EN 1877-1-2000 en Products and Systems for the Protection and Repair of Concrete Structures - Test Methods - Reactive Functions Related to Epoxy Resins - Part 1 Determination of Ep.pdf

1、STDmBSI BS EN 1877-1-ENGL 2000 Lb24bb9 0874067 O19 W BRITISH STANDARD BS EN 1877-1 2000 Products and systems for the protection and repair of concrete structures - Test methods - Reactive functions related to epoxy resins - Part 1: Determination of epoxy equivalent The European standard EN 1877-1:20

2、00 has the status of a British standard ICs 91.080.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMIITED BY COPYRIGE“ LAW STD.BS1 BS EN 1877-1-ENGL 2000 1b24bb9 08740b8 TSS BS EN 1877-1:2000 AmdNo. Date National foreword Comments This British standard is the official English language version of E

3、N 1877-12000. The UK participation in its preparation was entrusted by Technical Committee M17, Concrete, to Subcommittee B/517/8, protection and repair of concrete, which has the responsibility to: - aid enquirers to undexstand the te them in the UK A list of organizations represented on this subco

4、mmittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by

5、 using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contsact. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immu

6、nity from legal obligations. Summary of pages This document comprises a hnt cover, an inside hnt cover, the EN title page, pages 2 to 8, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued This British Standard, havin

7、g been prepared under the direction of the Sector Committee for Building and Civil Engineering, was published under the authority of the Standards Committee and comes into effect on 15 October Zoo0 O BSI 122000 ISBN O 580 36599 9 Amendments issued since publication STD*BSI BS EN L877-L-ENGL 2000 Lb2

8、4bb9 0874Ob9 991 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1877-1 July 2000 ICs 91.080.40 English version Products and systems for the protection and repair of concrete structures - Test methods - Reactive functions related to epoxy resins - Part 1: Determination of epoxy equivalent Produ

9、its et systmes pour la protection et la rparation des structures en bton - Mthodes dessai - Fonctions ractives des rsines poxydes - Pattie 1: Dtermination de lquivalent poxyde Produkte und Systeme for den Schutz und die Instandsetzung von Betontragwerken - Prfverfahren - Reaktive, funkdonelle Gruppe

10、n von Epoxidharzen - Teil 1 : Bestimmung des Epoxid-Aquivalents This European Standard was approved by CEN on 7 July 2000. CEN members are bound to comply with the CEWCENELEC Internai Regulations which stipulate the conditions for giving this European Standard the status of a national standard witho

11、ut 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 ma

12、de 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, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland

13、, Ireland, Italy, Luxembourg, Netherlands, Noway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMEE FOR STANDARDIZATION COMITE EUROPEEN DE NORMALISATION EUROPISCHES KOMITEE FUR NORMUNG Central Secretariat: rue de Stassart, 36 8-1050 Brussels Q 2000 CEN All rights of exploitati

14、on in any form and by any means resewed worldwide for CEN national Members. Ref. No. EN 187-1:2000 E STD-BSI BS EN 5877-L-ENGL 2000 M lb24bb9 0874070 603 M Page 2 EN 1877- 1 :2000 Contents Page Foreword . 3 1 Scope 4 2 Normative references 4 3 Terms and definitions . 4 4 Principle 4 5 Sampling . 4 6

15、 Apparatus . 5 7 Reagents . 5 a Preparation of the perchloric acid (O. 1 mou) in acetic acid 5 9 Standardization 6 10 Calculation of the concentration 6 11 12 Procedure . 6 13 Calculation . 7 14 Precision . 7 15 Test report 7 Bibliography . 8 Preparation of the Tetraethylammonium bromide reagent sol

16、ution 6 STD-BSI BS EN 1877-l-ENGL 2000 1b24bb9 0874071 54“ Page 3 EN 1877-1 :2000 Foreword This European Standard has been prepared by Technical Committee CEN/TC 104 “Concrete (performance, production, placing and compliance criteria)“, the secretariat of which is held by DIN. This European Standard

17、 shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2002, and conflicting national standards shall be withdrawn at the latest by December 2002. According to the CENICENELEC Internal Regulations, the national stand

18、ards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Noway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. This Europea

19、n Standard describes several type of test methods. Specifications for the products and systems for the protection and repair of concrete structures will be subject of separate standards. This European Standard is based on the IS0 3001 : 1997 standard. - STD-BSI BS EN L77-1-ENGL 5000 3bi?4bb9 0874072

