1、Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:07, Uncontrolled Copy, (c) BSIg49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58i
2、norganic chloride Potentiometric methodThe European Standard EN 15484:2007 has the status of a British StandardICS 71.080.60Ethanol as a blending component for petrol Determination of BRITISH STANDARDBS EN 15484:2007 BS 2000-552:2007BS EN 15484:2007Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDAR
3、DS, 12/12/2007 02:07, Uncontrolled Copy, (c) BSIThis BritiThe PTArequest to its EnBSNational forewordThis British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2007 BSI and Energy Institute 2007ISBN 978 0 580 56672 1Compliance with a British
4、Standard cannot confer immunity from legal obligations.Amendments issued since publicationAmd. No. Date Commentsboth 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 availab
5、le 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.sh Standard is the UK implementation of EN 15484:2007.
6、UK participation in its preparation was entrusted to Technical Committee I/13, Petroleum testing and terminology.list of organizations represented on this committee can be obtained on secretary.ergy Institute, under the brand of IP, publishes and sells all Parts of 2000, and all BS EN petroleum test
7、 methods that would be Part of BS 2000, EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15484August 2007ICS 71.080.60English VersionEthanol as a blending component for petrol - Determination ofinorganic chloride - Potentiometric methodEthanol comme base de mlange lessence - Dosage duchlorure minra
8、l - Mthode potentiomtriqueEthanol zur Verwendung als Blendkomponente inOttokraftstoff - Bestimmung des Gehalts an anorganischenChloriden aus dem Eindampfrckstand -Potentiometrisches VerfahrenThis European Standard was approved by CEN on 30 June 2007.CEN members are bound to comply with the CEN/CENEL
9、EC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CE
10、N 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 member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN mem
11、bers are the national standards bodies of 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, S
12、witzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No.
13、EN 15484:2007: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:07, Uncontrolled Copy, (c) BSIEN 15484:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents and materials 4 5 Apparatus .5 6 Samples and sampling5 7 Calibration 6 7.1 Prepara
14、tion of the blank test solution .6 7.2 Preparation of a 5,00 ml standard solution.6 7.3 Titration.6 7.4 Standardisation of 10,00 ml potassium chloride solution.7 7.5 Calculation of concentration of silver nitrate solution 7 7.6 Calculation of value of blank test.7 8 Sample analysis.7 8.1 Preparation
15、 of the dry residue7 8.2 Preparation of the sample solution7 8.3 Titration.8 9 Calculation8 10 Expression of results 8 11 Precision.8 11.1 Repeatability, r .8 11.2 Reproducibility, R 8 12 Test report 9 Annex A (informative) Measurement example .10 Annex B (informative) Interferences11 B.1 Introducti
16、on11 B.2 Other halogens.11 B.3 Oxidizing agents 11 B.4 Ammonium and iron (III) salts 11 B.5 Cyanides, thiocyanates and sulphides .11 Bibliography 12 Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:07, Uncontrolled Copy, (c) BSIEN 15484:2007 (E) 3 Foreword This document (EN 15484
17、:2007) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related produts 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
18、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. The method described in this document is based on ISO 6227 1 and a method from a European Regulation on wine 2. According to the CEN/CENELEC I
19、nternal 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, Ireland, Italy, Latvia, Lithuania, Luxembourg,
20、 Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:07, Uncontrolled Copy, (c) BSIEN 15484:2007 (E) 4 1 Scope This standard specifies a potentiometric method fo
21、r the determination of inorganic chloride content in ethanol from 4 mg/l to 30 mg/l. The chloride content is determined in aqueous solution after dissolution of the evaporation residue of the ethanol sample. WARNING Use of this standard may involve hazardous materials, operations and equipment. This
22、 standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use. NOTE For the purposes of thi
23、s document, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass fraction and the volume fraction. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For unda
24、ted 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 methods (ISO 3696:1987) 3 Principle A weighed test portion of ethan
25、ol sample is evaporated on a water bath. The dry residue is dissolved in deionised water. Inorganic chloride content is determined by potentiometric titration either manually or using automated equipment. 4 Reagents and materials All reagents shall be of analytical reagent grade or of higher purity.
