1、July 2009DEUTSCHE NORM English price group 7No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 75.160.20!$XTm“1534974www.
2、din.deDDIN EN 15691Ethanol as a blending component for petrol Determination of dry residue (involatile material) Gravimetric methodEnglish version of DIN EN 15691:2009-07Ethanol zur Verwendung als Blendkomponente in Ottokraftstoff Bestimmung des Trockenrckstandes (nichtflchtige Bestandteile) Gravime
3、trisches VerfahrenEnglische Fassung DIN EN 15691:2009-07www.beuth.deDocument comprises 9 pagesDIN EN 15691:2009-07 2 National foreword This standard has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biological or
4、igin” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Technical Committee NA 062-06-81 AA Spiegelausschuss zu CEN/TC19 Gasfrmige und flssige Kraft- und Brennstoffe, Schmierstoffe
5、und verwandte Produkte minerallstmmiger, synthetischer oder biologischer Herkunft of the Fachausschuss Minerall- und Brennstoffnormung (FAM). EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15691March 2009ICS 75.160.20English VersionEthanol as a blending component for petrol - Determination ofdry
6、residue (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
7、VerfahrenThis 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 bibliographi
8、cal 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 m
9、ember 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,
10、Latvia, 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 Brussel
11、s 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15691:2009: EEN 15691:2009 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Apparatus .45 Sampling .45.1 Preparation of samples .45.2 Verification an
12、d 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 7DIN EN 15691:2009-07 EN 15691:2009 (E) 3 Foreword This document (EN 15691:2009) has been prepared by Technical Committee CE
13、N/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and 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 la
14、test by September 2009, and conflicting national standards shall be withdrawn at the latest 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
15、 all such patent rights. This document was prepared by CEN/TC 19s Ethanol Task Force under responsibility 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 fo
16、llowing countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, S
17、lovenia, Spain, Sweden, Switzerland and United Kingdom. DIN EN 15691:2009-07 EN 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 stud
18、y 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 as
19、sociated 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 t
20、his 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 re
21、sidue 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, capabl
22、e 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 i
23、n 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. DIN EN 15691:2009-07 EN 15691:2009 (E) 5 5.2 Verification and quality control It is recommended to prepare a sodium
24、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 aqueous solution can be introduced in 1 l of this neutral alcohol without residue. This is a solutio
25、n 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 manipulate dishes, do not touch directly with fingers. Accurately weigh, to the nearest 0,1 mg, the
26、 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 allow to dry. NOTE In general, it takes about two hours to evaporate the alcohol on the water bath.
27、 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, the dishes with residue (M1). 7 Calculation The content of dry residue, D, expressed in mg/100
28、 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 Report the content of dry residue rounded to the nearest 1 mg/100 ml. 9 Precision 9.1 General The p
29、recision 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), molasses, pulp and corn. DIN EN 15691:2009-07 EN 15691:2009 (E) 6 NOTE The interlaboratory te
30、sting and the statistical evaluation are detailed in 2. In some occasions the repeatability is larger than the 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
31、 the standardized test method is applied fully once to a single sample. Unless otherwise stated, the probability 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 opera
32、tor, same apparatus, same laboratory and a short interval of time) should exceed the following value in mg/100 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 ab
33、solute difference between two single test results obtained under different conditions (different operators, different 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 a
34、verage value of results being compared. 10 Test report The test report shall contain at least the following information: 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) resu
35、lts of the test (see 8); e) any deviation, by agreement or otherwise, from the procedure specified in this European Standard, or regarded as optional; f) details of any incidents which may have influenced the test results; g) date of the test. DIN EN 15691:2009-07 EN 15691:2009 (E) 7 Bibliography 1
36、European Commission 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
37、for neutral alcohol 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 data in relation to methods of test (ISO 4259:2006) DIN EN 15691:2009-07
