SIST EN 14016-2:2004

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Bindemittel für Magnesiaestriche - Kaustische Magnesia und Magnesiumchlorid - Teil 2: PrüfverfahrenLiants pour chapes a base de magnésie - Magnésie caustique et chlorure de magnésium - Partie 2: Méthodes d'essaiBinders for magnesite screeds - Caustic magnesia and magnesium chloride - Part 2: Test methods91.100.50Veziva. Tesnilni materialiBinders. Sealing materialsICS:Ta slovenski standard je istoveten z:EN 14016-2:2004SIST EN 14016-2:2004en01-april-2004SIST EN 14016-2:2004SLOVENSKI
STANDARD



SIST EN 14016-2:2004



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14016-2January 2004ICS 91.100.50English versionBinders for magnesite screeds - Caustic magnesia andmagnesium chloride - Part 2: Test methodsLiants pour chapes à base de magnésie - Magnésiecaustique et chlorure de magnésium - Partie 2: Méthodesd'essaiBindemittel für Magnesiaestriche - Kaustische Magnesiaund Magnesiumchlorid - Teil 2: PrüfverfahrenThis European Standard was approved by CEN on 15 September 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards 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 translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.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 STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2004 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14016-2:2004: ESIST EN 14016-2:2004



EN 14016-2:2004 (E)2ContentspageForeword.31Scope.42Normative references.43Magnesium chloride test.43.1Sampling.43.1.1General.43.1.2Aqueous solution.43.1.3Solid salt.53.2Chemical analysis.53.2.1General.53.2.2Determination of water-insoluble constituents.53.2.3Sulfate content SO42-.63.2.4Calcium content Ca2+.73.2.5Magnesium content Mg2+.83.2.6Magnesium sulfate MgSO4, calcium sulfate CaSO4, calcium chloride CaCl2 and magnesiumchloride MgCl2.93.2.7Alkali chlorides (sodium chloride and potassium chloride).103.2.8Determination of the pH value.124Caustic magnesia test.124.1Sampling and preparation of the sample.124.2Chemical analysis.124.2.1General.124.2.2Hydrochloric acid insoluble residue.124.2.3Sesquioxides R2O3(Al2O3 + Fe2O3).134.2.4Calcium oxide CaO.144.2.5Determination of the free CaO content.154.2.6Magnesium oxide MgO.154.2.7Loss on ignition.164.3Bulk density.174.3.1General.174.4Fineness.184.4.1Apparatus.184.4.2Procedure and evaluation.184.5Setting time.194.5.1General.194.5.2Temperature and relative humidity.194.5.3Apparatus.194.5.4Magnesium chloride test solution.214.5.5Preparation of the magnesia paste of standard consistency.214.5.6Initial and final setting time.214.6Flexural strength and compressive strength.224.6.1General.224.6.2Preparation of the magnesia test mortar and the test specimens.224.6.3Procedure and evaluation.235Test report.23Bibliography.24SIST EN 14016-2:2004



EN 14016-2:2004 (E)3ForewordThis document (EN 14016-2:2004) has been prepared by Technical Committee CEN/TC 303 “Floor screeds and in-situ floorings in buildings”, the secretariat of which is held by BSI.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by July 2004, and conflicting national standards shall be withdrawn at the latest byJuly 2004.This document belongs to a series of standards on screed materials and floor screeds in buildings.No existing European Standard is superseded by this standard.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following coun-tries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Esto-nia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.SIST EN 14016-2:2004



