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1、BRITISH STANDARD BS EN 13506:2002 BS 6068-2.74: 2002 The European Standard EN 13506:2001 has the status of a British Standard ICS 13.060.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:10:09 GMT+00:00 2006, Uncontrol
2、led Copy, (c) BSI BS EN 13506:2002 This British Standard, having been prepared under the direction of the Health and Environment Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 25 January 2002 BSI 25 January 2002 ISBN 0 580 38
3、924 3 National foreword This British Standard is the official English language version of EN 13506:2001. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical and biochemical methods, which has the responsibility
4、to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Additional information BS EN 13506 is one of a series of standards on water quality, others of which have been or will be published as sections of BS 6068. This standard has therefore been given
5、 the secondary identifier BS 6068-2.74. The various sections of BS 6068 are comprised within Parts 1 to 7, which together with Part 0 are listed below: Part 0: Introduction; Part 1: Glossary; Part 2: Physical, chemical and biochemical methods; Part 3: Radiological methods; Part 4: Microbiological me
6、thods; Part 5: Biological methods; Part 6: Sampling; Part 7: Precision and accuracy. NOTEThe tests described in this British Standard should only be carried out by suitably qualified persons with an appropriate level of chemical expertise. Standard chemical procedures should be followed throughout.
7、Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Elect
8、ronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to underst
9、and the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover,
10、 an inside front cover, the EN title page, pages 2 to 16, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Oc
11、t 29 09:10:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13506 November 2001 ICS 13.060.50 English version Water quality - Determination of mercury by atomic fluorescence spectrometry Qualit de leau - Dosage du mercure par spectromtrie de fluoresc
12、ence atomique Wasserbeschaffenheit - Bestimmung von Quecksilber mittels Atomfluoreszenzspektrometrie This European Standard was approved by CEN on 4 October 2001. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standar
13、d 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 Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, Germ
14、an). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finl
15、and, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, 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
16、 2001 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13506:2001 E Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:10:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13506:2001 (E) 2 Contents page 1Scope 4 2Normative refe
17、rences 4 3Principle5 4Interferences.5 5Reagents and Standards.5 6Apparatus and instrumentation7 7Sample collection, preservation and storage.8 8Sample preparation procedure.9 9Instrumental set up9 10Procedure .9 11Data analysis and calculations.10 12Test report 11 13Precision data.12 Annex A (inform
18、ative) Additional Information13 Annex B (informative) Schematic Block Diagram14 Annex C (informative) Availability of Reagents etc. 15 Bibliography16 Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:10:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13506:2001 (E) 3 Foreword This European
19、Standard has been prepared by Technical Committee 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 May 2002, and conflicting na
20、tional standards shall be withdrawn at the latest by May 2002. Annexes designated “informative“ are only given for information. In this standard, annexes A, B and C are informative. WARNING Persons using this standard should be familiar with normal laboratory practice. This standard does not purport
21、 to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. According to the CEN/CENELEC Internal Regulations, the national standar
22、ds organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Copy
23、: sheffieldun sheffieldun, na, Sun Oct 29 09:10:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13506:2001 (E) 4 Introduction It is absolutely essential that tests conducted to this standard are carried out by suitably qualified staff. In natural water sources, mercury compounds generally occur in
24、very small concentrations of less than 0,1 g/l. 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 sediment and sludge. In order to fully decompose all of the mercury compounds, a
25、digestion procedure is necessary. Digestion can be omitted only if it is certain that the mercury concentration can be measured without this pre-treatment. 1 Scope This European Standard specifies a method for the determination of mercury in drinking, surface, ground and rain water. NOTEIt is permis
26、sible, that this standard is also applied to industrial and municipal waste water after an additional digestion step under appropriate conditions. The potential linear dynamic range is approximately 1 ng/l to 100 g/l. In practice, the working range is often from 10 ng/l to 10 g/l. Samples containing
27、 mercury at concentrations higher than the working range can be analysed following appropriate dilution of the sample. The method detection limit (MDL) will be dependent on the selected operating conditions and calibration range. With high purity reagents a MDL of less than 1 ng/l is obtainable. The
28、 relative standard deviation is typically less than 5 % for concentrations greater than twenty times the method detection limit. The sensitivity of this method is dependent on the selected operating conditions. 2 Normative references This European Standard incorporates by dated or undated reference,
29、 provisions from other publications. These normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated
