1、January 2010DEUTSCHE NORM English price group 7No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 91.100.30!$Nu“1564382ww
2、w.din.deDDIN EN 480-10Admixtures for concrete, mortar and grout Test methods Part 10: Determination of water soluble chloride contentEnglish version of DIN EN 480-10:2010-01Zusatzmittel fr Beton, Mrtel und Einpressmrtel Prfverfahren Teil 10: Bestimmung des wasserlslichen ChloridgehaltesEnglische Fas
3、sung DIN EN 480-10:2010-01SupersedesDIN EN 480-10:1997-02www.beuth.deDocument comprises pages10DIN EN 480-10:2010-01 National foreword This standard has been prepared by Technical Committee CEN/TC 104 “Concrete and related products” (Secretariat: DIN, Germany). The responsible German body involved i
4、n its preparation was the Normenausschuss Bauwesen (Building and Civil Engineering Standards Committee), Working Committee NA 005-07-23 AA Betonzusatzmittel. Amendments This standard differs from DIN EN 480-10:1997-02 as follows: a) The standard has been editorially revised. b) The reagents used hav
5、e been described in more detail. c) The procedures applied for Method 1 to Method 3 have been given in detail. Previous editions DIN EN 480-10: 1997-02 2 EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 480-10July 2009ICS 91.100.30 Supersedes EN 480-10:1996 English VersionAdmixtures for concrete, m
6、ortar and grout - Test methods - Part10: Determination of water soluble chloride contentAdjuvants pour bton, mortier et coulis - Mthodes dessai -Partie 10: Dtermination de la teneur en chlorure solubledans leauZusatzmittel fr Beton, Mrtel und Einpressmrtel -Prfverfahren - Teil 10: Bestimmung des was
7、serlslichenChloridgehaltesThis European Standard was approved by CEN on 23 June 2009.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 an
8、d bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre 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 responsibil
9、ity of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ir
10、eland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17,
11、B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 480-10:2009: EEN 480-10:2009 (E) 2 Contents Page Foreword 31 Scope 52 Principle 53 Apparatus .53.1 pH meter .53.2 Electrodes .53.3 Additional apparatus .63.4 Reagen
12、ts .64 Procedure .64.1 Preparation of sample .64.2 Determination .65 Results 76 Test report 8DIN EN 480-10:2010-01 EN 480-10:2009 (E) 3 Foreword This document (EN 480-10:2009) has been prepared by Technical Committee CEN/TC 104 “Concrete and related products”, the secretariat of which is held by DIN
13、. 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 January 2010, and conflicting national standards shall be withdrawn at the latest by January 2010. Attention is drawn to the possibility that some
14、 of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 480-10:1996. It has been drafted by Subcommittee 3 (SC 3) of TC 104 “Admixtures for concrete, mortar and
15、grout“. This draft European Standard is part of the series EN 480 “Admixtures for concrete, mortar and grout Test methods“ which comprises the following: Part 1 Reference concrete and reference mortar for testing Part 2 Determination of setting time Part 4 Determination of bleeding of concrete Part
16、5 Determination of capillary absorption Part 6 Infrared analysis Part 8 Determination of the conventional dry material content Part 10 Determination of water soluble chloride content Part 11 Determination of air void characteristics in hardened concrete Part 12 Determination of the alkali content of
17、 admixtures Part 13 Reference masonry mortar for testing mortar admixtures Part 14 Determination of the effect on corrosion susceptibility of reinforcing steel by potentiostatic electro-chemical test. This standard is applicable together with the other standards of the EN 480 series for testing admi
18、xtures in accordance with the EN 934 series of standards. The following amendments have been made to the 1996-09 edition of this standard: editorial revision; detailing of used reagents; detailing of the procedure applied for Method 1 to Method 3. DIN EN 480-10:2010-01 EN 480-10:2009 (E) 4 According
19、 to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, L
20、ithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 480-10:2010-01 EN 480-10:2009 (E) 5 1 Scope This draft European Standard specifies methods for determining water soluble halogens (except fluorid
21、es) in admixtures. The total water soluble halogen content is expressed as the chloride content. 2 Principle The object of the test is to determine the content of chloride ions (including other halogen ions except fluorides) in an admixture by precipitation of the chloride ions with a silver nitrate
22、 solution, according to the reaction: AgClAgCl +(solid) The end point of this reaction is determined with the aid of a pH meter. The volume of the sample required for this test has been calculated for an admixture of which the chloride content is lower than 0,1 % by mass. If the chloride content is
23、known, or can be assumed to be higher, the admixture has to be diluted in a precise ratio before carrying out the test. 3 Apparatus 3.1 pH meter Either: a) a pH millivoltmeter in which case the graph is plotted point by point, or b) a recording pH millivoltmeter connected to an automatic burette. 3.
