SIST EN 16192:2012
(Main)Characterization of waste - Analysis of eluates
Characterization of waste - Analysis of eluates
This European Standard specifies methods for the determination of the parameters pH, ammonium, AOX, As, Ba, Cd, Cl-, easily liberatable CN-, Co, Cr, Cr(VI), Cu, DOC/TOC, electrical conductivity, F-, Hg, Mo, Ni, NO2 -, Pb, phenol index, total S, Sb, Se, SO4 2-, TDS, V and Zn in aqueous eluates for the characterization of waste.
At the publication of this European standard EN 12506 and EN 13370 will be replaced.
Charakterisierung von Abfällen - Analyse von Eluaten
Diese Europäische Norm legt Verfahren zur Bestimmung der Parameter pH-Wert, Ammonium, AOX, As, Ba, Cd, Cl, leicht freisetzbares CN, Co, Cr, Cr(VI), Cu, DOC/TOC, elektrische Leitfähigkeit, F, Hg, Mo, Ni, NO2 , Pb, Phenolindex, Gesamt S, Sb, Se, , TDS, V und Zn in wässrigen Eluaten für die Charakterisierung von Abfällen fest.
Caractérisation des déchets - Analyse des éluats
La présente Norme européenne spécifie des méthodes de détermination des paramètres pH, ammonium, AOX, As, Ba, Cd, Cl-, CN- aisément libérable, Co, Cr, Cr(VI), Cu, COD/COT, conductivité électrique, F-, Hg, Mo, Ni, NO2-, Pb, indice phénol, S total, Sb, Se, SO42-, TDS, V et Zn dans les éluats aqueux en vue de la caractérisation des déchets.
Karakterizacija odpadkov - Analiza izlužkov
Ta evropski standard opredeljuje metode za določanje parametrov pH, amonij, organsko vezani halogeni, sposobni adsorpcije (AOX), As, Ba, Cd, Cl-, prosti CN-, Co, Cr, Cr(VI), Cu, DOC/TOC, električna prevodnost, F-, Hg, Mo, Ni, NO2 -, Pb, fenolni indeks, skupni S, S, Sb, Se, SO4 2-, celotne raztopljene snovi (TDS), V in Zn v vodnih izlužkih za karakterizacijo odpadkov.
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Karakterizacija odpadkov - Analiza izlužkovCharakterisierung von Abfällen - Analyse von EluatenCaractérisation des déchets - Analyse des éluatsCharacterization of waste - Analysis of eluates13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 16192:2011SIST EN 16192:2012en,fr,de01-februar-2012SIST EN 16192:2012SLOVENSKI
STANDARDSIST EN 13370:2004SIST EN 12506:20041DGRPHãþD
SIST EN 16192:2012
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16192
November 2011 ICS 13.030.99 Supersedes EN 12506:2003, EN 13370:2003English Version
Characterization of waste - Analysis of eluates
Caractérisation des déchets - Analyse des éluats
Charakterisierung von Abfällen - Analyse von Eluaten This European Standard was approved by CEN on 15 October 2011.
