1、BRITISH STANDARD Thermal insulating products for building equipment and industrial installations - Determination of trace quantities of water soluble chloride, fluoride, silicate, sodium ions and pH The European Standard EN 13468:2001 has the status of a British Standard ICs 91.120.10; 91.100.60 BS
2、EN 13468:2001 NO COPYING WITHOUT BI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BS EN 13468:ZOOl Amd. No. Date National foreword Comments This British Standard is the official English language version of EN 13468:2001. This British Standard, together with BS EN 13467:2001, BS EN 13469:2001, BS E
3、N 13470:2001, BS EN 13471:2001 and BS EN 13472:2001, partially supersedes BS 29721989. The UK participation in its preparation was entrusted by Technical Committee RHE29, Thermal insulating materials, to Subcommittee RHE/9/4, Nomenclature and specifications, which has the responsibility to: - - aid
4、enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, 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 represente
5、d on this subcommittee 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 Correspondenc
6、e 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 responsible for their correct application. Compliance with a British Standard does not of its
7、elf confer immunity from legal obligations. This British Standard, having been prepared under the direction of the Engineering Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on O9 November 2001 Summary of pages This document com
8、prises a front cover, an inside front cover, the EN title page, pages 2 to 17 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication 0 BSI O9 November 2001 ISBN O 580 38620 i EUROPEAN STANDARD NORME EUROPEN
9、NE EUROPISCHE NORM EN 13468 September 2001 ICs 91.100.60 English version Thermal insulating products for building equipment and industrial installations - Determination of trace quantities of water soluble chloride, fluoride, silicate, sodium ions and pH Produits isolants thermiques pour lquipement
10、du btiment et les installations industrielles - Dtermination des faibles quantits dions chlorure, fluorure, silicate et sodium solubles dans leau et mesure du pH Wnnedmmstoffe fr die Haustechnik und fr betriebstechnische Anlagen - Bestimmung des Gehalts von wasserlslichen Chlorid-. Fluorid-, Silikat
11、- und Natrium- Ionen und des pH-Wertes This European Standard was approved by CEN on 18 August 2001. CEN members are bound to comply with the CENICENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up
12、to-date lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under
13、the responsibility of a CEN member into its own language and notified to the Management Centre 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, Ireland, Italy, Luxembou
14、rg, Netherlands, Noway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMTTEE FOR STANDARDIZATION COMITE EUROPEEN DE NORMALISATION EUROPISCHES KOMITEE FUR NORMUNG Management Centre: rue de Stassart, 36 6-1050 Brussels O 2001 CEN All rights of exploitation in any form and by any
15、means reserved worldwide for CEN national Members. Ref. No. EN 13468:2001 E EN 13468:2001 (E) Contents Page Foreword . 3 1 Scope 4 2 Normative references 4 3 Terms and definitions . 4 4 principle . 4 5 Apparatus . 4 6 Test specimens 5 Calculation and expression of results 9 7 Procedure . 6 8 9 1 O A
16、ccuracy of measurement . 11 Test report 11 Annex A (normative) Spectrophotometric determination of fluoride with zirconium-SPADNS . 13 Annex B (informative) General information related to the use of this standard . 14 Annex C (informative) Example of ion chromatography equipment . 15 Annex D (inform
17、ative) Example of borosilicate glass equipment to prepare leaching solutions for thermal insulating products that float 16 Tables Table 1 -Test temperature and leaching time . 6 Table 2 - 95 % Confidence interval values 11 Table 3 - Trueness . 1 2 . EN 13468:2001 (E) Foreword This European Standard
18、has been prepared by Technical Committee CEN/TC 88 “Thermal insulating materials and products“, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by March 2002,
19、 and conflicting national standards shall be withdrawn at the latest by March 2002. This European Standard is one of a series of standards which specify test methods for determining dimensions and properties of thermal insulating materials and products. It supports a series of product standards for
