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2、opper content Graphite furnace atomic absorption spectrometric methodThe European Standard EN 15488:2007 has the status of a British StandardICS 71.080.60Ethanol as a blending component for petrol Determination of BRITISH STANDARDBS EN 15488:2007 BS 2000-556:2007BS EN 15488:2007Licensed Copy: Wang B
3、in, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:28, 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 56676 9Compliance wi
4、th a British 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 informati
5、on 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.National forewordsh Standard is the UK im
6、plementation of EN 15488:2007.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
7、, and all BS EN petroleum test methods that would be Part of BS 2000, EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15488August 2007ICS 71.080.60English VersionEthanol as a blending component for petrol - Determination ofcopper content - Graphite furnace atomic absorptionspectrometric methodthan
8、ol comme base de mlange lessence -Dtermination de la teneur en cuivre - Mthode parspectromtrie dabsorption atomique avec four en graphiteEthanol zur Verwendung als Blendkomponente inOttokraftstoff - Bestimmung des Kupfergehaltes -Graphitrohr-AtomabsorptionsspektrometrieThis European Standard was app
9、roved 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 EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalsta
10、ndards 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 version in any other language made by translationunder the responsibility of a CEN member into its own language and notified t
11、o the CEN Management Centre has the 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, Neth
12、erlands, Norway, Poland, Portugal,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
13、 any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15488:2007: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:28, Uncontrolled Copy, (c) BSIEN 15488:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative reference 4 3 Terms and definitions .4 4
14、 Principle5 5 Reagents and materials 5 6 Apparatus .5 6.1 Atomic absorption spectrometer .5 7 Samples and sampling6 8 Preparation of blank and calibration solutions 6 8.1 Intermediate calibration solution .6 8.2 Calibration solutions .6 9 Procedure .7 9.1 Instrument preparation .7 9.2 Calibration 7
15、10 Sample analysis.8 11 Calculation8 12 Expression of results 8 13 Precision.8 13.1 Repeatability.8 13.2 Reproducibility.9 14 Test report 9 Annex A (informative) Example of thermal program of the graphite furnace.10 Bibliography 11 Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02
16、:28, Uncontrolled Copy, (c) BSIEN 15488:2007 (E) 3 Foreword This document (EN 15488:2007) 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 Europe
17、an 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. This document is based on IP 478 1. According to the CEN/C
18、ENELEC 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, Ireland, Italy, Latvia, Lithuania, Lux
19、embourg, 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 02:28, Uncontrolled Copy, (c) BSIEN 15488:2007 (E) 4 1 Scope This standard specifies a procedure for th
20、e determination of copper content in ethanol from 0,07 mg/kg to 0,20 mg/kg using graphite furnace atomic absorption spectrometry. NOTE For the purpose of this document, the terms “% (m/m)” and “% (V/V)“ are used to represent the mass fraction, respectively the volume fraction of a material. WARNING
21、Use of this standard may involve hazardous materials, operations 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 th
22、e applicability of regulatory limitations prior to use. 2 Normative reference 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
23、ing 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 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 radian
24、t power P rate at which energy is transported in a beam of radiant energy 3.2 transmittance T ratio of the radiant power transmitted by a material to the radiant power incident upon it 3.3 absorbance A logarithm to the base 10 of the reciprocal of the transmittance NOTE Can be derived by the followi
25、ng equation: A = log (1/T) = -log (T) (1) 3.4 integrated absorbance Aiintegrated area under the absorbance peak generated by the atomic absorption spectrometer Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 12/12/2007 02:28, Uncontrolled Copy, (c) BSIEN 15488:2007 (E) 5 4 Principle The graph
26、ite furnace is aligned in the optical path of the atomic absorption spectrometer. A test portion is pipetted onto the platform or at the wall of the graphite furnace. The furnace is heated in consecutive thermal stages, firstly to dry the test portion completely without spattering, then to eliminate
27、 excess sample matrix, and finally to volatilise the analyte of interest. During this final stage, the amount of light absorbed by the copper atoms is measured over a specified period. The integrated absorbance Ai, produced by the copper in the test portion, is compared to a calibration curve constr
28、ucted from copper standards in ethanol solution. NOTE The second heating stage is used to eliminate as much of the sample matrix as possible before the atomization step, as non-dissociated molecular species are the most common form of interference. Spectrometers are equipped with background correcti
29、on capabilities to control further possibilities of erroneous results due to molecular absorption. 5 Reagents and materials 5.1 General All reagents shall be of analytical reagent grade or of higher purity. 5.2 Ethanol, 99,8 % (m/m) minimum purity. 5.3 Copper standard, aqueous solution containing 1
30、000 mg/l of copper as inorganic salt (e.g. nitrate), or a multi-element aqueous standard containing 1 000 mg/l of copper. 5.4 Water, for analytical laboratory use, conforming to grade 3 of EN ISO 3696. 5.5 Argon, regulated compressed gas of 99,999 % minimum purity for the graphite furnace gas flow s
