeium 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 us/em. 1 reagents of analytical quality (see als 3.6); 1 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. 48 F _Atworption tubes containing magnesium perchlorate (6.2.5) —_Atsonption tubes containing absorbent for earn ellie (6.2.2) Absorption tue containing carbon dione absorbent (6.2.2) and magnesium perchlorate (6.2.5) Absorption toner containing carbon diexite sworn (6.2.2) Figure 2. Apparatus for the determination of the carbon dioxide content (alternative method) 7.2.2 Concentrated hydrochloric acid (IC), 7.2.3 Dilute hydrochloric acid 1 + 19, 7.2.4 Concentrated phosphoric acid (yPO,). 7.2.5 Dilute phosphoric eid 1 + 19; store this solution in a polyethylene flask, {6 Concentrated nitric acid (INO). 7 Concentrated! perchloric acta (IICIO,). 7.2.8 Concentrated hydrofluoric acid (HF). 7.2.9 Sudium chloride (NaCl), dried at 105 °C to constant mass, 7.2.10 Potassium chloride (KC), dried at 105 °C to constant mass, 7.2.11 Alkali stock solution. Weigh about 0,566 of sodium chloride and about 0,475 4 of potassium chloride, transfer t flask, add 100 mal exc 1+ iM and dilute and make up to the mark with water. This solution Page 10 EN 196-21: 1989 contains approximately 0,300 g each of NazO and K,0. The actual contents can be determined from the original quantities from the following formulae: K,0 (in git) = 0,6138 x act mass of potassium chloride ” NayO (in g/1) = 05308 x actual sodium chloride in © 7.3 Apparatus 7.3.1 Balance, capable of weighing to the nearest 0.0001 7.3.2 Calibrated burettes 7.8.3 Flame photometer, with which the int of the sodium Tine at 589 nm and the po line at 768 nm can be measured: a sufficiently stable apparatus shall be ased. 7.34 Platinum dish: 7.8.5 Filter paper, medi diameter ap n pore size (pore roximately 7 pm). 7.8.6 Platinum stirrer, 7.4 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, ray 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 Ni 589 mm and for KO at 768 nm, Plot graphs of the measured intensities against 1 corresponding concentrations of sodium oxide potassium oxide in the calibration solutions. Dissolution of the test portion 7.5.1 Cements completely soluble in acid (Content of insoluble residue < 3%) Weigh 0,1 cement into a 50 ml beaker, make into a slurry with 10 ml of water and add 10 ml of 3 Ywrehlrie acl vapours form exponive mixtures with onanie cree ae the use of fame cpr Ashes with mesures when working wt ‘nyanie stances inthe same Fame eupboe 2749 c acid 1+ ‘until the cement has dissolved, breaking. down with a glass rod. Filter the susper through the filter paper (7. 100 mt 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 w: cool to ambient temperature. Add 10 ml of dilute phosphoric acid 1 + 19 to the solution, make up to the mark and mix thoroughly. 7.5.2 Cements not completely soluble in actd Use the method described below where the content Of insoluble residue, determined in accordat With elause 9 of EN 196-2, exceeds 3‘. Weigh 0,2 g of cement into a platinum dish and add ml of concentrated nitric acid (7.2.6). Heat the mixture, for example, on a hot-plate, and evaporate to dryness. Disperse the residue fron evaporation in 5 ml of water, add 2 ml of concentrated perchloric acid (7.2.7) 10 ml of concentrated hydrofloy Heat the mixture and evapo Prevent overheating by Trequent agitation by means of the platinum stirer (7.3.6). Add 40 ml of water and 20 tnl 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 (7.3.8) into a 200 ml volumetric flask washing through with hot water, Wash the filter paper and residue with hot water until the 200 mil volumetric flask contains a volun approximately 150 ml. Then allow the fit hing water to cool to am 20 mal of dilute phosphoric acid 1 + solution, make up to the thoroughly 7.6 Procedure pray the measuring solution produced as deseribed in 7.5.1 or 7.5.2 into the Fame of the fame photometer (7.3.8). Measure the intensity of the inn Tine a line at mm oxide or potassium respectively by on fra the intensit libration are. Add 19 to the Use the graphs plotted as in soxtium oxide and potassium oxide cone of the solution in mg/l or use the intensities and the associated concentra tion solutions with the next hi intensity for the Page 11 EN 196-21 : 1989 and potassium oxide concentrations “Table 1. Volumes of solutions for the preparation of calibration solutions and thelr sodium oxide | Tine ‘Alkali stock solution | Dil ay) rele ml ml Tydrochlorie acid Dilute phonphorle acld | NazO and KO rei concentrator = 10,0 38 1046 83 167 25,0 33,3 417 8 50,0 95,0 [100.0 99,6 ik solution Caleulate the sodium oxide (Cx,,0) oF potassium oxide (Cx,) concentration of the sample from the intensities Iya,0 oF Ik,u respectively using the following formulae: san + (Con = C0.) a= fin C0 ~ Grn + (Gon ~ Chin) * FF z where Cin 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; Is the concentration of the sodium oxide or potassium oxide respeetively in the calibration solution having a higher concentration than the measuring solution in mg; Is the intensity of the calibration solution wwing a lower concentration than the measured solution; is the intensity of the calibration solution aving a higher concentration than the measuring solution. 