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1、DRAFT FOR DEVELOPMENT DD CEN/TS 15412:2006 Solid recovered fuels Methods for the determination of metallic aluminium ICS 75.160.10 ? Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI DD CEN/TS 15412:2006 This Dra
2、ft for Development was published under the authority of the Standards Policy and Strategy Committee on 31 October 2006 BSI 2006 ISBN 0 580 48570 6 National foreword This Draft for Development was published by BSI. It is the UK implementation of CEN/TS 15412:2006. This publication is not to be regard
3、ed as a British Standard. It is being issued in the Draft for Development series of publications and is of a provisional nature. It should be applied on this provisional basis, so that information and experience of its practical application can be obtained. Comments arising from the use of this Draf
4、t for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be initiated not later than 3 years after its publication by the European organization so that a decision can be
5、 taken on its status. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the replies received by the end of the review period, the responsible BSI Committee will decide whether to support the conversion into a Eur
6、opean Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent to the Secretary of the responsible BSI Technical Committee at British Standards House, 389 Chiswick High Road, London W4 4AL. The UK participation in its preparation was entrusted to Technic
7、al Committee PTI/17, Solid biofuels. A list of organizations represented on PTI/17 can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Amendments issued since publicat
8、ion Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI TECHNICAL SPECIFICATION SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 15412 September 2006 ICS 75.160.10 English Version Solid
9、recovered fuels - Methods for the determination of metallic aluminium Combustibles solides de rcupration - Mthodes pour la dtermination de laluminium mtal Feste Sekundrbrennstoffe - Verfahren zur Bestimmung des Gehaltes an metallischem Aluminium This Technical Specification (CEN/TS) was approved by
10、CEN on 25 March 2006 for provisional application. The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard. CEN m
11、embers are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS) until the final decision about t
12、he possible conversion of the CEN/TS into an EN is reached. CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Pola
13、nd, Portugal, 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 2006 CENAll rights of exploitation in any form and by
14、any means reserved worldwide for CEN national Members. Ref. No. CEN/TS 15412:2006: E Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2 Contents Page Foreword3 Introduction.4 1 Scope5 2 Normative references5 3 T
15、erms and definitions .5 4 Safety remarks.5 5 Principle6 6 Apparatus.6 7 Reagents.7 8 Preparation of the test sample.7 9 Procedure.8 10 Calculation and evaluation.9 11 Quality control .9 12 Performance characteristics 10 13 Test report10 Annex A (normative) Guidelines - Characteristics of the laborat
16、ory sample for chemical analysis of SRF11 Bibliography13 CEN/TS 15412:2006 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 3 Foreword This document (CEN/TS 15412:2006) has been prepared by Technical Committee C
17、EN/TC 343 “Solid Recovered Fuels”, the secretariat of which is held by SFS. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to announce this CEN Technical Specification: Austria, Belgium, Cyprus, Czech Republic, Denmark, Es
18、tonia, 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. CEN/TS 15412:2006 Licensed Copy: London South Bank University, London So
19、uth Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 4 Introduction The metallic aluminium in solid recovered fuels is very problematic in combustion processes. Aluminium can form deposit on heat transfer surfaces and superheaters. For these reasons a method for the de
20、termination of total metallic aluminium is necessary. Other methods with low melting point such as tin, lead and zinc may cause similar problems but their content in solid recovered fuels is usually very low and then their effect is not significant. CEN/TS 15412:2006 Licensed Copy: London South Bank
21、 University, London South Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 5 1 Scope This Technical Specification specifies two different methods for the determination of metallic aluminium in solid recovered fuels: method a: dissolution of metallic aluminium and analy
22、sis by Inductively Coupled Plasma Optic Emission Spectrometry (ICP-OES) or by Flame Atomic Absorption Spectrometry (FAAS); method b: Differential Thermal Analysis (DTA) on the solid SRF. 2 Normative references The following referenced documents are indispensable for the application of this Technical
23、 Specification. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. CEN/TS 15357:2006, Solid recovered fuels Terminology, definitions and descriptions CEN/TS 15413, Solid recovered fuels Metho
24、ds for the preparation of the test sample from the laboratory sample prCEN/TS 15414-3, Solid recovered fuels Determination of moisture content using the oven dry method Part 3: Moisture in general analysis sample prCEN/TS 15403, Solid recovered fuels Methods for the determination of the ash content
25、EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) EN ISO 11885, Water quality Determination of 33 elements by inductively coupled plasma atomic emission spectroscopy (ISO 11885:1996) EN ISO 12020, Water quality Determination of aluminium Atomic abso
26、rption spectrometric methods (ISO 12020:1997) 3 Terms and definitions For the purposes of this Technical Specification, the terms and definitions given in CEN/TS 15357:2006 and the following apply. 3.1 metallic aluminium aluminium that could be extract from SRF by using a 0,75 mol/l NaOH solution, a
27、fter leaching with 0,14 mol/l HNO3 solution. This includes the metallic aluminium and some chemical forms of aluminium non-soluble in nitric acid but easily soluble in alkaline media 4 Safety remarks The safety in handling of potentially hazardous materials is dealt with in relevant national and Eur