20、 486 Page 4 EN 1877-1 2000 1 Scope This European Standard specifies a method for the determination of the epoxy equivalent and is applicable to all epoxy compounds, for products and systems for the protection and repair of concrete structure. This European standard does not apply to the measurement

21、of epoxide equivalent of nitrogen-containing resins. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For

22、 dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). EN 21512 Paints and va

23、rnishes - Sampling ofproducts in liquid orpaste form (IS0 1512 : 1991) 3 Terms and definitions For the purposes of this standard the following terms and definitions apply: 3.1 epoxide equivalent The mass of resin, in grams, which contains one mole of epoxide group. 3.2 expoxide number Molar mass of

24、epoxy - group x 1 O0 epoxide equivalent Content of epoxy groups in (?YO) in 1 O0 g epoxy resin 3.3 epoxide index 1 O00 epoxide equivalent Moles of epoxide per kilogram epoxy resin. 4 Principle Reaction of the epoxide groups with nascent hydrogen bromide produced by the action of 0,l moVI standard vo

25、lumetric perchloric acid solution on tetraethylammonium bromide. Determination of the endpoint either using crystal violet as indicator or by a potentiometric method. 5 Sampling A representative and homogeneous sample of the material to be tested shall be taken according to EN 21512. Eliminate miner

26、al filler and pigments with a suitable organic solvent before the determination of the epoxide equivalent. It should be checked, that any solvent has evaporated. STD-BSI BS EN 1877-1-ENGL 2000 W 1b24bb9 0874073 312 W Page 5 EN 1877-1 :2000 6 Apparatus - - - Pipette, capacity 10 ml - - In addition, w

27、hen prepared the Oll moIA perchloric acid in acetic acid. - - - - Balance, accurate to within 0,l mg. Calibrated burette, capacity 50 ml. Conical flask, 100 ml or 200 ml, with ground glass neck and ground glass stopper. Instrument and electrodes for potentiometric titration. Magnetic stirrer with po

28、lytetrafluoroethylene-coated bar. Calibrated thermometer to permit temperature measurements within an accuracy of * Oll K. Volumetric flask, 1 O00 mi. Graduated cylinders, 50 ml and 500 ml. 7 Reagents For the analysis, only reagents of analytical grade shall be used. - - Tetraethylammonium bromide.

29、- Tetrabuthylarnmonium iodide. - Acetic acid 99 % to 100 %. - Chloroform, methylenchloride, acetone. - Crystal violet, 0,l YO in solution in acetic acid. - Potassium hydrogen phthalate. Perchloric acid, 0,l mol in acetic acid (Standard volumetric solution). In addition, when prepared the Oll molA pe

30、rchloric acid in acetic acid. - Acetic acid 99 % to 100 %. - Acetic anhydride, purity 96 %. - Phenolphthalein, Oll % solution. - Perchloric acid, 70 YO. - - Distilled water. Sodium hydroxide solution Oll moIA. 8 Preparation of the perchloric acid (0,i molIl) in acetic acid WARNING The use of safety

31、goggles and a safety screen is recommended. Determination of the true percentage of the approximately 70 % (m/m) perchloric acid. Weigh approximately 0,3 g of the perchloric acid (El) in a 200 mi conical flask, add 50 ml distilled water and mix thoroughly. Titrate it against Oll mol/l sodium hydroxi

32、de solution (Vi) using the phenolphthalein indicator solution. The content of perchloric acid is given by the equation : where P Ei Vi FnaOH = is the factor of the 0,l molli sodium hydroxide solution. = content of the perchloric acid ; = is the mass in (g), of the approximate 70 YO perchloric acid ;

33、 = is the volume, in (mi), of the Oll mol/ sodium hydroxide solution ; Weigh the calculated mass of the 70 Yo aqueous solution of the perchloric acid to an accuracy of 0,l mg into a 1 O00 ml volumetric flask. Add 300 mi of the acetic acid followed by 50 ml of the acetic anhydride under cooling. The

34、temperature of the solution shall be kept at 20 OC. Dilute to 1000 ml with the acetic acid and mix thoroughly. The solution should not show any discoloration to yellow for a period of 12 h. Then carry out the standardization. STD.BS1 BS EN L77-L-ENGL 2000 - Lb24bb 0874074 259 Page 6 EN 1877-1:2000 9

35、 Standardization a) Standardize this solution by titrating it in a 200 ml conical flask to 300 mg to 500 mg potassium hydrogen phthalate dissolved in 15 ml acetic acid, using the crystal violet indicator solution. If necessary, dry the potassium hydrogen phthalate for 24 hours at 120 OC before use.

