BS EN 196-10-2016 Methods of testing cement Determination of the water-soluble chromium (VI) content of cement《测试水泥用方法 水泥的水溶解铬(VI)含量的测定》.pdf

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1、BS EN 196-10:2016Methods of testing cementPart 10: Determination of the water-solublechromium (VI) content of cementBSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN 196-10:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN

2、 196-10:2016. It supersedes BS EN 196-10:2006 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee B/516/12, Sampling and testing.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not pur

3、port to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 84581 9 ICS 91.100.10 Compliance with a British Standard cannot confer immunity from legal oblig

4、ations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS EN 196-10:2016EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 196-10 May 2016 ICS 91.100.10 S

5、upersedes EN 196-10:2006English Version Methods of testing cement - Part 10: Determination of the water-soluble chromium (VI) content of cement Mthodes dessais des ciments - Partie 10 : Dtermination de la teneur en chrome (VI) soluble dans leau des ciments Prfverfahren fr Zement - Teil 10: Bestimmun

6、g des Gehaltes an wasserlslichem Chrom (VI) in Zement This European Standard was approved by CEN on 20 December 2015. 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 a

7、ny alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other langu

8、age made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark

9、, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR

10、 STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 196-10:2016 EBS EN 196-10:2016EN 1

11、96-10:2016 (E) 2 Contents Page European foreword . 3 Introduction 4 1 Scope 5 2 Normative references 5 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 . 6 3.4 Blank determinations 6 4 Reagents .

12、 6 5 Apparatus . 7 6 Preparation of a test sample of cement. 8 7 Extraction procedure . 9 7.1 Principle . 9 7.2 Preparation of mortar . 9 7.3 Filtration . 10 8 Determination of chromium (VI) . 10 8.1 General . 10 8.2 Measurement of absorbance without oxidation . 10 8.3 Measurement of absorbance with

13、 oxidation 11 9 Calculation and expression of results . 12 9.1 Calculation 12 9.2 Expression of results . 13 10 Reporting of results . 13 11 Repeatability and reproducibility . 13 Annex A (normative) Evaluation of the compliance of cement with the regulatory limit in 47 to Annex XVII of Regulation (

14、EC) No. 1907/2006 on water-soluble hexavalent chromium content . 14 Annex B (informative) Guidance on the application of this European Standard to the determination of the water soluble chromium (VI) content of cement-containing preparations 24 Annex C (informative) Guidance on screening test method

15、 (1) using paste extraction - method based on DS 1020 . 26 Annex D (informative) Guidance on screening test method (2) using paste extraction method based on TRGS 613 29 Annex E (informative) Guidance on the photometric determination of chromium reduction capacity in cements . 33 Bibliography . 37 B

16、S EN 196-10:2016EN 196-10:2016 (E) 3 European foreword This document (EN 196-10:2016) has been prepared by Technical Committee CEN/TC 51 “Cement and building limes”, the secretariat of which is held by NBN. This European Standard shall be given the status of a national standard, either by publicatio

17、n of an identical text or by endorsement, at the latest by November 2016, and conflicting national standards shall be withdrawn at the latest by November 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held

18、responsible for identifying any or all such patent rights. This document supersedes EN 196-10:2006. In comparison to EN 196-10:2006, the following changes have been made: In Clause 2, the normative references have been updated; The standard has been editorially revised. EN 196 consists of the follow

19、ing parts, under the general title Methods of testing cement: Part 1: Determination of strength; Part 2: Chemical analysis of cement; Part 3: Determination of setting times and soundness; Part 4: Quantitative determination of constituents (CEN/TR 196-4); Part 5: Pozzolanicity test for pozzolanic cem

20、ent; Part 6: Determination of fineness; Part 7: Methods of taking and preparing samples of cement; Part 8: Heat of hydration - Solution method; Part 9: Heat of hydration - Semi-adiabatic method; Part 10: Determination of the water-soluble chromium (VI) content of cement. According to the CEN-CENELEC

21、 Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Icela

22、nd, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 196-10:2016EN 196-10:2016 (E) 4 Introduction This European Standard specifies the reference method for the de

23、termination of water-soluble chromium (VI) content of cement that consists of two stages, an extraction procedure and an analysis of the filtered extract. This European Standard test method has adopted the principle that extraction is carried out under conditions approximating as closely as possible

24、 to those during the commercial use of cement. Consequently extraction is by standard mortar and subsequent filtration. Other extraction procedures based on paste extraction have traditionally been used and are included in Annexes C and D for use as screening tests, in factory production control or

25、laboratories not having access to equipment specified in EN 196-1 for the production of mortar. The use of paste extraction is outside the normal conditions of use of cement. This European Standard test method has adopted the principle of analysis by spectrophotometry. The procedures set down genera

26、lly permit the analysis to be carried out without the need for an oxidation step. On rare occasions some cements may contain reducing species, not controlled by the routine method, that interfere with the analysis and require an oxidation step. Inter-laboratory testing has demonstrated that it is ne

