1、BRITISH STANDARD BS EN ISO 4615:1999 Plastics Unsaturated polyesters and epoxide resins Determination of total chlorine content The European Standard EN ISO4615:1999has the status of a British Standard ICS 83.080.10BSENISO4615:1999 This British Standard, having been prepared under the directionof th
2、e Sector Committeefor Materials and Chemicals, waspublished underthe authorityof the Standards Committee and comesinto effect on 15August1999 BSI 04-2000 ISBN 0 580 32893 7 National foreword This British Standard is the English language version of ENISO4615:1999. It is identical with ISO4615:1979. T
3、he UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepregs, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpreta
4、tion, or proposals for change, and keep the UK interests informed; monitor related international and European developments 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
5、 that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement international or European publications referred to in this document may be found in the BSI S
6、tandards Catalogue under the section entitled “International Standards Correspondence Index” or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsibl
7、e for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theENISOtitle page, page 2, theISO title page, pages ii to iv, pages 1 to 6 an
8、d a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBSENISO4615:1999 BSI 04-2000 i Contents Page National forew
9、ord Inside front cover Foreword 2 Foreword iii Text of ISO 4615 1ii blankEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM ENISO 4615 May 1999 ICS 83.080.00 English version Plastics Unsaturated polyesters and epoxide resins Determination of total chlorine content (ISO4615:1979) Plastiques Rsines de
10、polyesters non saturs et poxydes Dtermination de la teneur totale en chlore (ISO4615:1979) Kunststoffe Ungesttigte Polyester und Epoxidharze Bestimmung des Gesamtchlorgehaltes (ISO4615:1979) This European Standard was approved by CEN on16April1999. CEN members are bound to comply with the CEN/CENELE
11、C 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 standards may be obtained on application to the Central Secretariat or to any CEN
12、 member. This European Standard exists 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 status as the official versions. CEN me
13、mbers are the national standards bodies of Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normali
14、sation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1999 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4615:1999 EENISO4615:1999 2 BSI 04-2000 Foreword The text of the International
15、Standard from Technical Committee ISO/TC61“Plastics” of the International Organization for Standardization (ISO) has been taken over as an European Standard by Technical Committee CEN/TC249 “Plastics”, the secretariat of which is held by IBN. This European Standard shall be given the status of a nat
16、ional standard, either by publication of an identical text or by endorsement, at the latest by November 1999, and conflicting national standards shall be withdrawn at the latest by November1999. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
17、countries are bound to implement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the UnitedKingdom. Endorsement notice The text of the International
18、Standard ISO4615:1979has been approved by CEN as a European Standard without any modification.ENISO4615:1999 ii BSI 04-2000 Contents Page Foreword iii 1 Scope and field of application 1 2 Principle 1 3 Reagents 1 4 Apparatus 1 5 Test sample 1 6 Procedure 1 7 Expression of results 5 8 Test report 5 F
19、igure 1 Combustion bomb, gas-fired type (for method A) 2 Figure 2 Flask for oxygen combustion with platinum wire attached to stopper (for method B) 3 Figure 3 Preparation of holder for liquid test portion 5 Figure 4 Folding of filter paper containing solid test portion 6 Descriptors: Plastics, polye
20、ster resins, epoxy resins, chemical analysis, determination of content, chlorine, combustion analysis.ENISO4615:1999 BSI 04-2000 iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards institutes (ISO member bodies). The work of developin