7 Expression of results Caleulate 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. Naz0 = 0,1 Cys @) K,0 = 0,1 Cx ® where hago 18 the sodium oxide concentration of the measuring solution as calculated by formula (6) (in mg/l); is the potassium oxide concentration of the measuring solution as caleulated by formula (7) (in mg/). Ceo ‘The mean of the two results for each oxide shall be rounded to the nearest 0,01 3 ‘The total alkali content, A, is obtained by converting the potassium oxide content to equivalent sodium oxide from the formula ‘A = NaO + 0,658 K:0 7.8 Repeatability and reproducibility ‘The standard deviation of repeatability is: 0,01 % for the di 0,02 *% for the detert ‘The standard deviation of reproducibility is: 0,02 % for the determination of Na;0; 0,03 % for the determination of Page 12 EN 196-21 : 1989 BAA Filter paper diameter approximately, 8 B26 Heating lamp. mweditum porenity (pore 7 um. alkali content 8 Determination of th {alternative method) 8.1 Principle ‘Cements whieh are comp! with hydrochloric acid. C incompletely soluble are first evaporated with hydrofluoric acid sulphuric acid. Tae alkali 8.4 Plotting the calibration curve contents of the solutions are determined by means In the case of cements which are comple ‘of Flame ph & Platinum dish. BAT Calibrated burette sly metry. soluble in hydrochloric acid, evaporate 20 mL of ici L + to dryness, and, in the ts not completely soluble in acid, of hydrofluoric acid (8.2.3) and A) to dryness for the alibration solutions for 8.2 Reagents 8.2.1 Concentrated lyelrvehtovie acid (HCD, evaporate 1 of sulphuric purposes of prepst Dilute yilrvehtovie acid V+ 9. an{uF), 8.244 Concentiuted sulphuric acid (80). 3 Concentrated lydtrumluoric ac In both eases dissolve the residue from evaporation, with 2 ml of hydrochloric acid 1+ 9 and 3 ml of 8.2.5 Lithium chloride (LICD); dried at 120 °C. water, Transfer the solution to a 100 ml volumetric ji oer flask and add 10 ml of buffer solution (8.2.11). Ye dried at 105 °C tsar the following quantities of the stock solution (8.2.8) to the individual volumetric Masks at 105 °Cto using the calibrated burette (8.3.7). 8.2.6 Sodtium chloride (Si const 8.2.7 Matassium chloride (KC: dried constant mas. : Tara ae WF 8.2.8 Stock solution [Rock mitment Jo [fe ae Pa Dissolve 0,610 g of lithium chloride, 0, got ~ = soi erie 0187 ‘oride Ther make up the volumetie flasks to the mack in water ina 1000 ml Volumetric flask and make up — yeithe distilled wat to the mark, 8.2.9 Cesium ehlnride (CD. 8.2.10 Aluminium nitrate (AUNO4)s. 8110), 8.2.11 Bufier sulution® a E moe] % Dissolve 50 g of caesium eliride and 250 gor [S cr fel sem 0 and Na0 content of laminin nitrate in water and make up to Tremont) —[o[ eh 1 a0 [ on ea 10000 eae eae on solutions inte the Hane of the Apparatus photometer (8.3.3) ksi ast and set the indie spray the oth om soutions i of increasing concentration (2 10 7). Meastn intensities for NayO at 589 nm and for KO at 7H num, Plot graphs af the meastured intensities iugainst the corresponding concentiations of sodium foxide and potassium oxide in th calibration tus 10 0, onder the 1. Balance, capable of weighing to the nearest 0.0001 8.3.2 (05 £5) °C and 8.3.3 Flame photometer, intensities of the sodium line at 588m potassium Ih n The Flame phot Jertrie urea, which can be set at (120 £5) 2c. mote shall be oper me at Ia sufficiently stable photometer is used, itis only relatively low tempe avoid ecessary to establish the calibration curves front distortion of the determination by alkaline earths. time to time, However, the values measured for Hlasks 1 and 7 shall be ehwcked far each analysis These soatons can ab be obtain! nade up realy for 2751 ta 8.5 Procedure 8.5.1 Cements completely soluble in actd (content of insoluble residue <3 %) Weigh 0,2 4 cement into the platinum dish (8.3.5), make into a slurry with 3 ml of water and evaporate to drynes after adding 20 ml of dilute hydrochloric acid 1+ 9. Add hot water and 2 mi of dilute hydrochloric acid 1 + 9 to the residue and filter through the filter paper (6.3.4) into 2 100 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 the mark with water. 