27、cessary to include an initial assessment test in order to observe the effects on the analysis. By comparing the results obtained from the method with and without the oxidation step, it can be determined whether, for that cement, the reference method should include the oxidation step. Other instrumen

28、tal procedures may be used for the analysis of the filtered extract provided they are calibrated against the analysis of the filtered extract using the reference procedure. In case of dispute or failure to comply with a regulatory limit only the reference method shall be used. This European Standard

29、 test method has drawn heavily on the Danish Standard DS 1020 and the extraction procedure developed by the French cement industry association ATILH. Careful consideration has been given to the details of the German TRGS 613 method developed by Germanys Hazardous Materials Committee in support of In

30、dustrial Regulations for Hazardous Materials. Notice was also taken of the British Cement Association inherent colour method; the draft method produced by CEN/TC 193/WG1, reference N680, for cement-based adhesives; European Standard method EN 420 for protective gloves; and to the method, reference I

31、D-215, developed by the Occupational Safety and Health Administration, Salt Lake City, UT, USA. The USA Portland Cement Association, Research and Development report Serial No. 2554 “Review and evaluation of analytical methods for the determination of hexavalent chromium in hydraulic cements and clin

32、ker” by Waldemar A. Klemm was found to be most helpful in resolving technical issues. CEN/TR 14589 confirmed that chromium species and solubilities are sensitive to pH and redox conditions and care has been taken to address these in this European Standard by controlling sample exposure to air, by ad

33、ding the indicator to the alkaline filtered extract and by precisely specifying the pH for the analytical procedure. This European Standard test method was developed in order to provide a reference test method for use in the evaluation of compliance of cement with the requirements in entry 47 to Ann

34、ex XVII of Regulation (EC) 1907/20061of the European Parliament and of the Council of 18 December 2006 concerning the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH). A system for the evaluation of compliance of cement is set out in Annex A. 1Note that Regulation (EC) No

35、 1907/2006 is impacted by Commission Regulation (EU) No 126/2013 of 13 February 2013 amending Annex XVII to Regulation (EC) No 1907/2006 of the European Parliament and of the Council on the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH). BS EN 196-10:2016EN 196-10:2016

36、(E) 5 1 Scope This part of EN 196 specifies the method for the determination of the water-soluble chromium (VI) content of cement. A reference method is described consisting of two stages, an extraction procedure and an analysis of the filtered extract. Guidance on other extraction procedures, suita

37、ble for screening tests, for factory production control or other purposes, is given but in case of dispute or failure to comply with a regulatory limit only the reference method is used. The reference method has alternatives whereby the filtered extract may be subjected to an oxidation step or not.

38、The criteria by which the appropriate procedure is selected are set down. Other instrumental procedures may be used for the analysis of the filtered extract provided they are calibrated against the analysis of the filtered extract using the reference procedure. In the case of a dispute, only the ref

39、erence method is used. Annex A sets out a normative procedure to be followed in case this test method is used as the basis for evaluation of conformity of a cement with the regulatory limit in Regulation (EC) 1907/20062. This part of EN 196 describes a method that applies to cements. It may have wid

40、er applicability but this would need to be verified by testing on a product-by-product basis. Guidance in the possible application of this European Standard to the determination of the water-soluble chromium (VI) content of cement-containing preparations is given in Annex B. Annexes C and D provide

41、information on other test procedures based on paste extraction and thus depart from the performance of cement in its normal conditions of use. They may be carried out with or without the oxidation process. Users should be aware that results using these methods might be significantly different to tho

42、se obtained by the reference method. In the case of dispute or failure to comply with the regulatory limit only the reference method is used. Annex E provides guidance on a method for determination of the excess reducing agent content of cement as used in the factory internal control system of some

43、countries. Manufacturers using such an internal control method should ensure themselves of the relevance of results in comparison with testing by the reference method. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensab

44、le for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 196-1, Methods of testing cement - Part 1: Determination of strength EN 196-7, Methods of testing cement - Part 7

45、: Methods of taking and preparing samples of cement EN ISO/IEC 17020, Conformity assessment - Requirements for the operation of various types of bodies performing inspection (ISO/IEC 17020) EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 170

46、25) EN ISO/IEC 17065, Conformity assessment - Requirements for bodies certifying products, processes and services (ISO/IEC 17065) 2Note that Regulation (EC) No 1907/2006 is impacted by Commission Regulation (EU) No 126/2013 of 13 February 2013 amending Annex XVII to Regulation (EC) No 1907/2006 of t

47、he European Parliament and of the Council on the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH). BS EN 196-10:2016EN 196-10:2016 (E) 6 3 General requirements for testing 3.1 Number of tests Determination of water-soluble chromium (VI) content of cement, where the determ

48、ination is not part of a series subject to statistical control, shall be carried out in duplicate. Where the determination is one of a series subject to statistical control, a single test shall be the minimum required. In the case of a dispute, the number of tests shall be two (see also 3.3). 3.2 Re

49、peatability 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. Repeatability and reproducibility