SIST EN 196-2:2005
(Main)Methods of testing cement - Part 2: Chemical analysis of cement
Methods of testing cement - Part 2: Chemical analysis of cement
This document specifies the methods for the chemical analysis of cement.
This document describes the reference methods and, in certain cases, an alternative method which can be considered to be equivalent. In the case of a dispute, only the reference methods are used.
Any other methods may be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence.
This document describes methods which apply principally to cements, but which can also be applied to their constituent materials. They can also be applied to other materials, the standards for which call up these methods.
Standard specifications state which methods are used.
Prüfverfahren für Zement - Teil 2: Chemische Analyse von Zement
Dieses Dokument legt die Verfahren zur Durchführung der chemischen Analyse von Zement fest.
Dieses Dokument beschreibt die Referenzverfahren und in einigen Fällen Alternativverfahren, deren
Ergebnisse denen des Referenzverfahrens entsprechen. Im Streitfall sind die Referenzverfahren maßgebend.
Werden andere Verfahren angewendet, so sind diese gegen die Referenzverfahren oder gegen international
anerkannte Referenzmaterialien zu kalibrieren, um ihre Eignung nachzuweisen.
Dieses Dokument legt Verfahren fest, die in erster Linie für Zemente gelten. Die Verfahren können jedoch
auch auf deren Bestandteile angewendet werden. Die Verfahren gelten auch für andere Stoffe, sofern in den
entsprechenden Normen darauf verwiesen wird.
In den Anwendungsnormen ist festgelegt, welche Verfahren anzuwenden sind.
Méthodes d'essais des ciments - Partie 2: Analyse chimique des ciments
Le présent document décrit les méthodes d'analyse chimique des ciments.
Le présent document décrit les méthodes de référence et, dans certains cas, une variante qui peut etre considérée comme une méthode équivalente. En cas de litige, seules les méthodes de référence doivent etre utilisées.
D'autres méthodes encore peuvent etre utilisées, a condition qu’elles soient étalonnées, soit par rapport a des méthodes de référence, soit par rapport a des matériaux de référence acceptés internationalement, pour démontrer leur équivalence.
Le présent document décrit les méthodes qui s’appliquent principalement aux ciments, mais qui peuvent etre aussi appliquées a leurs matériaux constitutifs. Elles peuvent etre également appliquées a d’autres matériaux, pour lesquels les normes prescrivent ces méthodes.
Les spécifications normalisées indiquent les méthodes qui doivent etre utilisées.
Metode preskušanja cementa - 2. del: Kemijska analiza cementa
General Information
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Standards Content (Sample)
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
SIST EN 196-2:2005
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
EN 196-2:2005 (E) 2 Contents Page Foreword.4 1 Scope.6 2 Normative references.6 3 General requirements for testing.6 3.1 Number of tests.6 3.2 Repeatability and reproducibility.6 3.3 Expression of masses, volumes, factors and results.7 3.4 Ignitions.7 3.5 Determination of constant mass.7 3.6 Check for absence of chloride ions (silver nitrate test).7 3.7 Blank determinations.7 4 Reagents.8 5 Apparatus.19 6 Preparation of a test sample of cement.24 7 Determination of loss on ignition.24 7.1 Principle.24 7.2 Procedure.24 7.3 Calculation and expression of results.24 7.4 Correction for oxidation of sulfides.25 7.5 Repeatability and reproducibility.25 8 Determination of sulfate.25 8.1 Principle.25 8.2 Procedure.25 8.3 Calculation and expression of results.26 8.4 Repeatability and reproducibility.26 9 Determination of residue insoluble in hydrochloric acid and sodium carbonate.26 9.1 Principle.26 9.2 Procedure.26 9.3 Calculation and expression of results.27 9.4 Repeatability and reproducibility.27 10 Determination of residue insoluble in hydrochloric acid and potassium hydroxide.27 10.1 Principle.27 10.2 Procedure.27 10.3 Calculation and expression of results.28 10.4 Repeatability and reproducibility.28 11 Determination of sulfide.28 11.1 Principle.28 11.2 Procedure.28 11.3 Calculation and expression of results.28 11.4 Repeatability and reproducibility.29 12 Determination of manganese.29 12.1 Principle.29 12.2 Procedure.29 12.3 Calculation of results.29 12.4 Repeatability and reproducibility.30 12.5 Expression of results.30 13 Determination of major elements.30 SIST EN 196-2:2005
