1、BRITISH STANDARD Water quality Digestion for the determination of selected elements in water Part 1: Aqua regia digestion The European Standard EN IS0 15587-1:2002 has the status ofa British Standard ICs 13.060.50 BS EN IS0 15587-1 12002 BS 6068-2.76: 2002 Incovorating Corrigendum No. I BS EN IS0 15
2、587-1 12002 13917 Corrigendum No. 1 ISBN O 580 39252 X National foreword 14 May 2002 Incorporating the Annex ZA This British Standard is the official English language version of EN IS0 15587-1:2002. It is identical with IS0 15587-1:2002. The UKparticipation in its preparation was entrusted by Techni
3、cal Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical and biochemical methods, which has the responsibility to: - - aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change,
4、and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. - A list of organizations represented on this committee can be obtained on request to its secretary. This is one of a series ofstandards on water quality, others ofwhich have be
5、en, or will be, published as Sections of BS 6068. The various Sections of BS 6068 are comprised within Parts 1 to 7, which together with Part O, are listed below. Part O Introduction Part 1 Glossary Part 2 Physical, chemical and biochemical methods Part 3 Radiological methodr Part 4 Microbiological
6、methodr Part 5 Biological methods Part 6 Sampling Part 7 fiecision and accuracy NOTE qualified persons with an appropriate level of chemical expertise. Standard chemical procedures should be followed throughout. The tests described in this British Standard should only be carried out by suitably Cros
7、s-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 Electroni
8、c 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 ofitself confer immunity from legal obligations. This British Standard, having
9、 been prepared under the direction of the Health and Summary Of pages This document comprises a front cover, an inside front cover, the EN IS0 title page, the EN IS0 foreword page, the IS0 title page, pages ii to iv, pages 1 to 18, the Annex ZA page and a back cover. Environment Sector Strategy Comm
10、ittee, was and published under the authority ofthe Standards Strategy Committee on and The BSI copyright date displayed in this document indicates when the document was last issued. 28 March 2002 Amendments issued since publication OBSI 14 May 2002 Amd. No. I Date I Comments EUROPEAN STANDARD NORME
11、EUROPENNE EUROPAISCHE NORM EN IS0 15587-1 March 2002 ICs 13.060.50 English version Water quality - Digestion for the determination of selected elements in water - Part 1 : Aqua regia digestion (IS0 15587- 1:2002) Qualit de leau - Digestion pour la dtermination de certains lments dans leau - Partie 1
12、 : Digestion leau rgale (IS0 15587-1:2002) Wasserbeschaffenheit - Aufschluss fur die Bestimmung ausgewahlter Elemente in Wasser - Teil 1 Konigswasser- Aufschluss (IS0 15587-1 2002) This European Standard was approved by CEN on 1 March 2002 CEN members are bound to comply with the CENICENELEC Interna
13、l 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 Management Centre or to any CEN member. Th
14、is 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 Management Centre has the same status as the official versions. CEN members are the
15、 national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom kUROIEAN COMMIT1 kE FOR STANDARDIZATION COMIIE EUROPEFN DE NOKMALISAIION
16、PUROPAISC tlbC KOMITEE FUR NORMUNG Management Centre: rue de Stascart, 36 B-1050 Brussels O 2002 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN IS0 15587-1:2002 E EN IS0 15587-12002 I CORRECTED 2002-04-17 I Foreword This document
17、(IS0 15587-1 :2002) has been prepared by Technical Committee ISO/TC 147 Water quality” in collaboration with 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
18、identical text or by endorsement, at the latest by September 2002, and conflicting national standards shall be withdrawn at the latest by September 2002. According to the CENKENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this Euro
19、pean Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard IS0 15587-1 :2002 has be
20、en approved by CEN as a European Standard without any modifications. NOTE Normative references to International Standards are listed in annex ZA (normative). EN IS0 15587-12002 INTERNATIONAL STANDARD IS0 15587-1 First edition 2002-03-01 Water quality - Digestion for the determination of selected ele
21、ments in water - Part I: Aqua regia digestion Qualit de leau - Digestion pour la determination de certains lments dans leau - Partie I: Digestion leau rgale Reference number IS0 15587-1 :2002(E) II EN IS0 15587-1:2002 Contents Page Foreword . iv 1 Scope 1 2 Normative references 1 3 Terms and definit
22、ions . 2 4 Principle 2 5 Reagents . 3 6 Apparatus . 3 7 Sampling . 4 8 Procedure . 4 9 Test report 6 Annex A (informative) Digestion in an open system using electrical heating 7 Annex B (informative) Digestion in an open system using microwave-assisted heating . 9 Annex C (informative) Digestion in
23、a closed system using microwave-assisted heating 11 Annex D (informative) Digestion in a closed system using an autoclave . 15 Annex E (informative) Performance checks . 17 Bibliography 18 . 111 EN IS0 15587-1:2002 Foreword IS0 (the International Organization for Standardization) is a worldwide fede
24、ration of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that commi
25、ttee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordan
26、ce with the rules given in the ISOIIEC Directives, Part 3 The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires a
27、pproval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this part of IS0 15587 may be the subject of patent rights. IS0 shall not be held responsible for identifying any or all such patent rights. IS0 15587-1 was prepared by Te
28、chnical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical method. IS0 15587 consists of the following parts, under the general title Water quality - Digestion for the determination of selected elements in water: - Part I: Aqua regia digestion Part 2: Nitric a
