DIN EN 16576-2015 Automotive fuels - Determination of manganese and iron content in diesel - Inductively coupled plasma optical emission spectrometry (ICP OES) method German versio.pdf

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1、February 2015 Translation by DIN-Sprachendienst.English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC

2、S 75.160.20!%X“2296153www.din.deDDIN EN 16576Automotive fuels Determination of manganese and iron content in diesel Inductively coupled plasma optical emission spectrometry (ICP OES)method;English version EN 16576:2014,English translation of DIN EN 16576:2015-02Kraftstoffe fr Kraftfahrzeuge Bestimmu

3、ng des Gehaltes an Mangan und Eisen in Dieselkraftstoff Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES);Englische Fassung EN 16576:2014,Englische bersetzung von DIN EN 16576:2015-02Carburants pour automobiles Dtermination des teneurs en manganse et en fer dans carburants di

4、esel Mthode spectromtrique optique par plasma couplage inductif (ICP OES);Version anglaise EN 16576:2014,Traduction anglaise de DIN EN 16576:2015-02www.beuth.deDocument comprises 14 pagesIn case of doubt, the German-language original shall be considered authoritative.01.15DIN EN 16576:2015-02 2 A co

5、mma is used as the decimal marker. National foreword This document (EN 16576:2014) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biological origin” (Secretariat: NEN, Netherlands). The responsible German body

6、 involved in its preparation was the DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-06-11 AA Atomspektrometrie of the Fachausschuss Minerall- und Brennstoffnormung (FAM). EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16576 November 201

7、4 ICS 75.160.20 English Version Automotive fuels - Determination of manganese and iron content in diesel - Inductively coupled plasma optical emission spectrometry (ICP OES) method Carburants pour automobiles - Dtermination des teneurs en manganse et en fer dans carburants diesel - Mthode spectromtr

8、ique optique par plasma couplage inductif (ICP OES) Kraftstoffe fr Kraftfahrzeuge - Bestimmung des Gehaltes an Mangan und Eisen in Dieselkraftstoff - Optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES) This European Standard was approved by CEN on 20 September 2014. CEN members

9、 are bound to comply with the CEN/CENELEC 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

10、to the CEN-CENELEC 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 translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

11、 Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lit

12、huania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17,

13、B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16576:2014 EEN 16576:2014 (E) 2 Contents Page Foreword 3 1 Scope 4 2 Normative references 4 3 Principle 4 4 Reagents . 4 5 Apparatus . 5 6 Sampling . 6 7 Preparat

14、ion of solutions . 6 7.1 General 6 7.2 Preparation of the Internal standard solution for dilution . 6 7.3 Preparation of the manganese intermediate solution 7 7.4 Preparation of the iron intermediate solution . 7 7.5 Preparation of the calibration solutions 7 7.6 Preparation of manganese and iron qu

15、ality control solution . 7 8 Calibration 8 8.1 General 8 8.2 Calibration of the ICP OES spectrometer 8 8.3 Procedure A 8 8.4 Procedure B 8 8.5 Check of the calibration 9 9 Sample analysis . 9 9.1 Sample solution preparation 9 9.2 Sample solution measurement . 9 10 Calculation 10 11 Expression of res

16、ults 10 12 Precision . 10 12.1 General 10 12.2 Repeatability, r . 11 12.3 Reproducibility, R 11 13 Test report 11 Bibliography 12 DIN EN 16576:2015-02 EN 16576:2014 (E) 3 Foreword This document (EN 16576:2014) has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants a

17、nd 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 endorsement, at the latest by May 2015 and conflicting national stand

18、ards shall be withdrawn at the latest by May 2015. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document answers requirements

19、originating from the amended Fuels Quality Directive (FQD, 1). A similar technique for unleaded petrol is described in EN 16136 2. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria

20、, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden,

21、Switzerland, Turkey and the United Kingdom. DIN EN 16576:2015-02 EN 16576:2014 (E) 4 1 Scope This European Standard specifies a method based on inductively coupled plasma optical emission spectrometry (ICP OES) for the determination of manganese content and of iron content, each from about 0,5 mg/l

22、to about 7,0 mg/l in diesel fuels including those containing up to about 10 % (V/V) fatty acid methylester (FAME). WARNING The use of this European Standard may involve hazardous materials, operations and equipment. This European Standard does not purport to address all of the safety problems associ

23、ated with its use. It is the responsibility of the user of this European Standard to establish appropriate safety and health practices and to determine the applicability of regulatory limitations prior to use. NOTE 1 Manganese and iron contents higher than 7,0 mg/l can be measured after preliminary

24、dilution of the sample with a suitable solvent. However, the precision has not been established for such a procedure. NOTE 2 For the purposes of this European Standard, the term “% (V/V)” is used to represent the volume fraction () of a material. 2 Normative references The following documents, in wh

25、ole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 1042, Laboratory glassware One

26、 -mark volumetric flasks (ISO 1042) EN ISO 3170, Petroleum liquids Manual sampling (ISO 3170) EN ISO 3171, Petroleum liquids Automatic pipeline sampling (ISO 3171) EN ISO 3675, Crude petroleum and liquid petroleum products Laboratory determination of density Hydrometer method (ISO 3675) EN ISO 12185

