1、BRITISH STANDARDBS EN 14538:2006 BS 2000-547: 2006Fat and oil derivatives Fatty acid methyl ester (FAME) Determination of Ca, K, Mg and Na content by optical emission spectral analysis with inductively coupled plasma (ICP OES)The European Standard EN 14538:2006 has the status of a British StandardIC
2、S 67.200.10g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Licensed Copy: Wang Bin, na, Wed Apr 11 01:57:00 GMT+00:00 2007, Uncontrolled Copy, (c) B
3、SIBS EN 14538:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 January 2007 BSI and Energy Institute 2007ISBN 978 0 580 50177 7National forewordThis British Standard was published by BSI. It is the UK implementation of EN 14538:2006. Th
4、e UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum testing and terminology.A list of organizations represented on PTI/13 can be obtained on request to its secretary.Energy Institute, under the brand of IP, publishes and sells all Parts of BS 2000, and all BS
5、 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.Further information is available from: Energy Institute, 61 New Cavendish Street, Lo
6、ndon 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 British Standard cannot confer immunity from legal obligations.Amendments issued since pub
7、licationAmd. No. Date CommentsLicensed Copy: Wang Bin, na, Wed Apr 11 01:57:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14538June 2006ICS 67.200.10English VersionFat and oil derivatives - Fatty acid methyl ester (FAME) -Determination of Ca, K, Mg an
8、d Na content by optical emissionspectral analysis with inductively coupled plasma (ICP OES)Produits drivs des corps gras - Esters mthyliquesdacides gras (EMAG) - Dtermination de la teneur en Ca,K, Mg et Na par spectromtrie dmission optique avecplasma couplage inductif (ICP OES)Erzeugnisse aus pflanz
9、lichen und tierischen Fetten undlen - Fettsure-Methylester (FAME) - Bestimmung vonCa, K, Mg und Na durch optischeEmissionsspektralanalyse mit induktiv gekoppeltemPlasma (ICP OES)This European Standard was approved by CEN on 10 May 2006.CEN members are bound to comply with the CEN/CENELEC Internal Re
10、gulations 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 Central Secretariat or to any CEN member.This Eu
11、ropean 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 Central Secretariat has the same status as the officialversions.CEN members are the natio
12、nal standards bodies of Austria, Belgium, 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 Kingdo
13、m.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14538:2006: ELicensed Cop
14、y: Wang Bin, na, Wed Apr 11 01:57:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14538:2006 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Chemicals.4 5 Apparatus .4 6 Sampling.5 7 Preparation of the calibration solutions and the blank solution 5 7.1 General5 7.2 Bl
15、ank solution 6 7.3 Calibration solution with a nominal element content of 0,5 mg/kg6 7.4 Calibration solution with a nominal element content of 1 mg/kg .6 7.5 Calibration solution with a nominal element content of 5 mg/kg .6 7.6 Calibration solution with a nominal element content of 10 mg/kg.6 8 Cal
16、ibration 6 8.1 General6 8.2 Calibration 7 8.3 Check of calibration 7 9 Sample analysis.7 9.1 Sample preparation .7 9.2 Measurement7 10 Calculation7 11 Results 8 12 Precision.8 12.1 Repeatability.8 12.2 Reproducibility.8 13 Test report 8 Licensed Copy: Wang Bin, na, Wed Apr 11 01:57:00 GMT+00:00 2007
17、, Uncontrolled Copy, (c) BSIEN 14538:2006 (E) 3 Foreword This document (EN 14538:2006) 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 European
18、Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2006, and conflicting national standards shall be withdrawn at the latest by December 2006. According to the CEN/CENELEC Internal Regulations, the nation
19、al standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Port
20、ugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: Wang Bin, na, Wed Apr 11 01:57:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14538:2006 (E) 4 1 Scope This document specifies a procedure for the direct determination of the soap building elements Calc
21、ium (Ca), Magnesium (Mg), Sodium (Na) and Potassium (K) in fatty acid methyl esters (FAME) by ICP OES at levels of about 1 mg/kg to 10 mg/kg. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited
