1、April 2008DEUTSCHE NORM English price group 12No part of this standard 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 13.060.50!$Md“1426592www
2、.din.deDDIN EN ISO 17852Water quality Determination of mercury Method using atomic fluorescence spectrometry (ISO 17852:2006)English version of DIN EN ISO 17852:2008-04Wasserbeschaffenheit Bestimmung von Quecksilber Verfahren mittels Atomfluoreszenzspektrometrie (ISO 17852:2006)Englische Fassung DIN
3、 EN ISO 17852:2008-04SupersedesDIN EN 13506:2002-04www.beuth.deDocument comprises 21 pagesDIN EN ISO 17852:2008-04 2 This standard is part of the series Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlamm-untersuchung Kationen (Gruppe E) (German standard methods for the examination of wate
4、r, waste water and sludge Cations (group E) and describes method (AFS) E 35. National foreword This standard has been prepared by Technical Committee ISO/TC 147 “Water quality” in collaboration with Technical Committee CEN/TC 230 “Water analysis” (Secretariat: DIN, Germany). The responsible German b
5、ody involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Technical Committee NA 119-01-03-01-11 AK Atomspektrometrische Verfahren. This standard has been published to implement the Water Framework Directive (WFD), Directive 2000/60/EC of the European
6、Parliament and of the Council of 23 October 2000 establishing a framework for Community action in the field of water policy*). Designation of method E 35 “Determination of mercury Method using atomic fluorescence spectrometry (AFS)”: Method DIN EN ISO 17852 E 35 Expert assistance and specialized lab
7、oratories will be required to perform the analysis described in this standard. Existing safety regulations are to be taken into account. Depending on the objective of the analysis, a check shall be made on a case-by-case basis as to whether and to what extent additional conditions will have to be sp
8、ecified. WARNING Users of this standard should take note that during sample pre-treatment bromine vapours can be generated after the potassium bromide potassium bromate reagent has been added. Therefore, when carried out in the laboratory this step is to be carried out in the fume cupboard; extreme
9、care is to be taken when adding the reagent on site or in the sampling vehicle. Mercury and mercury compounds are extremely toxic and dangerous to the environment. Samples and solutions that contain or might contain mercury are to be handled with extreme care. Standard methods published as DIN Stand
10、ards are obtainable from Beuth Verlag GmbH, either individually or grouped in volumes. The standard methods included in the loose-leaf publication entitled Deutsche Einheits-verfahren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be published by Wiley-VCH Verlag and Beuth Verlag Gm
11、bH. new Regulation on Section 7a of the Gesetz zur Ordnung des Wasserhaushalts (German Water Management Act) concerning Anforderungen an das Einleiten von Abwasser in Gewsser together with the Abwasser-verordnung and the Gesetz zur Ordnung des Wasserhaushalts have been published by Beuth Verlag GmbH
12、 as a loose-leaf collection Analysenverfahren in der Abwasserverordnung Rechtsvorschriften und Normen (Supplements). Standards or draft standards bearing the group title “German standard methods for the examination of water, waste water and sludge” are classified under the following categories (main
13、 titles): *)Registered in the DITR database of DIN Software GmbH, available from: Beuth Verlag GmbH, 10772 Berlin. All standard methods relevant to the Abwasserverordnung (Waste Water Ordinance ) (AbwV) included in the DIN EN ISO 17852:2008-04 3 General information (group A) (DIN 38402) Sensory anal
14、ysis (group B) (DIN 38403) Physical and physicochemical parameters (group C) (DIN 38404) Anions (group D) (DIN 38405) Cations (group E) (DIN 38406) Substance group analysis (group F) (DIN 38407) Gaseous constituents (group G) (DIN 38408) Parameters characterizing effects and substances (group H) (DI
15、N 38409) Biological-ecological methods of analysis (group M) (DIN 38410) Microbiological methods (group K) (DIN 38411) Test methods using water organisms (group L) (DIN 38412) Individual constituents (group P) (DIN 38413) Sludge and sediments (group S) (DIN 38414) Bio-assays with microorganisms (gro
16、up T) (DIN 38415) In addition to the methods described in the DIN 38402 to DIN 38415 series of standards, there are a number of European and International Standards available as DIN EN, DIN EN ISO and DIN ISO Standards which also form part of the collection of German standard methods. Information on
17、 Parts of these series of standards that have already been published can be obtained from the offices of the Normenausschuss Wasserwesen, telephone +49 (30) 2601-2448, or from Beuth Verlag GmbH, Burggrafenstrae 6, 10787 Berlin, Germany. The DIN Standards corresponding to the International Standards
18、referred to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 5667-1 DIN EN ISO 5667-1 ISO 5667-2*)DIN EN ISO 5667-1 ISO 5667-3 DIN EN ISO 5667-3 ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DIN EN 13506:2002-04 as follows: a) The standard number has been changed. b) A ne