26、 4.1 Acetone. 4.2 Nitric acid, approximately 1,40 g/ml, about 68 % (m/m) solution. 4.3 Potassium nitrate, solution saturated at room temperature. 4.4 Silver nitrate solution 1, c (AgNO3) = 0,1 mol/l approximately. Dissolve 8,5 g of silver nitrate in a 500 ml one-mark volumetric flask, dilute to the
27、mark and mix. Store in a dark glass bottle. 4.5 Silver nitrate solution 2, c (AgNO3) = 0,004 mol/l approximately. Prepare the solution at the time of use from silver nitrate solution 1 (4.4), diluting when required in a one-mark volumetric flask. 4.6 Potassium chloride standard reference solution 1,
28、 c (KCl) = 0,100 mol/l. Weigh 3,727 6 g of potassium chloride to the nearest 0,000 1 g. Potassium chloride was previously dried for 1 h at about 130 C and cooled in a dessicator. Dissolve in a little water and transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to th
29、e mark and mix. This solution shall not be kept for more than one month. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:07, Uncontrolled Copy, (c) BSIEN 15484:2007 (E) 5 4.7 Potassium chloride standard reference solution 2, c (KCl) = 0,004 mol/l. Prepare the solution at the tim
30、e of use from the standard reference potassium chloride solution 1 (4.6), diluting when required in a one-mark volumetric flask. 4.8 Water, for analytical laboratory use, conforming to grade 3 of EN ISO 3696. 5 Apparatus 5.1 Evaporating dish, capacity 100 ml to 250 ml. 5.2 Water bath 5.3 Drying oven
31、, thermostatically controlled at (105 2) C. 5.4 Dessicator, containing freshly activated silica gel (or equivalent desiccant) with moisture a content indicator. 5.5 Analytical balance, capable of weighing to the nearest 0,1 mg. 5.6 Pipette, volumetric, class A, capable of delivering 25 ml. 5.7 Poten
32、tiometric titration apparatus, comprising: 5.7.1 Potentiometer, sensitivity at least 2 mV, covering the range 500 mV to +500 mV. 5.7.2 Reference electrodes. 5.7.2.1 Calomel electrode, fitted with a reservoir filled with saturated potassium chloride solution, or 5.7.2.2 Double junction silver/silver
33、chloride electrode. The outer electrolyte must be saturated potassium nitrate solution (4.3), the inner electrolyte may be potassium chloride 3 mol/l or saturated potassium nitrate (4.3). 5.7.3 Bridge, containing saturated potassium nitrate solution (4.3), to be connected to the calomel electrode (5
34、.7.2.1) and fitted with porous diaphragms at the ends. 5.7.4 Measuring electrodes, being either 5.7.4.1 Silver electrode, or 5.7.4.2 Chloride or silver ion-selective electrode. 5.8 One-mark flasks, 25 ml volume. 5.9 Magnetic stirrer, with a polytetrafluorethylene (PFTE)-coated rod. 5.10 Burettes, wi
35、th fine point tip, graduated in 0,02 ml or 0,01 ml divisions. 6 Samples and sampling Unless otherwise specified, laboratory samples shall be obtained by the procedures described in EN ISO 3170. High density polyethylene containers shall be used. The containers should be carefully cleaned and rinsed
36、with pure water before use to avoid contamination. Samples should be analysed as soon as possible after removal from bulk supplies, to prevent loss of chloride. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:07, Uncontrolled Copy, (c) BSIEN 15484:2007 (E) 6 Thoroughly mix sampl
37、es in their containers immediately prior to drawing test portions. 7 Calibration 7.1 Preparation of the blank test solution At the same time as the determination, carry out a blank test, using 25 ml of water (4.8). 7.2 Preparation of a 5,00 ml standard solution 7.2.1 Place the blank test solution in
38、 a beaker of suitable capacity. Add, using one of the burettes (5.10), 5,00 ml of the potassium chloride solution (4.7). 7.2.2 Add a quantity of the acetone (4.1) to obtain a ratio of acetone to aqueous solution preferably equal to 80/10 (V/V) but, in any case, not lower than 50/50 (V/V). 7.3 Titrat
