SIST EN 14385:2004
(Main)Stationary source emissions - Determination of the total emission of As, Cd, Cr, Co, Cu, Mn, Ni, Pb, Sb, TI and V
Stationary source emissions - Determination of the total emission of As, Cd, Cr, Co, Cu, Mn, Ni, Pb, Sb, TI and V
This European Standard specifies a manual reference method for the determination of the mass concentration of specific elements in exhaust gases from hazardous waste incinerators. The method is applicable to each of the specific elements in the concentration range of 0,005 mg/m3 to 0,5 mg/m3. Unless otherwise stated, gas volumes are expressed at dry conditions, normalised to 273 K and oxygen content 101,3 kPa, and normalized to a dry oxygen content of 11 % on the volume/volume basis.
Specific elements according to this European standard are antimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), lead (Pb), manganese (Mn), nickel (Ni), thallium (Tl), and vanadium (V).
This European standard is validated for the determination of the mass concentration of specific ele-ments in incineration exhaust gases with the composition given in Table 1.
This European standard is also applicable for exhaust gases from other sources with a similar flue gas composition.
Emissionen aus stationären Quellen - Bestimmung der Gesamtemission von As, Cd, Cr, Co, Cu, Mn, Ni, Pb, TI und V
Diese Europäische Norm legt ein manuelles Referenzmessverfahren zur Bestimmung der Massenkonzentration der zu bestimmenden Elemente im Abgas von Sondermüll- und Müllverbrennungsanlagen fest [1]. Das Verfahren ist für jedes der zu bestimmenden Elemente im Konzentrationsbereich von 0,005 mg/m3 bis 0,5 mg/m3 anwendbar. Sofern nicht anders beschrieben, werden die Konzentrationen, bezogen auf trockenes Abgas, Normbedingungen (273 K, 101,3 kPa) und auf 11 % Sauerstoff (Volumenanteil) angegeben.
Die zu bestimmenden Elemente nach dieser Europäischen Norm sind: Antimon (Sb), Arsen (As), Cadmium (Cd), Chrom (Cr), Kobalt (Co), Kupfer (Cu), Blei (Pb), Mangan (Mn), Nickel (Ni), Thallium (Tl) und Vanadium (V).
Diese Europäische Norm ist auch für die Messung von Abgasen bei anderen Anlagen mit einer Abgaszusammensetzung, ähnlich wie sie in Tabelle 1 gegeben ist, anwendbar. Die für Müllverbrennungsanlagen ermittelten Verfahrenskenngrößen können nicht für die Anwendung bei anderen Matrixgegebenheiten ohne zusätzliche Validierungsmessungen extrapoliert werden.
ANMERKUNG Diese Europäische Norm wurde mit den beschriebenen Materialien und Ausrüstungen sowie den dargelegten Probenahme- und Aufschlussverfahren usw. und den anschließend durchgeführten AAS- und ICP-Analysen validiert. Dies schließt nicht die Verwendung anderer Geräte/Vorgehensweisen aus, die die Anforderungen erfüllen und bewiesener Maßen äquivalent zu den beschriebenen Vorgehensweisen in dieser Europäischer Norm sind.
Diese Europäische Norm wurde zur Bestimmung der Massenkonzentrationen von Metallen und Metalloiden in Abgasen von Verbrennungsanlagen mit den in Abschnitt 9 genannten Unsicherheiten validiert.
Falls Quecksilber ebenfalls mit bestimmt werden soll, so kann dies durch die Probenahme im Teilstromverfahren erfolgen (EN13211).
Emissions de sources fixes - Détermination de l'émission totale de As, Cd, Cr, Co, Cu, Mn, Ni, Pb, Sb, TI et V
La présente Norme européenne spécifie une méthode manuelle de référence pour la détermination de la concentration massique d'éléments spécifiques dans les effluents gazeux des incinérateurs municipaux de déchets dangereux [1]. Cette méthode est applicable a chacun de ces éléments dans la plage de concentration comprise entre 0,005 mg/m3 et 0,5 mg/m3. Sauf indication contraire, les concentrations sont exprimées sur sec, dans les conditions normales de température 273 K et de pression 101,3 kPa. pour une teneur en oxygene de 11 % (v/v).
