1、DEUTSCHE NORM Februarv 2001 Phenolic resins Determination of the gel time of resols under specific conditions using automatic apparatus (IS0 9396 : 1997) Enalish version of DIN EN IS0 9396 DIN EN IS0 9396 - ICs 83.080.1 O Supersedes DIN IS0 9396, January 1992 edition. Kunststoffe - Phenolharze - Bes
2、timmung der Gelierzeit mit einem Automaten unter spezifischen Bedingungen (IS0 9396 : 1997) European Standard EN IS0 9396 : 2000 has the status of a DIN Standard. A comma is used as the decimal marker. National foreword This standard has been published in accordance with a decision taken by CEN/TC 2
3、49 to adopt, without alteration, International Standard IS0 9396 as a European Standard. The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Technical Committee Hartbare Harze. It should be noted that the outside diameter (not t
4、he inside diameter, as erroneously stated) of the test tube described in subclause 4.4 is to be (16 I0,2) mm. Amendments IS0 9396 having been adopted as a European Standard, the status of the corresponding DIN Standard (DIN IS0 9396) has been changed accordingly. Previous edition DIN IS0 9396: 1992-
5、01. EN comprises 6 pages. No pari of this standard may be reproduced without the prior permission of Ref. No. DIN EN IS0 9396 : 2001 -0 Y Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, s the exclusive right of sale for German Standards (DIN-Normen). English pr
6、ice group 06 Sales No. 1106 07.01 EUROPEAN STANDARD NORME EUFIOPEENNE EUROPISCHE NORM EN IS0 9396 September 2000 ICs 83.080 Supersedes EN IS0 9396 : 1995. English version Plastics Determination of the gel time of resols under specific conditions using automatic apparatus (IS0 9396 : 1997) Phenolic r
7、esins Plastiques - Rsines phnoliques - Dtermination du temps de glification des rsols dans des conditions spcifiques sur appareils automatiques (IS0 9396 : 1997) Kunststoffe - Phenolharze - Bestimmung der Gelierzeit mit einem Automaten unter spezifischen Bedingungen (IS0 9396 : 1997) This European S
8、tandard was approved by CEN on 2000-08-09. CEN members are bound to comply with the CENKENELEC 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 su
9、ch national stand- ards may be obtained on application to the Central Secretariat or to any CEN member. The European Standards exist 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 languag
10、e and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, the Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, the Netherlands, Norway, Portugal, Spain, Swe
11、den, Switzerland, and the United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels O 2000. CEN - All rights of exploitation in any form and by any means reserved worldwide for CEN
12、 national members. Ref. No. EN IS0 9396 : 2000 E Page 2 EN IS0 9396 : 2000 Foreword International Standard IS0 9396 : 1997 Plastics - Phenolic resins - Determination of the gel time of resols under specific conditions using automatic apparatus, which was prepared by ISO/TC 61 Plastics of the Interna
13、tional Organization for Standardization, has been adopted by Technical Committee CEN/TC 249 Plastics, the Secretariat of which is held by IBN, as a European Standard. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement
14、, and conflicting national standards withdrawn, by March 2001 at the latest. In accordance with the CENKENELEC Internal Regulations, the national standards organizations of the follow- ing countries are bound to implement this European Standard: Austria, Belgium, the Czech Republic, Denmark, Finland
15、, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, the Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, and the United Kingdom. Endorsement notice The text of the International Standard IS0 9396 : 1997 was approved by CEN as a European Standard without any modification. Page 3
16、 EN IS0 9396 : 2000 1.Scope This International Standard specifies a method for determining the gel time of phenolic resins at a given temperature, using automatic apparatus under specified conditions. The test temperatures are 1 O0 OC, 130 OC and 150 OC. The method specified employs a plunger driven
17、 to carry out a reciprocating vertical motion. This method applies to the following types of phenolic resin: - liquid resols - solid resols with low melting points Powdered resins with a short gel time, such as mixtures of novolak and hexamethylenetetramine, do not lend themselves to this type of de