36、Carry out the end-point determination using 4 to 6 drops of the crystal violet indicator solution, titrating until a stable green colour is obtained. Record the temperature Q of the standard volumetric solution. Carry out a double determination. NOTE: method for the standardization of the perchloric

37、 acid. If the potentiometric method is used for the determination of epoxide equivalent, it is recommended to use the same b) Alternative: Use the manufacturers concentration of the solution. 10 Calculation of the concentration The concentration c of the perchloric acid solution in moles per litre i

38、s given by the equation : E2 c= V2 + 0,2042 where E2 : is the mass, in (g), of potassium hydrogen phthalate used ; V2 : is the volume, in (mi), of the perchloric acid solution used in the titration. 11 Preparation of the Tetraethylammonium bromide reagent solution Dissolve 100 g of tetraethylammoniu

39、m bromide in 400 ml of the acetic acid. Add a few drops of the crystal violet indicator solution ; if it changes colour, bring it back to the original colour with the standard volumetric perchloric acid solution. NOTE For some epoxide compounds of low reactivity, the use of tetrabutylammonium iodide

40、 is advised, either as the solid or as a 10 % solution in chloroform ; in this case, light should be excluded as much as possible. Solutions of tetrabutyl- ammonium iodide in chloroform are unstable and should be freshly prepared for each titration. 12 Procedure - Weigh into the flask, to the neares

41、t 0,l mg, a test portion containing from 0,6 mmol to 0,9 mmol of epoxy groups (this corresponds to a mass of between 0,6 x EE mg and 0,9 x EE mg, where EE is the estimated epoxy equivalent). - Add 10 ml of solvent, then dissolve the test portion using the magnetic stirrer and, if necessary, by heati

42、ng slightly. - Cool to room temperature, add 20 ml of acetic acid and then, with the pipette, 10 ml of tetraethylammonium bromide solution. - If using the indicator method, add 4 to 6 drops of crystal violet solution and titrate the solution on the magnetic stirrer with the perchloric acid solution.

43、 - Carry out the titration until a stable green colour is obtained. - If using the potentiometric method, place the electrodes in the test solution and titrate the solution on the magnetic stirrer with the perchloric acid solution. - Note the temperature t of the perchloric acid solution in order to

44、 be able to allow for expansion of the solution with increasing temperature. - Carry out a blank test an the same time as the determination, following the same procedure and using the same reagents but omitting the test portion. STD*BSI BS EN 1877-L-ENCL 2000 LbS4bbS 0874075 195 Page 7 EN 1877-1 200

45、0 13 Calculation The epoxide equivalent E is given by the equation : 1000 rn EE = where m is the mass, in (g), of the test portion ; VO is the volume, in (mi), of the perchloric acid solution used in the blank test ; VI is the volume, in (mi), of the perchloric acid solution used in the determinatio

46、n ; t is the temperature, in (“C), of the perchloric acid solution at the time of the determination and blank test ; t, is the temperature, in (“C), of the perchloric acid solution at the time of standardization ; c is the concentration of the perchloric acid solution (usually 0,l rnoi) at the time

47、of standardization. NOTE acid solution (1,07 x by working in a temperature-controlled room. The use of the correction factor is recommended because of the significant coefficient of expansion of the perchloric K-l), which corresponds to a volume variation of 0,l % per Kelvin. Use of this factor can

48、be avoided 14 Precision Repeatability limit : 0,5 % Reproducibility limit : 1 %. 15 Testreport The test report shall include the following information : a) a reference to this European Standard ; b) all details necessary to identify the product tested ; c) the epoxide equivalent and the way in which

49、 it is expressed; d) the reagent used if it is not tetraethylammonium bromide ; e) any other factor likely to have affected the result ; f) any deviations, by agreement or otherwise, from the procedure described ; g) the date of test. STD-BSI BS EN 1877-1-ENGL 2000 D 1624669 0874076 021 Page 8 EN 1877-1 :2000 Bibliography IS0 3001 : 1997 Plastics - Epoxy compounds - Determination of epoxy equivalent. 1877-1 :2000 BSI 389 Chimvick High Road London w4 4AL BSI - British Standards Institution BSI is the independent national body responsible for preparing