30、in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). EN 25667-1, Water quality - Sampling - Part 1: Guidance on the design of sampling programmes (ISO 5667- 1:1980). EN 25667-2, Water quality - Sampling - Part 2: Gui
31、dance on sampling techniques (ISO 5667-2:1991). EN ISO 5667-3, Water quality - Sampling - Part 3: Guidance on the preservation and handling of samples (ISO 5667-3:1994). EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987). Licensed Copy: sheffieldun shef
32、fieldun, na, Sun Oct 29 09:10:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13506:2001 (E) 5 3 Principle An aliquot of sample is digested using chemically generated bromine 1 2. This is known to breakdown all of the commonly occurring organomercury species to mercury(II). Immediately prior to ana
33、lysis, 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 is purged from solution by an argon gas carrier stream. Moisture is continually removed from the gas stream and the mercury vapour i
34、s detected by atomic fluorescence spectrometry (AFS). The procedure is usually automated by means of an auto sampler and control software. 4 Interferences With mercury there is a risk that exchange reactions, that is adsorption and desorption, will occur on the walls of sampling and reaction vessels
35、. Mercury vapour can diffuse through various plastics; this phenomenon needs to be taken into consideration in the choice of tubing material. Glass or special plastics tubing, e.g. FEP tubes, may be used (FEP = perfluoro(ethylene- propylene). Silicone tubing, for example, is unsuitable. Suppression
36、effects resulting from quenching of the atomic fluorescence signal can be encountered. Dissolved gaseous 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 fro
37、m the carrier gas stream using a hygroscopic membrane before entering the detector3. Anions which complex strongly with mercury can cause suppression. These include sulfide, iodide and bromide. The potassium bromide - potassium bromate reagent (5.5) causes no suppression if it is applied as required
38、. The noble metals, such as gold, silver and platinum, amalgamate with mercury vapour and, therefore, may cause suppression. Volatile organics do not cause interference with the AFS method 4. 5 Reagents and Standards 5.1 General Reagents and water can contain mercury as an impurity. For high sensiti
39、vity use ultra-pure reagents or those with particularly low mercury content compared to the lowest analyte concentration. 5.2 Water Use water with a purity fulfilling the requirements for grade 1 water according to EN ISO 3696 for all sample preparations and dilutions. 5.3 Potassium bromate solution
40、, c(KBrO3) = 0,0333 mol/l Dissolve 1,39 g of potassium bromate in 250 ml of water (5.2). Potassium bromate can be purified, if necessary, by heating in a muffle furnace overnight at 250 C 20 C. Prepare weekly. 5.4 Potassium bromide solution, c(KBr) = 0,2 mol/l Dissolve 5,95 g of potassium bromide in
41、 250 ml of water (5.2). Potassium bromide can be purified, if necessary, by heating in a muffle furnace overnight at 300 C 20 C. Prepare monthly. Licensed Copy: sheffieldun sheffieldun, na, Sun Oct 29 09:10:09 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13506:2001 (E) 6 5.5 Potassium bromide - pot
42、assium bromate reagent Mix equal volumes of potassium bromate (5.3) and potassium bromide solution (5.4). A total volume of 200 ml will allow digestion for 100 samples. Prepare daily. NOTEPre-mixed ampoules for potassium bromate-bromide stock solution are commercially available (see C.1). This reage
43、nt has been found to contain negligible mercury concentrations. 5.6 L -ascorbic acid solution, ?(C6H8O6) = 100 g/l Dissolve 10 g of L-ascorbic acid in water (5.2) in a 100 ml volumetric flask and make up to volume. Prepare weekly. 5.7 Nitric acid, ?(HNO3) = 1,4 g/ml See C.2. 5.8 Potassium dichromate
44、 solution, ? (K2Cr2O7) = 0,05 g/l Dissolve 50 mg of K2Cr2O7 in 50 ml nitric acid (5.7) and dilute to 1 000 ml with water (5.2). 5.9 Hydrochloric acid (HCl), w(HCl) = 120 g/kg Dilute 167 ml of high purity hydrochloric acid w(HCl) = 360 g/kg (? (HCl) = 1,19 g/ml) to 500 ml with water (5.2). 5.10 Tin(I
45、I)chloride solution, ? (SnCl2 2 H2O) = 20 g/l Add 10,0 g of tin(II)chloride dihydrate to 150 ml of hydrochloric acid (5.9). Heat to dissolve. Dilute to 500 ml with water (5.2). To remove any traces of mercury, bubble the solution with argon, nitrogen or air e.g. at a flow rate of 2 l/min for 15 min.
46、 NOTEThe hydrochloric acid used to prepare this solution can be analytical grade since any mercury present will be removed on bubbling. 5.11 Reagent blank For each 100 ml, prepare a solution containing 15 ml of hydrochloric acid (5.9) and 2 ml of potassium bromide - potassium bromate reagent (5.5).
47、Add 100 l of ascorbic acid solution (5.6) for each 10 ml prepared 5. It is essential that the same reagents used for sample and standard preparation are used for preparation of the reagent blank. Treat the reagent blank like a sample. NOTEOn the continuous flow system, the reagent blank solution is
48、run as background for automatic blank subtraction. This solution can contain trace levels of detectable amounts of mercury. 5.12 Mercury standard solutions 5.12.1 Mercury stock solution A, ? (Hg) = 1 000 mg/l Use a commercially available quantitative standard solution. This solution is stable for at
49、 least six months. Alternatively use a stock solution prepared from ultra high purity grade chemicals (99,99 / 99,999 % (mass fraction) pure). Dissolve 0,1354 g of mercury(II)chloride HgCl2 in 20 ml water (5.2). Add 5 ml of nitric acid (5.7) and dilute to 100 ml. WARNING Do not dry the inorganic salt, it is highly toxic. 5.12.2 Mercury stock solution B, ?(Hg) = 10 mg/l Dilute 1 ml of stock solution A (5.12.1) with water (5.2) to approximately 20 ml. Add 2 ml of potassium bromide - potassium bromate reagent (5.5) and 15 ml of hydrochloric acid (5.9)