1、BSI Standards PublicationBS EN 16455:2014Conservation of culturalheritage Extraction anddetermination of soluble saltsin natural stone and relatedmaterials used in and fromcultural heritageBS EN 16455:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 16455:20
2、14.The UK participation in its preparation was entrusted to TechnicalCommittee B/560, Conservation of tangible cultural heritage.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions o
3、f a contract. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 79016 4ICS 97.195Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the
4、authority of theStandards Policy and Strategy Committee on 30 September 2014.Amendments issued since publicationDate Text affectedBS EN 16455:2014EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16455 September 2014 ICS 97.195 English Version Conservation of cultural heritage - Extraction and de
5、termination of soluble salts in natural stone and related materials used in and from cultural heritage Conservation du patrimoine culturel - Extraction et dtermination des sels solubles dans la pierre naturelle et les matriaux associs utiliss dans le patrimoine culturel Erhaltung des kulturellen Erb
6、es - Auflsung und Bestimmung von lslichen Salzen in Naturstein und artverwandten Materialien des kulturellen Erbes This European Standard was approved by CEN on 25 July 2014. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Euro
7、pean 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 CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official version
8、s (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 CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Be
9、lgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Swit
10、zerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN nation
11、al Members. Ref. No. EN 16455:2014 EBS EN 16455:2014EN 16455:2014 (E) 2 Contents Page Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Principle 6 5 Reagents, materials and analytical equipment .6 6 Procedure .6 6.1 Sampling .6 6.2 Analysis procedure6 6.2.1
12、General 6 6.2.2 Conductivity measurements .7 6.2.3 Ions measurement .7 7 Expression of results 7 7.1 Specific conductivity, (S cm1) 7 7.2 Individual ions 7 8 Test report 8 Bibliography 9 BS EN 16455:2014EN 16455:2014 (E) 3 Foreword This document (EN 16455:2014) has been prepared by Technical Committ
13、ee CEN/TC 346 “Conservation of cultural heritage”, the secretariat of which is held by UNI. 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 2015 and conflicting national standards shall be w
14、ithdrawn at the latest by March 2015. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulation
15、s, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
16、Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16455:2014EN 16455:2014 (E) 4 Introduction Soluble salts are often present in stones and other porous inorganic building material
17、s as alteration products of chemical or biological origin. They can originate from surface deposition of environmental pollutants or from water capillary transport from other external sources and also from materials themselves or from conservation interventions. Soluble salts present in porous inorg
18、anic materials can, (depending on material properties, environmental conditions or possible treatments the surrounding conditions), initiate physical-chemical degradation processes. This standard describes a procedure to extract soluble salts present in porous inorganic materials to determine the io
19、ns and to estimate the content of soluble salts. There are several test methods for the analysis of salts, for example: a) recognition of salt crystals by microscopy; b) qualitative chemical reactions. These make it possible to identify the type of anions and cations present in a solution, after dis
20、solution of salts in water (i.e. sulphates, nitrates, chlorides); c) semiquantitative tests. These are mostly based on colourimetric reactions that lead to the formation of coloured compounds formed by each anion and its specific reagent; d) X-ray diffraction, which provides information on the natur
21、e of a salt (in crystalline form) identifying the mineralogical composition of a compound; e) spectroscopic techniques like flame photometry, AAS (Atomic Absorption Spectrometry), ICP-AES (Inductively Coupled Plasma - Atomic Emission Spectrometry) for cations; f) ion chromatography which makes it po
22、ssible to identify and quantify separately anions and cations. BS EN 16455:2014EN 16455:2014 (E) 5 1 Scope This European Standard provides a methodology for the qualitative and quantitative analysis of anions and cations obtained by dissolution of soluble salts present in either natural stone or oth
23、er porous inorganic materials constituting cultural heritage and in materials and products used for their conservation. The methodology requires samples to have been taken from the cultural property. The main ions considered in this standard are: Cl-, NO2-, NO3-, SO42 -, Na+, K+, NH4+, Ca2+, Mg2+2 N
24、ormative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendmen
25、ts) applies. EN 15898:2011, Conservation of cultural property Main general terms and definitions EN 16085:2012, Conservation of Cultural property Methodology for sampling from materials of cultural property General rules ISO 3310-1, Test sieves Technical requirements and testing Part 1: Test sieves
26、of metal wire cloth ISO 3310-2, Test sieves Technical requirements and testing Part 2: Test sieves of perforated metal plate 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 15898:2011 and EN 16085:2012 and the following apply. 3.1 soluble salts salts
