1、 STD-BSI BS EN L334b-ENGL ZOO0 Lb24669 0875831 008 BRITISH STANDARD Characterization of sludges - Determination of trace elements and phosphorus - Aqua regia extraction methods The European Standard EN 133462000 has the status of a British Standard ICs 13.030.20 NO COPYING WlTEOT BSI PERMISSION EXCE
2、PT AS PERMED BY COPYRIGHT LAW BS EN 13346:2000 STD-BSI BS EN L334b-ENGL 2000 Lb24bb9 0875832 T44 Amd.No. IDate Committee and comes into effect on 15 October ZOO0 BS EN 133462000 Comments National foreword This British Standard is the official English language version of EN 133462000. The UK particip
3、ation in its preparation was entrusted to Technical Committee EW5, Sludge characte - present to the responsible European committee any enquiries on the - monitor related intemational and European developments and promulgate A list of organizations represented on this committee can be obtained on req
4、uest to its secretary. Further information Users of this standard are informed that the UK submitted some substantial comments at the final voting stage of the draft EN for the following reasons. 1) The scope fails to address the question of whether this method is appropriate for ali of the types of
5、 sludges in the scope of CENITC 308. For example, is it applicable to sludges containing large amounts of lime? Hence, modify the scope to answer the question of applicability to the scope of the TC. 2) The following note should be added to the scope: “he validation for this standard has only been c
6、arried out using materials as described in annex A For other sludges, the user should validate the method using recovery and reproducibili tests”. 3) The final phrase, “and sludge products,” in the first sentence of the scope should be removed as it is inappropriate. 4) This is not a single sandard
7、since there are 4 alternative methods of extraction and 3 aitemative methods of pretreatment. The test report in clause 12 should therefore specify which of the 12 permutations has been used. Therefore, either rewrite c) as “describe which method of pretreatment and which method of digestion was use
8、d” or modify the document so that there is only one standard method against which others may be benchmarked 5) In annex D, the data presented for Method D with reference materials appear to condemn this method as unfit since it is almost invariably outside the 95% confidence of the reference sample.
9、 Therefore, suggest deleting Method D. 6) It is recommended that an additional brief section on the use of adequate AQC as per CENITC 223 methods be added “The analysis described in this standard should be carried out within a quality control system utilizuig analytical quaiity control measures. Whe
10、re performance data are absent for the sample type, recovery and reproducibility data should be obtained as a minimum”. interpreation, or proposals for change, and keep the UK interests informed, them in the UK. This British Standard, having been prepared under the direction of the Health and Enviro
11、nment Sector Committee. Q BSI 10-2000 ISBN O 580 36291 4 STD-BSI BS EN L334b-ENGL 2000 = lb24bb7 0875833 780 W BS EN 13346:2000 Cr oss-r eferences The British Standards which implement internationai or European publications referred to in this document may be found in the BSI Stan- Catalogue under t
12、he section entitled “intemationai Standards Correspondence Index“, or by using the “F“ facility of the BSI Standards Electronic 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 applicati
13、on. Compliance with a British Standard does not of itself confer immunity from legai obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN tite page, pages 2 to 29 and a back cover. The BSI copyright notice displayed in this document indic
14、ates when the document was last issued. - O BSI 10-2000 i STD-BSI BS EN L334b-ENGL 2000 lb24bb9 0875834 BL7 EUROPEAN STANDARD NORME EUROPENNE EUROPASCHE NORM EN 13346 August 2000 ICs 13.030.20 English version Characterization of sludges - Determination of trace elements and phosphorus - Aqua regia e
15、xtraction methods Caractrisation des boues - Dtermination des lmenis traces et du phosphore - Mthodes dextraction Ieau rgale Charakterisierung von Schlmmen - Bestimmung von Spurenelementen und Phosphor - Extraktionsverfahren mit Knigswasser This European Standard was approved by CEN on 5 August 2000
16、. CEN members are bound to comply with the CENICENELEC Internal Regulations which stipulate the conditions for giving this Europmn Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning wch national standards may be obtained on a
17、pplication to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by trawlation under the responsibility of a CEN member into its own language and notified to the Central Secretariat ha
18、s the same status as he official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMIIT
19、EE FOR STANDARDIZATION EUROPISCHES KOMITEE FR NORMUNG COMIT EUROPEN DE NORMALISATION Centrai Secretariat: rue de Stassart, 36 8-1050 Brussels Q 2000 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13346:2000 E STD-BSI BS EN 13346-E
20、NGL 2000 1624669 0875835 753 Page 2 EN 13346:2000 Contents Page Foreword -. 3 Introduction - 4 1 2 3 4 5 6 7 8 9 io 11 12 13 Scope -. 5 Normative references 5 Terms and definitions -. 5 Principle . .- . 6 Reagents ._ 6 Apparatus . 6 Preparation of the laboratory sample 7 Procedure . 8 Blank test 9 M
21、easurements 10 Expression of results 1 O Test report ._ 10 Precision data IO Annex A (informative) Pretreatment of the sample 21 Annex B (informative) Calibration of the microwave oven . 23 Annex C (informative) Guidelines for measurement techniques 25 Annex D (informative) Precision data for method
22、s C and D with reference materials 27 Bibliography -. 29 O BSI 10-2000 STD.BSI BS EN L334b-ENGL 2000 Lb24bb 087583b h9T D Page 3 EN 13346:2000 Foreword This European Standard has been prepared by Technical Committee CEN/TC 308, Characterization of sludges, the Secretariat of which is held by AFNOR.
