1、Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:21, Uncontrolled Copy, (c) BSIg49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58p
2、hosphorus content Ammonium molybdate spectrometric methodThe European Standard EN 15487:2007 has the status of a British StandardICS 71.080.60Ethanol as a blending component for petrol Determination of BRITISH STANDARDBS EN 15487:2007 BS 2000-555:2007BS EN 15487:2007Licensed Copy: Wang Bin, ISO/EXCH
3、ANGE CHINA STANDARDS, 12/12/2007 02:21, Uncontrolled Copy, (c) BSIThis BritiThe PTArequest to its EnBSThis 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 56675 2Compliance 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 availa
5、ble 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.National forewordsh Standard is the UK implementation
6、 of EN 15487:2007.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
7、 EN petroleum test methods that would be Part of BS 2000, EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15487August 2007ICS 71.080.60English VersionEthanol as a blending component for petrol - Determination ofphosphorus content - Ammonium molybdate spectrometricmethodthanol comme base de mlange
8、lessence -Dtermination de la teneur en phosphore - Mthodespectromtrique au molybdate dammoniumEthanol zur Verwendung als Blendkomponente inOttokraftstoff - Bestimmung des Phosphorgehaltes -Spektrometrisches Verfahren mit AmmoniummolybdatThis European Standard was approved by CEN on 30 June 2007.CEN
9、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 bibliographical references concerning such nationalstandards may be obtained on applica
10、tion 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 member into its own language and notified to the CEN Management Centre has t
11、he 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, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal
12、,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland 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 reserv
13、edworldwide for CEN national Members.Ref. No. EN 15487:2007: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:21, Uncontrolled Copy, (c) BSIEN 15487:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents and materials 4 5 Apparatus .5 6 Sam
14、ples and sampling6 7 Calibration 6 7.1 Preparation of calibration solutions 6 7.2 Colour development 6 7.3 Spectrometric measurement 6 7.4 Calibration regression line .6 8 Procedure .7 8.1 Dry residue .7 8.2 Test portion 7 8.3 Colour development 7 8.3 Spectrometric measurement 7 9 Calculation7 10 Ex
15、pression of results 7 11 Precision.8 11.1 Repeatability.8 11.2 Reproducibility.8 12 Test report 8 Bibliography 9 Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:21, Uncontrolled Copy, (c) BSIEN 15487:2007 (E) 3 Foreword This document (EN 15487:2007) has been prepared by Technica
16、l 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 national standard, either by publication of an identical text or by endorsem
17、ent, 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 EN ISO 6878 1 and a method from a European Regulation on wine 2. According to the CEN/CENELEC Internal Regulations, the nationa
18、l 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, Malta, Netherlands, Norway, Pol
19、and, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:21, Uncontrolled Copy, (c) BSIEN 15487:2007 (E) 4 1 Scope This standard specifies a procedure for the determination of phosphorus content me
20、asured as orthophosphate, in ethanol from 0,15 mg/l to 1,50 mg/l by ammonium molybdate spectrometric method. The phosphorus 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, oper
21、ations and equipment. This 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. 2
22、Normative references The following referenced documents are indispensable for the 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 liqui
23、ds Manual sampling (ISO 3170:2004) EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 3 Principle After evaporation of the ethanol sample, the dry residue is dissolved in water. The aqueous solution is treated with an acid solution containing molybdate an