27、that readily dissolve in a solvent such as water in order to form a solution; the solubility is dependent on the salt and the temperature of water 3.2 conductivity measure of the ability of water to conduct an electrical current; it is highly dependent on the amount of dissolved solids (such as salt
28、) in the water 3.3 specific conductivity conductivity of a solution measured between two electrodes 1 cm2in area and 1 cm apart Note 1 to entry: The units are 1S cm . 3.4 porous inorganic material material including natural stones e.g. sandstone limestone and marble; as well as artificial materials
29、such as mortar, plaster brick and other materials BS EN 16455:2014EN 16455:2014 (E) 6 4 Principle Soluble salts are extracted from a powdered solid sub-sample by dissolution in a fixed volume of ultra-pure water. The content of soluble salts in the sample can be determined by measurement of conducti
30、vity and qualitative and quantitative ion analysis after filtration. 5 Reagents, materials and analytical equipment 5.1 Ultra pure water (specific conductivity 1 Scm1) 5.2 Anion and cation reference solutions in the range of the expected results 5.3 Common laboratory glassware or plasticware 5.4 Pes
31、tle and agate mortar 5.5 Series of sieves in accordance with ISO 3310-1 or ISO 3310-2 5.6 0,45m filter 5.7 Magnetic stirrer 5.8 Flask shaker 5.9 Temperature controlled oven capable of maintaining a temperature at (50 5) C 5.10 A balance capable of weighing to 0,01 mg 5.11 A conductivity meter capabl
32、e of measuring to 1 Scm15.12 Instrument for the analysis of anions and cations NOTE Ion Chromatography is the most widely applied technique. 6 Procedure 6.1 Sampling General rules for sampling are described in EN 16085:2012. In all cases the location, the number and the amount of the samples used sh
33、ould be documented in the final report. During the sampling, environmental temperature (C) and relative humidity (%) shall be measured. 6.2 Analysis procedure 6.2.1 General An appropriate amount (at least 100 mg 5 mg) of the sample shall be powdered until the powder grain size is less than 0,106 mm
34、(140 mesh). The powdered sub-sample has to be dried in an oven at a temperature of (50 5) C for (24 1) h or until a constant mass has been reached. Constant mass is assumed to have been attained when the difference between two weights at an interval of (24 2) h is less than 0,1 % of the sub-sample.
35、In a few cases, the available amount may not be sufficient to allow a correct quantification. The concentrations will be considered as a semiquantitative evaluation. An amount, ( P ), (100 5) mg of the powdered and dried sub-sample has to be weighed with an accuracy of 0,1 mg and transferred quantit
36、atively to a 100,0 mL (V ) volumetric flask. Ultra pure water with known specific BS EN 16455:2014EN 16455:2014 (E) 7 conductivity (b ) has to be added to mark on the volumetric flask. The flask has to be sealed and gently shaken for (24,0 0,2) h at room temperature (25 5) C. NOTE (72,0 0,2) h may b
37、e required for complete or near complete of some soluble salts. The resulting mixture shall be allowed to stand (minimum 2 h) until the insoluble material settles. 6.2.2 Conductivity measurements Prior to proceed to determine quantitatively the ions, to estimate the total content of soluble salts1)t
38、he specific conductivity of the clear solution (a ) shall be measured and compared with the conductivity of ultra pure water (b). 6.2.3 Ions measurement The solution from 6.2 is then filtered using a 0,45m filter, and after calibration of the measurement system a portion of filtrate shall be collect
39、ed and used to determine the concentration (C), in mg/L, of each individual ion. 7 Expression of results 7.1 Specific conductivity, (S cm1) ( )Pba100= where a is the specific conductivity of the sample solution (S cm1); b is the specific conductivity of the pure water (S cm1); 100 is the “reference
40、mass” of 100 mg; P is the actual mass of the solid powdered sample (mg). 7.2 Individual ions Results of the ions shall be recorded as: Percentage of the dry mass of the sample, %I ( ) 1001% =PFVCI where I is the mass percentage mg/mg % of a single anion or cation analysed (Cl-, , Ca2+); C is the con
41、centration in mg/L of a single ion in solution; 1) In the case of mortar samples and certain types of stone, e.g. gypsum rock, the results are not always reliable because of the possible dissolution or partial dissolution of components which may affect the conductivity. BS EN 16455:2014EN 16455:2014
42、 (E) 8 V is the water extraction volume (100 ml); F is factor for conversion from ml to L, F = 1 000 ml/L; P is the actual mass of the solid powdered sample (mg). ( )% 11000100Iew=meqgwhere ew is the equivalent weight of each single ion. 8 Test report The report shall contain the following informati
43、on: a) unique identification number of the report; b) the name, number, and date of issue of this European Standard; c) the name and address of the laboratory and the address where the test was carried out if different; d) the name and the address of the client (if appropriate); e) the nature of the
44、 sample, e.g. solid, powder, etc.; f) the date of delivery of the sample or of the specimens; g) the date when the specimens were prepared (if relevant) and the date of testing; h) the analytical method used, the limits of detection, and the measurement accuracy; i) the conductivity (S cm1) and the
45、ion content ( meq g); j) the stirring time in hours; k) any deviation from this standard and the reason for such deviation; l) remarks. BS EN 16455:2014EN 16455:2014 (E) 9 Bibliography 1 UNI 11087:2003 Beni culturali - Materiali lapidei naturali ed artificiali - Determinazione del contenuto di sali
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