《BS-EN-15489-2007 BS-2000-539-2007.pdf》由会员分享，可在线阅读，更多相关《BS-EN-15489-2007 BS-2000-539-2007.pdf（12页珍藏版）》请在三一文库上搜索。
1、BRITISH STANDARD BS EN 15489:2007 BS 2000-539:2007 Ethanol as a blending component for petrol Determination of water content Karl Fischer coulometric titration method The European Standard EN 15489:2007 has the status of a British Standard ICS 71.080.60 ? Licensed Copy: London South Bank University,
2、 London South Bank University, Wed Oct 17 01:21:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS EN 15489:2007 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 56677 6 National forew
3、ord This British Standard is the UK implementation of EN 15489:2007. 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 Insti
4、tute, under 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. Fu
5、rther information 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 Britis
6、h Standard 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 01:21:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE N
7、ORM EN 15489 August 2007 ICS 71.080.60 English Version Ethanol as a blending component for petrol - Determination of water content - Karl Fischer coulometric titration method Ethanol comme base de mlange lessence - Dtermination de la teneur en eau - Mthode de titrage coulomtrique Karl Fischer Ethano
8、l zur Verwendung als Blendkomponente in Ottokraftstoff - Bestimmung des Wassergehaltes - Coulometrisches Titrationsverfahren nach Karl Fischer 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 con
9、ditions for giving this European Standard the status 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 th
10、ree official versions (English, French, German). A version 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
11、 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, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN
12、 COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION 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 15489:2007: E Licensed Copy: Lo
13、ndon South Bank University, London South Bank University, Wed Oct 17 01:21:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15489:2007 (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 an
14、d sample handling. 5 8 Apparatus preparation 5 9 Apparatus verification 6 10 Procedure 6 11 Calculation. 7 12 Expression of results 7 13 Precision 7 13.1 General. 7 13.2 Repeatability, r 7 13.3 Reproducibility, R . 7 14 Test report . 8 Bibliography . 9 Licensed Copy: London South Bank University, Lo
15、ndon South Bank University, Wed Oct 17 01:21:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15489:2007 (E) 3 Foreword This document (EN 15489:2007) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biological o
16、rigin”, 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 February 2008, and conflicting national standards shall be withdrawn at the latest by February 2008
17、. This document was prepared by CEN/TC 19s Ethanol Task Force and is based on the Energy Institute standard IP 539 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, Bu
18、lgaria, 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: London South
19、 Bank University, London South Bank University, Wed Oct 17 01:21:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15489:2007 (E) 4 1 Scope This European Standard specifies a method for the direct determination of water in ethanol to be used in gasoline blends. It is applicable to ethanol having wate
20、r contents in the range 0,039 % (m/m) to 0,500 % (m/m). NOTE For the purposes of this document, the term “% (m/m)” is used to represent the mass fraction. WARNING Use of this standard may involve hazardous materials, operations and equipment. This standard does not purport to address all of the safe
21、ty problems associated with 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
22、application of 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) EN ISO 3696, Water for analytical laboratory us
23、e Specification and test methods (ISO 3696:1987) 3 Terms and definitions For the purposes of this European Standard, the following terms and definitions apply. 3.1 water content content of water determined by coulometric Karl Fischer procedure as given in this document 4 Principle A weighed test por
24、tion is injected into the titration vessel of a coulometric Karl Fischer apparatus in which iodine for the Karl Fischer reaction is generated coulometrically at the anode. When all the water has been titrated, excess iodine is detected by an electrometric end-point detector and the titration is term
25、inated. Based on the stoichiometry of the reaction, one mole of iodine reacts with one mole of water, thus the quantity of water is proportional to the total integrated current according to Faradays Law. 5 Reagents and materials Use only reagents of recognized analytical grade and water complying wi
26、th the requirements of grade 3 of EN ISO 3696. 5.1 Xylene, water free Remove dissolved water from the xylene by adding approximately 100 g of activated molecular sieve (5.3) to approximately 2 l of xylene. Allow to stand overnight. Licensed Copy: London South Bank University, London South Bank Unive
27、rsity, Wed Oct 17 01:21:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15489:2007 (E) 5 5.2 Karl Fischer reagent, pyridine free. Use commercially available reagents that meet the performance requirements described in clause 9. 5.2.1 Anode electrolyte solution (anolyte) 5.2.2 Cathode electrolyte so
28、lution (catholyte) 5.2.3 Single Karl Fischer Reagents, for use in place of dual electrolyte solutions (5.2.1 and 5.2.2) in cells with or without a diaphragm. 5.3 Molecular sieve pellets Activate by placing in an oven at 200 C to 250 C for 4 h. Remove from the oven and transfer immediately to either