Les éléments spécifiques considérés dans la présente Norme sont l'antimoine (Sb), l'arsenic (As), le cadmium (Cd), le chrome (Cr), le cobalt (Co), le cuivre (Cu), le plomb (Pb), le manganese (Mn), le nickel (Ni), le thallium (TI) et le vanadium (V).
La présente Norme européenne est également applicable aux effluents gazeux provenant d'autres sources de composition similaire tels que ceux figurant dans le tableau 1. Les caractéristiques de performance de la méthode déterminées pour les incinérateurs de déchets ne peuvent pas etre extrapolées a d'autres types de matrices sans que des essais de validation complémentaires n'aient été effectués.
NOTE La présente Norme européenne a été validée sur la base des performances des matériels, équipement, du prélevement et de la minéralisation décrits, etc. suivis des analyses par AAS et ICP. Ceci n'exclut par l'utilisation d'autres types de matériel qui répondent aux exigences fixées dans cette Norme européenne et dont l'équivalence a été prouvée.
La présente Norme européenne a été validée pour la détermination de la concentration massique des métaux dans les effluents gazeux d'incinération, avec les incertitudes décrites a l'article 9.
Si le mercure doit également etre déterminé, il est possible d'effectuer le prélevement a l'aide de la ligne de dérivation du systeme de prélevement (EN 13211).
Emisije nepremičnih virov – Določevanje celotne emisije As, Cd, Cr, Co, Cu, Mn, Ni, Pb, Sb, TI in V
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Emissionen aus stationären Quellen - Bestimmung der Gesamtemission von As, Cd, Cr, Co, Cu, Mn, Ni, Pb, TI und VEmissions de sources fixes - Détermination de l'émission totale de As, Cd, Cr, Co, Cu, Mn, Ni, Pb, Sb, TI et VStationary source emissions - Determination of the total emission of As, Cd, Cr, Co, Cu, Mn, Ni, Pb, Sb, TI and V13.040.40Stationary source emissionsICS:Ta slovenski standard je istoveten z:EN 14385:2004SIST EN 14385:2004en,fr,de01-junij-2004SIST EN 14385:2004SLOVENSKI
STANDARD
SIST EN 14385:2004
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14385February 2004ICS 13.040.40English versionStationary source emissions - Determination of the totalemission of As, Cd, Cr, Co, Cu, Mn, Ni, Pb, Sb, TI and VEmissions de sources fixes - Détermination de l'émissiontotale de As, Cd, Cr, Co, Cu, Mn, Ni, Pb, TI et VEmissionen aus stationären Quellen - Bestimmung derGesamtemission von As, Cd, Cr, Co, Cu, Mn, Ni, Pb, TIund VThis European Standard was approved by CEN on 2 July 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2004 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14385:2004: ESIST EN 14385:2004
EN 14385:2004 (E)2ContentspageForeword.3Introduction.41Scope.52Normative references.63Terms and definitions, symbols and abbreviations.64Principle.85Apparatus, chemicals and gases.96Sampling equipment.127Cleaning of the sampling equipment prior to sampling.138Procedure.149Expression of results.2310Test report.26Annex A (informative)
Examples of absorption vessels.27Annex B (informative)
Types of isokinetic equipment.29Annex C (informative)
Pre-cleaning procedures of the sampling equipment at the laboratory anddetermination of the absorption efficiency.30Annex D (informative)
Measurement results of two field tests.33Annex E (informative)
Pre-tests for the determination of the efficiency, of the digestion and of theperformance of the analytical procedures.36Annex ZA (informative)
Relationship with EU Directives.39Bibliography.40SIST EN 14385:2004
EN 14385:2004 (E)3ForewordThis document (EN 14385:2004) has been prepared by Technical Committee CEN/TC 264 “Air quality”, thesecretariat 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 orby endorsement, at the latest by August 2004, and conflicting national standards shall be withdrawn at the latest byAugust 2004.This document has been prepared under a mandate given to CEN by the European Commission and the EuropeanFree Trade Association, and supports essential requirements of EU Directives.For relationship with EU Directives, see informative Annex ZA, which is an integral part of this document.In this European Standard the Annexes A to E are informative.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark,Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.SIST EN 14385:2004