EN 14016-2:2004 (E)41 ScopeThis European Standard applies to caustic magnesia and magnesium chloride used for the manufacture of magne-site screed material and magnesite floor screeds as specified in EN 13813 and describes test methods by meansof which the fulfilment of the requirements in EN 14016-1 can be checked.2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).EN 196-1, Methods of testing cement - Part 1: Determination of strength.EN 196-3, Methods of testing cement - Part 3: Determination of setting time and soundness.EN 459-2, Building lime - Part 2: Test methods.EN 13813, Screed materials and floor screeds - Screed material - Properties and requirements.EN 13892-1, Methods of test for screed materials - Part 1: Sampling, making and curing specimens for test.EN 13892-2, Methods of test for screed materials - Part
2: Determination of flexural and compressive strength.EN 14016-1, Binders for magnesite screeds - Caustic magnesia and magnesiumchloride - Part 1: Definitions, re-quirements.ISO 3310-1, Test sieves - Technical requirements and testing - Part 1: Test sieves of metal wire cloth.3 Magnesium chloride test3.1 Sampling3.1.1 GeneralFor the chemical analysis, take a representative sample of the following minimum quantities from the batch to betested.¾ 2 000 g from an aqueous solution or¾ 1 000 g from solid salt.3.1.2 Aqueous solutionFor sampling, thoroughly stir the whole quantity in the vessel. If salts have crystallised out through storage at lowtemperatures, bring them into solution again by gentle warming and stirring. If the solution has precipitated salts, donot take the sample just from the clear solution or from parts of the solution that contain solid salt.If the vessel has been partially emptied before sampling and contains precipitated salt, it is not possible to obtain arepresentative sample.SIST EN 14016-2:2004



EN 14016-2:2004 (E)53.1.3 Solid saltSamples shall only be taken from the inside of the blocks or of the salt mass (melted, ground in flakes or granules,crystallised). In order to obtain correct representative samples, take several individual samples depending onquantity and type of packaging and combine them to make a cumulative sample. As magnesium chloride attracts aconsiderable amount of moisture from the air, sampling, size reduction and mixing of the individual samples shallbe carried out as rapidly as possible. Store the final samples in tightly stoppered bottles.3.2 Chemical analysis3.2.1 GeneralThis subclause describes reference methods for determining the requirements specified EN 14016-1. If other testmethods are used, it shall be demonstrated that the results obtained with them are equivalent to the results of thereference methods. In cases of dispute, the reference method shall be used.Only analytically pure reagents shall be used. Unless otherwise stated, % means percentage by mass. The term“water” shall be understood to mean distilled water or water of the same degree of purity. “r” always designates thedensity of a liquid at 20 °C. Dilutions are given as a volume sum, e.g. dilute hydrochloric acid 1 + 19 means that 1 part per volume of concentrated hydrochloric acid shall be mixed with 19 parts per volume of water.3.2.2 Determination of water-insoluble constituents3.2.2.1 Apparatus¾ Balance accurate to 0,000 1 g;¾ Platinum or porcelain crucible;¾ Electric oven, adjustable to (1 000 ± 25) °C;¾ Desiccator with drying agent.3.2.2.2 Reagents¾ Silver nitrate, AgNO3;¾ Nitric acid, concentrated, HNO3 (r = 1,40 g/cm3 to 1,42 g/cm3);¾ Silver nitrate solution.Dissolve 0,5 g of silver nitrate in 100 ml of water and add a few drops of nitric acid.3.2.2.3 Procedure and evaluationAdd 200 ml of water to 100 g of aqueous magnesium chloride solution or to 50 g of solid magnesium chloride,weighed to the nearest 0,000 1 g, in a 400 ml beaker (tall form). After 15 min of intensive stirring, filter through afilter paper (medium fast: 140 s filtration time using the Herzberg test system) into a 500 ml volumetric flask. Washthe filtration residue with hot water free from chloride (check with silver nitrate solution). The filtrate is used to de-termine the content of the water-soluble constituents and the pH value. Dry the filter paper and the contents in ared-hot crucible of known mass and reduce to ash. Then heat the crucible for 15 min at (1 000 ± 25) °C. Allow thecrucible and its contents to cool down to room temperature in the desiccator and weigh the residue to the nearest0,000 1 g. Calculate the water-insoluble constituents as a percentage by mass WC using the following equation:EAmmWC100´= in %whereSIST EN 14016-2:2004



