EN ISO 17852:2008

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Water quality - Determination of mercury - Method using atomic fluorescence spectrometry (ISO 17852:2006)VFHQþQHQualité de l'eau - Dosage du mercure - Méthode par spectrométrie de fluorescence atomique (ISO 17852:2006)Wasserbeschaffenheit - Bestimmung von Quecksilber - Verfahren mittels Atomfluoreszenzspektrometrie (ISO 17852:2006)13.060.50VQRYLExamination of water for chemical substancesICS:SIST EN ISO 17852:2008en,fr,deTa slovenski standard je istoveten z:EN ISO 17852:200801-julij-2008SIST EN ISO 17852:2008SLOVENSKI
STANDARDSIST EN 13506:20031DGRPHãþD

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN ISO 17852January 2008ICS 13.060.50Supersedes EN 13506:2001
English VersionWater quality - Determination of mercury - Method using atomicfluorescence spectrometry (ISO 17852:2006)Qualité de l'eau - Dosage du mercure - Méthode parspectrométrie de fluorescence atomique (ISO 17852:2006)Wasserbeschaffenheit - Bestimmung von Quecksilber -Verfahren mittels Atomfluoreszenzspektrometrie (ISO17852:2006)This European Standard was approved by CEN on 8 December 2007.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 CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, 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 STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2008 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 17852:2008: E

Endorsement notice The text of ISO 17852:2006 has been approved by CEN as EN ISO 17852:2008 without any modifications.

INTERNATIONALSTANDARDISO17852First edition2006-06-01Reference numberISO17852:2006(E)© ISO2006Water quality— Determination of mercury— Method using atomic fluorescence spectrometryQualité de l'eau— Dosage du mercure— Méthode par spectrométrie de fluorescence atomique

ISO17852:2006(E)ii© ISO2006–All rights reservedPDF disclaimerThis PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shallnot be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. Indownloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariataccepts no liability in this area.Adobe is a trademark of Adobe Systems Incorporated.Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creationparameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In theunlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.©ISO2006All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below orISO's member body in the country of the requester.ISO copyright officeCase postale 56  CH-1211 Geneva 20Tel.+ 41 22 749 01 11Fax+ 41 22 749 09 47E-mailcopyright@iso.orgWebwww.iso.orgPublished in Switzerland

ISO17852:2006(E)© ISO2006–All rights reservediiiContents Page1Scope . 12Normative references . 13Principle . 24Interferences . 25Reagents and standards . 26Apparatus and instrumentation . 57Sample collection and pre-treatment . 68Instrumental set up . 69Procedure . 710Test report . 811Precision . 8AnnexA(informative)Additional information . 9AnnexB(informative)Schematic block diagram . 10AnnexC(informative)Availability of reagents . 11AnnexD(informative)Precision data . 12Bibliography . 13

ISO17852:2006(E)iv© ISO2006–All rights reservedForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies(ISO member bodies). The work of preparing International Standards is normally carried out through ISOtechnical committees. Each member body interested in a subject for which a technical committee has beenestablished has the right to be represented on that committee. International organizations, governmental andnon-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the InternationalElectrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part2.The main task of technical committees is to prepare International Standards. Draft International Standardsadopted by the technical committees are circulated to the member bodies for voting. Publication as anInternational Standard requires approval by at least 75% of the member bodies casting a vote.Attention is drawn to the possibility that some of the elements of this document may be the subject of patentrights. ISO shall not be held responsible for identifying any or all such patent rights.ISO17852 was prepared by Technical Committee ISO/TC147, Water quality, Subcommittee SC2, Physical,chemical and biochemical methods.This International Standard is the equivalent of European Standard EN13506. The preservation procedure withpotassium dichromate solution, described in EN13506, was replaced by a combined on site preservation anddigestion procedure with the potassium bromide - potassium bromate reagent (see 5.4)

ISO17852:2006(E)© ISO2006–All rights reservedvIntroductionIn natural water sources, mercury compounds generally occur in very small concentrations of less than .Higher concentrations may be found, for example, in industrial waste water.Both inorganic and organic compounds of mercury may be present. Mercury can also accumulate in sedimentand sludge.In order to fully decompose all of the mercury compounds, a digestion procedure is necessary. Digestion can beomitted only if it is certain that the mercury concentration can be measured without this pre-treatment.The user should be aware that particular problems could require the specification of additional marginalconditions.0,1µg/l