31、ystem. 5.6 Nitric acid (HNO3), c(HNO3) 0,5 mol/l Cautiously add 50 ml 2 ml of nitric acid ( = 1,40 g/ml) to 500 ml 10 ml water (5.4). Mix and allow to cool to room temperature. Make up to 1 000 ml with water (5.4). 6 Apparatus 6.1 Atomic absorption spectrometer 6.1.1 Capable of setting the wavelengt
32、h at 324,8 nm or 327,4 nm, with the appropriate slit, e.g. as specified by the manufacturer, and using peak area integration for the signal and background readings. It shall be equipped with the features described in 6.1.2 to 6.1.4. NOTE The wavelength of 327,4 nm can be used for the measurements, h
33、owever, the precision for results measured at this wavelength was not determined. 6.1.2 Copper hollow cathode lamp 6.1.3 Background correction system, capable to cover the 324,8 nm or 327,4 nm wavelength. 6.1.4 Graphite furnace accessory, which uses pyrolytically coated graphite tubes with or withou
34、t integrated platforms. 6.2 Autosampler, capable of reproducibly delivering 10 l 0,1 l aliquots to the graphite furnace. 6.3 Micropipette, capable of reproducibly delivering volumes in the range 20 l to 100 l with an accuracy of 0,4 l at 50 l. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 1
35、2/12/2007 02:28, Uncontrolled Copy, (c) BSIEN 15488:2007 (E) 6 6.4 Polyethylene containers, 25 ml volume. Rinse the containers with water (5.4). 6.5 Analytical balance, capacity of 100 g and capable of weighing to the nearest 0,01 g. 6.6 Ultrasonic bath 7 Samples and sampling Unless otherwise specif
36、ied, 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 pure water to avoid contamination. Samples should be analysed as soon as possible after removal from bu
37、lk supplies, to prevent loss of copper. NOTE High density polyethylene containers are used to prevent losses of copper by wall adsorption. 8 Preparation of blank and calibration solutions 8.1 Intermediate calibration solution Weigh a polyethylene container (6.4) and transfer with a micropipette (6.3
38、) 100 l of copper standard (5.3). Add water (5.4) to the container to bring the mass up to approximately 10,0 g and re-weigh to the nearest 0,01 g. Seal the container, mix well and mark with the copper content calculated as following: wcmVS = (2) where S is the copper content of the intermediate cal
39、ibration solution in mg/kg; Vcis the volume of copper standard (5.3) in l; mwis the mass of water (5.4) in g. NOTE This procedure leads to intermediate calibration solution with nominal copper content corresponding to 10 mg/kg. The intermediate solution is stable for up to one week. 8.2 Calibration
40、solutions The calibration solutions shall be prepared daily. Weigh five polyethylene containers (6.4), add about 5 g ethanol (5.2) to each container and then respectively 20 l, 40 l, 60 l, 80 l and 100 l of intermediate calibration solution (8.1). Reserve a sixth container for the preparation of the
41、 blank. Add ethanol (5.2) to each of the six containers to bring the mass up to approximately 10,0 g and re-weigh to the nearest 0,01 g. Seal each container, mix well and mark with the copper content (including the blank) calculated as following: Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS
42、, 12/12/2007 02:28, Uncontrolled Copy, (c) BSIEN 15488:2007 (E) 7 eimSVC= (3) where C is the copper content of the calibration solution in g/kg; S is the copper content of the intermediate calibration solution (8.1) in mg/kg; Viis the volume of intermediate calibration solution (8.1) in l; meis the
43、mass of ethanol (5.2) in g. NOTE This procedure leads to calibration solutions with nominal copper contents corresponding to 0 g/kg, 20 g/kg, 40 g/kg, 60 g/kg, 80 g/kg and 100 g/kg respectively. 9 Procedure 9.1 Instrument preparation 9.1.1 Set the spectrometer (6.1) at a wavelength of 324,8 nm or 32
44、7,4 nm, and the appropriate slit width. 9.1.2 Condition new (or re-installed) graphite tube assemblies with the temperature program provided by the spectrometer manufacturer. 9.1.3 Adjust the autosampler (6.2) tip as near as possible to the graphite platform surface but avoid contact between tip and
45、 surface. Use the blank solution (8.2) to evaluate the correct delivery of ethanol solutions. The delivered aliquot should distribute evenly onto the platform. Autosampler cups made of polyethylene, polypropylene or polytetra-fluorethylene (PTFE) can be used. Use nitric acid (5.6) as the rinse solut
46、ion of the autosampler. Due to the high volatility and surface tension of ethanol, the positioning of the tip and the correct delivery of sample aliquots should be checked periodically, as uneven delivery leads to erroneous measurements. Check the correct delivery of aliquots when the integrated abs
47、orbance of two repeated injections differ by more than 15 %. 9.2 Calibration 9.2.1 Apply the thermal program for copper analysis as given in the instrument manufacturers instructions. Due to the different design of graphite furnace atomizers, the thermal program shall be developed according to the a
48、tomizer characteristics. Refer to the instrument manual to set the best temperatures for copper pyrolisis and atomization steps. A thermal program is given as an example in Annex A. 9.2.2 Temperatures, ramp and hold times of drying steps shall be optimised so that the sample dries completely without
49、 spattering. 9.2.3 The ramp time for the pyrolisis step may be lengthened if it appears that an excess amount of smoke from the sample matrix is generated very quickly as the furnace heats from the second drying step (Drying 2) to the pyrolisis. Also, all smoke shall be evolved at least 5 s before the end of the pyrolisis step. If smoke still evolves at the end of the pyrolisis step, the hold time shall be lengthened. 9.2.4 For the spectrometer trace of absorbance versus atomization hold time, the absorbance at the end of the atom
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