1、BS EN 15691:2009 ICS 75.160.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDEthanol as a blendingcomponent for petrol Determinationof total dry residue(involatile material) Gravimetric methodBS 2000-576:2009Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS
2、, 07/08/2009 03:18, Uncontrolled Copy, (c) BSIThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 30 April2009 BSI 2009ISBN 978 0 580 58693 4Amendments/corrigenda issued since publicationDate CommentsBS EN 15691:2009National forewordThis British Stan
3、dard is the UK implementation of EN 15691:2009.The UK participation in its preparation was entrusted to TechnicalCommittee PTI/13, Petroleum testing and terminology.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to i
4、nclude all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.Energy Institute, under the brand of IP, publishes and sells all Parts of BS 2000, and all BS EN petroleum test methods
5、that would be Part of BS 2000, both in its annual publication “Standard methods for analysis and testing of petroleum and related products and British Standard 2000 Parts” and individually.Further information is available from: Energy Institute, 61 New Cavendish Street, London W1G 7AR. Tel: 020 7467
6、 7100. Fax: 020 7255 1472.Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 07/08/2009 03:18, Uncontrolled Copy, (c) BSIBS EN 15691:2009EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15691March 2009ICS 75.160.20English VersionEthanol as a blending component for petrol - Determination ofdry r
7、esidue (involatile material) - Gravimetric methodEthanol comme base de mlange lessence -Dtermination du rsidu sec (produits non volatils) -Mthode gravimtriqueEthanol zur Verwendung als Blendkomponente inOttokraftstoff - Bestimmung des Trockenrckstandes(nichtflchtige Bestandteile) - Gravimetrisches V
8、erfahrenThis European Standard was approved by CEN on 24 January 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographic
9、al references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN me
10、mber into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, L
11、atvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels
12、 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15691:2009: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 07/08/2009 03:18, Uncontrolled Copy, (c) BSIBS EN 15691:2009EN 15691:2009 (E) 2 Contents Page Foreword 31 Scope
13、 42 Normative references 43 Principle 44 Apparatus .45 Sampling .45.1 Preparation of samples .45.2 Verification and quality control 56 Procedure .57 Calculation 58 Expression of results 59 Precision .59.1 General 59.2 Repeatability, r .69.3 Reproducibility, R 610 Test report 6Bibliography 7Licensed
14、Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 07/08/2009 03:18, Uncontrolled Copy, (c) BSIBS EN 15691:2009EN 15691:2009 (E) 3 Foreword This document (EN 15691:2009) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic a
15、nd biological origin”, the secretariat of which is held by NEN. 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 September 2009, and conflicting national standards shall be withdrawn at the latest
16、by September 2009. 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 was prepared by CEN/TC 19s Ethanol Task Force under r
17、esponsibility of its Working Group 21 and is based on a test method mentioned in a European Wine Regulation 1. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
18、 Cyprus, Czech Republic, Denmark, Estonia, 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. Licensed Copy: Wang Bin, ISO/EXCHANG
19、E CHINA STANDARDS, 07/08/2009 03:18, Uncontrolled Copy, (c) BSIBS EN 15691:2009EN 15691:2009 (E) 4 1 Scope This European Standard specifies a procedure for the determination of dry residue in ethanol by gravimetric (desiccation) method in the range (10 to 25) mg/100 ml. NOTE In an interlaboratory st
20、udy 2 the method described has been tested at levels down to 3,5 mg/100 ml, but the precision appeared to be insufficient at such low levels. WARNING Use of this document may involve hazardous equipment, materials and operations. This method does not purport to address to all of the safety problems
21、associated with its use, but it is the responsibility of the user to search and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2 Normative references The following referenced documents are indispensable for the application of
22、 this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 3170, Petroleum liquids Manual sampling (ISO 3170:2004) 3 Principle Dry residue is determined by the weighing of the
23、residue left by evaporation of alcohol on a boiling water bath and drying in a drying oven. Dry residue includes all matter that is non-volatile under specified physical conditions. 4 Apparatus 4.1 Evaporating dish (100 to 250 ml). 4.2 Boiling water bath. 4.3 Pipette, 100 ml, class A. 4.4 Oven, capa
24、ble of being held at a temperature of (103 2) C. 4.5 Desiccator, containing freshly activated silica gel (or equivalent desiccant) with moisture content indicator. 4.6 Analytical balance, capable of weighing with an accuracy of 0,1 mg. 5 Sampling 5.1 Preparation of samples Unless otherwise specified
25、 in the commodity specification, samples shall be taken as described in EN ISO 3170. Collect the samples in glass bottles. Samples shall be stored at room temperature prior to analysis. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 07/08/2009 03:18, Uncontrolled Copy, (c) BSIBS EN 15691:200