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 CEN-CENELEC 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 CEN-CENELEC Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16192:2011: ESIST EN 16192:2012
EN 16192:2011 (E) 2 Contents Page Foreword .3Introduction .41 Scope .52 Normative references .53 Terms and definitions .64 Sample pretreatment .75 Blank determination .76 Interference .87 Selection of the suitable test method .88 Expression of results . 119 Test report . 11Annex A (informative)
Validation of EN 12506:2003 and EN 13370:2003 . 12A.1 General . 12A.2 Interlaboratory study . 12A.3 Selection of laboratories . 12A.4 Selection of samples . 12A.5 Validation scope . 13A.6 Results and statistics . 16A.7 Conclusion . 24Annex B (informative)
Additional validation data . 25B.1 Round robin test for the determination of Ba, Cd, Cr, Mo, Sb and Se in eluates . 25B.1.1 General . 25B.1.2 Round robin samples . 25B.1.3 Results of the round robin test . 25B.1.4 Conclusion from the round robin test . 29B.2 Round robin tests in the framework of acceptability of waste at landfills . 29Bibliography . 31 SIST EN 16192:2012
EN 16192:2011 (E) 3 Foreword This document (EN 16192:2011) has been prepared by Technical Committee CEN/TC 292 “Characterization of waste”, the secretariat of which is held by NEN. 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 May 2012, and conflicting national standards shall be withdrawn at the latest by May 2012. 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. This document supersedes EN 12506:2003 and EN 13370:2003. Details of significant technical changes between this European Standard and the previous edition are: This European Standard, EN 16192, is now a single document (instead of two) for the analysis of eluates specifying methods for the determination of the parameters pH, ammonium, AOX, As, Ba, Cd, Cl-, easily liberatable CN-, Co, Cr, Cr(VI), Cu, DOC/TOC, electrical conductivity, F-, Hg, Mo, Ni, NO2-, Pb, phenol index, total S, Sb, Se, SO42-, TDS, V and Zn in aqueous eluates for the characterization of waste. In Clause 7 the parameters, previously described in two documents, are now all integrated in Table 1. In Table 1 for all parameters EN and ISO standards are updated, removed if withdrawn and new relevant standards are added, i.e.: addition of the parameters Sb and Se together with the related analytical methods; revision of the standards EN ISO 11885 (ICP-OES) and EN ISO 10304-1 (IC); addition of the ICP-MS method (EN ISO 17294-1:2006 and EN ISO 17294-2:2004); addition of the AAS with graphite furnace technique (EN ISO 15586:2003); addition of the flow analysis techniques for Cl- (EN ISO 15682:2001), Cr(VI) (EN ISO 23913:2009) and SO42- (ISO 22743:2006); addition of the parameter TDS (total dissolved solids) together with the related analytical method; addition of the parameter DOC (dissolved organic carbon) to the parameter TOC (total organic carbon); revision of the standards EN ISO 11732 (ammonium by flow analyser); replacement of EN 1485 (AOX) by EN ISO 9562:2004; revision and addition of new standards for Hg determination – EN 1483 and EN ISO 17852. In Annex B (informative) additional validation data are added obtained from a round robin test for the determination of Ba, Cd, Cr, Mo, Sb and Se in eluates and from round robin tests in the framework of acceptability of waste at landfills, both organized in Belgium. 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. SIST EN 16192:2012
EN 16192:2011 (E) 4 Introduction This European standard is intended to be used for the characterization of waste as defined in the Council Directive 75/442/EEC on waste, as amended by Council Directive 91/156/EEC of 18th March 1991, and national regulations, whose final destination for disposal is landfill. In the Council Decision of 19 December 2002 establishing criteria and procedures for the acceptance of waste at landfills pursuant to Article 16 of and Annex II to Directive 1999/31/EC, the test methods are described for determining the acceptability of waste at landfills. In section 3 of the Annex of this Decision the European standards EN 12506 and EN 13370 are included which are replaced by this European Standard.
This European Standard deals with the determination of chemical constituents, electrical conductivity, pH and total dissolved solids (TDS) in eluates which have been obtained by leaching of waste samples for example using EN 12457 “Characterization of waste - Leaching - Compliance test for leaching of granular waste materials and sludges” (Part 1 to Part 4). In principle, it may be used for the analysis of every kind of eluate as long as the performance characteristics of the applied analytical method fulfill the specific requirements. SIST EN 16192:2012
EN 16192:2011 (E) 5 1 Scope This European Standard specifies methods for the determination of the parameters pH, ammonium, AOX, As, Ba, Cd, Cl-, easily liberatable CN-, Co, Cr, Cr(VI), Cu, DOC/TOC, electrical conductivity, F-, Hg, Mo, Ni, NO2-, Pb, phenol index, total S, Sb, Se, SO42-, TDS, V and Zn in aqueous eluates for the characterization of waste. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 1483:2007, Water quality — Determination of mercury — Method using atomic absorption spectrometry EN 1484:1997, Water analysis — Guidelines for the determination of total organic carbon (TOC) and dissolved organic carbon (DOC) EN 15216:2007, Characterization of waste — Determination of total dissolved solids (TDS) in water and eluates EN 26777:1993, Water quality — Determination of nitrite — Molecular absorption spectrometric method (ISO 6777:1984) EN 27888:1993, Water quality — Determination of electrical conductivity (ISO 7888:1985) prEN ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