22、 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 3171, Petroleum liquids - Automatic pipeline sampling (ISO 3171:1988) 3 Principle An exactly weighed test portio
23、n is diluted with kerosene using a 1:1 weight ratio. The resulting solution is directly injected into the plasma of the ICP OES spectrometer. For reference and calibration purposes, calibration samples with known contents of the element(s) under investigation in the range of 0,5 mg/kg to 10 mg/kg ar
24、e used. The sum of the content of Calcium and the content of Magnesium, and the sum of the content of Sodium and the content of Potassium are reported. 4 Chemicals Unless otherwise stated, only chemicals of recognized analytical quality shall be used. 4.1 Paraffin oil, low viscosity, Pharmacopeia (E
25、UPHARM EP5), e.g. Merck 1071741)4.2 Kerosene, boiling range included between 150 C and 325 C, e.g. Aldrich 32.946-01)4.3 Element Standard solutions, dissolved in oil, 500 mg/kg per element. These are available as single element standards, like e.g. Merck 115053 (Ca), 115057 (Mg), 115054 (K) and 1150
26、58 (Na), or also at least partially as multi-element standards, (e.g. Spex)1). 4.4 Argon, with minimum purity w (Ar) = 99,996 % (V/V) 5 Apparatus Commercial laboratory and glass equipment, in conjunction with the following: 5.1 100 ml bottles with cap, preferably made of Polyethylene (PE), brown 5.2
27、 250 ml bottles with cap, preferably made of Polyethylene (PE), brown 1) Merck, Aldrich and Spex standards are examples of a suitable product available commercially. This information is given for the convenience of users of this standard and does not constitute an endorsement by CEN of these product
28、s. Licensed Copy: Wang Bin, na, Wed Apr 11 01:57:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14538:2006 (E) 5 NOTE In order to minimize pollution of the solutions, it is recommended to prepare all the determination solutions in polyethylene bottles. Do not touch surfaces that could come in conta
29、ct with working solutions. New glassware should be filled with sodium-free water and to be left for two days before use to remove soluble sodium. This is especially important when this procedure is used for the determination of sodium and/or potassium. 5.3 ICP OES spectrometer 5.3.1 General ICP OES
30、spectrometers (simultaneous or sequence devices) equipped for the analysis of organic liquids are suitable. Both setup and operation of the ICP OES spectrometer shall be done in accordance with operating instructions of the manufacturer. NOTE 1 Depending on the type and construction of the ICP OES s
31、pectrometer (radial, axial, detectors sensitivity, etc.) it may sometimes be necessary to select wavelengths different from those listed here. In such cases, a separate optimization of the instrument parameters and possibly also of the optimal dilution (see 9.1) is strongly recommended. NOTE 2 The c
32、alibration solution with an element content of 1 mg/kg (7.4) can be used to check the correct instrument performance. 5.3.2 Recommended wavelengths for Calcium and Magnesium The following wavelengths are recommended for the analysis, because they have been found to exhibit minimal interference in da
33、ily practice: Calcium 422,673 nm; Magnesium 279,553 nm. Depending on the ICP OES spectrometers optical configuration also other specific wavelengths can be selected, like 317,933 nm, 393,366 nm or 396,847 nm for Calcium and 285,213 nm for Magnesium, if these lines are free from interferences (see al
34、so Note 1 under 5.3.1). 5.3.3 Recommended wavelengths for Sodium and Potassium The following wavelengths are recommended for the analysis, because they have been found to exhibit minimal interference in daily practice (see also Note 1 under 5.3.1). Sodium 588,995 nm or 589,592 nm; Potassium 769,897
35、nm or 766,490 nm. 6 Sampling Samples shall be taken as described in EN ISO 3170 or EN ISO 3171 and/or in accordance with the requirements of national standards or regulations for the sampling of automotive diesel fuel. Bottles made of plastic (PE or PTFE) preferably should be used. 7 Preparation of
36、the calibration solutions and the blank solution 7.1 General In order to avoid inhomogenities, the standard solutions (4.3) should be shaken vigorously before use. Licensed Copy: Wang Bin, na, Wed Apr 11 01:57:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14538:2006 (E) 6 The masses given in 7.3,
