SIST EN 13468:2002

SLOVENSKI STANDARD
SIST EN 13468:2002
01-marec-2002
Toplotnoizolacijski proizvodi za opremo stavb in industrijske inštalacije –
Ugotavljanje sledi vodotopnih klorovih, fluorovih, silikatnih in natrijevih ionov ter
pH vrednosti
Thermal insulating products for building equipment and industrial installations -
Determination of trace quantities of water soluble chloride, fluoride, silicate, sodium ions
and pH
Wärmedämmstoffe für die Haustechnik und für betriebstechnische Anlagen -
Bestimmung des Gehalts von wasserlöslichen Chlorid-, Fluorid-, Silikat- und Natrium-
Ionen und des pH-Wertes
Produits isolants thermiques pour l'équipement du bâtiment et les installations
industrielles - Détermination des faibles quantités d'ions chlorure, fluorure, silicate et
sodium solubles dans l'eau et mesure du pH
Ta slovenski standard je istoveten z: EN 13468:2001
ICS:
91.100.60 0DWHULDOL]DWRSORWQRLQ Thermal and sound insulating
]YRþQRL]RODFLMR materials
SIST EN 13468:2002 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 13468:2002

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SIST EN 13468:2002
EUROPEAN STANDARD
EN 13468
NORME EUROPÉENNE
EUROPÄISCHE NORM
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 l'équipement du bâtiment Wärmedämmstoffe für die Haustechnik und für
et les installations industrielles - Détermination des faibles betriebstechnische Anlagen - Bestimmung des Gehalts von
quantités d'ions chlorure, fluorure, silicate et sodium wasserlöslichen Chlorid-, Fluorid-, Silikat- und Natrium-
solubles dans l'eau et mesure du pH Ionen und des pH-Wertes
This European Standard was approved by CEN on 18 August 2001.
CEN members are bound to comply with the CEN/CENELEC 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 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 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, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2001 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 13468:2001 E
worldwide for CEN national Members.

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SIST EN 13468:2002
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
7 Procedure.6
8 Calculation and expression of results .9
9 Accuracy of measurement .11
10 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 (informative) 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 .11
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SIST EN 13468:2002
EN 13468:2001 (E)
Foreword
This European Standard 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, 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 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 89/106/EEC) through the consideration of the essential
requirements.
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
Annex 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 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 CEN/CENELEC Internal Regulations, the 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 Kingdom.
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SIST EN 13468:2002
EN 13468:2001 (E)
1 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 extract. 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 conditions may influence the risk of stress corrosion cracking. See informative annex B 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 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 amendments).
ISO 10136-1, Glass and Glassware - Analyses of extract solutions – Part 1: Determination of silicon
dioxide by molecular absorption spectrometry.
ISO 10136-2, Glass and Glassware - Analyses of extract solutions – Part 2: Determination of sodium
oxide and potassium oxide by flame spectrometric methods.
3 Terms and definitions
This European Standard contains no terms and definitions.
4 Principle
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 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 clean 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
5.1.1 1000 ml borosilicate glass flask;
5.1.2 Water condenser;
5.1.3 Heater, complying with the requirements of 7.2;
5.1.4 Prewashed filter, diameter of pores 0,45 m;
5.1.5 Cork borer having a diameter which enables to take the specified mass for the test specimen;
5.1.6 Disposable gloves;
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SIST EN 13468:2002
EN 13468:2001 (E)
5.1.7 Plastic bag or container;
5.1.8 Balance, permitting reading to ± 0,01 g.
5.2 Analyses
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 Spectrophotometer;
5.2.6 pH meter/millivolt 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 0,5 S/cm;
5.3.2 0,01 N sodium cloride (NaCl);
5.3.3 0,01 N silver nitrate (AgNO );
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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 distributed 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
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 the 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 ± 5) C. In case of dis-
pute they shall be stored at (23 ± 2) C for the time stated in the relevant product standard.
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SIST EN 13468:2002
EN 13468:2001 (E)
7 Procedure
7.1 Test conditions
The test shall be carried out at (23 ± 5) C.
7.2 Test procedure
7.2.1 Preparation of the leaching solution
Take (20 ± 0,1) g or (7,5 ± 0,05) g of the test specimen (m), as specified in the relevant product standard
and place it in the wide-mouth glass flask. Add (400 ± 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 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 the maximum service temperature specified for the product the test temperature and
leaching time shall be chosen as specified in Table 1.
Table 1 - Test temperature and leaching time
Maximum service temperature Test temperature
Leaching time
C C h
(100 ± 1) 0,5
100
(90 ± 1) 1,0
 90 to < 100
 80 to < 90 (80 ± 1) 2,0
(70 ± 1) 4,0
 70 to < 80
< 70 (60 ± 1) 8,0
Remove the flask with the condenser, from the heat and cool for 10 min to 15 min until the temperature
reaches room temperature, e.g. in a water bath. Filter the leaching solution.
Make a "blank" test, using the same procedure as above, but without a test specimen of 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 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 mg/kg 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 mg/kg.
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SIST EN 13468:2002
EN 13468:2001 (E)
7.2.2.2 Ion-chromatographic determination (IC)
The ion-chromatographic determination of chloride-ions shall be carried out in accordance with the
equipment manufacturer's operating instruction.
5 ml of the filtered solution is injected into the test loop through a disposable, chloridefree filter. The
volume of the te
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