1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationDD CEN/TS 15412:2010Solid recovered fuels Methods for the determinationof metallic aluminiumDD CEN/TS 15412:2010 DRAFT FOR DEVELOPMENTNational forewordThis Draft for Development
2、is the UK implementation of CEN/TS 15412:2010. It supersedes DD CEN/TS 15412:2006 which iswithdrawn.This publication is not to be regarded as a British Standard.It is being issued in the Draft for Development series of publicationsand is of a provisional nature. It should be applied on thisprovision
3、al basis, so that information and experience of its practicalapplication can be obtained.Comments arising from the use of this Draft for Developmentare requested so that UK experience can be reported to theinternational organization responsible for its conversion toan international standard. A revie
4、w of this publication willbe initiated not later than 3 years after its publication by theinternational organization so that a decision can be taken on itsstatus. Notification of the start of the review period will be made inan announcement in the appropriate issue of Update Standards.According to t
5、he replies received by the end of the review period,the responsible BSI Committee will decide whether to support theconversion into an international Standard, to extend the life of theTechnical Specification or to withdraw it. Comments should be sentto the Secretary of the responsible BSI Technical
6、Committee at BritishStandards House, 389 Chiswick High Road, London W4 4AL.The UK participation in its preparation was entrusted to TechnicalCommittee PTI/17, Solid biofuels.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not pur
7、port to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 69178 2ICS 75.160.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This Draft for Development was published under the authority ofthe S
8、tandards Policy and Strategy Committee on 31 August 2010.Amendments issued since publicationDate Text affectedDD CEN/TS 15412:2010TECHNICAL SPECIFICATION SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 15412 June 2010 ICS 75.160.10 Supersedes CEN/TS 15412:2006English Version Solid recovered f
9、uels - Methods for the determination of metallic aluminium Combustibles solides de rcupration - Mthode de dtermination de laluminium total Feste Sekundrbrennstoffe - Verfahren zur Bestimmung des Gehaltes an metallischem Aluminium This Technical Specification (CEN/TS) was approved by CEN on 27 March
10、2010 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 members are requi
11、red 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 the possible conv
12、ersion of the CEN/TS into an EN is reached. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, P
13、oland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and b
14、y any means reserved worldwide for CEN national Members. Ref. No. CEN/TS 15412:2010: EDD CEN/TS 15412:2010CEN/TS 15412:2010 (E) 2 Contents Page Foreword 3Introduction . 41 Scope 42 Normative references 43 Terms and definitions . 44 Safety remarks . 55 Principle 55.1 Method A. 55.2 Method B. 56 Appar
15、atus . 56.1 Method A. 56.2 Method B . 67 Reagents . 67.1 General 67.2 Method A. 67.3 Method B . 78 Preparation of the test sample . 79 Procedure . 79.1 Sample conservation and pre-treatment . 79.2 Sample preparation . 79.3 Method A. 89.3.1 General 89.3.2 Leaching of lightly soluble aluminium compoun
16、ds . 89.3.3 Dissolution of metallic aluminium . 89.4 Method B. 89.5 Determination of metallic aluminium . 89.5.1 Method A. 89.5.2 Method B. 810 Calculation and evaluation . 810.1 General 810.2 Method A. 910.3 Method B. 911 Quality control . 912 Performance characteristics 913 Test report 9Annex A (n
17、ormative) Guidelines - Characteristics of the laboratory sample for chemical analysis of SRF 11DD CEN/TS 15412:2010CEN/TS 15412:2010 (E) 3 Foreword This document (CEN/TS 15412:2010) has been prepared by Technical Committee CEN/TC 343 “Solid Recovered Fuels”, the secretariat of which is held by SFS.
18、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 CEN/TS 15412:2006. According to the CEN/CENELEC Internal Regu
19、lations, the national standards organizations of the following countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembour
20、g, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DD CEN/TS 15412:2010CEN/TS 15412:2010 (E) 4 Introduction The metallic aluminium in solid recovered fuels is very problematic in combustion processes. Aluminium can form de
21、posit on heat transfer surfaces and superheaters. For these reasons a method for the determination of total metallic aluminium is necessary. Other metals 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 th
22、en their effect is not significant. 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 analysis by Inductively Coupled Plasma Optic Emission Spectrometry (ICP-OES)
23、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 document. For dated references, only the edition cited applies. For undated refer
24、ences, the latest edition of the referenced document (including any amendments) applies. prEN 15357:2009, Solid recovered fuels Terminology, definitions and descriptions prEN 15403, Solid recovered fuels Determination of the ash content prEN 15413, Solid recovered fuels Methods for the preparation o
25、f the test sample from the laboratory sample prEN 15414-3, Solid recovered fuels Determination of moisture content using the oven dry method Part 3: Moisture in general analysis sample EN ISO 3696:1995, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) EN ISO 11885:2
26、009, Water quality Determination of selected elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO 11885:2007) EN ISO 12020:2000, Water quality Determination of aluminium Atomic absorption spectrometric methods (ISO 12020:1997) 3 Terms and definitions For the purposes o