EN 14016-2:2004 (E)6mAis the final mass in g;mEis the initial mass of aqueous magnesium chloride solution or solid magnesium chloride in g.Make up the filtrate in the 500 ml volumetric flask containing the water-soluble constituents with water to the mark.3.2.3 Sulfate content SO42-3.2.3.1 Apparatus¾ Platinum crucible;¾ Electric oven, adjustable to (800 ± 25) °C;¾ Desiccator with drying agent.3.2.3.2 Reagents¾ Hydrochloric acid, concentrated, HCl (r = 1,18 g/cm3 to 1,19 g/cm3;¾ Hydrochloric acid, dilute 1 + 11;¾ Barium chloride – 2 – hydrate BaCl2 × 2H2O;¾ Barium chloride solution:Dissolve 120 g of barium chloride in water to make up 1 000 ml;¾ Silver nitrate AgNO3;¾ Nitric acid HNO3;¾ Silver nitrate solution:Dissolve 0,5 g of silver nitrate in 100 ml of water and add a few drops of nitric acid.3.2.3.3 Procedure and evaluationIf aqueous magnesium chloride solution is the material to be tested for determination of the sulfate content, pipette25 ml of the solution prepared as described in 3.2.2 into a 400 ml beaker. Use 50 ml of the solution as specified in3.2.2 for the determination if the material to be tested is solid magnesium chloride. Dilute the solution with water toapproximately 250 ml and adjust the pH value to 2,0 to 2,5 with dilute hydrochloric acid. Depending on the bariumsulfate content to be expected, add 3 ml to 5 ml of hot barium chloride solution in drops (1 ml of barium chloridesolution to 100 mg of barium sulfate) to the boiling solution whilst stirring vigorously. Boil for a further 15 min to en-sure good precipitation. Allow to stand overnight and filter the precipitate through a filter paper (slow: 1 500 s filtra-tion time according to the Herzberg test system) and wash chloride free with boiling water (check with silver nitratesolution). Transfer the filter paper and the contents to a red-hot crucible of known mass and reduce to ash at full airflow. Then, heat at (800 ± 25) °C to constant mass (± 0,000 5 g). Allow the crucible and its contents to cool down toroom temperature in the desiccator and then finally weigh the residue to the nearest 0,000 1 g. If the material to betested is aqueous magnesium chloride solution, calculate the percentage by mass of sulfate content using the fol-lowing equation:Sulfate content -24totalSO = EAmxm100232,81´ in %If the material to be tested is solid magnesium chloride, calculate the percentage by mass of sulfate content usingthe following equation:Sulfate content -24totalSO = EAmm100116,42´´ in %SIST EN 14016-2:2004



EN 14016-2:2004 (E)7wheremA1 is the final mass of barium sulfate in the aqueous magnesium chloride solution as the material to be testedin grams;mA2 is the final mass of barium sulfate in the solid magnesium chloride as the material to be tested in grams;mE is the initial mass of aqueous magnesium chloride solution or solid magnesium chloride specified in 3.2.2 ingrams.3.2.4 Calcium content Ca2+3.2.4.1 Reagents¾ Sodium hydroxide NaOH;¾ Sodium hydroxide solution approximately 1 mol/l:dissolve 40 g of sodium hydroxide in water and make upto 1 000 ml of solution; keep the solution in a polyethylene bottle;¾ Murexide:purpuric acid, ammonium salt;¾ Naphtol green B:1-nitroso-2-naphthol-6-sulfonic acid, iron-sodium salt;¾ Sodium chloride NaCl;¾ Murexide mixed indicator:Grind 0,1 g of murexide and 0,3 g of naphthol green B with 30 g of sodium chloride;¾ EDTA:ethylenediamine tetraacetic acid, disodium salt, dihydrate;¾ EDTA solution 0,01 mol/l (a commercially available ready-to-use solution may be used).3.2.4.2 Procedure and evaluationTo analyse aqueous magnesium chloride solution and solid magnesium chloride, pipette 50 ml and 100 ml respec-tively of the solution prepared as described in 3.2.2 into a 500 ml volumetric flask and make up to the mark withwater. Pipette 100 ml of this solution into a 250 ml beaker (tall form). Adjust the pH value of the solution to at least13 (check) using sodium hydroxide solution. After adding approximately 0,1 g of murexide mixed indicator, titratethe solution on a white base against a white background (approximately 10 cm away) with 0,01 mol/l of EDTA solu-tion stirring continuously (e.g. using a magnetic stirrer). The end point is indicated by a change in colour from red toviolet.Determine the blank value in parallel.Other common indicators may also be used, e.g. calconcarboxylic acid (colour change: wine red to blue). Traces ofiron, manganese, zinc and copper interfere with the titration. Depending on the type and quantity of the interferingelements, add 10 drops of 10 % sodium sulfide solution or triethanolamine solution 1 + 4 to the solution before ti-tration.If the material to be tested is magnesium chloride solution, calculate the calcium content as the percentage bymass of Ca2+ using the following equation:Calcium content +2totalCa= EmBV100)(02004,01´-´ in %If the material to be tested is solid magnesium chloride, calculate the calcium content as the percentage by mass ofCa2+ using the following equation:SIST EN 14016-2:2004