EN 196-2:2005 (E) 3 13.1 Principle.30 13.2 Decomposition with sodium peroxide.30 13.3 Precipitation and determination of silica — Double evaporation method (reference method).33 13.4 Precipitation and determination of silica — Polyethylene oxide method (alternative method).33 13.5 Decomposition with hydrochloric acid and ammonium chloride and precipitation of silica (alternative method).34 13.6 Determination of pure silica.35 13.7 Decomposition of the evaporation residue.35 13.8 Determination of soluble silica.36 13.9 Determination of total silica.36 13.10 Determination of iron (III) oxide.37 13.11 Determination of aluminium oxide.38 13.12 Determination of calcium oxide by EGTA (reference method).38 13.13 Determination of magnesium oxide by DCTA (reference method).39 13.14 Determination of calcium oxide by EDTA (alternative method).40 13.15 Determination of magnesium oxide by EDTA (alternative method).41 14 Determination of chloride.42 14.1 Principle.42 14.2 Procedure.42 14.3 Calculation and expression of results.43 14.4 Repeatability and reproducibility.43 15 Determination of carbon dioxide (reference method).43 15.1 Principle.43 15.2 Apparatus.43 15.3 Procedure.43 15.4 Calculation and expression of results.44 15.5 Repeatability and reproducibility.44 16 Determination of carbon dioxide (alternative method).44 16.1 Principle.44 16.2 Apparatus.44 16.3 Procedure.45 16.4 Calculation and expression of results.45 16.5 Repeatability and reproducibility.45 17 Determination of alkali (reference method).46 17.1 Principle.46 17.2 Reagents.46 17.3 Preparation of calibration solutions and calibration curves.46 17.4 Dissolution of the test portion.46 17.5 Procedure.47 17.6 Calculation and expression of results.48 17.7 Repeatability and reproducibility.48 18 Determination of alkali (alternative method).48 18.1 Principle.48 18.2 Reagents.49 18.3 Construction of the calibration curves.49 18.4 Procedure.49 18.5 Calculation and expression of results.50 18.6 Repeatability and reproducibility.50
SIST EN 196-2:2005
EN 196-2:2005 (E) 4 Foreword This document (EN 196-2:2005) has been prepared by Technical Committee CEN/TC 51 ‘Cement and building limes’, the secretariat of which is held by IBN/BIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by August 2005, and conflicting national standards shall be withdrawn at the latest by August 2005. This document supersedes EN 196-2:1994 and EN 196-21:1989. This European Standard on the methods of testing cement comprises the following Parts: EN 196-1, Methods of testing cement — Part 1: Determination of strength EN 196-2, Methods of testing cement — Part 2: Chemical analysis of cement EN 196-3, Methods of testing cement — Part 3: Determination of setting time and soundness EN 196-5, Methods of testing cement — Part 5: Pozzolanicity test for pozzolanic cements EN 196-6, Methods of testing cement — Part 6: Determination of fineness EN 196-7, Methods of testing cement — Part 7: Methods of taking and preparing samples of cement EN 196-8, Methods of testing cement — Part 8: Heat of hydration — Solution method EN 196-9, Methods of testing cement — Part 9: Heat of hydration — Semi-adiabatic method NOTE A previous part, EN 196-21: Methods of testing cement — Part 21: Determination of the chloride, carbon dioxide and alkali content of cement, has been revised and incorporated into EN 196-2. Another document, ENV 196-4 Methods of testing cement — Part 4: Quantitative determination of constituents, has been drafted and will be published as a CEN Technical Report. This edition introduces the following technical changes based on comments received by the secretariat: a) EN 196-21 has been consolidated into EN 196-2; b) calibration against internationally accepted reference materials is permitted; c) the number of tests to be carried out, when the analysis is part of a series subject to statistical control, has been reduced to one; d) a requirement for blank determinations has been included; e) limiting ranges have been set for masses, volumes and temperatures wherever these are significant; f) the required accuracy of the balance is consistent with that of equipment traditionally used; g) a specification for a laboratory oven has been included; h) the calibration procedure for standard silica solution has been simplified; i) additional indicators have been included for the visual determination of EDTA titrations; SIST EN 196-2:2005