29、cid digestion Annexes A to E of this part of IS0 15587 are for information only. iv EN IS0 15587-1:2002 Water quality - Digestion for the determination of selected elements in water - Part 1: Aqua regia digestion WARNING - Persons using this part of IS0 15587 should be familiar with normal laborator
30、y practice. This part of IS0 15587 does not purport 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. 1 Scope This part of
31、 IS0 15587 specifies a method for extracting trace elements from a water sample using aqua regia as a digestion agent. The method is applicable to all types of waters with a suspended solids mass concentration of less than 20 g/l and a mass concentration of total organic carbon (TOC) expressed as ca
32、rbon of less than 5 g/l. The aqua regia digestion method is empirical and it might not release elements completely. However, for most environmental applications, the result is fit for purpose. Aqua regia digestion is suitable for the release of: Ag, AI, As, B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe, Hg, K,
33、Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Se, Sn, Sr, TI, V, Zn. It is not suitable for the digestion of refractory compounds such as SO, Tio, and Alzo,. The presence of chloride in the digestion solution may limit the application of analytical techniques. The method is generic and may be implemented using a w
34、ide variety of equipment provided - the digestion composition is unchanged, - the digestion temperature is known, and the digestion duration is in accordance with this temperature 2 Normative references The following normative documents contain provisions which, through reference in this text, const
35、itute provisions of this part of IS0 15587. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of IS0 15587 are encouraged to investigate the possibility of applying the most recent editions of th
36、e normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of IS0 and IEC maintain registers of currently valid International Standards. IS0 3696: 1987, Water for analytical laboratory use - Specification and test methods
37、IS0 5667-3:1994, Water quality - Sampling - Pari 3: Guidance on the preservation and handling of samples 1 EN IS0 15587-12002 3 Terms and definitions For the purposes of this part of IS0 15587, the following terms and definitions apply 3.1 aqua regia solution obtained by mixing one volume of nitric
38、acid with three volumes of hydrochloric acid 3.2 wet digestion treatment with reactive liquid chemicals with the aim of bringing analytes into solution so as to be suitable for subsequent analysis NOTE The degree to which analytes are brought into solution suitable for subsequent analysis may depend
39、 on the principle of the subsequent analysis. Some analytical methods require the element in solution to be independent of its chemical state, others require a specific valence or a specific ionic species, for instance hydride atomic spectrometry, photometry and electrochemical methods. For the latt
40、er, special attention should be paid to the presence of chemically stable organometals 5. 4 Principle The test portion is digested with aqua regia at a defined temperature. The temperature is at least the boiling point (103 “C at 101,3 kPa) and at most 175 “C. At the boiling point (101,3 kPa), the m
41、inimum duration to release the digestible fraction is 120 min. The maximum duration is set at four times the minimum duration at that temperature. By convention, both the required minimum and maximum duration is assumed to halve with every 15 “C increase in temperature above the boiling point (see F
42、igure 1). After digestion the digest is clarified, if necessary. c v) 2 160 - % 150 n 140 130 120 110 IO0 90 80 10 100 t 1 O00 Digestion duration (min) Figure 1 - Range of permitted digestion temperature and duration 2 EN IS0 15587-12002 5 Reagents During analysis, use only reagents of recognized an
43、alytical grade that meet the purity requirements of the subsequent analysis. Verify their purity by performing a blank test. 5.1 subsequent analysis. Water, complying with grade 1 of IS0 3696. Grade 2 may be used if it meets the purity requirements for the 5.2 Hydrochloric acid, c(HCI) = 12,O mol/l,
44、 p = 1,2 kg/l, approximately 37 % by mass. 5.3 Nitric acid is available both as p(HN03) = 1,40 kg/l, approximately 65 Yo by mass and p(HN0,) = 1,42 kg/l, approximately 69 Yo by mass. Both are suitable. Nitric acid, c(HN03) = 15,8 mol/l, p= 1.4 kg/l. 5.4 Antifoaming agent, for instance n-dodecane (C,
45、2H26). 6 Apparatus 6.1 digest solution. Digestion vessel, temperature- and pressure-resistant and capable of containing the mixture of sample and If a closed vessel is applied, its inner wall shall be inert and shall not release substances to the digest in excess of the purity requirements of the su
46、bsequent analysis. 6.2 condenser) and designed to minimize losses. Vapour recovery system, capable of recovering the evaporated digest during open digestion (e.9. refliux Materials in contact with the vapour shall be inert and shall meet the purity requirements of the subsequent analysis. 6.3 specie
47、s which may pass through the vapour recovery system (6.2). Volatile species trap, in an open digestion system capable of trapping one or more volatile measurement This trap may comprise condensation equipment or equipment to absorb these species in nitric acid or aqua regia. Materials in contact wit
48、h the vapour shall be inert and shall meet the purity requirements of the subsequent analysis. 6.4 Heating device, capable of maintaining the target temperature for the required time period. 6.5 analysis. Filter paper, cellulose-based ashless type, with a median pore size adapted to the apparatus us
49、ed for It shall not be able to release substances to the digest in excess of the purity requirements of the subsequent analysis and shall not absorb substances from the digest beyond the level of negligible impact on trueness of the analytical result. 6.6 for instance with warm nitric acid (5.3) diluted to 10 % by volume with water (5.1). Anti-bumping granules or roughened glass beads, having a diameter of 2 mm to 3 mm and acid-washed 6.7 Volumetric flask, usually of nominal capacity of 50 ml or 100 ml. 6.8 Graduated pipettes or dispensers, of appropriate volume