EN 14016-2:2004 (E)8Calcium content +2totalCa= EmBV100)(01002,02´-´ in %whereV1 is the volume of 0,01 mol/l EDTA solution used when determining the aqueous magnesium chloride solu-tion, in millilitres;V2 is the volume of 0,01 mol/l EDTA solution used when determining the solid magnesium chloride, in millili-tres;B is the blank value in millilitres;mE is the initial mass of aqueous magnesium chloride solution or solid magnesium chloride specified in 3.2.2 ingrams.3.2.5 Magnesium content Mg2+3.2.5.1 Reagents¾ Ammonium chloride NH4Cl;¾ Ammonia solution (r = 0,91 g/cm3) NH3;¾ Ammonium chloride buffer:Dissolve 70 g of ammonium chloride and 570 ml of ammonia solution with wa-ter and make up to 1 000 ml;¾ Eriochrome black T:2-hydroxy-1-(1’-hydroxy-2-azonaphthyl)-6-nitronaphthalene-4-sulfonic acid, sodiumsalt;¾ Eriochrome black T indicator:grind1 g of eriochrome black T with 100 g of sodium chloride;¾ EDTA:ethylenediamine tetraacetic acid, disodium salt, dihydrate;¾ EDTA solution 0,1 mol/l (a commercially available ready-to-use solution may be used);¾ Sodium sulfide Na2S × nH2O;¾ Triethanolmine N(CH2CH2OH)3 (r = 1,12 g/cm3);¾ Triethanolmine solution 1 + 4.3.2.5.2 Procedure and evaluationPipette 10 ml of the solution prepared as specified in 3.2.4 (500 ml volumetric flask) into a 250 ml beaker (tall form)and dilute to approximately 100 ml. Adjust the pH value of the solution with 10 ml of ammonium chloride buffer.After adding approximately 0,1 g of eriochrome black T indicator, titrate the solution on a white base against awhite background (approximately 10 cm away) with EDTA solution, 0,1 mol/l, stirring continuously (e.g. using amagnetic stirrer). The end point is indicated by a change in colour from red to blue.Determine the blank value in parallel.Other common indicators may also be used. Traces of iron, manganese, zinc and copper interfere with the titration.Depending on the type and quantity of the interfering elements, add 10 drops of 10 % sodium sulfide solution ortriethanolamine solution 1 + 4 to the solution before titration.Other common indicators may also be used.SIST EN 14016-2:2004



EN 14016-2:2004 (E)9The percentage of magnesium determined Mg total comprises the magnesium bound to chloride and sulfate. Theresult also contains the calcium content of the corresponding water-soluble salts also determined during titration.If the material to be tested is magnesium chloride solution, calculate the total magnesium content as the percent-age by mass of Mg total using the following equation:Magnesium content Mg total= EmBV100)(2152,13´-´ in %If the material to be tested is solid magnesium chloride, calculate the total magnesium content as the percentageby mass of Mg total using the following equation:Magnesium content Mg total= EmBV100)(6076,04´-´ in %whereV3 is the volume of 0,1 mol/l EDTA solution used when determining the aqueous magnesium chloride solution,in ml;V4 is the volume of 0,1 mol/l EDTA solution used when determining the solid magnesium chloride solution, inml;B is the blank value in ml;mE is the initial mass of aqueous magnesium chloride solution or solid magnesium chloride specified in 3.2.2in g.3.2.6 Magnesium sulfate MgSO4, calcium sulfate CaSO4, calcium chloride CaCl2 and magnesium chlorideMgCl2If the total sulfate content is greater than the sulfate content bonded as calcium sulfate i.e.-24totalSO>4172,13967,32totalCa+´ in %then sulfate is present as magnesium sulfate and calcium sulfate.Sulfate content-244MgSOSO=-24totalMgSOSO - 4172,13967,32+´totalCa in %Magnesium sulfate MgSO4=-×244253,1MgSOSO in %Calcium sulfate CaSO4=+×23967,3totalCa in %Calculate the sulfate-bonded magnesium content as a percentage by mass of 4MgSOMG using the following equa-tion:Sulfate-bonded magnesium49201,04MgSOMgMgSO´=, in %Calculate the magnesium chloride content from the total magnesium content and the sulfate-bonded magnesiumcontent as the difference between the two percentages by mass in accordance with the following equation:SIST EN 14016-2:2004