21、g International Standards is carried out through ISO technical committees. Every member body interested in a subject for which a technical committee has been set up has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO,
22、 also take part in the work. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the ISO Council. International Standard ISO4615was developed by Technical Committee ISO/TC61, Plastics
23、, and was circulated to the member bodies in August1978. It has been approved by the member bodies of the following countries: The member body of the following country expressed disapproval of the document on technical grounds: United Kingdom Austria Hungary South Africa, Rep. of Belgium Iran Sweden
24、 Bulgaria Italy Switzerland Canada Japan Turkey Czechoslovakia Korea, Rep. of USA Egypt, Arab Rep. of Mexico USSR Finland Netherlands Yugoslavia Germany, F.R. New Zealand Greece Romaniaiv blankENISO4615:1999 BSI 04-2000 1 1 Scope and field of application This International Standard specifies two met
25、hods for the determination of the total chlorine content of unsaturated polyesters and epoxide resins, namely: method A: combustion in a bomb; method B: combustion in a flask. NOTE 1Determination of combined chlorine and bromine content or bromine content only, is also possible by these methods. The
26、 appropriate procedure shall be agreed upon by the purchaser and the supplier. NOTE 2These methods are not applicable to the determination of total chlorine in epoxy resins containing chlorine as an impurity. 2 Principle Oxidation of a test portion with sodium peroxide (method A) or gaseous oxygen (
27、method B) followed by electrometric or volumetric titration of the resulting chlorides. 3 Reagents During the analysis, use only reagents of known analytical quality, and only distilled water or water of at least equivalent purity. 3.1 Silver nitrate, standard volumetric solution, c(AgNO 3 ) = 0,1mo
28、l/l. 1) NOTEFor testing resins of low total chlorine content less than2% (m/m), a standard volumetric solution of silver nitrate, c(AgNO 3 ) = 0,05 mol/l, 2)may be used. 3.2 Nitric acid, 126 g/l solution. For method A only: 3.3 Nitric acid, concentrated, = 1,42 g/ml. 3.4 Sodium peroxide, granulated.
29、 3.5 Starch or sucrose as combustion aids. For method B only: 3.6 Oxygen, gaseous. 3.7 Sodium nitrate 3.8 Potassium hydroxide solution, 100 g/l. 3.9 Hydrogen peroxide solution, 300 g/l. 4 Apparatus 4.1 Balance, to weigh to an accuracy of0,0001g. 4.2 Equipment for Volhard titration or for electrometr
30、ic titration, with a burette having a capacity and accuracy appropriate to the chosen method (A or B). For method A only: 4.3 Combustion bomb (for example Parr bomb or another bomb which gives the same results), electrically fired or gas-fired. A suitable gas-fired bomb is shown in Figure 1. 4.4 Nic
31、kel crucible with lid, to fit into the bomb (gas-fired). Suitable dimensions are: diameter 25 mm, height 40 mm. 4.5 Safety oven 4.6 Beaker, of capacity 600 ml. For method B only: 4.7 Round-bottomed flask of capacity500ml, with head for oxygen combustion (see Figure 2). A platinum wire1mm in diameter
32、 and120mm long in the shape of a tapered spiral is attached to the stopper, a suitable spiral being 15mm in diameter and15mm long. It is recommended that metal gauze be wrapped around the flask for safety or that a safety cage be used. NOTEA safety bulb can be fitted to the flask to permit expansion
33、 of the gases to reduce the hazard. 4.8 Filter paper, free from halogens and ash. 4.9 Adhesive tape of cellulose acetate or regenerated cellulose, coated with polyvinyl acetate, of width30mm. 4.10 Beaker, of capacity 100 ml. 5 Test sample If the sample is in the solid state, it shall be in powdered
34、or granular form, or if necessary shall be cut into pieces 1to3mm in size. When an electrically fired bomb is used, it is preferable that the material be powdered. 6 Procedure 6.1 Method A (combustion bomb) 6.1.1 Test portion Weigh, to the nearest 0,0005g,0,1g maximum of the test sample. 1) Hitherto
35、 expressed as 0,1 N standard volumetric solution. 2) Hitherto expressed as 0,05 N standard volumetric solution.ENISO4615:1999 2 BSI 04-2000 Figure 1 Combustion bomb, gas-fired type (for method A)ENISO4615:1999 BSI 04-2000 3 6.1.2 Determination 6.1.2.1 First place 7 to 7,5 g of the sodium peroxide(3.
