EN 196-2:2005

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Metode preskušanja cementa - 2. del: Kemijska analiza cementaPrüfverfahren für Zement - Teil 2: Chemische Analyse von ZementMéthodes d'essais des ciments - Partie 2: Analyse chimique des cimentsMethods of testing cement - Part 2: Chemical analysis of cement91.100.10Cement. Mavec. Apno. MaltaCement. Gypsum. Lime. Mortar71.040.40Kemijska analizaChemical analysisICS:Ta slovenski standard je istoveten z:EN 196-2:2005SIST EN 196-2:2005en01-april-2005SIST EN 196-2:2005SLOVENSKI
STANDARDSIST EN 196-21:1995SIST EN 196-2:19951DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 196-2
February 2005 ICS 91.100.10 Supersedes EN 196-2:1994, EN 196-21:1989 English version
Methods of testing cement - Part 2: Chemical analysis of cement
Méthodes d'essais des ciments - Partie 2: Analyse chimique des ciments
Prüfverfahren für Zement - Teil 2: Chemische Analyse von Zement This European Standard was approved by CEN on 29 December 2004.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. 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 Central Secretariat has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36
B-1050 Brussels © 2005 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 196-2:2005: ESIST EN 196-2:2005

used. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 196-7, Methods of testing cement — Part 7: Methods of taking and preparing samples of cement ISO 385-1, Laboratory glassware — Burettes — Part 1: General requirements ISO 835-1, Laboratory glassware — Graduated pipettes — Part 1: General requirements 3 General requirements for testing 3.1 Number of tests Analysis of a cement may require the determination of a number of its chemical properties. For each determination one or more tests shall be carried out in which the number of measurements to be taken shall be as specified in the relevant clause of this document. Where the analysis is one of a series subject to statistical control, determination of each chemical property by a single test shall be the minimum required. Where the analysis is not part of a series subject to statistical control, the number of tests for determination of each chemical property shall be two (see also 3.3). In the case of a dispute, the number of tests for determination of each chemical property shall be two (see also 3.3). 3.2 Repeatability and reproducibility Repeatability - Precision under repeatability conditions where independent test results are obtained with the same method on identical test items (material) in the same laboratory by the same operator using the same equipment within short intervals of time. Reproducibility - Precision under reproducibility conditions where test results are obtained with the same method on identical test items (material) in different laboratories with different operators using different equipment. SIST EN 196-2:2005

1 000 ml. 4.42 Silver nitrate (AgNO3), dried to constant mass at (150 ± 5) °C. 4.43 Silver nitrate solution. Dissolve 5 g of silver nitrate (AgNO3) (4.42) in water, add 10 ml of concentrated nitric acid (HNO3) (4.12) and make up to 1 000 ml with water. 4.44 Silver nitrate solution 0,05 mol/l. Dissolve (8,494 0 ± 0,000 5) g of silver nitrate (AgNO3) (4.42) in water in a 1 000 ml volumetric flask and make up to the mark. Store in a brown glass container and protect from the light. SIST EN 196-2:2005

50 ml in a volumetric flask. 4.56 Ammonium acetate solution. Dissolve 250 g of ammonium acetate (CH3COONH4) in water and make up to 1 000 ml. 4.57 Triethanolamine N(CH2CH2OH)3 (>99 %) diluted to 1 + 4 solution. 4.58 Reducing solution. Dissolve 1 g of tin (II) chloride (SnCl2.2H2O) (4.33) in water to which has been added 1 ml of concentrated hydrochloric acid (4.1). Make up to 100 ml with water. Use within one day. 4.59 Buffer solution of pH 1,40. Dissolve (7,505 ± 0,001) g of amino-acetic acid (4.23) and
(5,850 ± 0,001) g of sodium chloride (NaCl) (4.37) in water and make up to 1 000 ml. Dilute 300 ml of this solution to 1 000 ml with hydrochloric acid 1 + 99 (4.8). 4.60 Standard potassium iodate solution, approximately 0,016 6 mol/l. Weigh, to ± 0,000 5 g,
(3,6 ± 0,1) g, of potassium iodate (KIO3) (4.34) (m1) and place in a 1000 ml volumetric flask. Add 0,2 g of sodium hydroxide (4.29), 25 g of potassium iodide (KI), dissolve all the solids in freshly boiled and cooled water and make up to the mark using the same water. Calculate the factor F of the potassium iodate solution from the following formula: 856631,m
=F (1) where m1 is the mass of the portion of potassium iodate, in grams. 4.61 Sodium thiosulfate solution approximately 0,1 mol/l 4.61.1 Preparation SIST EN 196-2:2005