23、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 February 2001, and conflicting national standards shall be withdrawn at the latest by February 2001. According to the CENICENELEC Internal Regulatio
24、ns, the national standards 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, Noway, Portugal, Spain, Sweden, Switzerland and the United
25、 Kingdom. The annexes A to D are informative. O BSI 10-2000 Page 4 EN 13346:2000 Introduction Elements extractable in aqua regia cannot be described as “total“; conversely they cannot be regarded as the “bio-available“ fraction, as the extraction procedure is too vigorous to represent all biological
26、 processes. One extraction method is proposed, using aqua regia. Four heating processes are described, they use the same reagents therefore the same principle of chemical reaction. Method A is a vigorous digestion procedure allowing larger test portions. Method B is a fast procedure carried out in a
27、 single vessel, smaller test portions are used. Methods C and D are microwave heating procedures using closed and open systems respectively. Q BSI 10-2000 Page 5 EN 13346:2000 1 Scope This standard specifies methods for the extraction, with aqua regia, of trace elements and phosphorus from sludges a
28、nd sludge products. The resulting solution is suitable for the determination of As, Cd, Cr, Cu, Hg, Ni, Pb, Se, Zn and P using spectrometric techniques. NOTE 1 should be expected. With high solute concentrations in extract solutions, spectral interferences and background enhancement NOTE 2 This meth
29、od can be used for other elements except that portion of the elements bonded to silica. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the pub
30、lications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. EN 1233, W
31、ater quality - Determination of chromium - Atomic absorption spectrometric methods. EN 1483, Water quality - Determination of mercury. EN 12880, Characterization of sludges - Determination of dry residue and water content. EN IS0 3696, Water for analytical laboratory use - Specification and test met
32、hods (IS0 3696:1987). EN IS0 5961, Water quality - Determination of cadmium by atomic absorption spectrometry (IS0 5961:1994). EN IS0 11885, Water quality - Determination of 33 elements by inductively coupled plasma atomic emission spectroscopy (IS0 1 1885: 1996). EN IS0 11969, Water quality - Deter
33、mination of arsenic - Atomic absorption spectrometric method (hydride technique) (IS0 1 1969: 1996). IS0 5725-2, Accuracy (trueness and precision) of measurement methods and resulfs - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method. IS
34、0 8288, Water quality - Determination of cobalt, nickel, copper, zinc, cadmium and lead - Flame atomic absorption spectrometric methods. 3 Terms and definitions For the purposes of this European Standard, the following terms and definitions apply. 3.1 aqua regia digestion solution obtained by mixing
35、 one volume of nitric acid and three volumes of hydrochloric acid 3.2 dry mass (dry matter) the mass of solids obtained after the specified drying process. It is expressed as grams or kilograms EN 128801 BSI 10-2000 STDSBSI BS EN 1334b-ENGL 2000 Lb24669 0875837 377 Page 6 EN 13346:2000 4 Principle T
36、he laboratory sample is prepared in order to obtain a representative test portion which is extracted with aqua regia according to one of the following heating procedures: - boiling for about 2 h with a reflux condenser, followed by filtration and making up to volume in a volumetric flask (method A);
37、 - boiling for about 15 min in a calibrated glass tube, making up to volume in the same tube, allowing to settle and then decanting the supernatant solution for analysis (method B); - microwave digestion for about 20 min in a closed vessel followed by filtration and making up to volume in a volumetr
