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1、BRITISH STANDARD BS EN 15485:2007 BS 2000-553:2007 Ethanol as a blending component for petrol Determination of sulfur content Wavelength dispersive X-ray fluorescence spectrometric method The European Standard EN 15485:2007 has the status of a British Standard ICS 71.080.60 ? Licensed Copy: London S
2、outh Bank University, London South Bank University, Wed Oct 17 01:21:09 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS EN 15485:2007 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 5
3、6826 8 National foreword This British Standard is the UK implementation of EN 15485:2007. 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 se
4、cretary. Energy Institute, 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”
5、 and individually. Further 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. Com
6、pliance with a British 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 01:21:09 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME E
7、UROPENNE EUROPISCHE NORM EN 15485 August 2007 ICS 71.080.60 English Version Ethanol as a blending component for petrol - Determination of sulfur content - Wavelength dispersive X-ray fluorescence spectrometric method thanol comme base de mlange lessence - Dosage du soufre - Mthode par fluorescence X
8、 dispersive en longueur donde Ethanol zur Verwendung als Blendkomponente in Ottokraftstoff - Bestimmung des Schwefelgehaltes - Wellenlngendispersive Rntgenfluoreszenz-Spektrometrie (wdRFA) This European Standard was approved by CEN on 30 June 2007. CEN members are bound to comply with the CEN/CENELE
9、C Internal Regulations which stipulate the conditions 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 C
10、EN member. This European Standard exists in three 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. CE
11、N 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, Romania, Slovakia, Slovenia, Spain, Sw
12、eden, Switzerland and United Kingdom. EUROPEAN 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 Member
13、s. Ref. No. EN 15485:2007: E Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:09 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15485:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references4 3 Principle4 4 Reagents and materials 4 5 Apparatus .4
14、6 Samples and sampling5 7 Preparation of calibration solutions5 7.1 Blank calibration solution.5 7.2 Stock solution5 7.3 Calibration solutions.5 7.4 Storage and stability of the calibration solutions6 8 Settings.6 8.1 Measuring parameters 6 8.2 Optimization.6 8.3 Performance check of the spectromete
15、r.6 9 Calibration6 9.1 General6 9.2 Calibration solutions.7 9.3 Calibration curves7 9.4 Checking.7 10 Procedure .7 11 Expression of results 8 12 Precision.8 12.1 Repeatability.8 12.2 Reproducibility.8 13 Test report8 Bibliography9 Licensed Copy: London South Bank University, London South Bank Univer
16、sity, Wed Oct 17 01:21:09 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15485:2007 (E) 3 Foreword This document (EN 15485:2007) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biological origin”, the secretaria
17、t 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. The method described
18、 in this document is based on EN ISO 20884 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, Germa
19、ny, 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 Bank University, London South Bank University, Wed Oct 17 01:21:09 GMT+00
20、:00 2007, Uncontrolled Copy, (c) BSI EN 15485:2007 (E) 4 1 Scope This document specifies a wavelength-dispersive X-ray fluorescence (WDXRF) test method for the determination of the sulfur content of ethanol from 7 mg/kg to 20 mg/kg. NOTE For the purposes of this European Standard, the term “% (m/m)“
21、 is used to represent the mass fraction of a material. 2 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 (includ
22、ing any amendments) applies. EN ISO 3170, Petroleum liquids Manual sampling (ISO 3170:2004) 3 Principle The sample under analysis is exposed in a sample cell to the primary radiation of an X-ray tube. The count rates of the S-K X-ray fluorescence and the count rate of the background radiation are me
23、asured. The sulfur content of the sample is determined from a calibration curve defined for the relevant measuring range. NOTE Whilst the Siegbahn X-ray line notation (S-K) is used in this document, the corresponding IUPAC X-ray line notation is S K-L2,3. 4 Reagents and materials 4.1 Dibutylsulfide,
24、 of nominal sulfur content 21,92 % (m/m), or 4.2 Dibutyldisulfide, of nominal sulfur content 35,95 % (m/m), used as a calibrating substance for sulfur. 4.3 Ethanol absolute, where the purity is not less than 99 %, for use as a blank solution, high purity grade, with a sulfur content 1 mg/kg. Check t
25、he blank solution prior to use with the spectrometer (5.1). A signal for sulfur shall not be detectable. 5 Apparatus 5.1 Wavelength dispersive X-ray fluorescence spectrometer, with the capability for measuring the count rates of the S-K X-ray fluorescence radiation and the background radiation. The
26、minimum requirements for the spectrometer are given in Table 1. Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:09 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15485:2007 (E) 5 Table 1 Spectrometer requirements Component Requirement Recommendations Anode
27、Rhodium, scandium or chromium Voltagea) No less than 30 kV 30 kV Currenta) No less than 50 mA 100 mA Collimator Coarse Analysing crystal Germanium, pentaerythrite, or graphite Germanium Optical path Helium Sample cup windowb) Polyester film, sulfur-free, 4 m maximum Polyester film 3,5 m Detector Pro
28、portional counter with pulse-height analyser a Lower power systems may be used, provided that these have been validated to meet the precision requirements specified in Clause 12. b Other sample window materials with the same or better transparency, purity and stability, can also be used. 5.2 Analyti
29、cal balance, capable of weighing to the nearest 0,1 mg. 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 with p