Standardization 4.61.2.1 This standardization is carried out preferably using the standard potassium iodate solution (4.60). For this standardization, pipette 20 ml of the standard potassium iodate solution (4.60) into a 500 ml conical flask and dilute with approximately 150 ml of water. Acidify with 25 ml of hydrochloric acid 1+1 (4.2) and titrate with the approximately 0,1 mol/l sodium thiosulfate solution (4.61.1) to a pale yellow colour. Add 2 ml of the starch solution (4.49) and continue the titration until the colour changes from blue to colourless. Calculate the factor f of the sodium thiosulfate solution from the formula: VF
=V
,F
,
,
=f1120856630121467016020××××× (2) where F is the factor of the standard potassium iodate solution (4.60); V1 is the volume of the approximately 0,1 mol/l sodium thiosulfate solution used for the titration, in millilitres; 3,566 8 is the mass of potassium iodate corresponding to a solution with exactly 0,016 67 mol/l of potassium iodate, in grams; 214,01 is the molecular mass of KIO3, in grams. 4.61.2.2 The standardization may alternatively be carried out using a known quantity of potassium iodate. For this standardization, weigh, to ± 0,000 5 g, (0,070 ± 0,005) g of potassium iodate (4.34) (m2) and place in a 500 ml conical flask. Dissolve in approximately 150 ml of water. Add about 1 g of potassium iodide, acidify with 25 ml of hydrochloric acid 1+1 (4.2) and titrate with the approximately 0,1 mol/l sodium thiosulfate solution (4.61.1) until a pale yellow colour is obtained. Then add 2 ml of the starch solution (4.49) and titrate until the colour changes from blue to colourless. Calculate the factor f of the sodium thiosulfate solution from the formula: Vm
, =V,m
=f22224363280856630001××× (3) where m2 is the mass of potassium iodate, in grams; V2 is the volume of the approximately 0,1 mol/l sodium thiosulfate solution used for the titration, in millilitres; 3,566 8 is the mass of potassium iodate corresponding to a solution with exactly 0,016 67 mol/l of potassium iodate, in grams. 4.62 Standard manganese solution 4.62.1 Anhydrous manganese sulfate Dry hydrated manganese sulfate (MnSO4.xH2O) to constant mass at (250 ± 10) °C. The composition of the product obtained corresponds to the formula MnSO4. SIST EN 196-2:2005

(2,0 ± 0,1) g of anhydrous sodium carbonate (4.39). Heat the mixture and fuse it at a bright-red heat for at least 15 min. After cooling to room temperature, place the fused solid in a polyethylene beaker and dissolve it in water, then transfer the solution quantitatively to a 200 ml volumetric flask and make up to the mark with water. Store the solution in a polyethylene container. This solution contains 1 mg of SiO2 per millilitre. 4.63.3 Standard solution Pipette 5 ml of the basic solution into a 250 ml volumetric flask and make up to the mark with water. Store the solution in a polyethylene container. This solution contains 0,02 mg silica per millilitre. Use within one week. 4.63.4 Compensating solutions Prepare the compensating solutions according to the procedure adopted in the determination of silica content (13.3 to 13.5) by dissolving the amounts of the reagents given in Table 2 in water and making up to 500 ml. 4.63.5 Construction of the calibration curve Add from a burette the volumes of the silica calibration solutions given in Table 3 into 100 ml polyethylene beakers each containing a magnetic stirrer bar. Add 20 ml of the compensating solution by pipette and make up to 40 ml with water from a burette. The volumes required for this are also given in Table 3. While stirring with a magnetic stirrer, add 15 drops of hydrofluoric acid 1+3 (4.11). Stir for at least 1 min. Then pipette 15 ml of the boric acid solution (4.51) into the solution. SIST EN 196-2:2005