EN 14385:2004 (E)4IntroductionThis European Standard specifies a method for the determination of the total mass concentration of specificelements in flue gases of waste incinerators. During the establishment of this European Standard field tests wereperformed in order to determine some performance characteristics. These tests showed that in the “gaseous”phase most of the elements can not be determined quantitatively in the absorption solutions. Therefore, the resultsof this method are expressed as the total element mass concentrations (i.e. sum of gaseous, dissolved in droplets,solid and adsorbed on particles). This means that when the specific elements are mainly in the solid phase nosignificant losses (biases) should occur due to the poor absorption efficiency for the elements in the gaseousphase. The quality check requirement for approval of the results is the mass in the last absorber expressed as aminimum percentage of the total mass; this minimum is set at a rather high level, based on the experiences of theabsorption efficiencies in the field tests.When this European Standard is applied for conditions that are different from those investigated during the fieldtests at municipal waste incinerators, the results may not be the same as experienced during these field testsdescribed.SIST EN 14385:2004
EN 14385:2004 (E)51 ScopeThis European Standard specifies a manual reference method for the determination of the mass concentration ofspecific elements in exhaust gases from hazardous and municipal waste incinerators [1]. The method is applicableto each of the specific elements in the concentration range of 0,005 mg/m3 to 0,5 mg/m3. Unless otherwise stated,concentrations are expressed at volumes under dry conditions, normalised to 273 K, 101,3 kPa, and oxygencontent with a volume fraction of 11 %.Specific elements according to this European standard are antimony (Sb), arsenic (As), cadmium (Cd), chromium(Cr), cobalt (Co), copper (Cu), lead (Pb), manganese (Mn), nickel (Ni), thallium (Tl), and vanadium (V).This European Standard is also applicable for exhaust gases from other sources with a flue gas composition,similar to that given in Table 1. The performance characteristics of the method determined for waste incinceratorscannot be extrapolated to be used for other types of matrix without any further validation work.NOTEThis European Standard has been validated with the described materials, equipment, sampling and digestionperformances etc., followed by analyses with AAS and ICP. This does not exclude the use of other types that meet therequirements and proven to be equivalent to the described European Standard.This European Standard has been validated for the determination of the mass concentration of metals inincineration exhaust gases, within the uncertainties stated in clause 9.If mercury is to be determined as well, this may be sampled in a side stream arrangement of the sampling train(EN 13211).Table 1 — Exhaust gas matrixParameterto bedeterminedMass concentration rangetotalsuspendedmatter0 mg/m3to20 mg/m3TOCa)0 mg/m3to20 mg/m3HCl0 mg/m3to20 mg/m3HF0 mg/m3to2 mg/m3SO20 mg/m3to100 mg/m3CO0 mg/m3to250 mg/m3NOx as NO20 mg/m3to500 mg/m3Volume fraction rangeCO23 %to15 % (dry, actual)H2O (ga)10 %to35 % (actual)O23 %to17 % (dry, actual)Temperature60 °Cto200 °Ca)total organic carbonSIST EN 14385:2004
EN 14385:2004 (E)62 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text, and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).EN 13284-1:2001, Stationary source emissions – Determination of low range mass concentration of dust – Part 1:Manual gravimetric methodEN 13211:2001, Air quality – Stationary source emissions – Manual method of determination of the concentrationof total mercuryISO 5725-2, Accuracy (trueness and precision) of measurement methods and results - Part 2 : Basic method forthe determination of repeatability and reproducibility of a standard measurement method3 Terms and definitions, symbols and abbreviations3.1 Terms and definitionsFor the purposes of this European Standard, the following terms and definitions apply.3.1.1 absorbera device in which specific elements are absorbed into an absorption liquid3.1.2 chemical blanka solution used to check the purity of the chemicals employed by the laboratoryNOTEThe chemical blank value is determined by analysing the chemical blank solution (produced as described in 5.2.10)for the specific elements. This chemical blank is to be used as blank for all digestions using acids from one and the same batch.Furthermore, this chemical blank should be used for dilution of laboratory standards.3.1.3 filter blankthe filter blank value is determined for each specific element by treatment and analysis of an unused filter