30、ure water to avoid contamination. Samples should be analysed as soon as possible after removal from bulk supplies to prevent loss of sulfur. Thoroughly mix samples in their containers immediately prior to withdrawal of the test portions. NOTE Particular attention should be paid to avoid contaminatio
31、n of sampling bottles from phosphorus containing detergents. 7 Preparation of calibration solutions 7.1 Blank calibration solution Use ethanol (4.3) as a blank solution. 7.2 Stock solution Weigh a quantity of the required calibrating substance (4.1 or 4.2) to the nearest 0,1 mg, and dilute with blan
32、k solution (7.1) at room temperature so that a stock solution with an accurately known sulfur content (to the nearest 1 mg/kg) of approximately 1 000 mg/kg is obtained. NOTE Care should be taken due to volatility of the calibrating substance. 7.3 Calibration solutions Weigh the stock solution (7.2)
33、to the nearest 0,1 mg into bottles and dilute with blank solution (7.1) so that standard solutions with sulfur contents in accordance with Table 2 are provided by stirring at room Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:09 GMT+00:00 2007, Uncontrol
34、led Copy, (c) BSI EN 15485:2007 (E) 6 temperature. The sulfur contents in the calibration solutions are indicated in milligrams per kilogram rounded to the nearest 0,1 mg/kg. Table 2 Calibration solutions Number Sulfur content mg/kg 0 (blank solution) 0,0 1 5,0 2 10,0 3 20,0 7.4 Storage and stabilit
35、y of the calibration solutions Calibration solutions prepared in accordance with Table 2 have a limited stability and shall be used on the same day they are prepared. NOTE While stock solutions may be stable for a longer time, calibration solutions may not. 8 Settings 8.1 Measuring parameters For op
36、timum measuring parameters, refer to Table 1. 8.2 Optimization The spectrometer shall be optimized in accordance with the manufacturers specifications in order to achieve the optimum signal-to-noise ratio. The calibration solution with 20 mg/kg sulfur is recommended for optimization. The counting ti
37、me shall be adjusted such that, for the 20 mg/kg calibration solutions, an optimal signal-to- noise ratio and signal area, for example resulting from 15 000 net counts, is obtained. This optimized counting time shall be used for both calibration (see 9) and measurement (see 10). 8.3 Performance chec
38、k of the spectrometer Prior to a measurement series (calibration and/or measurement), but in any case at least once daily, the manufacturers specifications shall be used to check that the spectrometer is operating correctly, so that an optimum performance and a consistent standard of highest possibl
39、e quality is ensured. NOTE 1 Many modern WDXRF systems use drift monitoring and correction to ensure that systems produce accurate data over long periods of time without the need to recalibrate. NOTE 2 Performance checks should be performed on a regular basis, since such checks will give valuable in
40、formation about the status and stability of the spectrometer. 9 Calibration 9.1 General Take care to ensure that the spectrometer is in an optimized condition after having executed all provisions given in Clause 8 and operating optimally before calibration (see 8.3). Licensed Copy: London South Bank
41、 University, London South Bank University, Wed Oct 17 01:21:09 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 15485:2007 (E) 7 9.2 Calibration solutions Transfer the calibration solutions (7.3) into suitable sample cups and fill them half full (see the note below). Depending on the concentration rang
42、e, all calibration solutions prepared in accordance with Table 2 shall be measured consecutively in ascending order. The count rate, Is, of the S-K X-ray fluorescence radiation at 0,537 3 nm, and the count rate, IB, of the background radiation at 0,545 nm, shall be measured consecutively. NOTE Too s
43、mall sample quantities will give a low result or relatively more evaporation/concentration effects when measuring volatile samples, whilst too much quantity of sample will give more sagging of the cell window especially when light aromatic samples are measured. 9.3 Calibration curves The net count r
44、ate, I0, is calculated according to equation (1). To determine the calibration curve, the relevant net count rate, I0, is plotted against the corresponding sulfur content of the calibration solution; the calibration curve shall then be calculated and stored using the linear model according to equati
45、on (2). The regression calculation may be carried out either separately or using the spectrometer calculator. I0 BS II = (1) where I0 is the net count rate for the relevant determination; Is is the count rate of the S-K X-ray fluorescence radiation at 0,537 3 nm; IB is the count rate of the backgrou
46、nd radiation at 0,545 nm; ( )bxaxI+= 0 (2) where x is the sulfur content of the relevant calibration solution, expressed in milligrams per kilogram (mg/kg); a, b are the parameters from the regression calculation; I0(x) is the net count rate computed from the regression calculation for the content,
47、x. 9.4 Checking Check the WDXRF system daily or before a measurement series by using quality control samples with known sulfur contents. Check immediately when using a new batch of films. If the check result differs by more than the 0,71 R, where R is the reproducibility of this test method (see 12.
48、2), execute a recalibration. NOTE It is recommended to execute a control chart analysis. 10 Procedure Fill a sample cup with a sufficient quantity of the sample under analysis so that an approximate medium height level is achieved (see the note to 9.2). Expose the sample to the radiation of the X-ra
49、y tube. Measure consecutively the count rate, Is, of the S-K X-ray fluorescence radiation at 0,537 3 nm and the count rate, IB, of the background radiation at 0,545 nm. Calculate the net count rate, I0, according to equation (1). Read the sulfur content in milligrams per kilogram from the calibration curve (see 9.3) for the measuring range of 7 mg/kg to 20 mg/kg sulfur. If the sulfur content Licensed Copy: London South Bank University, London South Bank University, Wed O