Precipitation by double evaporation (13.3) Precipitation by polyethylene oxide (13.4) Decomposition by HCl and NH4Cl
(13.5) HCl conc. ml 75 70 15 H2SO4 1 + 1 ml 1 1 - HNO3 conc. ml - - 1 Polyethylene oxide solution ml - 5 - NH4Cl g - - 1 Na2CO3 g 1,75 1,75 1,75 NaCl g 0,25 0,25 0,25 Na2O2 g 3 3 -
Table 3 — Composition of the silica calibration solutions and their silica content Serial No. Blank 1 2 3 4 Standard SiO2 solution (ml) 0 2 5 10 20 Water (ml) 20 18 15 10 0 Silica content (mg SiO2/100 ml) 0 0,04 0,10 0,20 0,40
Add from a pipette 5 ml of the ammonium molybdate solution (4.54). Adjust the pH of this solution to (1,60 ± 0,05) by adding, drop by drop, sodium hydroxide solution (4.30) or hydrochloric acid 1 + 2 (4.3) using the pH meter (5.18.1) calibrated with a buffer solution of similar pH (e.g. 1,40 see 4.59). Transfer the solution to a 100 ml volumetric flask and rinse the beaker with dilute hydrochloric acid (4.9). After 20 min, add from a pipette 5 ml of the citric acid solution (4.52), stir and leave to stand for 5 min. Then add from a pipette 2 ml of the reducing solution (4.58). (Time 0). Make up to the mark with dilute hydrochloric acid (4.9) and mix. At time (0 + 30) min measure the absorbance with the photometer (5.10) using a cell (5.11) of 1 cm optical length against the blank solution prepared in the same way, using the wavelength 815 nm. Construct a curve giving the measured absorbance as a function of the corresponding silica contents given in Table 3. The blank solution used in constructing the calibration curve may be used as the blank solution here. The calibration curve enables the silica content in mg SiO2/100 ml to be determined. 4.64 Standard calcium ion solution, approximately 0,01 mol/l Weigh, to ± 0,000 5 g, (1,00 ± 0,01) g of calcium carbonate (4.53) (m4) and place it in a 400 ml beaker with approximately 100 ml of water. Cover the beaker with a watch glass and carefully introduce approximately
10 ml of hydrochloric acid 1 + 2 (4.3). Stir with a glass rod and ensure that dissolution is complete, bring to the boil in order to expel the dissolved carbon dioxide. Cool to room temperature, transfer to a 1 000 ml volumetric flask, washing the beaker and watch glass carefully, and make up to the mark with water. 4.65 EDTA solution, approximately 0,03 mol/l 4.65.1 Ethylenediaminetetra-acetic acid disodium salt dihydrate (EDTA) 4.65.2 Preparation Dissolve (11,17 ± 0,01) g of EDTA in water and make up to 1 000 ml. Store in a polyethylene container. SIST EN 196-2:2005

, = V ,
,m
=fD3434652160300910050××××
(5) where m4 is the mass of calcium carbonate taken to prepare the standard calcium ion solution (4.64), in grams; V3 is the volume of the EDTA solution used for the titration, in millilitres. b) Visual determination of the end-point (alternative method) Add, without weighing, about 0,1 g of either the calcon indicator (4.71) or the Patton and Reeders indicator (4.76). Stir and titrate with the approximately 0,03 mol/l EDTA solution (4.65) until the colour changes from pink to blue (calcon) or purple to blue (Patton and Reeders), volume V3, and one drop in excess does not further increase the intensity of the blue colour. Calculate the standardization factor fD of the EDTA solution using equation (5). 4.66 Copper complexonate solution Pipette 25 ml of the copper sulfate solution (4.55) into a 400 ml beaker and add from a burette an equivalent volume V5 of the approximately 0,03 mol/l EDTA solution (4.65). Determine the required volume V5 of EDTA solution as follows. Pipette 10 ml of the copper sulfate solution (4.55) into a 600 ml beaker. Dilute to approximately 200 ml with water and add 10 ml of concentrated ammonium hydroxide (4.25) and, without weighing, about 0,1 g of murexide indicator (4.69). Titrate with the approximately 0,03 mol/l EDTA solution (4.65) until the colour changes from pink to violet (V4). Calculate the volume V5 of the approximately 0,03 mol/l EDTA solution to be added to 25 ml of the copper sulfate solution to obtain copper complexonate from the formula: V
, = V4552× (6) where V4 is the volume of the approximately 0,03 mol/l EDTA solution for the titration, in millilitres. SIST EN 196-2:2005
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