(ISO/DIS 5667-3:2010) EN ISO 9562:2004, Water quality — Determination of adsorbable organically bound halogens (AOX) (ISO 9562:2004) EN ISO 10304-1:2009, Water quality — Determination of dissolved anions by liquid chromatography of ions — Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate (ISO 10304-1:2007) EN ISO 10304-3:1997, Water quality — Determination of dissolved anions by liquid chromatography of ions — Part 3: Determination of chromate, iodide, sulfite, thiocyanate and thiosulfate (ISO 10304-3:1997) EN ISO 11732:2005, Water quality — Determination of ammonium nitrogen — Method by flow analysis (CFA and FIA) and spectrometric detection (ISO 11732:2005) EN ISO 11885:2009, Water quality — Determination of selected elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO 11885:2007) EN ISO 11969:1996, Water quality — Determination of arsenic — Atomic absorption spectrometric method (hydride technique) (ISO 11969:1996) EN ISO 13395:1996, Water quality — Determination of nitrite nitrogen and nitrate nitrogen and the sum of both by flow analysis (CFA and FIA) and spectrometric detection (ISO 13395:1996) EN ISO 14402:1999, Water quality — Determination of the phenol index by flow analysis (FIA and CFA)
(ISO 14402:1999) EN ISO 14403:2002, Water quality — Determination of total cyanide and free cyanide by continuous flow analysis
(ISO 14403:2002) EN ISO 14911:1999, Water quality — Determination of dissolved Li+, Na+, NH4+, K+, Mn2+, Ca2+, Mg2+, Sr2+ and Ba2+ using ion chromatography — Method for water and waste water (ISO 14911:1998) EN ISO 15586:2003, Water quality — Determination of trace elements using atomic absorption spectrometry with graphite furnace (ISO 15586:2003) SIST EN 16192:2012
EN 16192:2011 (E) 6 EN ISO 15682:2001, Water quality — Determination of chloride by flow analysis (CFA and FIA) and photometric and potentiometric detection (ISO 15682:2000) EN ISO 17294-1:2006, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-MS) — Part 1: General guidelines (ISO 17294-1:2004) EN ISO 17294-2:2004, Water quality — Application of inductively coupled plasma mass spectrometry (ICP-MS) — Part 2: Determination of 62 elements (ISO 17294-2:2003) EN ISO 17852:2008, Water quality — Determination of mercury — Method using atomic fluorescence spectrometry
(ISO 17852:2006) EN ISO 23913:2009, Water quality — Determination of chromium(VI) — Method using flow analysis (FIA and CFA) and spectrometric detection (ISO 23913:2006) ISO 6439:1990, Water quality — Determination of phenol index — 4-Aminoantipyrine spectrometic methods after distillation ISO 6703-2:1984, Water quality — Determination of cyanide — Part 2: Determination of easily liberatable cyanide ISO 7150-1:1984, Water quality — Determination of ammonium — Part 1: Manual spectrometric method ISO 8288:1986, Water quality — Determination of cobalt, nickel, copper, zinc, cadmium and lead — Flame atomic absorption spectrometric methods ISO 9297:1989, Water quality — Determination of chloride — Silver nitrate titration with chromate indicator (Mohr's method) ISO 9965:1993, Water quality — Determination of selenium — Atomic absorption spectrometric method (hydride technique) ISO 10359-1:1992, Water quality — Determination of fluoride — Part 1: Electrochemical probe method for potable and lightly polluted water ISO 10523:2008, Water quality — Determination of pH ISO 11083:1994, Water quality — Determination of chromium (VI) — Spectrometric method using 1,5-diphenylcarbazide ISO 22743:2006, Water quality — Determination of sulfates — Method by continuous flow analysis (CFA) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 sample portion of material selected from a larger quantity of material 3.2 eluate solution obtained by a leaching test 3.3 laboratory sample sample or subsample(s) sent to or received by the laboratory 3.4 test sample; analytical sample sample, prepared from the laboratory sample, from which test portions are removed for testing or analysis SIST EN 16192:2012
EN 16192:2011 (E) 7 3.5 test portion; analytical portion quantity of material of proper size for measurement of the concentration or other properties of interest, removed from the test sample NOTE 1 The test portion can be taken from the laboratory sample directly if no preparation of sample is required (e.g. with liquids), but usually it is taken from the prepared test sample. NOTE 2 A unit or increment of proper homogeneity, size and fineness, needing no further preparation, can be a test portion. 3.6 leachant aqueous solution used in a leaching test 3.7 leaching test laboratory test for the determination of the release of matter from a waste into water or an aqueous solution 4 Sample pretreatment The eluate shall be analyzed for the total content of its constituents. If precipitation occurs between the preparation of the eluate and the analysis it is necessary to ensure by appropriate methods (e.g. redissolution, separate analysis of solution and precipitate) that the total content of the parameters of interest is determined. If the eluate results from a procedure including 0,45 µm membrane filtration analytical results refer to the content dissolved by the leaching process. Eluates are susceptible to be changed to different extents as a result of physical, chemical or biological reactions which may take place between the time of leaching and the analysis. pH shall be determined immediately after preparation of the eluates and prior to sample pretreatment.