24、2 Electrodes Either: a) a combination of two electrodes consisting of: 1) an indicator: silver; 2) a reference: mercuric sulphate (electrolyte KNO3) or calomel with agar gel (electrolyte KNO3); or b) a combined electrode (indicator and reference) Ag - AgCl (electrolyte KNO3). NOTE Other electrodes s
25、uch as ion selective electrodes may be used provided the results will be unaffected. DIN EN 480-10:2010-01 EN 480-10:2009 (E) 6 3.3 Additional apparatus 3.3.1 Balance with an accuracy of 0,1 mg reading up to 200 g 3.3.2 20 ml burette graduated with accuracy of 0,05 ml 3.3.3 250 ml and 500 ml beakers
26、 3.3.4 1 000 ml measuring flask 3.3.5 Heating device with a magnetic stirrer 3.3.6 10 ml, 20 ml and 50 ml graduated flasks 3.4 Reagents All reagents shall be of analytical grade. 3.4.1 Concentrated nitric acid (HNO3) 3.4.2 Hydrogen peroxide (H2O2), 30 % by mass (110 volumes) 3.4.3 Sodium hydroxide s
27、olution (naOH), 33 % by mass 3.4.4 Distilled or demineralized water 3.4.5 Ethanol (C2H5OH) 3.4.6 Acetone (C3H7O) 3.4.7 Silver nitrate solution (AgNO3), pre-prepared 0,01 mol/l, normality N determined to 0,0001 4 Procedure 4.1 Preparation of sample 4.1.1 Liquid admixture From a liquid admixture a sam
28、ple of (10 1) g is weighed to 0,01 g and placed into a 250 ml or a 500 ml beaker. 4.1.2 Powder admixture From a powder admixture a sample (5 1) g is weighed to 0,01 g. The sample is placed into a 250 ml or a 500 ml beaker. 4.2 Determination 4.2.1 General Depending upon the composition of the admixtu
29、re one of the following methods shall be used. DIN EN 480-10:2010-01 EN 480-10:2009 (E) 7 4.2.2 Method 1 If the admixture does not contain constituents that will interfere with the test, such as lignosulphonates, thiocyanates or reducing agents, dilute the sample or dissolve it and make the solution
30、 up to 100 ml with distilled or demineralized water. Then add 80 ml of acetone followed by dilute nitric acid until the pH is (2,0 + 0,5) and carry out the titration of the chloride ions with the silver nitrate solution, recording the volume (V) used to 0,05 ml. Carry out a blank titration under the
31、 same conditions and record the volume (Vo) to 0,05 ml. 4.2.3 Method 2 If the admixture does contain, or can be assumed to contain lignosulphonate or reducing agents, the sample shall be diluted or dissolved and made up to 100 ml with distilled or demineralized water. Then add 5 ml of sodium hydroxi
32、de solution followed by 10 ml of hydrogen peroxide. This can cause an exothermic reaction. In order to avoid loss of chloride ions, make sure that the pH remains above 8,5 by adding, if necessary, more sodium hydroxide solution. Bring the solution very slowly to the boiling point by means of a heati
33、ng device with a magnetic stirrer and boil for 30 minutes1). Leave the solution to cool to (20 + 2) oC. Then add 80 ml of acetone followed by dilute nitric acid until the pH is (2,0 + 0,5) and carry out the titration of the chloride ions using the silver nitrate solution, recording the volume used (
34、V) to 0,05 ml. Carry out a blank titration under the same conditions and record the volume (Vo) to 0,05 ml. 4.2.4 Method 3 NOTE Carry out this test in an extraction cabinet to minimise the risk from the exothermic reaction and the escape of hydrogen cyanide. The operator should wear suitable protect
35、ive clothing. If the admixture does contain, or can be assumed to contain thiocyanate, dissolve the sample if necessary and dilute to 100ml using distilled or demineralised water then place the sample in a 500 ml beaker in order to avoid losses by overflow. Carefully add 5 ml of sodium hydroxide sol
36、ution followed by 10 ml of hydrogen peroxide. This can cause an extremely exothermic reaction. After this reaction has subsided, add again 10 ml of hydrogen peroxide and repeat the addition three times. In order to avoid loss of chloride ions and minimise the escape of hydrogen cyanide, make sure th
37、at the pH remains above 8,5 at all times by adding, if necessary, more sodium hydroxide solution. Heat the solution slowly to the boiling point and keep it boiling for 2 h. Leave the solution to cool slowly to (20 + 2) o C. Then transfer the solution into a 250 ml beaker using distilled or demineral
38、ized water to wash out the 500 ml beaker. Add 80 ml of acetone followed by dilute nitric acid until the pH is (2,0 + 0,5) and carry out the titration of the chloride ions using the silver nitrate solution, recording the volume used (V) to 0,05 ml. Carry out a blank titration under the same condition
39、s and record the volume (Vo) to 0,05 ml 5 Results The results shall be expressed in % by mass. 1) Some admixtures may foam while boiling. This may be reduced by the addition of ethanol. DIN EN 480-10:2010-01 EN 480-10:2009 (E) 8 Chloride content wcl=()%55,3mnVVoby mass where V is the volume of silve
40、r nitrate solution used in the test in millilitres; Vois the volume of silver nitrate solution used in the blank titration in millilitres; N is the normality of silver nitrate solution in mol per litre; m is the mass of the sample in grams. 6 Test report The test report shall include at least the fo
41、llowing information: a) Name or code of admixture tested (with information relating to its marking); b) Date of test; c) Name of the laboratory; d) Name of operator; e) Number of test standard (EN 480-10) f) Details of the equipment used; g) Method of test used (i.e. method 1, 2 or 3).; if method 2
42、or 3 has been used, the volume of hydrogen peroxide, the boiling time and any other necessary comments shall be included; h) Origin of the sample and date when taken; i) Chloride ion content that shall be reported to the nearest 0,01 %. NOTE All three methods give the total halogen ion content (except fluoride) as chloride. In the case of method 2, any thiocyanate will also be included as chloride. DIN EN 480-10:2010-01