28、opean regulations, which every laboratory should refer to. In addition the following information is given: most of reagents used within this Technical Specification are strongly corrosive and toxic. Safety precautions are absolutely necessary due to strong corrosive reagents at high temperature; CEN
29、/TS 15412:2006 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 6 the reaction of metallic aluminium (and other metals such as zinc, lead and tin) with NaOH solution generates gaseous hydrogen that can form expl
30、osive mixtures in the air; all procedures have to be performed in a hood or in closed force-ventilated equipment. By the use of strong oxidising reagents the formation of explosive organic intermediates is possible especially when dealing with samples with a high organic content. Do not open pressur
31、ised vessels before they have cooled down. Avoid contact with the chemicals and the gaseous reaction products. 5 Principle 5.1 Method A The test portion of 1 mm maximum particle size is leached with 0,14 mol/l nitric acid solution and shaken. After that the mixture is filtered. The elemental alumini
32、um is digested by heating the sample with alkali. After that the mixture is filtered and then the aluminium content is determined by ICP-OES or FAAS. 5.2 Method B The test portion of 1 mm maximum particle size is ashed and then introduced with the proper program in the DTA analyser and the DTA curve
33、 is recorded. 6 Apparatus 6.1 Method A 6.1.1 Balances Analytical balance resolution 0,1 mg. 6.1.2 General laboratory equipment Including volumetric graduated flasks and pipettes of adequate size; filter equipment of adequate chemical resistance and purity or centrifuge. The use of glass ware shall b
34、e excluded when NaOH is used. 6.1.3 Shaking table 6.1.4 Hotplate Resistance heated, with temperature regulation up to 120 C. 6.1.5 Inductively coupled plasma (ICP-OES) Normal commercial instrumentation. 6.1.6 Flame atomic absorption spectrometer (FAAS) Normal commercial instrumentation. 6.2 Method B
35、 6.2.1 Differential thermal analyser (DTA) Commercial differential thermal analyser or differential thermal analyser/thermogravimetric analyser (DTA/TGA) CEN/TS 15412:2006 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy
36、, (c) BSI 7 6.2.2 Platinum pans 7 Reagents All reagents shall be at least of analytical grade and suitable for their specific purposes. Other specific reagents are listed and described in the reference methods for digestion or instrumental determination listed in Clause 2. 7.1 Method A 7.1.1 Water o
37、f grade 1 as specified by EN ISO 3696:1995. 7.1.2 Sodium hydroxide (NaOH), 0,75 mol/l. 7.1.3 Nitric acid (HNO3), 0,14 mol/l. 7.1.4 Concentrated nitric acid (HNO3), 14 mol/l. 7.1.5 Aluminium standard solution, 1 000 mg/l. Commercial available standard solution for spectroscopy. 7.1.6 Calibration solu
38、tions The calibration solutions are made by mixing 10 ml of 0,75 mol/l NaOH (7.1.2) with 3 ml concentrated HNO3 (7.1.3) in 100 ml graduated flask. A suitable amount of aluminium standard is then added and the solution is diluted to 100 ml with water. 7.2 Method B 7.2.1 Aluminium powder, purity 96,7
39、% or higher. 7.2.2 Sand Purified, high quartz content sand. 7.2.3 Aluminium calibration mixture Appropriate solid mixtures prepared by mixing sand (7.2.2) and metallic aluminium (7.2.1), according to the expected content of metallic aluminium in SRF samples. 8 Preparation of the test sample The test
40、 sample is the general analysis test sample with a nominal top size of 1 mm or less, which shall be prepared in accordance with CEN/TS 15413 and for the method B prepared in accordance with prCEN/TS 15403. For the method A the sample can be either dry or air-dried and for the method B the sample can
41、 be either dry or air-dried fuel ash, prepared according to prCEN/TS 15403. CEN/TS 15412:2006 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 8 9 Procedure 9.1 Sample conservation and pre-treatment The laborato
42、ry samples shall be stored according to guidelines defined in Annex A. Furthermore any possible source of contamination during the laboratory sample preparation (e.g. grinding with metallic apparatus, mainly aluminium or aluminium alloy) shall be avoided or reduced as much as possible. The laborator
43、y sample should be stored and delivered in sealed high-density plastic containers. 9.2 Sample preparation The test portion shall be prepared from the laboratory sample according to CEN/TS 15413. In addition, for the purposes of this method, the target size should be 1 mm or below. For method B the t
44、est portion is obtained by ashing an appropriate amount of the original sample. Depending on the used method, the amount of test portion ranges between 50 mg (method b) to 2 g (method a). Whereas the determination is carried out on dry basis, the moisture content shall be determined according to prC
45、EN/TS 15414-3. 9.3 Method A 9.3.1 General Accurately weight about 2 g of the test sample in 250 ml Erlenmeyer flask. Carry out two blank tests, using the same procedure but omitting the test portion. 9.3.2 Leaching of lightly soluble aluminium compounds Add 100 ml of 0,14 mol/l nitric acid (7.1.3) p
46、ut the Erlenmeyer flask on the shaking table. Shake the sample for one hour. Filter the sample and rinse 3 times the Erlenmeyer flask and the filter 20 ml aliquots of water (7.1.1). 9.3.3 Dissolution of metallic aluminium Transfer the filter with the sample into a narrow PTFE container. Add 100 ml o
47、f 0,75 mol/l sodium hydroxide (7.1.2), heat to boiling and let the solution gently boil for 1,5 h. Remove the sample from the heating plate and add 100 ml water and let the solution cool down. The solution is filtered and the filtrate is transferred into a plastic 500 ml graduated flask. Rinse the P
48、TFE vessel and the filter with 3 aliquots of 25 ml each of water (7.1.1). Add 15 ml concentrated nitric acid (7.1.4) into the graduated flask and dilute with water to 500 ml. 9.4 Method B The sample is ashed according to the general principle of prCEN/TS 15403. Accurately weight about 50 mg of ash d
49、irectly in the platinum pan. The thermogram is recorded. CEN/TS 15412:2006 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 9 9.5 Analysis of content of metallic aluminium 9.5.1 Method A The content of aluminium in the final solution from method A shall be determined by FAAS or ICP-OES according to the general principles of EN ISO 12020 or EN ISO 11885. 9.5.2 Method B The metallic alum