24、d antimony ions to obtain an antimony phosphomolybdate complex. The complex is then treated with ascorbic acid to form a strongly coloured molybdenum blue complex. The content of phosphorus is obtained by measuring the absorbance of the complex at 880 nm. 4 Reagents and materials 4.1 All reagents sh
25、all be of analytical reagent grade or of higher purity. 4.2 Water, for analytical laboratory use, conforming to grade 3 of ISO 3696. 4.3 Sulphuric acid solution, c(H2SO4) 9 mol/l Add 500 ml 5 ml water (4.2) to a 2 l beaker. Cautiously add, with continuous stirring and cooling, 500 ml 5 ml sulphuric
26、acid, = 1,84 g/ml. Mix well and allow the solution to cool to room temperature. 4.4 Hydrochloric acid solution, c(HCl) 2,4 mol/l Cautiously add in a 1 000 ml volumetric flask (5.4), 200 ml 10 ml of concentrated hydrochloric acid ( = 1,18 g/ml) to 500 ml 10 ml water (4.2). Mix and cool to room temper
27、ature. Make up to 1 000 ml with water (4.2). 4.5 Sodium hydroxide solution, c(NaOH) = 2 mol/l Dissolve 80 g 1 g sodium hydroxide pellets in water (4.2) in a 1 000 ml volumetric flask (5.4), cool and dilute to 1 l with water (4.2). 4.6 Ascorbic acid solution, c(C6H8O6) = 100 g/l Dissolve 10 g 0,5 g a
28、scorbic acid in 100 ml 5 ml water (4.2). NOTE The solution is stable for 2 weeks if stored in an amber glass bottle in a refrigerator and can be used as long as it remains colourless. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:21, Uncontrolled Copy, (c) BSIEN 15487:2007 (E)
29、 5 4.7 Acid molybdate solution Dissolve 13 g 0,5 g ammonium heptamolybdate tetrahydrate (NH4)6Mo7O244H2O in 100 ml 5 ml water (4.2). Dissolve 0,35 g 0,05 g antimony potassium tartrate hemihydrate K(SbO)C4H4O6H2O in 100 ml 5 ml water (4.2). Add the molybdate solution to 300 ml 5 ml sulphuric acid (4.
30、3) with continuous stirring. Add the tartrate solution and mix well. NOTE The reagent is stable for at least 2 months if stored in an amber glass bottle. 4.8 Orthophosphate stock standard solution, c(P) = 50 mg/l Dry a few grams of potassium dihydrogen phosphate (KH2PO4) to constant mass at 105 C. W
31、eigh about 0,220 g of KH2PO4with a precision of 0,000 1 g and dissolve in about 800 ml 10 ml water (4.2) in a 1 000 ml volumetric flask. Add 10 ml 0,5 ml sulphuric acid (4.3) and make up to the mark with water (4.2). Alternatively, use a commercially available stock solution. NOTE The solution is st
32、able for at least 3 months if stored in a well stopped glass bottle. Refrigeration to about 4 C is recommended. 4.9 Orthophosphate standard solution, c(P) = 2 mg/l Pipette 20 ml 0,01 ml orthophosphate stock standard solution (4.8) into a 500 ml volumetric flask. Make up to the mark with water (4.2)
33、and mix well. Prepare and use this solution each day as required. 5 Apparatus 5.1 Water bath 5.2 Evaporating dish, capacity 100 ml to 250 ml. 5.3 Volumetric pipettes , Class A. 5.4 Volumetric flasks, Class A. 5.5 Burettes, calibrated burettes of 10 ml and 50 ml capacity with 0,05 ml and 0,1 ml subdi
34、vision respectively. 5.6 Desiccator, containing freshly activated silica gel (or equivalent desiccant) with moisture content indicator. 5.7 Oven, thermostatically controlled at (105 2) C. 5.8 Spectrometer, suitable for measuring absorbance at 880 nm and capable of accepting optical cells with a thic
35、kness 10 mm. 5.9 Laboratory glassware Before use, wash all glassware, for example with hydrochloric acid (4.4), at approximately 40 C to 50 C and rinse thoroughly with water (4.2). Detergents containing phosphate shall not be used. Preferably the glassware should be used only for the determination o
36、f phosphorus. After use, clean it as described above and keep covered until needed again. Rinse glassware used for the colour development and optical cells occasionally with sodium hydroxide solution (4.5), followed by thorough rinsing with water (4.2), to remove deposits of the coloured complex whi
