DIN EN 16455-2014 Conservation of cultural heritage - Extraction and determination of soluble salts in natural stone and related materials used in and from cultural heritage German.pdf

1、December 2014Translation by DIN-Sprachendienst.English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、 97.195!%Zd“2275565www.din.deDDIN EN 16455Conservation of cultural heritage Extraction and determination of soluble salts in natural stone andrelated materials used in and from cultural heritage;English version EN 16455:2014,English translation of DIN EN 16455:2014-12Erhaltung des kulturellen Erbes

3、Auflsung und Bestimmung von lslichen Salzen in Naturstein und artverwandtenMaterialien des kulturellen Erbes;Englische Fassung EN 16455:2014,Englische bersetzung von DIN EN 16455:2014-12Conservation du patrimoine culturel Extraction et dtermination des sels solubles dans la pierre naturelle et les m

4、atriauxassocis utiliss dans le patrimoine culturel;Version anglaise EN 16455:2014,Traduction anglaise de DIN EN 16455:2014-12www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 11 pages11.14 DIN EN 16455:2014-12 2 A comma is used as the dec

5、imal marker. National foreword This document (EN 16455:2014) has been prepared by Technical Committee CEN/TC 346 “Conservation of cultural heritage” (Secretariat: UNI, Italy). The responsible German body involved in its preparation was the DIN-Normenausschuss Bauwesen (DIN Standards Committee Buildi

6、ng and Civil Engineering), Working Committee NA 005-01-36 AA Erhaltung des kulturellen Erbes (SpA zu CEN/TC 346). The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3310-1 DIN ISO 3310-1 ISO 3310-2 DIN ISO 3310-2 National Annex NA (informa

7、tive) Bibliography DIN ISO 3310-1, Test sieves Technical requirements and testing Part 1: Test sieves of metal wire cloth DIN ISO 3310-2, Test sieves Technical requirements and testing Part 2: Test sieves of perforated plates EN 16455September 2014 ICS 97.195 English Version Conservation of cultural

8、 heritage - Extraction and determination 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

9、Erhaltung des kulturellen Erbes - 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 co

10、nditions 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 CEN-CENELEC Management Centre or to any CEN member. This European Standard exi

11、sts 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 CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national st

12、andards bodies of Austria, Belgium, 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,

13、Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. 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 national Members. Ref. No. EN 16455:2014 EEUROPEAN COMMITTEE FOR STANDARDIZATI

14、ONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 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 Pr

15、ocedure .6 6.1 Sampling .6 6.2 Analysis procedure6 6.2.1 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 DIN EN 16455:2014-12EN 16455:2014 (E) 3 Foreword This do

16、cument (EN 16455:2014) has been prepared by Technical Committee 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 lates

17、t by March 2015 and conflicting national standards shall be withdrawn 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 pa

18、tent rights. According to the CEN-CENELEC Internal Regulations, 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

19、, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16455:2014-12EN 16455:2014 (E) 4 Introduction Soluble salts are oft

20、en present in stones and other porous inorganic building materials 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

21、conservation interventions. Soluble salts present in porous inorganic 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 solubl

22、e salts present in porous inorganic materials to determine the ions 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 identif

23、y the type of anions and cations present in a solution, after dissolution 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 reage

24、nt; d) X-ray diffraction, which provides information on the nature 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 S

25、pectrometry) for cations; f) ion chromatography which makes it possible to identify and quantify separately anions and cations. DIN EN 16455:2014-12EN 16455:2014 (E) 5 1 Scope This European Standard provides a methodology for the qualitative and quantitative analysis of anions and cations obtained b

26、y dissolution of soluble salts present in either natural stone or other 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 thi

27、s standard are: Cl-, NO2-, NO3-, SO42 -, Na+, K+, NH4+, Ca2+, Mg2+2 Normative 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,

28、the latest edition of the referenced document (including any amendments) 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

29、, Test sieves Technical requirements and testing Part 1: Test sieves 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 15898:201

30、1 and EN 16085:2012 and the following apply. 3.1 soluble salts salts 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; i

31、t is highly dependent on the amount of dissolved solids (such as salt) 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

32、e.g. sandstone limestone and marble; as well as artificial materials such as mortar, plaster brick and other materials DIN EN 16455:2014-12EN 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

33、 soluble salts in the sample can be determined by measurement of conductivity 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 th

34、e expected results 5.3 Common laboratory glassware or plasticware 5.4 Pestle 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

35、A balance capable of weighing to 0,01 mg 5.11 A conductivity meter capable 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

36、 all cases the location, the number and the amount of the samples used should 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 sa

37、mple shall be powdered until the powder grain size is less than 0,106 mm (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

38、weights at an interval of (24 2) h is less than 0,1 % of the sub-sample. 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-sa

39、mple has to be weighed with an accuracy of 0,1 mg and transferred quantitatively to a 100,0 mL (V ) volumetric flask. Ultra pure water with known specific DIN EN 16455:2014-12EN 16455:2014 (E) 7 conductivity (b ) has to be added to mark on the volumetric flask. The flask has to be sealed and gently

40、shaken for (24,0 0,2) h at room temperature (25 5) C. NOTE (72,0 0,2) h may be 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 determi

41、ne quantitatively the ions, to estimate the total content of soluble salts1)the 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

42、 calibration of the measurement system a portion of filtrate shall be collected 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 i

43、s the specific conductivity of the pure water (S cm1); 100 is the “reference 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 percen

44、tage mg/mg % of a single anion or cation analysed (Cl-, , Ca2+); C is the concentration 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 o

45、f components which may affect the conductivity. DIN EN 16455:2014-12EN 16455:2014 (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 o

46、f each single ion. 8 Test report The report shall contain the following information: 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;

47、 d) the name and the address of the client (if appropriate); e) the nature of the 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

48、 of detection, and the measurement accuracy; i) the conductivity (S cm1) and the ion content ( meq g); j) the stirring time in hours; k) any deviation from this standard and the reason for such deviation; l) remarks. DIN EN 16455:2014-12EN 16455:2014 (E) 9 Bibliography 1 UNI 11087:2003 Beni culturali - Materiali lapidei naturali ed artificiali - Determinazione del contenuto di sali solubili DIN EN 16455:2014-12