1、- STDDBSI BS EN IS0 3001-ENGL 1999 W 2b24bb9 07827LL bob BRITISH STANDARD Plastics - Epoxy compounds - Determination of epoxy equivalent The European Standard EN IS0 3001:1999 has the status of a British Standard IS EN IS0 l001:1999 ICs 83.080.01 I NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITT
2、ED BY COPYRIGK LAW BS EN IS0 3001:1999 been prepared under the direction of the Sector Amd.No. Date Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 May 1999 O BSI 05-1999 ISBN O 580 32302 1 National foreword Text affecte
3、d This British Standard is the English language version of EN IS0 3001:1999. It is identical with IS0 3001:1999. It supersedes BS 27824. Methods 433C and 433D31997 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting
4、plastics and prepregs, which has the responsibility to: - aid enquirem to undemtand the te$ - present to the responsible internationallEuropean committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; - monitor related international and European dev
5、elopments and promulgate them in the UK A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international public
6、ations with their corresponding European publications. The British Standards which implement these international or European publications may be found in the BSI Standards Catalogue under the section entitled “Intedonal Standards Correspondence Index”, or by using the “Find” facility of the BSI Stan
7、dards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pa
8、ges This document comprises a front cover, an inside front cover, the EN IS0 title page, the EN IS0 foreword page, the IS0 title page, page V, is the volume, in millilitres, of perchloric acid solution (4.6.1) used in the blank test; V, is the volume, in millilitres, of perchloric acid solution (4.6
9、.1) used in the determination. 4.7 Tetraethylammonium bromide, reagent solution. Dissolve 100 g of tetraethylammonium bromide in 400 ml of glacial acetic acid (4.1). Add a few drops of crystal violet solution (4.5). If it changes colour, bring it back to the original (blue-green) colour with standar
10、d volumetric perchloric acid solution (4.6). For some epoxy compounds of low reactivity, the use of tetrabutylammonium iodide is advised, either as the solid or as a 10 % solution in chloroform. In this case, light shall be excluded as much as possible. Solutions of tetrabutylammonium iodide in chlo
11、roform are unstable and shall be freshly prepared for each titration. 5 Apparatus 5.1 Potentiometric titration apparatus, equipped with a silver electrode and a silver chloride or mercury sulfate electrode. 5.2 Balance, accurate to within 0,l mg. 5.3 Conical flask, capacity 100 ml or 200 ml, with gr
12、ound-glass neck and ground-glass stopper. 5.4 Microburette, with closed reservoir, or calibrated burette, capacity 10 ml. 5.5 Glass apparatus, with ground joints, vents being protected from moisture by calcium chloride tubes. 2 STD.BSI BS EN IS0 3130L-ENGL 1779 Lb24bb9 U782717 7T7 m EN IS0 3001:1999
13、 5.6 Magnetic stirrer, with polytetrafluoroethylene-coated bar. 5.7 Thermometer, calibrated to permit temperature measurements to within i 0,l OC. 5.8 Pipette, capacity 10 ml. 5.9 Volumetric flask, capacity 1 O00 ml. 5.10 Measuring cylinders, capacity 50 ml and 500 ml. 6 Procedure 6.1 Weigh into the
14、 flask, to the nearest 0,1 mg, a test portion containing 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). 6.2 Add 10 ml of chloroform (4.3), then dissolve the test portion using the magnetic stirrer
15、(5.6) and, if necessary, by heating slightly. Cool to room temperature, add 20 ml of glacial acetic acid (4.1) and then, with the pipette (5.8), 10 ml of tetraethylammonium bromide solution (4.7). In the case of high-molecular-mass epoxy resins, increase the chloroform volume to 30 ml. 6.3 If using
16、the indicator method, add 4 to 6 drops of crystal violet solution (4.5) and titrate the solution on the magnetic stirrer with perchloric acid solution (4.6). Carry out the titration until a stable green colour is obtained. 6.4 If using the potentiometric method, place the electrodes in the test solu
17、tion. Adjust the speed of the magnetic stirrer to give vigourous stirring without splattering. Titrate the solution with perchloric acid solution (4.6). 6.5 Note the temperature t of the perchloric acid solution in order to be able to allow for expansion of the solution with increasing temperature.
