1、DEUTSCHE NORM Februarv 2001 Determination of the tendency of compounds and products based on chloride and anv other acidic txoducts at elevated temreratures vinyl chloride homopolymers and copolymers to evolve hydrogen DIN - Part 3: Conductometricmethod (IS0 182-3 : 1993) IEN IS0 182-3 English versi
2、on of DIN EN IS0 182-3 ICs 83.080.20 Kunststoffe - Bestimmung der Neigung von Formmassen und Erzeugnissen auf der Basis von Vinylchlorid- Homopolymeren und -Copolymeren, bei erhhten Temperaturen Chlorwasserstoff und andere saure Pro- dukte abzugeben - Teil 3: Leitfhigkeitsverfahren (IS0 182-3 : 1993
3、) European Standard EN IS0 182-3 : 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 249 to adopt, without alteration, International Standard IS0 182-3 as a European Standard.
4、 The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Technical Committee PVC-Formmassen. DIN EN IS0 182-4 and DIN IS0 565 are the standards corresponding to International Standards IS0 182-4 and IS0 565, respectively, referred t
5、o in clause 2 of the EN. National Annex NA Standards referred to (and not included in Normative references and Annex ZA) DIN EN IS0 182-4 Determination of the tendency of compounds and products based on vinyl chloride homopolymers and copolymers to evolve hydrogen chloride and any other acidic prod-
6、 ucts at elevated temperatures - Part 4: Potentiometric method (IS0 182-4 : 1993) Test sieves - Metal wire cloth, perforated metal plate and electroformed sheet - Nomi- na1 sizes of openings (IS0 565 : 1990) DIN IS0 565 EN comprises 15 pages. No pari of this standard may be reproduced without the pr
7、ior permission of Ref. No. DIN EN IS0 182-3 : 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 price group 11 Sales No. 11 11 06.01 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NO
8、RM EN IS0 182-3 September 2000 ICs 83.080 English version Plastics Determination of the tendency of compounds and products based on vinyl chloride homopolymers and copolymers to evolve hydrogen chloride and any other acidic products at elevated temperatures Part 3: Conductometric method (IS0 182-3 :
9、 1993) Plastiques - Dtermination de la tendance des compositions base dhomopolymres et copolymres du chlorure de vinyle dgager du chlorure dhydrogne et ventuelle- ment dautres produits acides tempratures leves - Partie 3: Mthode conductimtrique (IS0 182-3 : 1993) Kunststoffe - Bestimmung der Neigung
10、 von Formmassen und Erzeugnissen auf der Basis von Vinylchlorid-Homopolymeren und -Copolymeren, bei erhhten Tempe- raturen Chlorwasserstoff und andere saure Produkte abzugeben -Teil 3: Leitfhig keitsverfahren (IS0 182-3 : 1993) This European Standard was approved by CEN on 2000-09-08. CEN members ar
11、e 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 such national stand- ards may be obtained on application to
12、 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 language and notified to the Central Secretariat has the same st
13、atus 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, Sweden, Switzerland, and the United Kingdom. CEN European Co
14、mmittee 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 national members. Ref. No. EN IS0 182-3 : 2000 E Page 2
15、EN IS0 182-3 : 2000 Foreword International Standard IS0 182-3 : 1993 Plastics - Determination of the tendency of compounds and products based on vinyl chlo- ride homopolymers and copolymers to evolve hydrogen chloride and any other acidic prod- ucts at elevated temperatures - Part 3: Conductometric
16、method, which was prepared by ISO/TC 61 Plastics of the International 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 standar
17、d, either by publication of an identical text or by endorsement, 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 S
18、tandard: Austria, Belgium, the Czech Republic, Denmark, Finland, 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 182-3 : 1993 was approve
19、d by CEN as a European Standard without any modification. NOTE: Normative references to international publications are listed in Annex ZA (normative). WARNING - The use of this part of IS0 182 may involve hazardous materials, operations and equipment. This part of IS0 182 does not purport to address
20、 all of the safety problems associated with its use. It is the responsibility of the user of this part of IS0 182 to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1 Scope 1.1 This part of IS0 182 specifies a method for the d
