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1、BRITISH STANDARD BS EN 15491:2007 BS 2000-538:2007 Ethanol as a blending component for petrol Determination of total acidity Colour indicator titration method The European Standard EN 15491:2007 has the status of a British Standard ICS 71.080.60 ? Licensed Copy: London South Bank University, London
2、South Bank University, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS EN 15491:2007 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2007 BSI and Energy Institute 2007 ISBN 978 0 580 56679 0 National foreword This
3、 British Standard is the UK implementation of EN 15491:2007. The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum testing and terminology. A list of organizations represented on this committee can be obtained on request to its secretary. Energy Institute, un
4、der the brand of IP, publishes and sells all Parts of BS 2000, and all BS EN petroleum test methods 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 in
5、formation is available from: Energy Institute, 61 New Cavendish Street, London W1G 7AR. Tel: 020 7467 7100. Fax: 020 7255 1472. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standa
6、rd cannot confer immunity from legal obligations. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1
7、5491 August 2007 ICS 71.080.60 English Version Ethanol as a blending component for petrol - Determination of total acidity - Colour indicator titration method Ethanol comme base de mlange lessence - Dtermination de lacidit totale - Mthode de titrage par indicateur color Ethanol zur Verwendung als Bl
8、endkomponente in Ottokraftstoff - Bestimmung der Gesamtsurezahl - Farbindikator-Titration This European Standard was approved by CEN on 30 June 2007. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status
9、of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards 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 ve
10、rsion in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic,
11、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. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMA
12、LISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2007 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15491:2007: E Licensed Copy: London South Bank University, London South Bank Univers
13、ity, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15491:2007 (E) 2 Contents Page Foreword. 3 1 Scope 4 2 Normative references . 4 3 Terms and definitions. 4 4 Principle. 4 5 Reagents and materials 4 6 Apparatus 5 7 Sampling and sample handling. 6 8 Procedure 6 9 Calculation. 6 1
14、0 Expression of results 6 11 Precision 7 11.1 General. 7 11.2 Repeatability, r 7 11.3 Reproducibility, R . 7 12 Test report . 7 Bibliography . 8 Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15491:2007 (E)
15、 3 Foreword This document (EN 15491:2007) has been prepared by Technical Committee CEN/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 natio
16、nal standard, either by publication of an identical text or by endorsement, at the latest by February 2008, and conflicting national standards shall be withdrawn at the latest by February 2008. This document was prepared by CEN/TC 19s Ethanol Task Force and is based on the Energy Institute standard
17、IP 538 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Irelan
18、d, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI
19、 EN 15491:2007 (E) 4 1 Scope This European Standard specifies a method for determining the total acidity, calculated as acetic acid, of ethanol to be used in petrol blends. It is applicable to ethanol having total acid contents of between 0,003 % (m/m) to 0,015 % (m/m). NOTE For the purposes of this
20、 European Standard, the term “% (m/m)” and “% (V/V)” are used to represent the mass fraction and the volume fraction respectively. WARNING Use of this standard may involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associated w
21、ith its use. It is the responsibility of the user of this standard to 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 this docu
22、ment. 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) EN ISO 3696, Water for analytical laboratory use Specification and test
23、 methods (ISO 3696:1987) 3 Terms and definitions For the purposes of this European Standard, the following terms and definitions apply. 3.1 total acidity acidity, calculated as acetic acid, determined by titration and colour indicator as given in this standard 4 Principle A test portion of the ethan
24、ol is mixed with an equal volume of neutralized, carbon dioxide free water. The acid content is titrated with potassium hydroxide solution, to the neutral endpoint of phenolphthalein. The total acidity is then calculated as acetic acid. 5 Reagents and materials Use only reagents of recognized analyt
25、ical grade and water complying with the requirements of grade 3 of EN ISO 3696. 5.1 Potassium hydrogen phthalate 5.2 Potassium hydroxide solution 0,01 mol/l, a solution prepared in accordance with 5.2.1 or a commercially available standardized potassium hydroxide solution of equivalent concentration
26、 and purity. The reagent shall be protected against carbon dioxide absorption and restandardized frequently enough to detect concentration changes of 0,000 5 mol/l. Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) B
27、SI EN 15491:2007 (E) 5 5.2.1 Dissolve approximately 0,6 g potassium hydroxide in 1 l of water and standardize using potassium hydrogen phthalate in accordance with 5.2.2. 5.2.2 Dry a quantity of potassium hydrogen phthalate (5.1) in an oven at approximately 120 C for approximately 2 h. Place in a de
28、siccator and allow to cool. Weigh approximately 0,1 g to the nearest 0,1 mg into a 250 ml flask and record this mass. Add approximately 50 ml of carbon dioxide free water (5.5) and swirl to dissolve. Add 2 drops of phenolphthalein indicator solution (5.3) and using a 50 ml burette (6.5), titrate to