26、9EN 15691:2009 (E) 5 5.2 Verification and quality control It is recommended to prepare a sodium chloride solution with a content of 100 mg/l in ethanol from neutral ethanol free of dry residue and from an aqueous sodium chloride solution the content of which is 10 g/l. For example, 10 ml of the aque
27、ous solution can be introduced in 1 l of this neutral alcohol without residue. This is a solution with a dry residue content of 10 mg/100 ml. 6 Procedure Place clean dry evaporating dishes (4.1) into the oven for 30 minutes, then place them into the desiccator (4.5) for 30 minutes. Use a tool to man
28、ipulate dishes, do not touch directly with fingers. Accurately weigh, to the nearest 0,1 mg, the clean dry evaporating dishes (4.1) (M0). Pipette (4.3) 100 ml of sample or quality control and introduce respectively into the dishes. Place the dishes with sample on the boiling water bath (4.2) and all
29、ow to dry. NOTE In general, it takes about two hours to evaporate the alcohol on the water bath. Place the dishes in the oven (4.4) at (103 2) C for 30 minutes and then transfer dishes with residue into a desiccator (4.5). Allow the dishes to cool for 30 minutes and then weigh, to the nearest 0,1 mg
30、, the dishes with residue (M1). 7 Calculation The content of dry residue, D, expressed in mg/100 ml is given by: 01MMD = (1) where D is the expression for dry residue, M1is the mass, in mg, of the dish and residue after drying, M0is the mass, in mg, of the clean dry dish. 8 Expression of results Rep
31、ort the content of dry residue rounded to the nearest 1 mg/100 ml. 9 Precision 9.1 General The precision given was derived from statistical analysis by EN ISO 4259 3 of the results of interlaboratory testing of a matrix of ethanol liquids, produced from biomaterials such as wine (fermentation result
32、), molasses, pulp and corn. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 07/08/2009 03:18, Uncontrolled Copy, (c) BSIBS EN 15691:2009EN 15691:2009 (E) 6 NOTE The interlaboratory testing and the statistical evaluation are detailed in 2. In some occasions the repeatability is larger than the
33、 reproducibility, caused by outliers, but the evaluation did not show major mistakes in the set up of the interlaboratory testing. The term “single test result” means the value obtained when the standardized test method is applied fully once to a single sample. Unless otherwise stated, the probabili
34、ty shall be 95 %. 9.2 Repeatability, r The repeatability limit is the value below which the absolute difference between two single test results obtained under the same conditions (same operator, same apparatus, same laboratory and a short interval of time) should exceed the following value in mg/100
35、 ml in one case in twenty: r = 0,191 X + 0,000 55 (2) where X is the average value of results being compared. 9.3 Reproducibility, R The reproducibility limit is the value below which the absolute difference between two single test results obtained under different conditions (different operators, di
36、fferent apparatus and/or different laboratories and/or different time) should not exceed the following value in mg/100 ml in one case in twenty: R = 0,184 8 X + 0,000 81 (3) where X is the average value of results being compared. 10 Test report The test report shall contain at least the following in
37、formation: a) reference to this European Standard, i.e. EN 15691; b) all information necessary for the complete identification of the sample; c) applied sampling procedure (see 5.1); d) results of the test (see 8); e) any deviation, by agreement or otherwise, from the procedure specified in this Eur
38、opean Standard, or regarded as optional; f) details of any incidents which may have influenced the test results; g) date of the test. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 07/08/2009 03:18, Uncontrolled Copy, (c) BSIBS EN 15691:2009EN 15691:2009 (E) 7 Bibliography 1 European Commiss
39、ion regulation (EC) N 625/2003 of 2 April 2003 amending Regulation (EC) No 1623/2000 laying down detailed rules for implementing Council Regulation (EC) No 1493/1999 on the common organisation of the market in wine with regard to market mechanisms: Annex IV Community analysis method for neutral alco
40、hol Method 10: Determination of dry residue 2 Research Report on determination of the dry extract content of ethanol gravimetric method, January 2007, available from UNGDA, 174 blvd Camlinat, 92247 MALAKOFF Cedex, France, 3 EN ISO 4259, Petroleum products Determination and application of precision
41、data in relation to methods of test (ISO 4259:2006) Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 07/08/2009 03:18, Uncontrolled Copy, (c) BSIEnergy InstituteBuying Parts of BS 2000Orders for BS 2000 publications should be addressed to either:Energy Institute Library and Information Service
42、61 New Cavendish StreetLondonW1G 7ARTel: +44 (0)20 7467 7100Fax: +44 (0)20 7255 1472www.energyinst.org.ukOrder standards securely via:www.energyinstpubs.org.ukor:British Standards Institution Customer Services389 Chiswick High RoadLondonW4 4ALTel: +44 (0)20 8996 9001Fax: +44 (0)20 8996 Order hard co
43、py standards securely via: exists in all BS 2000 publications. No part of this publication may be reproduced in any form without the prior permission in writing of BSI and the Energy Institute. Enquiries about copyright should be made to the Secretary of PTI/13 at the Energy Institute.PTI/13BS 2000 SeriesLicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 07/08/2009 03:18, Uncontrolled Copy, (c) BSI