36、4) in the crucible (4.4) (for the gas-fired bomb), or in the fusion cup of the bomb (for the electrically fired bomb), then add the test portion(6.1.1) mixed with 0,16to 0,17g of the starch or sucrose, then an additional 7to7,5g of the sodium peroxide. The filling with sodium peroxide should be carr
37、ied out behind a shield protecting the operator. Mix all components by stirring, then place the crucible, with the lid in position, inside the bomb and close the bomb tightly. If an electrically fired bomb is used, assemble the bomb and tap it to settle the charge. 6.1.2.2 Fire the bomb. IMPORTANT W
38、ARNING If a gas-fired bomb is used, place the bomb in the safety oven (4.5). Adjust the flame beforehand, using an empty bomb in the safety oven, so that the top of the flame is a few millimetres from the base of the bomb. Then remove the empty bomb. Heat the test bomb to300to400 C for about10min. I
39、gnition usually starts at50to60 C, and is detected by a cracking sound, and the fact that the bottom of the bomb starts to glow. The heating of the bomb is of extreme importance because underheating will cause incomplete oxidation of the organic matter and low chlorine results, whereas overheating m
40、ay cause damage to the bomb cup and even an explosion. These bombs are not intended to operate at a red heat, but there is no serious danger involved in this method of oxidation provided that the proper charges are used in a bomb that is in satisfactory condition, and that the proper heating techniq
41、ue is used. Discard the bomb if the sides or bottom become visibly swollen, or if the interior surfaces become worn or corroded at any point to an inside diameter1,5% below the original value. It is essential to read carefully the manufacturers instructions, particularly with reference to safety pre
42、cautions. 6.1.2.3 Cool the bomb. Open it and, if a gas-fired bomb is used, remove the crucible, carefully place it in100ml of water in the beaker (4.6) and immediately cover the beaker with a watch glass. When the reaction has subsided, wash down the inside of the bomb and the plug, collecting the w
43、ashings in the beaker. If an electrically fired bomb is used, dismantle it after cooling, remove the head and tip it into100ml of water in the beaker (4.6). Lay the fusion cup in the same beaker and immediately cover with a watch glass. CAUTION If the bomb is cooled in water, take care that the wate
44、r does not reach the joint between the plug and the bomb. Figure 2 Flask for oxygen combustion with platinum wire attached to stopper (for method B)ENISO4615:1999 4 BSI 04-2000 IMPORTANT WARNING When doubt exists as to whether the reaction has taken place, do not dissolve the contents of the bomb in
45、to water according to the normal procedure because this might lead to a violent explosion. The contents of the bomb should be spread out onto dry sand, after which they should be sprayed with water from a safe distance and then washed with more water. 6.1.2.4 Heat the beaker and its contents to boil
46、ing, then cool. Rinse the crucible and lid, or the fusion cup and head, into the beaker with water, then remove them. 6.1.2.5 Slowly add20ml of the concentrated nitric acid (3.3), stirring constantly, followed by the nitric acid solution (3.2) until the mixture is neutral. Then add an additional2ml
47、of the nitric acid solution(3.2). NOTEMethyl orange is a suitable indicator for the neutralization. 6.1.2.6 Dilute the contents of the beaker to about200ml with water, and determine the chlorine content, by electrometric titration or by the Volhard method, with the silver nitrate solution(3.1). 6.1.
48、3 Blank test Carry out a blank test by firing the same amount of the sodium peroxide (3.4) and starch or sucrose (3.5) as was used with the test portion, and repeating the procedure (but omitting the test portion) specifiedin6.1.2. 6.2 Method B (oxygen flask) 6.2.1 Test portion 6.2.1.1 CASE OF A LIQ
49、UID Cut out30mm 30mm square of adhesive tape(4.9) see Figure 3a). Stick on it a square of filter paper (4.8) with a tail see Figure 3b). Wind it around a glass rod, starting at the side parallel and closer to the tail, so as to form a small cylinder, keeping the filter paper inside see Figure 3c). Close the extremity of the cylinder opposite the tail by flattening and pinching. Weigh the cylinder to the nearest0,0001g. Then deposit the liquid sample of0,025to0,035g through the upper end of the cylinder by
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