EN 14016-2:2004 (E)10Magnesium chloride MgCl2= 3,9173 × )(4MgSOtotalMgMg- in %If the total sulfate content is less than the sulfate content bonded as calcium sulfate, i.e.4172,1397,3224+´ 1)Constant mass is reached if two successive weighings 24 h apart, differ by less than 0,1 %.SIST EN 14016-2:2004



EN 14016-2:2004 (E)11Volumetric flask12345NaCl stock solution in ml05101520Then fill the volumetric flasks to the mark with water. For an initial mass of 100 g of MgCl2 solution or 50 g of solidMgCl2 and after taking 20 ml of the solution described in 3.2.2 and dilution as described in 3.2.7.5, the measuredvalues of volumetric flasks 1 to 5 correspond to the following percentages by mass of sodium chloride:Volumetric flask12345NaCl in %0,000,501,001,502,00If a photometer of sufficient consistency is used, it is only occasionally necessary to record the calibration curve inits entirety. However, in each analysis, check the measured values of volumetric flasks 1 to 5. Sufficient consis-tency is given if, after having reset the zero point with water, the same calibration curve is obtained using the samecalibration solutions.3.2.7.4 Determination of the calibration curves for potassium chlorideIntroduce 5 ml of the sodium chloride stock solution, 5 ml of the calcium sulfate stock solution and 1 g of magne-sium chloride into each of five 250 ml volumetric flasks. Then, from a calibrated burette, add the following quantitiesof the potassium chloride stock solutions to the individual flasks:Volumetric flask12345KCl stock solution in ml0,000,501,001,502,00Then fill the volumetric flasks to the mark with water. For an initial mass of 100 g of MgCl2 solution or 50,0000 g ofsolid MgCl2 and after taking 20 ml of the solution described in 3.2.2 and dilution as described in 3.2.7.6, the meas-ured values of volumetric flasks 1 to 5 correspond to the following percentages by mass of potassium chloride:Volumetric flask12345KCl in %0,000,501,001,502,00If a photometer of sufficient consistency is used, it is only occasionally necessary to record the calibration curve inits entirety. However, in each analysis, check the measured values of flasks 1 to 5. Sufficient consistency is givenif, after having reset the zero point with water, the same calibration curve is obtained using the same calibrationsolutions.3.2.7.5 Procedure and evaluation for sodium chlorideTo determine the sodium chloride content, if the material to be tested is aqueous magnesium chloride solution, usea solution obtained by making up 20 ml of the solution described in 3.2.2 to 1 000 ml. To determine the sodiumchloride content if the material to be tested is solid magnesium chloride, use a solution obtained by making up20 ml of the described solution to 500 ml. Measure each solution in the flame photometer. The reading gives thesodium chloride content on the basis of the calibration curve.3.2.7.6 Procedure and evaluation for potassium chlorideCarry out the flame photometric determination on the solution prepared as described above. The reading gives thepotassium chloride content on the basis of the calibration curve.SIST EN 14016-2:2004



EN 14016-2:2004 (E)123.2.8 Determination of the pH valueDetermine the pH value of the solution described in 3.2.2 containing the water-soluble constituents electrometri-cally or using indicators, e
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