27、f this document, the terms and definitions given in prEN 15357:2009 and the following apply. 3.1 metallic aluminium aluminium that could be extract from SRF by using a 0,75 mol/l NaOH solution, after leaching with 0,14 mol/l HNO3solution DD CEN/TS 15412:2010CEN/TS 15412:2010 (E) 5 NOTE This includes
28、 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 relevant national and European regulations, which every laboratory should refer to. I
29、n 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; the reaction of metallic aluminium (and other metals such as zi
30、nc, lead and tin) with NaOH solution generates gaseous hydrogen that can form explosive 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 esp
31、ecially when dealing with samples with a high organic content. Do not open pressurised 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 a
32、cid solution and shaken. After that the mixture is filtered. The elemental aluminium 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
33、 and then introduced with the proper program in the DTA analyser and the DTA curve is recorded. 6 Apparatus 6.1 Method A 6.1.1 Balances Analytical balance resolution 0,1 mg. DD CEN/TS 15412:2010CEN/TS 15412:2010 (E) 6 6.1.2 General laboratory equipment Including volumetric graduated flasks and pipet
34、tes of adequate size; filter equipment of adequate chemical resistance and purity or centrifuge. The use of glass ware shall be excluded when NaOH is used. 6.1.3 Shaking table 6.1.3 Hotplate Resistance heated, with temperature regulation up to 120 C. 6.1.4 Inductively coupled plasma (ICP-OES) Normal
35、 commercial instrumentation. 6.1.5 Flame atomic absorption spectrometer (FAAS) Normal commercial instrumentation. 6.2 Method B 6.2.1 Differential thermal analyser (DTA) Commercial differential thermal analyser or differential thermal analyser/thermogravimetric analyser (DTA/TGA). 6.2.2 Platinum pans
36、 7 Reagents 7.1 General 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. 7.2 Method A 7.2.1 Water of grade 1 as specif
37、ied by EN ISO 3696:1995. 7.2.2 Sodium hydroxide (NaOH), 0,75 mol/l. 7.2.3 Nitric acid (HNO3), 0,14 mol/l. 7.2.4 Concentrated nitric acid (HNO3), 14 mol/l. 7.2.5 Aluminium standard solution, 1 000 mg/l. Commercial available standard solution for spectroscopy. 7.2.6 Calibration solutions The calibrati
38、on solutions are made by mixing 10 ml of 0,75 mol/l NaOH (7.2.2) with 3 ml concentrated HNO3(7.2.3) in 100 ml graduated flask. A suitable amount of aluminium standard is then added and the solution is diluted to 100 ml with water. DD CEN/TS 15412:2010CEN/TS 15412:2010 (E) 7 7.3 Method B 7.3.1 Alumin
39、ium powder, purity 96,7 % or higher. 7.3.2 Sand Purified, high quartz content sand. 7.3.3 Aluminium calibration mixture Appropriate solid mixtures prepared by mixing sand (7.3.2) and metallic aluminium (7.3.1), according to the expected content of metallic aluminium in SRF samples. 8 Preparation of
40、the test sample The test sample is the general analysis test sample with a nominal top size of 1 mm or less, which shall be prepared in accordance with prEN 15413 and for the method B prepared in accordance with prEN 15403. For the method A the sample can be either dry or air-dried and for the metho
41、d B the sample can be either dry or air-dried fuel ash, prepared according to prEN 15403. NOTE 1 In some cases Calcite (calcium carbonate) in the sample can effect on results interpretation in method B. In such cases ashing is recommended at higher temperatures, e.g. 850 C. NOTE 2 Special care shoul
42、d be taken to avoid segregation of aluminium particles when preparing test portion (method A). 9 Procedure 9.1 Sample conservation and pre-treatment The laboratory samples shall be stored according to guidelines defined in Annex A. Furthermore any possible source of contamination during the laborato
43、ry sample preparation (e.g. grinding with metallic apparatus, mainly aluminium or aluminium alloy) shall be avoided or reduced as much as possible. The laboratory sample should be stored and delivered in sealed high-density plastic containers. 9.2 Sample preparation The test portion shall be prepare
44、d from the laboratory sample according to prEN 15413. In addition, for the purposes of this method, the target size should be 1 mm or below. For method B the test portion is obtained by ashing an appropriate amount of the original sample. Depending on the used method, the amount of test portion rang
45、es 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 prEN 15414-3. DD CEN/TS 15412:2010CEN/TS 15412:2010 (E) 8 9.3 Method A 9.3.1 General Accurately weight about 2 g of the test sample in 250 ml Er
46、lenmeyer flask. Carry out two blank tests, using the same procedure but omitting the test portion. NOTE 1 A glass fibre filter, 10 cm, GF 6 (retention of particles larger than 1 m) with Bchner funnel with suction may be used when necessary. NOTE 2 Some turbidity may remain after filtration and shoul
47、d not interfere with the determination. 9.3.2 Leaching of lightly soluble aluminium compounds Add 100 ml of 0,14 mol/l nitric acid (7.2.3) put 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 with 20 ml
48、aliquots of water (7.2.1). 9.3.3 Dissolution of metallic aluminium Transfer the filter with the sample into a narrow PTFE container. Add 100 ml of 0,75 mol/l sodium hydroxide (7.2.2), heat to boiling and let the solution gently boil for 1,5 h. Remove the sample from the heating plate and add 100 ml
49、water and let the solution cool down. The solution is filtered and the filtrate is transferred into plastic 500 ml graduated flask. Rinse the PTFE vessel and the filter with 3 aliquots of 20 ml each of water (7.2.1). Add 15 ml concentrated nitric acid (7.2.4) 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 prEN 15403. Weight