It is therefore essential to take the necessary precautions to minimize these reactions and in the case of many parameters to analyze the eluate sample with a minimum of delay. The maximum delay is given in
prEN ISO 5667-3 or in the respective analytical standards. Precautions should be taken before and during transport as well as during the time in which the samples are preserved in the laboratory before being analyzed, to avoid alteration of the test portion. Split the eluate in an adequate number of test portions for different chemical analyses and preserve them according to the requirements in the analytical standards or prEN ISO 5667-3. One specific test portion may be an untreated aliquot of the laboratory sample for the analysis of chromates such as chloride, fluoride, sulfate, nitrite and chromium(VI) as well as for the determination of electrical conductivity. For trace metal analysis test portions usually need to be acidified to pH ≤ 2. NOTE 1 For safety reasons it is recommended to acidify the test portion under a hood as volatile toxic substances can be generated. NOTE 2 In cases where high contents of soluble solids are leached, acidification of the eluates can lead to precipitation of salts. This can be avoided by dilution prior to acidification. 5 Blank determination The blank contribution of the applied analytical procedures shall be determined as described in the analytical standards and considered in the calculation of the results when appropriate. SIST EN 16192:2012
EN 16192:2011 (E) 8 6 Interference A large number of compounds can interfere with the determination of the parameters concerned. These potential interferences are listed in the individual standards in question. Several types of interference effects can contribute to inaccuracies in the determination of the various parameters, especially at low concentrations. These potential interference effects are listed in the individual standards and shall be considered separately for each analytical technique. Chemical interferences are characterized by molecular compound formation, ionization effects, solute vaporization, precipitation and effects of decomposition of organic matter. Addition of buffer and/or preservation methods may reduce these effects. Physical interferences can be caused by changes of viscosity and surface tension. They can cause significant inaccuracies especially in eluate samples containing high concentrations of acids and/or dissolved components. The colour or turbidity of eluates can cause interference in spectrophotometric determination. 7 Selection of the suitable test method Select the appropriate standardized test method listed in Table 1 according to the type of waste eluate, the concentration range of the parameter of interest and the expected interferences. For analytical quality control purposes ENV ISO 13530 and EN ISO/IEC 17025 should be considered. It is pointed out that the standardized test methods listed in Table 1 have primarily been developed for the analysis of water samples. Most of them were validated in an interlaboratory trial for a limited number of waste eluate matrices (see Annex A). Their suitability for other waste eluates shall be checked in the laboratory performing the analysis. Additional validation data obtained in the evaluation of the analytical performance of laboratories are given in Annex B. Those standards cited in Table 1 that have not been validated in the CEN/TC 292 interlaboratory trial in 1999-2001, have the matrix waste water and/or leachates included in their scope, and they proved to be applicable for the analysis of eluates in routine analyses.