29、a dry glass bottle fitted with a gas-tight closure or a desiccator. Allow to cool before use. 6 Apparatus 6.1 Automatic coulometric Karl Fischer titrator, capable of meeting the requirements given in clause 9. 6.2 Syringes, of glass, with needles of suitable length such that the tip can reach under
30、the surface of the anolyte when inserted through the inlet-port septum. The bores of the needles used shall be kept as small as possible, but large enough to avoid problems arising from back pressure or blocking whilst sampling. NOTE 1 Needles with bores between 0,5 mm and 0,8 mm have been found sui
31、table. NOTE 2 Recommended syringe sizes are: a) 10 l with a fixed needle for periodic checking of the titrator performance, and b) 1 ml or 2 ml for the ethanol test portion. 6.3 Balance, capable of weighing to 0,1 mg. 7 Sampling and sample handling 7.1 Samples shall be taken as described in EN ISO 3
32、170. 7.2 Take care to minimise the uptake of atmospheric moisture during sampling and sample handling. NOTE The use of a glass bottle that can be sealed with a septum has been found suitable for sampling and sample handling. A test portion of the sample can be taken through the septum with a syringe
33、 fitted with a needle. 8 Apparatus preparation 8.1 Follow the manufacturers directions for preparation and operation of the titration apparatus. 8.2 Seal all joints and connections to the titration cell to prevent atmospheric moisture from entering. 8.3 If a single Karl Fischer solution (5.2.3) is u
34、sed, add this solution to the cell. 8.4 If separate electrolyte solutions are used, add the anolyte (5.2.1) to the outer compartment of the titration cell to the level recommended by the manufacturer. Add the catholyte (5.2.2) to the inner compartment of the titration cell to a level 2 mm to 3 mm be
35、low the level of the anolyte. Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15489:2007 (E) 6 8.5 Turn on the titrator and stirrer. Allow the residual moisture in the titration cell to be titrated until the
36、 end- point is reached. Do not proceed beyond this stage until the background current (or background titration rate) is constant and less than the maximum recommended by the manufacturer of the instrument. NOTE High background current for a prolonged period can be attributable to moisture on the ins
37、ide walls of the titration cell. Gentle swirling of the cell will wash the inside with electrolyte. Also check all fittings to ensure atmospheric moisture does not enter the cell. It is recommended that the titrator be permanently switched on to stabilize to a low background current. 8.6 If the vess
38、el becomes contaminated with a previously tested organic sample, thoroughly clean the anode and cathode compartments with xylene (5.1). If the frit becomes blocked, thoroughly clean with xylene. Do not use acetone or other ketones for cleaning or drying the apparatus. 9 Apparatus verification The wa
39、ter titrated is a direct function of the coulombs of electricity consumed. However, reagent performance deteriorates with use and shall be regularly monitored by accurately injecting 10 l of water. Suggested monitoring intervals are done initially when fresh reagents are used and then after every 10
40、 injections. Replace the anolyte (5.2.1) and catholyte (5.2.2) solutions, or the single Karl Fischer solution (5.2.3), whenever one of the following occurs: a) result from a 10 l injection of water is outside 10 000 g 200 g, or persistently high; b) unstable background current, or phase separation i
41、n the outer compartment, or organic products coating the electrodes; c) total sample content of the titration cell exceeds one third of the volume of the anolyte; d) titrator displays error messages which suggests replacing the electrolytes (see the manufacturers instructions). 10 Procedure 10.1 Usi
42、ng a clean, dry syringe (6.2) to withdraw at least three portions of the sample and discard as waste. Immediately withdraw a 1 ml to 2 ml test portion of the sample, clean the needle with a paper tissue and using the balance (6.3) weigh the syringe and contents to the nearest 0,1 mg. 10.2 Insert the
43、 needle through the inlet-port septum, start the titration and, with the tip of the needle just below the liquid surface, inject the entire test portion. Withdraw the syringe, wipe the needle with a clean tissue, and reweigh the syringe to the nearest 0,1 mg. 10.3 The apparatus will automatically ti
44、trate the water present. After the end-point is reached, record the water titrated from the display on the titrator (6.1). Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15489:2007 (E) 7 11 Calculation Calc
45、ulate the water content of the sample, Cs, expressed in % (m/m), using the following equation: 4 1 2 s 10 = m m C (1) where m1 is the mass of the test portion, expressed in grams; m2 is the mass of water displayed by the titrator, expressed in micrograms. 12 Expression of results Report the water co
46、ntent of the sample to the nearest 0,001 % (m/m). 13 Precision 13.1 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 bio materials such as raw wine, molasses, pulp and c
47、orn. NOTE The interlaboratory testing and the statistical evaluation are detailed in Research Report: IP 539 2. 13.2 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
48、 the long run, in the normal and correct operation of the test method, exceed the following value in only one case in twenty. r = 0,011 16 (X + 1) (2) where X is the average of results being compared. Typical values are given in Table 1. 13.3 Reproducibility, R The difference between two single and
49、independent results, obtained by different operators working in different laboratories on identical test material, would in the long run, in the normal and correct operation of the test method, exceed the following value only in one case in twenty. R = 0,018 80 (X + 1) (3) where X is the average of results being compared. Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15489:2007 (