18、6.6 Carry out a blank test at the same time as the determination, following the same procedure and using the same reagents but omitting the test portion. 7 Expression of results Calculate the epoxy equivalent EE, in grams per mole, by the following equation, rounding to three places of d ec i m a I
19、s : 1 O00 m EE = (V, -Vo) 1 - - ( :i;). where m is the mass, in grams, of the test portion; Vo is the volume, in millilitres, of perchloric acid solution (4.6) used in the blank test; VI is the volume, in millilitres, of perchloric acid solution (4.6) used in the determination; t is the temperature,
20、 in degrees Celsius, of the perchloric acid solution (4.6) at the time of the determination and blank test; 3 EN IS0 3001:1999 Titration Repeatability Reproducibility method Sr r SR R Potentiometric 0,61 1,72 1,22 3,41 Indicator 0,68 1,91 1 ,O4 2,91 1 rc c is the temperature, in degrees Celsius, of
21、the perchloric acid solution (4.6) at the time of standardization; is the concentration, in moles per litre, of the perchloric acid solution (4.6) (usually 0,l moVI) at the time of standardization. I Average value of EE 187,O 188,2 NOTE The use of the correction factor is necessary because of the si
22、gnificant coefficient of expansion of the perchloric acid solution (1,07 x 10-3 “C-1), which corresponds to a volume variation of 0,l % per degree Celsius. Use of this factor can be avoided by working in a temperature-controlled room. The result is sometimes expressed as the epoxy index, expressed i
23、n moles of epoxy groups per kilogram, calculated as follows: Titration method Potentiometric 1 O00 Epoxy index EI = - EE Repeatability Reproducibility Average value of EE Sr r SR R 0,87 2,43 6,68 18,71 916,3 8 Precision Indicator The precision of this method was determined in accordance with IS0 572
24、5, Accuracy (trueness and precision) of test methods and results, following round-robin testing organized in Japan in 1996. 2,94 8,24 8,Ol 2244 91 9,2 Solid bisphenol A type epoxy resins 4 STD.BSI BS EN IS0 30UL-ENGL L779 IB LbZqbb7 0782721 555 EN IS0 3001:1999 9 Testreport The test report shall inc
25、lude the following particulars: a reference to this International Standard; all details necessary for complete identification of the sample; the reagent used, if not tetraethylammonium bromide; the result of the test and the way in which it is expressed; details of any operation not included in this
26、 Intemational Standard as well as details of any incident likely to have affected the result; the date of the test. 5 STD-BSI BS EN IS0 3001-ENGL 1779 118 1b24bb7 0782722 q1 D EN IS0 3001:1999 Annex A (normative) Modification applicable to epoxyamines A.1 Scope When determinations are carried out on
27、 nitrogen-containing epoxy resins (.e. epoxyamines) using the method described in the body of this International Standard, the values determined for the epoxy equivalent are too low. This is due to a reaction between the perchloric acid and the amino nitrogen, leading to the formation of a salt. If
28、account is taken of the perchloric acid involved in the formation of the salt, then the method can also be used to determine the epoxy equivalent of epoxyamines. A.2 Principle The amino nitrogen in a test portion of the epoxyarnine is titrated with a 0,l molA standard volumetric perchloric acid solu
29、tion. The second blank value thus obtained is used as a correction factor in the calculation of the epoxy equivalent, as shown in clause A.4. A.3 Procedure Determine the second blank value in accordance with clause 6 of this International Standard, but without addition of tetraethylammonium bromide
30、solution (4.7). A.4 Expression of results Calculate the epoxy equivalent EE of the epoxyarnine, in grams per mole, by the following equation: 1 O00 m EE = “1 1 000 where ml is the mass, in grams, of the test portion used in the second blank test; V, is the volume, in millilitres, of perchloric acid
31、solution (4.6) used in the second blank test; the other symbols are as defined in clause 7 of this International Standard. 6 BS EN IS0 3001:1999 BSI 389 Chiswick High Road London w4 4AL BSI - British Standards Institution BSI is the independent national body responsible for preparing British Standar
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