whichhas been taken from the same batch as the sample filters. The treatment of the filter blank is specified in 8.7.3. Thefilter blank gives the blank values for the filter and treatment only. This value may be subtracted from the analyticalvalue. The filter blank is not the same as the field blank (see 8.5)3.1.4 field blanksamples of filter, absorption and rinsing solutions taken at sites without sampling gas and analysed as a normalsample (explanation see 8.5)In every campaign of sampling, at least one sampling blank should be taken at each duct or chimney wheresampling is to be carried out.3.1.5 filtered materialmaterials collected on the filter3.1.6 filter passing materialcomponents passing the filter and recovered in the rest of the absorbing systemSIST EN 14385:2004
EN 14385:2004 (E)73.1.7 fritted gas distributora part of the absorber where the gas stream is distributed into the absorption liquid3.1.8 representative samplingsampling as stated in EN 13284-1:20013.1.9 specific elementsAntimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), lead (Pb), manganese (Mn),nickel (Ni), thallium (Tl), vanadium (V) and their compounds3.1.10 total specific elementssum of all specific elements of 3.1.9 apart from Cd and Tl contained in the exhaust gas, i.e. the sum of the filteredand filter passing parts of these elements3.1.11 sampling campaignsampling at one duct or location during one site visit3.2 Symbols3.2.1 ACross section area, in square metres (m²)3.2.2 QFlow rate of the sampled gas, in cubic metres per hour or litres per minute (m³/h or l/min)3.2.3 TTemperature, in Kelvin (K)3.2.4 VGas volume dry at standard conditions, in cubic metres or litres (m³ or l)3.2.5 LLeakage rate (volume ratio)3.2.6 OOxygen volume content of the flue gas, in percentage (%)3.2.7 mMass, in milligrams (mg)3.2.8 nNumber of absorption vessels3.2.9 pPressure, in kilopascals (kPa)3.2.10 Mass concentration, e.g. in milligrams per cubic metre (mg/m³); grams per litre (g/l)3.2.11 cMass concentration, in grams per litre (g/l)3.2.12 Absorption efficiency3.2.13 w Mass fraction in percent (%)3.2.14
r420Density, in kilograms per litre (kg/l) at 20 °C related to the water of 4 °C3.2.15 Specific conductivity, in micro-Siemens per metre
(µSm-1)3.2.16 Specific resistance, in mega-Ohm and metre (MSIST EN 14385:2004
EN 14385:2004 (E)83.3 Abbreviations3.3.1 CRMCertified reference material3.3.2 ElSpecific element3.3.3 FEPPolyperfluoroethene / -propene3.3.4 PEPolyethene3.3.5 PFAPerfluoroalkoxy compounds3.3.6 PPPolypropene3.3.7 PTFEPolytetrafluoroethene3.3.8 ambAmbient; index3.3.9 gasGaseous; index3.3.10 mainMain stream; index3.3.11 sideSide stream; index3.3.12 mesDry, temperature, pressure at measuring conditions; index3.3.13 bHumidity, pressure, temperature at measuring conditions; index3.3.14 fWet at standard conditions; index3.3.15 solParticle bound; index3.3.16 normNormalized to a dry oxygen content of 11 % (volume fraction); index3.3.17 perPermitted; index3.3.18 obsObserved; index3.3.19 intInternal; index3.3.20 0Temperature at standard condition of 273 K, pressure at standard condition of 101,3 kPa, dry volume at273 K and 101,3 kPa; index4 PrincipleA known volume of flue gas is extracted isokinetically and representatively from a duct or chimney during a certainperiod of time at a controlled flow rate following EN 13284-1:2001. The dust in the sampled gas volume is collectedon a filter. Thereafter, the gas stream is passed through a series of absorbers containing absorption solutions andthe filter passing fractions of the specific elements are collected within these solutions.The filter, absorption solution and rinsing solutions are recovered for analysis.The filter sample is digested in a closed PTFE vessel.The absorption liquids and the rinsing solutions are prepared for analysis.SIST EN 14385:2004
EN 14385:2004 (E)9The samples are analyzed and the final result is expressed as the total mass concentration for each specificelement and no distinction shall be made between filtered and filter passing fractions.5 Apparatus, chemicals and gases5.1 Apparatus5.1.1 GeneralAll parts coming into contact with the sample are to be made of corrosion resistant and inert material, i.e.borosilicate glass, quartz glass, PTFE, or titanium. As commercial titanium can contain some of the specificelements to be determined, care has to be taken to avoid contamination5.1.2 Apparatus for sampling5.1.2.1 Nozzle (see a)1 of Figure B.1)The diameter shall be chosen to be compatible with the required gas