If the methods referred to in Table 1 are found to be inappropriate by reason of, for example, detection limits, repeatability or interferences, other methods validated for water analysis e.g. discrete analyzer, can be used. Their suitability for waste eluates shall be checked in the laboratory performing the analysis. The reason for the deviation shall be stated in the test report. Table 1 — Parameters and test methods
Parameter Test method pH ISO 10523:2008 Ammonium EN ISO 11732:2005 EN ISO 14911:1999 ISO 7150-1:1984 AOX EN ISO 9562:2004 As EN ISO 11885:2009 EN ISO 11969:1996 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 Ba EN ISO 11885:2009 EN ISO 17294-1:2006 EN ISO 17294-2:2004 SIST EN 16192:2012
EN 16192:2011 (E) 9
Table 1 (continued) Parameter Test method Cd ISO 8288:1986 EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 Cl- ISO 9297:1989 EN ISO 10304-1:2009 EN ISO 15682:2001 CN-easily liberatable EN ISO 14403:2002a ISO 6703-2:1984 Co EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 Cr EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 Cr(VI) ISO 11083:1994 EN ISO 10304-3:1997 EN ISO 23913:2009 Cu ISO 8288:1986 EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 DOC/TOC EN 1484:1997 Electrical conductivity EN 27888:1993 F- EN ISO 10304-1:2009b ISO 10359-1:1992 Hg EN 1483:2007 EN ISO 17852:2008 Mo EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004
SIST EN 16192:2012
EN 16192:2011 (E) 10 Table 1 (continued) Parameter Test method Ni ISO 8288:1986 EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 NO2- EN 26777:1993 EN ISO 10304-1:2009 EN ISO 13395:1996 Pb ISO 8288:1986 EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 Phenol index EN ISO 14402:1999c ISO 6439:1990 Total S EN ISO 11885:2009 Sb EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 Se EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 ISO 9965:1993 SO4 2- EN ISO 10304-1:2009 ISO 22743:2006 TDS EN 15216:2007 V EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 Zn ISO 8288:1986 EN ISO 11885:2009 EN ISO 15586:2003 EN ISO 17294-1:2006 EN ISO 17294-2:2004 a free cyanide is equivalent to easily liberatable cyanide for eluates with low organic content after distillation. b for eluates with low organic content. c after distillation. SIST EN 16192:2012
EN 16192:2011 (E) 11 8 Expression of results Specific instructions for the calculation of the results given in the individual analytical standards shall be strictly observed. The results of the tests except for pH and electrical conductivity shall be expressed as a concentration of the constituents in the eluate, expressed in µg/l or mg/l. The amount of constituent leached relative to the total mass of the sample, in mg/kg of dry matter, can be calculated using the liquid to solid ratio of the leaching test. 9 Test report The work carried out by the testing laboratory shall be covered by a report which accurately, clearly and unambiguously presents the test results and all other relevant information. Each test report shall include at least the following information: a) reference to this European Standard and supplementary standards; b) name and address of testing laboratory; c) unique identification of report (such as serial number) and of each page and total number of pages of the report; d) description and identification of the laboratory sample; e) date of receipt of laboratory sample and date(s) of performance of test; f) identification of the test specification or description of the method or procedure; g) description of eluate sampling and treatment, where relevant; h) any deviations, additions to or exclusions from the test specification, and any other information relevant to a specific test; i) measurements, examinations and derived results, supported by tables, graphs, sketches and photographs as appropriate, and any failures identified;
j) a statement on measurement uncertainty (where needed); k) a signature and title or an equivalent marking of person(s) accepting technical responsibility for the test report and date of issue; l) a statement that the test results relate only to the laboratory sample; m) a statement that the report shall not be reproduced except in full without the written approval of the testing laboratory. SIST EN 16192:2012
EN 16192:2011 (E) 12 Annex A (informative)
Validation of EN 12506:2003 and EN 13370:2003 A.1 General During 1999 - 2001 a project for validation of these standards has been organized and carried out. The validation included an interlaboratory study for evaluation of performance characteristics of methods included in these standards (reproducibility and repeatability). A.2 Interlaboratory study The purpose of the validation trial was to check the suitability of the cited standards for analysis of waste eluates.