37、ch has a tendency to stick as a thin film on the wall of glassware. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:21, Uncontrolled Copy, (c) BSIEN 15487:2007 (E) 6 6 Samples and sampling Unless otherwise specified, laboratory samples shall be obtained by the procedures describ
38、ed in EN ISO 3170. High density polyethylene containers shall be used. The containers should be carefully cleaned and rinsed with pure water to avoid contamination. Particular attention should be paid to avoid contamination from phosphorus containing detergents. Samples should be analysed as soon as
39、 possible after removal from bulk supplies to prevent possible loss of phosphorus. Thoroughly mix samples in their containers immediately prior to withdrawal of the test portions. NOTE High density polyethylene containers are used in order to prevent losses of phosphorus by wall absorption. 7 Calibr
40、ation 7.1 Preparation of calibration solutions Transfer, by means of a volumetric pipette (5.3), 2,5 ml, 5,0 ml, 10,0 ml, 20,0 ml, 30,0 ml, and 40,0 ml of orthophosphate standard solution (4.9) to 50 ml volumetric flasks. Dilute with water (4.2) to about 40 ml. As an alternative, volumes from 2,5 ml
41、 to 10,0 ml can be transferred using a 10 ml burette (5.5) and volumes from 20,0 ml to 40,0 ml using a 50 ml burette (5.5). Transfer about 40 ml of water (4.2) to a 50 ml volumetric flask (blank solution). 7.2 Colour development Add to each flask, while swirling, 1 ml of ascorbic acid (4.6) followed
42、 by 2 ml of acid molybdate solution (4.7). Make up to the mark with water (4.2) and mix well. Phosphorus concentration in the calibration solutions is given in Table 1. Table 1 Phosphorus concentration of calibration solutions Calibration solution Orthophosphate solution ml Phosphorus concentration
43、mg/l 1 (blank) 0 0 2 2,5 0,1 3 5,0 0,2 4 10,0 0,4 5 20,0 0,8 6 30,0 1,2 7 40,0 1,6 7.3 Spectrometric measurement Set up the spectrometer (5.8) according to the manufacturer instructions. Measure, using 10 mm cells, the absorbance of each solution at 880 nm after a period between 10 min and 30 min. U
44、se water (4.2) in the reference cell. 7.4 Calibration regression line Plot the absorbance (as the y-axis) against phosphorus concentration in mg/l (as the x-axis) of the calibration solutions. The relationship between absorbance and concentration is linear. Calculate the linear regression Licensed C
45、opy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:21, Uncontrolled Copy, (c) BSIEN 15487:2007 (E) 7 bXaY += (1) where Y is the absorbance; X is the phosphorus concentration in mg/l; a is the slope of the linear regression; b is the intercept of the linear regression. Verify the linear regre
46、ssion from time to time for slope and intercept, especially if new batches of chemicals are used. 8 Procedure 8.1 Dry residue Add (50 0,5) ml ethanol sample to the evaporating dish (5.2) using a 25 ml pipette (5.3). Place the dish with sample on the water bath (5.1) and allow to dry. Place the dish
47、in the oven (5.7) at 105 C for 30 minutes and then transfer the dish in a desiccator (5.6). Allow the dish to cool for 30 minutes. NOTE The time usually required to obtain the dry residue ranges from 2 hours to 3 hours. 8.2 Test portion Add about 10 ml water (4.2) to the evaporating dish (5.2) and w
48、arm gently to solubilize the dry residue. Transfer the solution to a 50 ml volumetric flask (5.4). Repeat the treatment with 10 ml water (4.2) to rinse carefully the evaporating dish (5.2) and to transfer quantitatively the residue. 8.3 Colour development Add to the flask, while swirling, 1 ml of as
49、corbic acid (4.6) followed by 2 ml acid molybdate solution (4.7). Make up to the mark with water (4.2) and mix well. 8.3 Spectrometric measurement Follow the procedure outlined in 7.3. 9 Calculation Calculate the phosphorus content P, expressed in mg/l, using the equation: abAP=(2) where A is the absorbance of the test portion; b is the intercept of the calibration regression (see 7.4); a is the slope of the calibration regression, expressed in l/mg (see 7.4). 10 Expression of results Report the phosphoru