sampling volume flow rate; the choice of thenozzle shall be in accordance with EN 13211 and EN 13284-1:2001.5.1.2.2 Filter housing and filter support (see a)3 of Figure B.1)The filter housing and filter support shall be in accordance with EN 13284-1:2001.5.1.2.3 Sampling probe (see a)2 of Figure B.1)Temperature controlled5.1.2.4 AbsorbersFritted gas bubblers or impingers are to be used; for examples see annex A. For the main stream arrangementcooling of the absorbers to a temperature below 30 °C can be useful to avoid excessive evaporation from the firstabsorption bottle.5.1.2.5 Connection fittings and tubingBall joints and other connectors made of the materials stated in 5.1.1 are allowed. PTFE lined seals are alsoallowed.For the main-stream arrangement of the sampling equipment, the material requirements specified in 5.1.1 shall beapplied from the nozzle to the last absorber; for the side-stream arrangement these materials shall be applied fromthe nozzle to the T-piece and from the T-piece to the last absorber in the side-stream sampling train.The length of connections (such as tubing) from the sampling probe to the absorbers shall be less than 1 m.The total inner surface of all silicone tubing connections that can become exposed to the gases is limited in relationto the sampled gas flow rate. The flow rate dependent total inner surface (A/Q) of the exposed silicone tubing in thesampling equipment, shall be less than 0,003 3 m2/(m3 h-1) or 2 cm2/(l min-1) respectively.5.1.2.6 Suction unitDepending on the arrangement of the equipment (see annex B) two suction units can be required for one samplingline.The suction unit(s) shall be gas tight, corrosion-proof and capable of extracting at least the desired gas flow rate(s)at the low pressure conditions present in the flue gas duct. Wide adjustments of the sample flow rate(s) shall befacilitated using regulating and/or by-pass valves. Shut-off valve(s) for stopping the gas flow, or back flow due tothe low pressure in the duct, should also be available.SIST EN 14385:2004
EN 14385:2004 (E)10If a variant of the sampling train with flow division is chosen, the ratio of the main and side streams has to be keptconstant (± 10 %).NOTE 1Measures for the protection of the suction unit(s) such as filters, water traps etc. can be useful.NOTE 2Corrosion-proof and gas-tight flow meters (variable area meters, orifice plates etc.) are strongly recommended tocheck the sampling flow rate.5.1.2.7 Gas volume meteringTwo gas volume measuring methods may be used:¾ gas flow measurement (Method I);¾ gas volume measurement (Method II).Both methods are described in EN 13284-1:2001. Method II is more accurate than method I.5.1.2.7.1 Gas volume metersThe specifications for gas volume meters are given in EN 13284-1:2001, annex F (a wet gas volume meter mayalso be used).Specifications for the gas volume measurement are:a) When employing a dry gas volume meter a condenser and/or a gas drying system shall be used which canachieve a residual water vapour content of less than 10 g/m3 (equivalent to a dew point of 10,5 °C or a volumecontent c(H2O) = 1,25 %);b) The gas volume meters (wet or dry) shall have a relative uncertainty not exceeding 2 % of the volume (actualconditions);c) In order to calculate the gas volume at standard conditions the temperature measurement at the gas volumemeter shall have an uncertainty not exceeding 2,5 K (i.e. 1 % of absolute temperature) and the pressuremeasurement at the gas volume meter shall have an uncertainty not exceeding 1 kPa (i.e. 10 mbar, or 1 %).5.1.2.7.2 Gas flow metersThis is to be used for checking the actual volume flow rate. The measurement uncertainty of the flow meter shall beless than 5 %.5.1.2.8 Storage bottlesThe bottles for the storage of the unused absorption solutions (before sampling) as well as the exposed absorptionsolutions containing the absorbed elements (samples) shall be made of PE. The caps shall be made of PTFE, PFA,FEP, PP, or uncoloured PE.WARNINGUsing the storage bottles with absorption solution see Warning of 8.2.3.5.1.3 Apparatus for analysis5.1.3.1 Digestion deviceHeating plate or microwave oven for digestion in a closed PTFE vessel at increased temperature and pressure.5.1.3.2 Digestion PTFE vesselsPressure tight PTFE vessels with lids to be used for sample digestion at increased temperature and pressure,matching the digestion device, capacity e.g. 100 ml to 200 ml.SIST EN 14385:2004