EN 196-2:2005 (E) 5 j) an ignition temperature of (950 ± 25 ) °C has been set for the determination of loss on ignition and the ignition of barium sulfate and insoluble residues; k) determination of sulfate before and after ignition in the determination of loss on ignition becomes the reference method when correcting for sulfide; l) determination of silica by the double evaporation method becomes the reference method; m) in the determination of carbon dioxide by decomposition with sulfuric acid an additional, empty, gas washing bottle is included as a safety precaution against the reverse flow of sulfuric acid should pressure be lost; n) in the determination of alkali the influence of phosphoric acid on the potassium emission from the calibration solutions is suppressed by the addition of calcium to the calibration solutions. The procedure is adjusted accordingly. Analytical methods utilising x-ray fluorescence (XRF) were considered during this revision but no published, standardised method was considered sufficiently comprehensive to be included. A new work item has been established by CEN/TC51 in order to prepare a method based on XRF. XRF and other instrumental methods such as differential thermal analysis for determination of carbon dioxide, atomic absorption spectroscopy, etc. may be used as alternative methods provided they are calibrated against the reference methods, or against internationally accepted reference materials. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: 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. SIST EN 196-2:2005
EN 196-2:2005 (E) 6 1 Scope This document specifies the methods for the chemical analysis of cement. This document describes the reference methods and, in certain cases, an alternative method which can be considered to be equivalent. In the case of a dispute, only the reference methods are used. Any other methods may be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence. This document describes methods which apply principally to cements, but which can also be applied to their constituent materials. They can also be applied to other materials, the standards for which call up these methods. Standard specifications state which methods are
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
EN 196-2:2005 (E) 7 Repeatability and reproducibility in this document are expressed as repeatability standard deviation(s) and reproducibility standard deviation(s) in e.g. absolute percent, grams, etc., according to the property tested. 3.3 Expression of masses, volumes, factors and results Express masses in grams to the nearest 0,000 1 g and volumes from burettes in millilitres to the nearest 0,05 ml. Express the factors of solutions, given by the mean of three measurements, to three decimal places. Express the results, where a single test result has been obtained, as a percentage generally to two decimal places. Express the results, where two test results have been obtained, as the mean of the results, as a percentage generally to two decimal places. If the two test results differ by more than twice the standard deviation of repeatability, repeat the test and take the mean of the two closest test results. The results of all individual tests shall be recorded. 3.4 Ignitions Carry out ignitions as follows. Place the filter paper and its contents into a crucible which has been previously ignited and tared. Dry it, then incinerate slowly in an oxidising atmosphere in order to avoid immediate flaming, while ensuring complete combustion. Ignite the crucible and its contents at the stated temperature then allow to cool to the laboratory temperature in a desiccator. Weigh the crucible and its contents. 3.5 Determination of constant mass Determine constant mass by making successive 15 min ignitions followed each time by cooling and then weighing. Constant mass is reached when the difference between two successive weighings is less than 0,000 5 g. 3.6 Check for absence of chloride ions (silver nitrate test) After generally five to six washes of a precipitate, rinse the base of the filter stem with a few drops of water. Wash the filter paper and its contents with several millilitres of water and collect this in a test tube. Add several drops of silver nitrate solution (4.43). Check the absence of turbidity or precipitate in the solution. If present, continue washing while carrying out periodic checks until the silver nitrate test is negative. 3.7 Blank determinations Carry out a blank determination without a sample, where relevant, following the same procedure and using the same amounts of reagents. Correct the results obtained for the analytical determination accordingly. SIST EN 196-2:2005