18、termination. Such resins crosslink as soon as fusion starts and become too viscous in the test tube to give meaningful results. Resins containing large amounts of a solvent with a low boiling point are especially unsuitable for this type of determination. With such resins, a boiling and distillation
19、 process takes place as the resin hardens. It might be of interest to determine the time taken for the resin to gel in the presence of a catalyst. The catalyst shall be added in well defined proportions. The type of catalyst used and its treatment shall be stated in the test report. 2. Preparation o
20、f test portions 2.1 Test liquid resols as produced. 2.2 Test solid resols as produced. 3. Principle A plunger placed in a test tube containing the substance to be examined is driven to carry out a reciprocating motion. The gel time is reached when the viscosity of the specimen is such that the tube
21、is lifted with the plunger, thus stopping a timer. Page 4 EN IS0 9396 : 2000 4. Apparatus 4.1 Automatic apparatus for measuring gel time (see figure 1): The cycle time of the plunger shall be 1 O s or as otherwise agreed between the parties concerned. The frequency shall be mentioned in the test rep
22、ort. 4.2 Thermostatically controlled bath, maximum temperature 200 OC, tolerance i 0,5 “C for the temperature chosen for the test (see 5). The density of the bath liquid, e.g. silicone oil, shall be I g/cm3 f 0,l g/cm3. 4.3 Plunger: metal wire with helix, length approx. 23 cm, diameter approx. 1 mm;
23、 helix at the end of the wire, height approx. 5 mm, diameter 5 mm to 6 mm. 4.4 Test tube, with a mass of 10 g f 1 g and the following dimensions: inside diameter 16 mm f 0,2 mm, length 160 mm f 4 mm. 4.5 Metal ring, weighing 10 g or 20 g, to hold down the test tube (4.4) in the bath (4.2). 4.6 Balan
24、ce, accurate to Oll g. 5. Procedure Perform the test in duplicate, or on a greater number of test portions as agreed between the parties concerned. Weigh 5 g +/- Oll g of resin into the test tube (4.4). Place the metal ring (4.5) round the top of the tube to hold it down in the bath (4.2) and to pre
25、vent it being lifted prematurely as the viscosity rises before the gel point is reached. The mass of the ring shall be 1 O g for liquid resols 20 g for solid or powdered resols. or The test temperature shall be 1 O0 OC, 130 OC or 150 OC, as agreed between the parties concerned. Start up the apparatu
26、s (4.1) as soon as the test tube containing the resin to be tested is in its holder. In the case of liquid resins, connect up the plunger immediately. For solid resins, it will be necessary to wait until the resin has melted. During the test, the test tube shall remain immersed to a depth of 11 cm i
27、n the liquid in the thermostatically controlled bath, with part of the test tube holder also being immersed. Page 5 EN IS0 9396 : 2000 The gel time is reached, when the test tube follows the to-and-fro motion of the plunger, .e. when the test tube starts to move in its holder. The apparatus will sto
28、p automatically when the gel time is reached. 6. Precision (test error) 6. I Repeatability (r) The value below which the absolute difference between two single test results, each the mean of duplicates, obtained on identical material by one operator in one laboratory within a short interval of time
29、using the standardized test method, may be expected to lie with a 95 % probability is 2-8 % (depending on resin type) 6.2 Reproducibility (R) The value below which the absolute difference between two test results, each the mean of duplicates, obtained on identical materials by operators in different
30、 laboratories using the standardized test method, may be expected to lie with a 95 % probability is 20 % 7. Test report The test report shall contain the following information: a) a reference to this International Standard; b) all details necessary for the complete identification of the sample of re
31、sin tested; c) the arithmetic mean of the individual values measured for the gel time, expressed in minutes to the nearest 0,l min. d) the temperature at which the test was performed; e) the frequency of the plunger motion. Page 6 EN IS0 9396 : 2000 Dimensions in millimetres 4 6 7 8 9 10 11 Key 1 El
32、ectric timer 2 Timer seeing button 3 4 Plunger drive motor 5 6 Metal ring 7 Test tube holder 8 Testtube 9 10 Phenolic resin 11 Start button for plunger and timer Stop lever for plunger and timer Plunger (of material other than aluminium) Thermostatically controlled bath containing a liquid suitable for use at the highest temperature employed Figure 1 - Reciprocating-plunger apparatus for determining gel time