EN 14385:2004 (E)115.1.3.3 Measuring flasksFor the unused and exposed absorption solutions, the capacity will depend on their application, e.g. 50 ml, 100 ml,and 1 000 ml. The flasks are to be made of borosilicate glass, quartz glass, or PE.5.1.3.4 Storage flasksFor the digestion solutions, the capacity will depend on their application, e.g. 100 ml and 1 000 ml. Again they areto be made of borosilicate glass, quartz glass, or PE.5.1.3.5 Pipettes and dispensersThese are to be made of borosilicate glass, quartz glass, or PE.5.2 Chemicals and filter material5.2.1 GeneralOnly reagents of recognised analytical grade are to be used (e.g. supra pure). All these materials are to have thelowest possible content of the elements to be determined. The chemicals used shall have a blank value for each ofthe elements of less than 1,0 µg/l.WARNINGTake care that all reagents used, are in accordance with the appropriate health and safety regulations. Carry out arisk assessment on the overall analytical protocol, which will include COSHH (Control of Substances Hazardous to Health)assessments for all reagents used. Particular attention is made to the use of hydrofluoric acid (HF) and develop a separate"safe working" protocol and used by the laboratory to address the unique safety issues relating to HF.5.2.2 FilterFor any series of test, use only filters from one batch, which should have a low and constant metal content. Thefilter material shall have a blank value for each of the elements (per cubic metre of sampled flue gas anticipated) ofless than 1 µg/m³. Only flat filters made of quartz fibre, glass fibre or PTFE are to be used. For the filter efficiency,the same specifications as in EN 13284-1:2001 are required (see Note). This efficiency shall be certified by thesupplier. The filter material shall be suitable for application up to the maximum temperature anticipated.According to EN 13284-1:2001 the filter material shall have an efficiency of at least 99,5 % on a test aerosol with amaximum abundance at a particle diameter of 0,3 µm at the maximum flow rate anticipated, (or at least 99,9 % ona test aerosol of 0,6 µm mean diameter).When using filters with organic binders precautions shall be taken to ensure that during digestion all sampledelements attached to the filter material will be digested. The organic binders or the reaction products from thesebinders after digestion shall not influence the analysis.NOTEGenerally the use of filters with organic binders is not recommended.5.2.3 Hydrofluoric acidHF; mass fraction w » 40 %, r420= 1,16 kg/l, for filter digestion5.2.4 Hydrogen peroxideH2O2; mass fraction w » 30 %, r420= 1,11 kg/l5.2.5 Nitric acidHNO3; mass fraction w » 65 %, r420= 1,40 kg/l, for filter digestionSIST EN 14385:2004
EN 14385:2004 (E)125.2.6 Hydrochloric acidHCl; mass fraction w » 35 %, r420= 1,18 kg/l.5.2.7 WaterH2O; doubly distilled or of the same quality, specific conductivity < 10 µSm-1 (i.e. specific resistance
> 0,1 MWm).5.2.8 Absorption solutionPrepare a mixture from equal volumes of nitric acid (5.2.5) and hydrogen peroxide (5.2.4) and dilute one volumepart of this mixture with nine volume parts of water (5.2.7). This results in mass contents w(HNO3) » 3,3 % andw(H2O2) » 1,5 %. As hydrogen peroxide tends to decompose with time then this solution should be preparedfreshly. Keep a portion of the solution for analysis as a blank equivalent to the absorption solution used at site.5.2.9 Boric acid solution (H3BO3)To obtain a cold saturated boric acid solution with a mass content w » 5 %, dissolve 55 g of boric acid in 1 000 mlwarm water (5.2.7) and let the solution cool down to room temperature.5.2.10 Chemical blank solution for digestionTo be obtained as follows: Add 200 ml of saturated H3BO3 (5.2.9), 30 ml of HNO3 (5.2.5) and 20 ml HF (5.2.3) to avolumetric flask with approximately 700 ml of water (5.2.7). Fill up to 1 000 ml with water (5.2.7), and mix well.Transfer the mixture to a 1 000 ml storage bottle. Mark it ”chemical blank” and add any other relevant information(date etc.).The chemical blank solution shall be used as blank for all digestions by using acids from one batch. Furthermore,this chemical blank solution shall be used for dilution of laboratory standards (see 3.1.3 and 8.7.3).5.2.11 Rinsing acidHNO3, mass content w » 25 %, for rinsing the digestion equipment. Thoroughly mix about 275 ml of HNO3 (5.2.5)with 300 ml of water (5.2.7) and make up to 1 l with water (5.2.7).5.2.12 Standard solutionsThese are to contain the specific elements to be determined with (element) = 1 g/l; pH £ 1Use commercially available standard solutions and dilute them to the appropriate concentrations.5.2.13 Certified reference materialCommercially available certified reference material (CRM), e.g. pulverized fly ash (BCR 038), shall be used.5.2.14 GasesThese gases will depend on the chosen analytical technique and will be described in the manufacturer's operatinginstructions.6 Sampling equipment6.1 General requirementsThe sampling equipment consists of:¾ a temperature controlled sampling probe with the entry nozzle;SIST EN 14385:2004