20、thermal insulating materials and products which derive from the Council Directive of 21 December 1988 on the approximation of laws, regulations and administrative provisions of the Member States relating to construction products (Directive 89/1 OG/EEC) through the consideration of the essential requ
21、irements. This standard contains the following normative annex: Annex A - Spectrophotometric fluoride determination of Fluoride with zirconium-SPADNS and three informative annexes: Annex B - General information related to the use of this standard Annex C - Example of ion chromatography equipment Ann
22、ex D - Example of borosilicate glass equipment for preparation of leaching solutions for thermal insulating products that float This European Standard has been prepared for products used to insulate building equipment and industrial installations, but it may also be applied to products used in other
23、 areas. No existing European Standard is superseded. This European Standard has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and supports essential requirements of EU Directive(s). According to the CENKENELEC Internal Regulations, the
24、 national standards 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, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingd
25、om. 3 EN 13468:2001 (E) i Scope This standard specifies the equipment and procedures for determining trace quantities of the water soluble chloride, fluoride, silicate and sodium ions in an aqueous extract of the product. It also describes a procedure for the determination of the pH of the aqueous e
26、xtract. The standard is applicable to thermal insulating products. NOTE The determination of these parameters may be relevant for thermal insulating products intended for application to stainless austenitic steel surfaces. The presence of chloride, fluoride, silicate and sodium ions under certain co
27、nditions may influence the risk of stress corrosion cracking. See informative annex 6 for further information. 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
28、 in the text, and the publications are listed hereafter. For 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. The latest edition of this undated reference applies (including ame
29、ndments). IS0 1 O1 36-1, Glass and Glassware - Analyses of extract solutions - Pari 1: Determination of silicon dioxide by molecular absorption spectrometry. IS0 1 O1 36-2, Glass and Glassware - Analyses of extract solutions - Pari 2: Determination of sodium oxide and potassium oxide by flame spectr
30、ometric methods. 3 Terms and definitions This European Standard contains no terms and definitions. 4 Principie Test specimens of the insulating product are boiled or heated in deionized water to leach out soluble ions. Tests to determine water soluble chloride, fluoride, silicate and sodium ions are
31、 performed on aliquots of the filtered aqueous extract. A pH value is determined on one of the aliquots. 5 Apparatus All equipment and working instruments used for this purpose must be free from soluble chloride, fluoride, silicate, sodium ions, and grease. Chloride free solvents shall be used to cl
32、ean equipment and working instruments (avoid chlorinated solvents). During the performance of the analytic procedure extraneous sources of these ions shall be reduced or eliminated. 5.1 Preparation of aqueous extract 5.1 .I 1 O00 ml borosilicate glass flask; 5.1.2 Water condenser; 5.1.3 Heater, comp
33、lying with the requirements of 7.2; 5.1.4 Prewashed filter, diameter of pores 0.45 pm; 5.1.5 Cork borer having a diameter which enables to take the specified mass for the test specimen; 5.1.6 Disposable gloves; 4 5.1.7 Plastic bag or container; 5.1.8 Balance, permitting reading to I 0,Ol g. 5.2 Anal
34、yses 5.2.1 Ion Chromatography equipment (IC). See informative annex C for example of suitable equipment; 5.2.2 Titration equipment with automatic end point; 5.2.3 Atomic Absorption Spectrophotometer (AAS): 5.2.4 Atomic Emission Spectrometer with Inductively Coupled Plasma (ICP-AES); 5.2.5 Spectropho
35、tometer; 5.2.6 pH meterlmillivolt meter; 5.2.7 Fluoride ion selective electrode. NOTE Any device providing the same result with at least the same accuracy may be used. 5.3 Materials 5.3.1 deionized water, conductivity less than 03 pS/cm; 5.3.2 0,Ol N sodium cloride (NaCI); 5.3.3 0,Ol N silver nitrat