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INTERNATIONAL STANDARDISO17852:2006(E)© ISO2006–All rights reserved1Water quality— Determination of mercury— Method using atomic fluorescence spectrometryWARNING—Persons using this International Standard should be familiar with normal laboratorypractice. This standard does not purport to address all of the safety problems, if any, associated with itsuse. It is the responsibility of the user to establish appropriate safety and health practices and toensure compliance with any national regulatory conditions.IMPORTANT—It is absolutely essential that tests conducted according to this International Standardare carried out by suitably qualified staff.1ScopeThis International Standard specifies a method for the determination of mercury in drinking, surface, ground andrain water using atomic fluorescence spectrometry.NOTEThis International Standard may be applied to industrial and municipal waste water after an additional digestion stepunder appropriate conditions.The potential linear dynamic range is approximately
to . In practice, the working range is oftenfrom
to .Samples containing mercury at concentrations higher than the working range can be analysed followingappropriate dilution of the sample.The method detection limit () will be dependent on the selected operating conditions and calibration range.With high purity reagents, a
of less than
is obtainable.The relative standard deviation is typically less than
for concentrations greater than twenty times themethod detection limit.The sensitivity of this method is dependent on the selected operating conditions.2Normative referencesThe following referenced documents are indispensable for the application of this document. For datedreferences, only the edition cited applies. For undated references, the latest edition of the referenced document(including any amendments) applies.ISO3696, Water for analytical laboratory use— Specification and test methodsISO5667-1, Water quality— Sampling— Part1: Guidance on the design of sampling programmes andsampling techniquesISO5667-2, Water quality— Sampling— Part2: Guidance on sampling techniquesISO5667-3, Water quality— Sampling— Part3: Guidance on the preservation and handling of water samples1ng/l100µg/l10ng/l10µg/lxDLxDL1ng/l5%

ISO17852:2006(E)2© ISO2006–All rights reserved3PrincipleAtomic fluorescence is an emission process in which atoms are excited by the absorption of a beam ofelectromagnetic radiation. The excited species then relax to the ground state, giving up their excess energy asphotons. Intensity of the photons is measured.An aliquot of sample is digested using chemically generated bromine and bromine chloride (BrCl)[1],[2]. This isknown to break down all of the commonly occurring organomercury species to mercury(II). Immediately prior toanalysis, the excess bromine is removed by ascorbic acid (see A.2).Elemental mercury vapour is generated from the digested sample by reduction with tin(II) chloride, and ispurged from solution by an argon gas carrier stream. Moisture is continually removed from the gas stream andthe mercury vapour is detected by atomic fluorescence spectrometry (AFS). The procedure is usuallyautomated by means of an autosampler and control software.4InterferencesWith mercury there is a risk that exchange reactions, that is adsorption and desorption, will occur on the wallsof sampling and reaction vessels.Mercury vapour can diffuse through various plastics; this phenomenon needs to be taken into consideration inthe choice of tubing material. Glass or special plastics tubing, e.g. FEP1) tubes, may be used. Silicone tubing,for example, is unsuitable.Suppression effects resulting from quenching of the atomic fluorescence signal may be encountered. Dissolvedgaseous species are usually removed during the digestion stage.The presence of water vapour or aerosol in the fluorescence cell may cause suppression due to quenching.Water vapour should be removed from the carrier gas stream using a hygroscopic membrane before enteringthe detector[3].Anions which complex strongly with mercury can cause suppression. These include sulfide, iodide andbromide. The potassium bromide - potassium bromate reagent (5.4) causes no suppression if it is applied asrequired.The noble metals, such as gold, silver and platinum, amalgamate with mercury vapour and, therefore, maycause suppression.Volatile organics do not cause interference with the AFS method[4].5Reagents and standardsReagents and water can contain mercury as an impurity. For high sensitivity, use ultra-pure reagents or thosewith particularly low mercury content compared to the lowest analyte c
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