21、etermination of the thermal stability at elevated temperature of compounds and products based on vinyl chloride homopolymers and copolymers (in the following text abbreviated as PVC) which undergo dehydrochlorination (the evolution of hydrogen chlor- ide). 1.2 The method may be used as a quality con
22、trol test during manufacture and conversion of PVC com- pounds. It may also be used for the characterization of PVC compounds and products, especially with re- gard to the effectiveness of their heat-stabilizing sys- tems. It is suitable for coloured PVC compounds and prod- ucts where a discolourati
23、on test under the action of heat may be unsatisfactory. 1.3 The method is recommended for compounded PVC materials and products only, although it can be used for polymers in powder form under appropriate conditions, to be agreed upon between the interested parties. The method is not recommended for
24、PVC compounds in the form of dry blends, since such materials may not be sufficiently homogeneous. 1.4 PVC compounds and products may evolve other decomposition products, in addition to hydrogen chloride, at elevated temperatures. A limited number of these decomposition products may affect the con-
25、ductivity of water when they are absorbed into it. Compensation for this effect is not within the scope of this part of IS0 182, and therefore care is necess- ary in attempting to compare results for dissimilar compounds and products. In this case a method suit- able for the determination of chlorid
26、e ion (CI7 in the absorbing solution shall be used (see IS0 182-4). 1.5 The method may also be applied to other plas- tics materials which can evolve hydrogen chloride or other hydrogen halides when heated under the con- ditions prescribed by the relevant specifications, or as agreed upon between th
27、e interested parties. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of IS0 182. At the time of publication, the editions indicated were valid. All standards are subject Page 3 EN IS0 182-3 : 2000 to revisio
28、n, and parties to agreements based on this pan of IS0 182 are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 182-4:1993, Plastics - Determinatio
29、n of the tendency of compounds and products based on vinyl chloride homopolymers and copolymers to evolve hy- drogen chloride and any other acidic products at ele- vated temperatures - Part 4: Potentiometric method. IS0 565:1990, Test sieves - Metal wire cloth, per- forated metal plate and electrofo
30、rmed sheet - Nom- inal sizes of openings. IS0 4793:1980, laboratory sintered (fritted) filters - Porosity grading, classification and designation. IS0 6353-2: 1 983, Reagents for chemical analysis - Part 2: Specifications - First series. 3 Definition For the purposes of this part of IS0 182, the fol
31、lowing definit ion applies. 3.1 stability time, ts: Time, measured by reference to a predetermined change in the conductivity of ab- sorbing demineralized water, required for a certain amount of hydrogen chloride to be evolved when a prescribed mass of PVC compound or product is maintained at an ele
32、vated temperature under the test conditions specified in this part of IS0 182. 4 Principle A test portion of the PVC compound or product is maintained at an agreed temperature in a nitrogen gas stream and the hydrogen chloride evolved is absorbed in a given amount of demineralized water. The amount
33、of hydrogen chloride evolved is determined in relation to the recorded change in conductivity of the water. 5 Reagents During the test, use only reagents of recognized ana- lytical grade in accordance with IS0 6353-2. 5.1 Pure nitrogen, containing less than 6 ppm oxy- gen and less than 0,l ppm carbo
34、n dioxide by volume. The purity shall be such that when the gas is passed through demineralized water (see 5.3) for 1 h at a rate of 7,2 I/h -t 0,l I/h, the conductivity of the water re- mains unchanged. The gas shall be dried by passing it through a suitable drying agent, and the flow-rate through
35、the dehydrochlorination cell adjusted by means of a nee- dle valve and measured using a suitable flowmeter. 5.2 Hydrochloric acid, aqueous solution, c(HCI) = 0,l mol/l. 5.3 Demineralized water, with a pH of 4.0 i 0,l and a conductivity not greater than 40 FS/cm, ad- justed by the addition of 0,l mol