19、w approach involving a combined preservation and digestion step that is carried out on site has been introduced; in this step the potassium bromide potassium bromate reagent and other substances are added directly to the samples. Thus, potassium chromate does not have to be added to stabilize the sa
20、mples and the digestion step does not have to take place in the laboratory, as is usually the case. c) Precision data from EN 13506:2002-04 are given in Annex D of DIN EN ISO 17852. d) The standard has been editorially revised. Previous editions DIN EN 13506: 2002-04 *)With the publication of ISO 56
21、67-1:2006 Part 2 of the standard was integrated into Part 1 and in this manner replaced. DIN EN ISO 17852:2008-04 4 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN EN ISO 5667-1, Water quality Sampling Part 1: Guidance
22、 on the design of sampling programmes and sampling techniques DIN EN ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination o
23、f repeatability and reproducibility of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17852 January 2008 ICS 13.060.50 Supersedes EN 13506:2001 English Version Water quality - Determination of mercury - Method using atomic fluorescence spectrometry (ISO 17852:
24、2006) Qualit de leau - Dosage du mercure - Mthode par spectromtrie de fluorescence atomique (ISO 17852:2006)Wasserbeschaffenheit - Bestimmung von Quecksilber - Verfahren mittels Atomfluoreszenzspektrometrie (ISO 17852:2006) This European Standard was approved by CEN on 8 December 2007. CEN members a
25、re 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
26、 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 translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the sa
27、me status as the official 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,
28、Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means res
29、erved worldwide for CEN national Members. Ref. No. EN ISO 17852:2008: EContents PageDIN EN ISO 17852:2008-04 EN ISO 17852:2008 (E)2 :Foreword 3 Introduction . 4 1 Scope 5 2 Normative references 5 3 Principle 6 4 Interferences 6 5 Reagents and standards . 6 6 Apparatus and instrumentation . 9 7 Sampl
30、e collection and pre-treatment . 10 8 Instrumental set up 10 9 Procedure . 11 10 Test report 12 11 Precision . 12 Annex A (informative) Additional information 13 Annex B (informative) Schematic block diagram . 14 Annex C (informative) Availability of reagents . 15 Annex D (informative) Precision dat
31、a 16 Bibliography 17 ForewordDIN EN ISO 17852:2008-04 EN ISO 17852:2008 (E)3 The text of ISO 17852:2006 has been prepared by Technical Committee ISO/TC 147 “Water quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 17852:2008 by Technical Committee
32、CEN/TC 230 “Water analysis“, the secretariat 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 or by endorsement, at the latest by July 2008, and conflicting national standards shall be withdrawn at the latest
33、 by July 2008. 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 13506:2001. According to the CEN/CENELEC In
34、ternal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg,
35、Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 17852:2006 has been approved by CEN as EN ISO 17852:2008 without any modifications. IntroductionIn natural water sources, mercury compounds
36、 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 comp
37、ounds, 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.0,1g/lDIN EN ISO 17852
38、:2008-04 4 EN ISO 17852:2008 (E)WARNING 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 saf
39、ety 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 determin
40、ation of mercury in drinking, surface, ground andrain water using atomic fluorescence spectrometry.NOTE This International Standard may be applied to industrial and municipal waste water after an additional digestion stepunder appropriate conditions.The potential linear dynamic range is approximatel
41、y 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.Wi
42、th 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.2 Normative referencesThe following ref
43、erenced 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.ISO 3696, Water for analytical laboratory use Specification and test
44、methodsISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes andsampling techniquesISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples1 ng/l 100g/l10 ng/l 10g/lxDLxDL1 ng/l5%5 EN ISO 17852:2008 (E)DIN EN ISO 17852:2
45、008-04 ISO 5667-2N1)N1)National footnote: With the publication of ISO 5667-1:2006 Part 2 of the standard was integrated into Part 1 and in this manner replaced. , Water quality Sampling Part 2: Guidance on sampling techniques3PrincipleAtomic fluorescence is an emission process in which atoms are exc
46、ited 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 isk
47、nown 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
48、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.4 InterferencesWith mercury there is a risk that exchange
49、 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 duri