39、ion Introduce into the beaker a magnetic stirrer rod (5.9), place the beaker on the stirrer and set it in motion. Introduce in the solution the measuring electrode (5.7.4) and the reference electrode (5.7.2). If, however, a calomel electrode (5.7.2.1) is used, introduce one end of the bridge (5.7.3)
40、 instead of the reference electrode and immerse the other end in a beaker of water containing the calomel electrode. Connect the electrodes to the potentiometer (5.7.1) and record the initial value of the potential, after having checked the zero setting of the instruments. Execute the titration by a
41、dding silver nitrate solution (4.5) in successive increments of 0,1 ml each. After each addition, wait for the potential to reach the steady value. In the first two columns of a table, note the successive volumes added and the corresponding potentials. In a third column, note the successive incremen
42、ts (1E) of the potential E. In a fourth column, note the differences (2E), positive or negative, between the successive increments (1E) of the potential E. The end of the titration corresponds to the addition of the 0,1 ml (V1) of the silver nitrate solution, which gives the maximum value of 1E. The
43、 exact volume (Veq), in ml, of silver nitrate solution (4.5) corresponding to the end of the reaction is given by the equation (for better comprehension see the example in Annex A): +=BbVVV10eq(1) where V0is the volume, in ml, of the silver nitrate solution (4.5) which gives the maximum increment of
44、 1E; V1is the volume, in millilitres, of the silver nitrate solution (4.5); b is the first negative increment of 2E; B is the sum of the absolute values of the last positive increment of 2E and the first negative increment of 2E. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:0
45、7, Uncontrolled Copy, (c) BSIEN 15484:2007 (E) 7 7.4 Standardisation of 10,00 ml potassium chloride solution. Repeat the operations specified in Error! Reference source not found. and 7.3, this time using 10,00 ml instead of 5,00 ml, of potassium chloride solution (4.7). 7.5 Calculation of concentra
46、tion of silver nitrate solution The concentration of the silver nitrate solution, c(AgNO3), expressed as moles of AgNO3 per litre, is given by the equation: ()()()3235KClAgNOVVcc=(2) where c(KCl) is the concentration, in mol/l, of potassium chloride solution (4.7); V2is the value, in ml, of Veqcorre
47、sponding to the titration of 10 ml of potassium chloride solution (4.7), in the presence of blank test solution; V3is the value, in ml, of Veqcorresponding to the titration of 5 ml of potassium chloride solution (4.7), in the presence of blank test solution; 5 being the difference, in ml, between th
48、e two volumes of potassium chloride solution (4.7). 7.6 Calculation of value of blank test The value of the reagent blank test, V4, is given, in ml, by the equation: 2342 VVV = (3) where V2 and V3are as defined in 7.5. 8 Sample analysis IMPORTANT One should always be aware of interferences originati
49、ng from specific elements in the sample. Some known interferences are indicated in Annex B. 8.1 Preparation of the dry residue Add 25 ml (VE) of test portion to the evaporating dish (5.1). Place the dish with sample on the boiling water bath (5.2) and allow to dry. Place the dish in the oven (5.3) at 105 C for 30 min and then transfer the dish to a desiccator (5.4). Allow the dish to cool for 30 min. Add 10 ml of water (4.8), to the evaporating dish and heat gently until complete dissolution of the dry residue. Transfer the solution t
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