36、e (ASNO3); 6 Test specimens 6.1 General To ensure that the results are representative of the product care shall be taken that the test specimens are not subjected to any outside contamination. 6.2 Dimensions of test specimens Take out each test specimen by using a cork borer at positions evenly dist
37、ributed over the total surface of a full size product. To avoid contamination chloride-free gloves must be worn and the test specimen is placed in a closed polyethylene bag. Depending on the product family the weight of each test specimen shall be at least 7,5 g or 20 g. 6.3 Number of test specimens
38、 The number of test specimens shall be as specified in the relevant product standard. If the number is not specified, then at least three test specimens (3 weights of 7,5 g or 20 g) shall be used. NOTE In the absence of a product standard or any other European technical specification the number of t
39、he test specimens may be agreed between parties. 6.4 Conditioning of test specimens The test specimens shall be stored for at least 6 h and not more than 24 h at (23 15) OC. In case of dis- pute they shall be stored at (23 k 2) OC for the time stated in the relevant product standard. 5 EN 13468:2001
40、 (E) Maximum service temperature Test temperature “C “C 1100 (100 * 1) 7 Procedure Leaching time h O, 5 7.1 Test conditions I 70 The test shall be carried out at (23 k 5) “C 7.2 Test procedure (60 f 1) I 8,O 7.2.1 Preparation of the leaching solution Take (20 f 0,l) g or (73 f 0.05) g of the test sp
41、ecimen (m), as specified in the relevant product standard and place it in the wide-mouth glass flask. Add (400 f 5) ml deionized water (V). The flask shall be closed with a ground-in stopper and shaken until the test specimen is completely wetted and submerged. If the test specimen floats it should
42、be held under water (example, see informative annex D. Fix the water condenser to the flask and electrically heat for 5 min to 10 min until the leaching solution has reached the test temperature. The leaching process shall be continued, under reflux conditions, for the specified time. Depending on t
43、he maximum service temperature specified for the product the test temperature and leaching time shall be chosen as specified in Table 1. I 2 90 to 100 I (90 * 1) I I 280to 90 I (80 f 1) I 28 l 40 270toc 80 (70 t 1) Make a “blank“ test, using the same procedure as above, but without a test specimen o
44、f insulating product. The filtered solutions will subsequently be used for the analyses. NOTE Other test methods than decribed below may be used if the same result with at least the same accuracy is obtained. 7.2.2 Chloride determination 7.2.2.1 General One of the following methods shall be used on
45、a fresh aliquot of the filtered solution. In case of dispute the method decribed in 7.2.2.2 is the reference method. The repeatability of the methods is calculated as the standard deviation on 10 determinations taken from the same leaching solution. The standard deviation shall be smaller than 0,5 m
46、glkg for concentrations smaller than 8,3 mg/kg and smaller than 6 % of the mean of the 10 determinations for concentrations larger than or equal to 8,3 mglkg. 6 EN 13468:2001 (E) 7.2.2.2 Ion-chromatographic determination (IC) The ion-chromatographic determination of chloride-ions shall be carried ou
47、t in accordance with the equipment manufacturers operating instruction. 5 ml of the filtered solution is injected into the test loop through a disposable, chloridefree filter. The volume of the test loop of the IC-apparatus is chosen (normally 50 pl). NOTE Depending on the kind of binding and/or wat
48、erproofing agent, mineral wool products may release organic contaminants during the boiling process which may cause peaks that are close to the chloride peaks in the ion- chromatogramme. A clear separation of test peaks shall be obtained during the IC determination. 7.2.2.3 AgN03 titration The deter
49、mination of chloride ions by polarization titration shall be according to the alternating current vol- tage method with amperometric indication. Precautions shall be taken to avoid interference from other ions, e.g. fluoride. The following procedure shall be carried out on aliquots of the filtered solution (minimum 200 ml, V,) from the tested product and the blank. Where necessary to remove organic contaminents Iml to 2 ml HNOS (65 % “O3, diluted 1:l) and 0,5 g of fine activated carbon shall be added to the solution before filtering through a prewashed filter. For cellular g