38、ic flask (method C); - microwave digestion for about 30 min in an open vessel followed by filtration and making up to volume in a volumetric flask (method D). NOTE Other heating procedures can be used providing they demonstrate equivalent performance. 5 Reagents 5.1 General The reagents used shall b
39、e of sufficient purity so as not to introduce a significant error into the subsequent analysis. A reagent blank comprising the same quantity of acids shall be taken through the entire procedure with each batch of analysis. 5.2 Water Deionized or distilled water used shall conform to purity grade 2 o
40、f EN IS0 3696. 5.3 Hydrochloric acid, solution c(HCI) = 12,O molll. About 37 % (dm), p = 1 ,I8 g/ml. 5.4 Nitric acid, solution, c(HN03) = 15,8 mol/l. About 65 % (dm), p = 1,42 g/ml. 5.5 Nitric acid solution, about 1 % (VW) for cleaning. Take 10 ml of nitric acid (5.4) and dilute to 1 I in a flask wi
41、th water. This dilute nitric acid shall be used to clean the glassware. 5.6 n-Dodecane or other suitable antifoaming agents (for addition in method B). 6 Apparatus 6.1 General All glassware and plasticsware shall be adequately cleaned and stored in order to avoid any contamination. NOTE deposits. It
42、 can be necessary to periodically clean the reaction vessel with a suitable surfactant to remove stubborn Q BSI 10-2000 STDmBSI BS EN 1334b-ENGL 2000 I Lb24bb9 08758LIO 010 Page 7 EN 13346:2000 6.2 Reaction vessels a) glass flask, 250 ml for example (for method A); b) calibrated borosilicate glass t
43、ube 50 ml, for example, with a glass or polypropylene stopper (for method B); c) plastics vessel (at least 1 O0 mi) made of pertluoroalkoxy polymer (PFA) or tetrafluoromethoxyl polymer (TFM) equipped with a system capable of controlling overpressure in order to avoid explosion of the vessel (for met
44、hod C); d) digestion vessel made of borosilicate glass with a volume of at least 50 ml (for method D). NOTE Quartz vessels can be used instead of glass vessels. 6.3 Reflux condenser Adaptable to reaction vessels used in methods A or D. 6.4 Heating devices a) a heating mantle or aluminium block heate
45、r (for methods A and B respectively); b) a microwave oven with programmable power to control fast exothermic reaction and closed microwave vessels equipped with a safety system for method C. A domestic microwave oven is not allowed; c) a microwave oven with a programmer module (for method D). NOTE F
46、or example an apparatus with microwave frequencies 2,451 GHz, electronic automatic power control which can be pilot-operated from 10 % to 99 % with 5 % increment for maximal power released of 200 W and a pump for reagent. 6.5 Filter papers Filter paper cellulose based, hardened and resistant to aqua
47、 regia. 6.6 Volumetric flasks, capacity 25 ml, 50 ml or 100 ml. 6.7 Analytical balance, with an accuracy of 1 mg or better 6.8 methods A and B). Boiling aids, anti bumping granules or glass beads, diameter 2 mm to 3 mm, acid washed (for 7 Preparation of the laboratory sample Weigh a representative a
48、mount of the wet sample, to give a sufficient dry mass for the method used, in a porcelain dish and prepare it according to EN 12880. Take the dried sample and grind with contaminant free pestle and mortar or mill. Keep the sample under dry conditions. NOTE Other methods of dried sample preparation
49、are presented in annex A. O BSI IO-2000 STDoBSI BS EN 13346-ENGL 2000 N Zb24bb7 08758ir1 T57 m Page 8 EN 13346:2000 8 Procedure 8.1 Extraction procedure under reflux conditions (method A) Weigh approximately 3 g, to the nearest 0,001 g, of the prepared sample (clause 7) and transfer to the 250 ml reaction vessel 6.2 a). Moisten with about 0,5 ml to 1 ,O ml of water (5.2) and add, with mixing, (21 f 0,l) ml of hydrochloric acid (5.3) followed by (7 f 0,l) ml of nitric acid (5.4) dropwise if necessary to reduce foaming. Connect the condenser (6.3) to
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