EN 196-2:2005 (E) 8 4 Reagents Use only reagents of analytical quality. References to water mean distilled or de-ionised water having an electrical conductivity ≤ 0,5 mS/m. Unless otherwise stated percent means percent by mass. Unless otherwise stated the concentrated liquid reagents used in this document have the following densities () (in g/cm3 at 20 °C): hydrochloric acid 1,18 to 1,19 acetic acid 1,05 to 1,06 nitric acid 1,40 to 1,42 phosphoric acid 1,71 to 1,75 perchloric acid 1,60 to 1,67 ammonium hydroxide 0,88 to 0,91 The degree of dilution is always given as a volumetric sum, for example: dilute hydrochloric acid 1 + 2 means that 1 volume of concentrated hydrochloric acid is to be mixed with 2 volumes of water. 4.1 Concentrated hydrochloric acid (HCl) 4.2 Dilute hydrochloric acid 1 + 1 4.3 Dilute hydrochloric acid 1 + 2 4.4 Dilute hydrochloric acid 1 + 3 4.5 Dilute hydrochloric acid 1 + 9 4.6 Dilute hydrochloric acid 1 + 11 4.7 Dilute hydrochloric acid 1 + 19 4.8 Dilute hydrochloric acid 1 + 99 4.9 Dilute hydrochloric acid of pH (1,60 ± 0,05). Prepare by adjusting the pH of two litres of water to (1,60 ± 0,05) by adding five or six drops of concentrated hydrochloric acid. Control using the pH meter (5.18.1). Store the solution in a polyethylene container. 4.10 Concentrated hydrofluoric acid (> 40 %) (HF) 4.11 Dilute hydrofluoric acid 1 + 3 4.12 Concentrated nitric acid (HNO3) 4.13 Dilute nitric acid 1 + 2 4.14 Dilute nitric acid 1 + 100 4.15 Concentrated sulfuric acid (>98 %) (H2SO4) 4.16 Dilute sulfuric acid 1 + 1 4.17 Dilute sulfuric acid 1 + 4 4.18 Concentrated perchloric acid (HClO4) SIST EN 196-2:2005
EN 196-2:2005 (E) 9 4.19 Concentrated phosphoric acid (H3PO4) 4.20 Dilute phosphoric acid 1 + 19; store this solution in a polyethylene container. 4.21 Boric acid (H3BO3) 4.22 Concentrated acetic acid (CH3COOH) 4.23 Amino-acetic acid (NH2CH2COOH) 4.24 Metallic chromium (Cr), in powder form 4.25 Concentrated ammonium hydroxide (NH4OH) 4.26 Dilute ammonium hydroxide 1 + 1 4.27 Dilute ammonium hydroxide 1 + 10 4.28 Dilute ammonium hydroxide 1 + 16 4.29 Sodium hydroxide (NaOH) 4.30 Sodium hydroxide solution 4 mol/l. Dissolve 160 g of sodium hydroxide (4.29) in water and make up to 1 000 ml. Store in a polyethylene container. 4.31 Sodium hydroxide solution 2 mol/l. Dissolve 80 g of sodium hydroxide (4.29) in water and make up to 1 000 ml. Store in a polyethylene container. 4.32 Ammonium chloride (NH4Cl) 4.33 Tin (II) chloride (SnCl2.2H2O) 4.34 Potassium iodate (KIO3), dried to constant mass at (120 ± 5) °C. 4.35 Potassium periodate (KIO4) 4.36 Sodium peroxide (Na2O2), in powder form. 4.37 Sodium chloride (NaCl), dried to constant mass at (110 ± 5) °C. 4.38 Potassium chloride (KCl), dried to constant mass at (110 ± 5) °C. 4.39 Sodium carbonate (Na2CO3), dried to constant mass at (250 ± 10) °C. 4.40 Mixture of sodium carbonate and sodium chloride. Mix 7 g of sodium carbonate (4.39) with 1 g sodium chloride (NaCl) (4.37). 4.41 Barium chloride solution. Dissolve 120 g of barium chloride (BaCl2.2H2O) in water and make up to
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
EN 196-2:2005 (E) 10 4.45 Sodium carbonate solution. Dissolve 50 g of anhydrous sodium carbonate (4.39) in water and make up to 1 000 ml. 4.46 Potassium hydroxide solution. Dissolve 250 g of potassium hydroxide (KOH) in water and make up to 1 000 ml. Store in a polyethylene container. 4.47 Ammoniacal zinc sulfate solution. Dissolve 50 g of zinc sulfate (ZnSO4.7H2O) in 150 ml water and add 350 ml of concentrated ammonium hydroxide (4.25). Leave to stand for at least 24 h and filter. 4.48 Lead acetate solution. Dissolve
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