36、il hydrochloric acid. 6 Apparatus The general arrangement of the apparatus is shown in figure 1. The figure shows a re-usable dehydrochlorination cell A. This cell may be replaced by a disposable cell B. 6.1 Dehydrochlorination cells. 6.1.1 Cell A (re-usable), with shape and dimensions as shown in f
37、igure2. A recommended procedure for cleaning the cell is given in annex A. 6.1.2 Cell B (disposable), with shape and dimen- sions as shown in figure3. NOTE 1 Other types of cell may be employed if it has been proved that the results obtained are equivalent to those obtained with one of the cells des
38、cribed in 6.1.1 and 6.1.2. 6.2 Test portion holder, for use with cell A. The test portion is supported on a porous sintered-glass disc (grade P 100, IS0 4793). 10 mm in diameter. To prevent blocking of the porous disc, it is advisable to place a thin, soft layer of glass wool between it and the test
39、 portion. A recommended procedure for cleaning the disc sup- port is given in annex A. Page 4 EN IS0 182-3 : 2000 2 10 8 9 12 13 6 7 11 16 1s 1 1 Nz cy:inder 2 Purification train 3 Ball flowmeter 4 Electronic temperature S Temperature sensor 6 Heating bath 7 PVC test portiorl 8 Dehydrochlorination c
40、ell I 4 ontroller (SC i I ie division O 9 Thermometer (scale division 0.1 0 10 Silicone oil 11 Magnetic stirrer C) 12 Absorbing solution 13 Measuring electrode(s) 14 Conductance meter 15 Recorder Figure 1 - General arrangement of apparatus C C c Spurs 11 coils Sintered-glass 10 mm diameter Page 5 EN
41、 IS0 182-3 : 2000 Dimer.sions in millimetres disc, (removo It Figure 2 - Cell A (reusable) for dehydrochlorination of PVC samples Page 6 EN IS0 182-3 : 2000 C u- h Dimensions in millimetres 4 U-tube (wall thickness li 0 int. 6 - Figure 3 - Cell B (disposable) for dehydrochlorination of PVC samples 6
42、.3 Glass connection tube, for use with cell A, having dimensions as shown in figure4. The con- nection tube is secured to cell A by two springs fixed to hooks on the ground-glass joints. The tube shall be provided with an insulating jacket. 6.4 Expansion joints and cell connections, for use with cel
43、l B. Cell B is connected to the apparatus through flexible polytetrafluoroethylene (PTFE) and silicone rubber tubes. Special joints allow for thermal expansion. The complete joint arrangement is shown in figure 5. 6.5 Oil bath, with a capacity of at least 10 I. The bath shall be capable of operating
44、 in the temperature range 170 “C to 210 “C and of maintaining the test temperature with an accuracy of I 0,l “C. The bath shall be designed so that the temperature distribution is even throughout, and shall have a ther- mal capacity sufficient to avoid temperature change when the dehydrochlorination
45、 cell is immersed in it. 6.6 Thermometer, with a scale suitable for reading the heating bath temperature in the range 170 “C to 210 “C and with a scale division of 0,l “C. 6.7 Balance, with a scale division of 1 mg. 6.8 Measurement cell. A suitable measurement cell is shown in figure6 If the diamete
46、rs of the measurement electrode and the feed tube for the gases from decomposition of the test portion are sufficiently small, a 300 ml Erlenmeyer flask is a suitable alternative measure- ment cell. A recommended procedure for cleaninc the cell is given in annex A. 6.9 Magnetic stirrer, capable of p
47、roviding gentle agitation within the measurement cell. 6.10 ConductanTe meter, with a conductivity probe constant of 1 cm- , giving direct readings in FS/cm, and preferably equipped with an automatic tempera- ture compensating device and an output for a chart recorder. NOTE 2 Graphite electrodes hav
48、e been shown to operate in a more trouble-free manner than platinized platinum electrodes. 6.11 Stopclock, or other suitable timing device, if not included in the recorder. 6.12 Flowmeter, for example a rotameter, or other suitable device capable of measuring a gas flow-rate within the range 120 cm3
49、/min f 4 cm3/min. 7 Preparation of test samples The measured stability times is depend to some ex- tent on the surface area of the prepared test portions as well as on their thermal history. Any cutting or grinding of a material necessary to produce the test portions shall be conducted in a uniform manner, avoiding heating of the material. NOTE 3 Cryogenic grinding is recommended. 7.1 PVC plastisols Spread these materials on glass plates and gel them in an oven at an agreed temperature so that sheets 0,5 mm thick are formed. Cut these sheets into squares ap