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 KO and Na,0 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 dryress 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 deseribed in 8.5.1. 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 ‘The mean of the two results for each 0 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 Na,0; 0,02 % for the determination of K30. ‘The standard deviation of reproducibility is 0,02 % for the determination of Naz0; 0,03 % for the determination of K20. BS EN 196-21 : 1992 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 conerete NA.1 General ‘This method of test is intended to be used for th determination of the alkali content of cement only for the purpose of calculating the reactive alka content of the conerete mix when 2 containing an alkali reactive constitu aan unfamiliar cement/aggregate combination, is in use (see 4.2.4 of BS 5328 : Part 1). NA.2 Apparatus 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 NaO per litre.) Dry a quantity of analytical reagent grade, or purer, NaCl 250 °C, weigh 0.1886 4, dissolve i water and dilute to 1000 ml. NA.3.2 Putassium stock solution, (100 mg of KO per litre.) Dry a quantity of analytical reagent grade, or purer, KCI at 250 °C, weigh 0.1583 8, dissolve in water and dilute to’1000 ml. NA.3.3 Ahuninium solution, (20 of At 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 super-purity alumin between 0.5 mm and 3 mm thick, cut two pieces, one about 120 mm x 360'mm and the other about 120 mm > 200 mm. Bend the larger piece to fit inside a 2.1 boro plastics beaker, then bend t Inside the larger one. Near the middle of the t f each piece drill a hole and twist a separate piece of thick aluminium, each one to make electrical connections. Cl bath sheets by washing successively et fs the he pte 21 gf aunts bl ed spirits. Allow the sheets to dry, nto + 0.05 gand place them in th vaker ensuring that they do not make contact with each other, Cover the beaker with zefilastics cover and take the wire leads out through ho 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 ead from the inner sheet to the negative terminal of a source of direct current which can bbe varied from 0 V to 12 V). While stirring, add 200 ml of nitric acid to 800 ml of warm water (about 50 °C) in a ‘separate beaker and trunsfer this solution to the beaker containing the electrodes. Switch on the power supply and increase the applied voltage to obtain a current of about 8 A. When it is considered that sufficient aluminium has dissolved), switeh off and disconnect the power supply. Remove, wash, dry and reweigh the aluminium shects together with any pieces that may have become detached. Calculate 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, ) Cut sufficient super-purity alumin ‘or wire into small pieces and wash succes with dilute hydrochloric acid (I+ 9), water and industrial methylated spirits, Dry, weigh out 20.0 g and transfer a little at a time, usit ‘Tongs, to a gently boiling solution of 100 ml of nitrie acid in 500 ml of water to which 2 ml of, saturated mercuric chloride solution hive 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 ml. NA.3.4 Calcium solution, (6. sh of CaO per litre.) cer, cover with 100 ml of water and carefully add 25 ml of HINO. When solution is complete dilute to 1000 ml with w ‘Test for sodium and potassium con the following procedure, Prepare solutions A, Band C, using the quantities given in table NA.1 With the sodium fight filter in place, set the flame photometer to read 0 with solution and 100 % y solution C and recand the ive. Replace the soitum light filter by: the ht filter and repeat the procedure. If than 2 for NasO (0.1 nye) or T for Ky0 (0,1 mg/l) are obtained rejec solution and propare a new solution, Jing 4 purer source of CaCO, read 420 A ower eure ar tants perme 1992 NA.4 Calibration Prepare calibration solutions using the quant sven in table NA With the sodium light filter in place set the fame photometer to read 0 with seale-zero solution and 100 with scale-100 solution. Record the readings el for cach of the intermediate ealibration ions. checking and adjusting if necessary, the 100 settings between each reading. Replace the sodjum light filter by the potassium light filter ‘and repeat the calibration procedure. Construct the calibration graphs of instrument reading against milligrams per litre of Nag0 or K30. NOTE 1, For instruments ‘Accordance withthe manufacturers striction [NOTE 2, In some exes different Na0 and or KO ‘concentration ranges may le req. Slt is be necessary ti the alka ete of the

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