37、7.4, 7.5 and 7.6 correspond to a nominal element content of 500 mg/kg per element in the standard solutions (4.3) and (4.4). Calculate the exact concentrations for the calibration solutions, taking into account the exact weights. All prepared solutions shall be homogenized by vigorous shaking. NOTE
38、1 As a strong general recommendation, the solutions used for calibration should be freshly prepared. If that is not possible, the samples should be stabilized using a suitably small amount of a stabilizing agent like 2-Ethylhexanoic acid, which has been shown to be free of the elements under investi
39、gation. Experience from daily practice has shown that such stabilized samples can be used for about 14 days. However, there is also sufficient evidence that calibration standard (7.3) in particular is not sufficiently stable, so that it is strongly recommended to prepare fresh solutions for each new
40、 calibration. NOTE 2 The dilution factors for the blank solution, the calibration solutions and sample solution should be selected such that the viscosities are as close to one another as possible. This can often be achieved by using a somewhat higher dilution factor. 7.2 Blank solution Approximatel
41、y 30 g paraffin oil (4.1) is weighed, with a precision of 0,01 g, into a 250 ml PE bottle (5.2), filled up with kerosene (4.2) to a total sample mass of approximately 100 g, with a precision of 0,01 g. 7.3 Calibration solution with a nominal element content of 0,5 mg/kg For each element, approximate
42、ly 0,1 g standard solution (4.3) is weighed, with a precision of 0,000 1 g, into a 250 ml PE bottle (5.2). Then approximately 30 g paraffin oil is added, with a precision of 0,01 g. Subsequently, kerosene (4.2) is added to make up to a total sample weight of approximately 100 g, with a precision of
43、0,01 g. Special attention shall be executed in using this calibration solution, as it is not as stable as the other ones. 7.4 Calibration solution with a nominal element content of 1 mg/kg For each element, approximately 0,2 g standard solution (4.3) is weighed, with a precision of 0,000 1 g, into a
44、 250 ml PE bottle (5.2). Then approximately 30 g paraffin oil is added, with a precision of 0,01 g. Subsequently, kerosene (4.2) is added to make up to a total sample weight of approximately 100 g, with a precision of 0,01 g. 7.5 Calibration solution with a nominal element content of 5 mg/kg For eac
45、h element, approximately 1 g standard solution (4.3) is weighed, with a precision of 0,000 1 g, into a 250 ml PE bottle (5.2). Then approximately 30 g paraffin oil is added, with a precision of 0,01 g. Subsequently, kerosene (4.2) is added to make up to a total sample weight of approximately 100 g,
46、with a precision of 0,01 g. 7.6 Calibration solution with a nominal element content of 10 mg/kg For each element, approximately 2 g standard solution (4.3) is weighed, with a precision of 0,000 1 g into a 250 ml PE bottle (5.2). Then approximately 30 g paraffin oil is added, with a precision of 0,01
47、 g. Subsequently, kerosene (4.2) is added to make up to a total sample weight of approximately 100 g, with a precision of 0,01 g. 8 Calibration 8.1 General The ICP OES spectrometer setup and instrument check is performed according to the instructions from the manufacturer. A separate calibration fun
48、ction for each element under investigation shall be established. Licensed Copy: Wang Bin, na, Wed Apr 11 01:57:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 14538:2006 (E) 7 8.2 Calibration The calibration of the ICP OES spectrometer shall be done by the measurement of the blank solution (7.2) and
49、 of the standard solutions (7.3 to 7.6). For the determination of the elements the wavelengths recommended in 5.3 shall be used. It is important to ensure that the wavelengths used in calibration also match exactly the ones used in the measurement. For each element under investigation, a calibration curve is constructed using linear regression with concentration as independent variable (X) and signal as dependent variable (Y). This can either be done manually or with use of a computer. The calibration curve will have the form Y = m X + b, where m is the slope and