EN 14385:2004 (E)13¾ a filter housing with filter support and filterThe filter housing may be located either:– in the duct or chimney, mounted directly behind the entry nozzle (in-stack filtration); or– outside the duct or chimney, mounted directly behind the suction tube (out-stack filtration).In the latter case (out-stack filtration) the filter housing shall be temperature controlled.¾ a series of at least three absorbers;¾ suction unit(s) with gas metering device(s) and flow regulator(s).6.2 Isokinetic sampling equipmentSampling shall be carried out isokinetically according to EN 13284-1:2001.Only the additional specific requirements for the sampling of total specific elements are stated here.Two types of absorber systems may be employed, a so-called main-stream or a side-stream arrangement. In themain-stream system all the sampled flue gas is passed through the absorbers, while in the side-streamarrangement only a part of the sampled flue gas is passed through the absorbers.Examples of both systems of the isokinetic sampling equipment are given in annex B.The sampling probe shall be temperature controlled. In addition, when the out-stack filter arrangement is used thefilter housing shall be temperature controlled too. In the case of the side-stream arrangement the T-piece (i.e. theconnection to and the distribution T-piece itself), shall also be temperature controlled. Insulation without additionalheating of these parts is not allowed.NOTEInsulation alone of the connector and the T-piece is insufficient for maintaining the same gas temperature as in thesampling probe. The heat input from the sampled gas is insufficient to compensate for the thermal losses even with insulation.The parts of the equipment that are in contact with the sampled flue gas shall only be composed of the specificmaterials prescribed in 5.1.2.Additional measurement equipment is needed to monitor the isokinetic conditions. For the description of thisequipment, and the associated specific requirements, reference is made to EN 13284-1:2001.6.3 AbsorbersFor an efficient absorption of gaseous phase metals, three absorbers shall be placed in series. The analyticalprocedures and/or sampling procedures shall be arranged in such a way that the detection limit for each elementshould be at least 1 µg/m³. If the element mass concentration of the third absorber is more than 10 % of the totalconcentration in the sampled gas for one or more elements then the overall result shall be rejected.7 Cleaning of the sampling equipment prior to samplingThose parts of the sampling train being in contact with the sampled gas shall be cleaned prior to sampling.The following inner parts shall be cleaned: Nozzle, probe, filter housing, filter support, T-piece (if applied),absorbers, connection tubing, storage bottles for absorption solutions and samples, transport containers for filters(e.g. petri dishes).Some examples of cleaning procedures are given in annex C.SIST EN 14385:2004
EN 14385:2004 (E)148 Procedure8.1 General requirementsThe sampling shall be performed according to EN 13284-1:2001. This includes the procedure of the representativegrid sampling, as well as maintaining isokinetism.The sampling probe, the out-stack filter and the T-piece (see 6.2) shall be maintained at a temperature of at least20 K above the flue gas temperature, or 20 K above the dew point, whichever is the highest.The sampling time shall meet legal or other regulatory requirements.NOTEThe sample volume taken should be sufficient to meet the required detection limit. This will depend on the analyticalinstrumentation used.8.2 Preparation and installation of equipment8.2.1 Filter installationThe filter shall be installed in the filter housing attached to the probe. Care shall be taken in handling the filter inorder to avoid contamination.NOTEIf a sufficient number of filter support or filter casetts are available the filters can be mounted in the filter housings inthe l
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