A.3 Selection of laboratories A questionnaire has been circulated by all CEN/TC 292/WG 2 and WG 3 members to collect a list of interested European laboratories. 41 laboratories gave their commitment to participate in the interlaboratory trial. All of them were asked to declare that they fulfil the minimum requirements to carry out the analyses according to the standards. According to ISO 5725 series no selection has been made in advance on the basis of the supposed "ability" of laboratories, their accreditation, etc. It is therefore legitimate to regard the participating laboratories as a good average of "normal" European laboratories. A.4 Selection of samples To test the analytical procedures on a proper number of eluates, four different materials were considered to produce bulk amounts of waste eluates: — contaminated soil (COS), — sewage sludge (SEW), — sand blasting waste (SBW), — fly ash filter cake from municipal solid waste incinerator (FFC), Additionally, three synthetic solutions were prepared (SYN1, SYN2 and SYN3). The analytical procedures mentioned in the cited standards require different conservation methods. Since it was impossible to produce waste eluates using all the different conservating agents and methods according to the corresponding standards, it was decided to use only two conservation methods:
— addition of HNO3 to a pH of about 2, — no conservation agents but storage of the eluates at 4°C in the dark. The waste eluates and synthetic solutions stabilized with HNO3 were filled into polyethylene bottles and other samples into glass bottles. Table A.1 shows the different conservation procedures as mentioned in the standards and used in this trial. SIST EN 16192:2012
EN 16192:2011 (E) 13 A.5 Validation scope In this trial not all parameter/method combinations were validated for the different samples. In Table A.1 an overview is given of the validation scope.
The parameter/method combinations marked with an x in Table A.1 were successfully validated. A remark is given in Table A.1 for those parameter/method combinations where the validation was not successful, because: — the element concentrations in some samples did not match the working range for the analytical method; — the number of participants and/or the number of results was too low; — matrix dependent interferences occured. In the other cases no validation study was performed. Complementarily some of the standards cited in EN 12506:2003 and EN 13370:2003 have been validated by ISO on waste water. SIST EN 16192:2012
EN 16192:2011 (E) 14 Table A.1 — Validated parameter/method/sample combinations
Parameter Standard Prescribed conservation in standard Used Conservation in trial COSFFC SBW SEW SYN1 SYN2 SYN3
Validated by ISO on waste water Ammonium NH4 ISO 7150-1 Immediate analysis or H2SO4 pH 2 None, 4 oC
x
x
Ammonium NH4 EN ISO 11732 Immediate analysis or H2SO4 pH 2 None, 4 oC
x
x
x AOX EN 1485 HNO3 pH 2 HNO3 pH 2 x
x
x As EN ISO 11885 HNO3 pH 2 HNO3 pH 2 x
x
a
x As EN ISO 11969 HCl pH 2 HNO3 pH 2 x
b
Ba EN ISO 11885 HNO3 pH 2 HNO3 pH 2
x x
x
Cd ISO 8288 HNO3 pH 2 HNO3 pH 2 x
x x
Cd EN ISO 11885 HNO3 pH 2 HNO3 pH 2 x
x
Cl- ISO 9297 None, 4 oC None, 4 oC
x x
x Cl- EN ISO 10304-1 None, 4 oC None, 4 oC
x x x
x Cyanide easily liberatable ISO 6703-2 NaOH pH 8 None, 4 oC
c
a x
Cyanide easily liberatable EN ISO 14403 NaOH pH 12 None, 4 oC
x a
x Co EN ISO 11885 HNO3 pH 2 HNO3 pH 2 x
x
Cr EN ISO 11885 HNO3 pH 2 HNO3 pH 2
x
x
Cr(Vl) ISO 11083 Buffer pH 7 None, 4 oC
x
x
x Cu ISO 8288 HNO3 pH 2 HNO3 pH 2 x
x x
Cu EN ISO 11885 HNO3 pH 2 HNO3 pH 2 x
x
x
Electrical conductivity EN 27888 None, 4 oC None, 4 oC x x x x x x
x F- EN ISO 10304-1 None, 4 oC None, 4 oC
x x
F- ISO 10359-1 None, 4 oC None, 4 oC
x x
Hg EN 1483 K2Cr2O7 pH 1 HNO3 pH 2
a
...
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