29、neutral endpoint with the potassium hydroxide solution. Carry out a blank determination using the same volume of carbon dioxide free water (5.5). Calculate the concentration C, in moles per litre, of the potassium hydroxide solution from the equation: () 01 23,204 1000 VV m C = (1) where m is the ma
30、ss, in grams, of potassium hydrogen phthalate; V1 is the volume, in millilitres, of potassium hydroxide solution for the titration; V0 is the volume, in millilitres, of potassium hydroxide used for the blank. 5.3 Phenolphthalein indicator solution, approximately 10g/l Weigh approximately 1 g of phen
31、olphthalein into the 100 ml volumetric flask (6.1). Add approximately 20 ml of ethanol (5.4) and swirl until dissolved. Make up to 100 ml with ethanol. 5.4 Ethanol, approximately 95 % (V/V). 5.5 Carbon dioxide free water NOTE A suitable way of preparing carbon dioxide free water is to place approxim
32、ately 100 ml of water in a 250 ml conical flask (6.3), fitted with a standard ground glass joint, heat to boiling on either a hot plate or gas burner and boil for 2 min to 3 min. Remove the flask and its contents from the heat and insert a soda-lime filled guard tube (6.7) and cool to ambient temper
33、ature before use. 5.6 Soda lime, for the guard tube (optional). 5.7 Nitrogen, carbon dioxide free (optional). 6 Apparatus 6.1 Volumetric flask, Class A, 100 ml capacity. 6.2 Measuring cylinder, 100 ml capacity. 6.3 Conical flask, glass, with standard ground glass joint, approximately 250 ml capacity
34、. 6.4 Burette, Class A 50 ml capacity. 6.5 Burette, Class A 10 ml capacity and graduated in 0,05 ml, or less, subdivisions. 6.6 Pipette, Class A 50 ml capacity. 6.7 Glass guard tube, with ground glass joint to fit the conical flask (6.3) (optional). Licensed Copy: London South Bank University, Londo
35、n South Bank University, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15491:2007 (E) 6 7 Sampling and sample handling 7.1 Unless otherwise specified, laboratory samples shall be obtained by the procedures described in EN ISO 3170. 7.2 Take care to minimise the uptake of atmosphe
36、ric carbon dioxide during sampling and sample handling. 8 Procedure 8.1 Fill the 10 ml burette (6.5) with the potassium hydroxide solution (5.2). 8.2 Using the measuring cylinder (6.2) measure approximately 50 ml of carbon dioxide free water (5.5) into the conical flask (6.3). Add two drops of pheno
37、lphthalein solution (5.3). Titrate with the standardized potassium hydroxide solution (5.2) to a faint pink endpoint. 8.3 Using the pipette (6.6) add 50 ml of the test portion to the neutralised water. Stopper the flask and swirl to mix the test portion and the water. 8.4 Remove the stopper and imme
38、diately titrate the mixture using the standardized potassium hydroxide to a faint pink end point. Take care not to prolong the titration as the up-take of atmospheric carbon dioxide by the ethanol water mix will appreciably affect the result. NOTE Atmospheric carbon dioxide can be prevented from ent
39、ering the titration flask by bubbling nitrogen (5.7) through the solution during the titration. 8.5 If the density of the ethanol to be tested is not known, determine it, in g/ml, at 15 C to two decimal places. 9 Calculation Calculate the total acidity, As, as acetic acid, of the sample in % (m/m),
40、using the following equation: 0,12 s = VC A (2) where C is the concentration, in moles per litre, of potassium hydroxide solution, see equation (1); V is the volume, in millilitres, of potassium hydroxide solution required to neutralize 50 ml of test portion; is the density, in grams per millilitre,
41、 of the test portion at 15 C. 10 Expression of results Report the total acidity content of the sample to the nearest 0,001 % (m/m). Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15491:2007 (E) 7 11 Precisi
42、on 11.1 General The precision given was derived from statistical analysis by EN ISO 4259 2 of the results of interlaboratory testing of a matrix of ethanol samples produced in Europe from biomaterials such as raw wine, molasses, pulp and corn. NOTE The interlaboratory testing and the statistical eva
43、luation are detailed in Research Report IP 538 3. 11.2 Repeatability, r The difference between two test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material would in the long run, in the normal and correct operation of the test
44、 method, exceed the following value in only one case in twenty. r = 0,000 960 4 11.3 Reproducibility, R The difference between two single and independent results, obtained by different operators working in different laboratories on identical test material, would in the long run, in the normal and co
45、rrect operation of the test method, exceed the following value only in one case in twenty. R = 0,001 370 12 Test report The test report shall contain at least the following information: a) reference to this European Standard, i.e. EN 15491; b) type and complete identification of the product tested;
46、c) result of the test (see 10); d) any deviation, by agreement or otherwise, from the procedure specified; e) date of the test. Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15491:2007 (E) 8 Bibliography 1
47、 IP 538/06, Determination of the total acidity of ethanol Colour indicator titration method. Available from the Energy Institute, 61 New Cavendish Street, London, W1G 7AR, UK. 2 EN ISO 4259, Petroleum products Determination and application of precision data in relation to methods of test (ISO 4259:2
48、006). 3 Research Report: IP 538/06, Precision evaluation on IP 538, Determination of the total acidity of ethanol Colour indicator titration method. Available from the Energy Institute, 61 New Cavendish Street, London, W1G 7AR, UK. Licensed Copy: London South Bank University, London South Bank Unive
49、rsity, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI blank Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:07 GMT+00:00 2007, Uncontrolled Copy, (c) BSI Energy Institute Buying Parts of BS 2000 Orders for BS 2000 publications should be addressed to either: Energy Institute Library and Information Service 61 New Cavendish Street London W1G 7AR Tel: +44 (0)20 7467 7100 Fax: +44 (0)20 7255 1472 www.ener