27、, Crude petroleum and petroleum products Determination of density Oscillating U -tube method (ISO 12185) 3 Principle A diesel fuel sample is diluted with a hydrocarbon solvent. The solution is introduced directly into the plasma of an ICP OES spectrometer. Iron and manganese contents are calculated

28、by comparison with calibration solutions prepared from suitable iron and manganese compounds. An internal standard is employed to correct viscosity effects. 4 Reagents Unless specified otherwise, only chemicals which are known to have a high degree of purity shall be used. 4.1 Kerosene, boiling rang

29、e between 150 C and 250 C, analytical reagent grade. Other grades of kerosene with analyte concentrations below the detection limits for the two elements under investigation may be used. In this case, perform a wavelength check for absence of signals from the corresponding elements as well as for ab

30、sence of spectral interference. 4.2 Manganese standard solution, dissolved in oil, (Mn) = 100 mg/kg. DIN EN 16576:2015-02 EN 16576:2014 (E) 5 A multi-element standard solution may also be used instead of the single element standard solution. Some element standard solutions are supplied with differen

31、t element content on the market. These solutions may be used instead of the required solutions, but an initial mass to mass dilution has to be done. 4.3 Iron standard solution, dissolved in oil, (Fe) = 100 mg/kg. A multi-element standard solution may also be used instead of the single element standa

32、rd solution. Some element standard solutions are supplied with different element content on the market. These solutions may be used instead of the required solutions, but an initial mass to mass dilution has to be done. 4.4 Internal standard solutions (cobalt, scandium, yttrium), dissolved in oil, f

33、or example with 1 000 mg/kg per element, available as single element standards. NOTE The element standard solutions are commonly available as single element standards with various element content. 4.5 Argon, with a purity of 99,995 % (V/V). Small amounts of oxygen (purity O2 99,995 % (V/V) may be ad

34、ded, for instance in accordance with the operating instructions of the equipment manufacturer, to the argon gas stream using a metering valve (30 ml/min to 100 ml/min) to prevent carbon deposits in the area of the plasma torch. 5 Apparatus 5.1 Laboratory equipment 5.1.1 General All glassware shall b

35、e cleaned carefully before use. 5.1.2 Glassware, usual laboratory glassware, together with the following: 5.1.2.1 Beakers, 50 ml. 5.1.2.2 Volumetric flasks, 20 ml, 50 ml and 500 ml, according to EN ISO 1042, with taper sleeve and plug. 5.1.3 Bottles, 50 ml and 500 ml, with screw caps, high-density p

36、olyethylene (HDPE). 5.1.4 Graduated pipettes or variable volume automatic pipettes, fitted with disposable polypropylene tips. 5.2 Analytical balance, capable of weighing to the nearest 0,1 mg. 5.3 ICP OES spectrometer 5.3.1 General ICP OES spectrometer equipped for the analysis of organic liquids,

37、with a high-frequency generator and a nebulizer suitable for organic solvents. The use of a feed pump for sample introduction into the nebulizer is required. Both setup and operation of the ICP OES spectrometer shall be done in accordance with operating instructions of the manufacturer. 5.3.2 Wavele

38、ngths Table 1 gives the recommended wavelengths. As the magnitude of the background signal highly depends on spectral structures caused by the samples nature and origin, only net intensities are to be used for calculations. DIN EN 16576:2015-02 EN 16576:2014 (E) 6 Table 1 Recommended wavelengths Ele

39、ment Wavelength nm Manganese 257,610 259,372 260,569 279,482 279,827 293,931 Iron 234,350 238,204 240,488 259,940 261,187 Cobalt 238,892 Scandium 361,383 Yttrium 224,306 360,073 371,029 6 Sampling IMPORTANT The laboratory shall receive a sample which is truly representative and was not damaged or al

40、tered during transport or storage. Unless otherwise specified in the commodity specification, samples shall be taken as described in EN ISO 3170 or EN ISO 3171 and/or in accordance with the requirements of national regulations for the sampling of the product under test. The samples shall be filled i

41、nto clean containers. 7 Preparation of solutions 7.1 General In order to avoid inhomogeneity, the element standard solutions (4.2, 4.3 and 4.4) shall be shaken vigorously before use. It is strongly advised to use freshly prepared calibration solutions. 7.2 Preparation of the Internal standard soluti

42、on for dilution Weigh 5 g of cobalt, scandium or yttrium stock solution (4.4) with a precision of 0,1 g in a 500 ml volumetric flask (5.1.2.2). Fill up to 500 ml with kerosene solvent (4.1). The prepared solution shall be homogenized by vigorous shaking. DIN EN 16576:2015-02 EN 16576:2014 (E) 7 NOTE

43、 Experience from daily practice with yttrium used as internal standard has shown that internal standard solutions can be used for about two weeks. Internal standard solution with different element content may be used instead of the 1 000 mg/kg one. In that case, the mass has to be adjusted in order

44、to get a minimum content of 10 mg/l in the internal standard solution for dilution. 7.3 Preparation of the manganese intermediate solution Weigh 3,00 g 0,01 g of manganese standard solution (4.2) into a 50 ml HDPE bottle (5.1.3). Add kerosene solvent (4.1) to 15,00 g 0,01 g. In case manganese standa

45、rd solutions (4.2) with different manganese content are used, the mass of standard solution shall be adjusted accordingly to achieve 20 mg/kg manganese content. 7.4 Preparation of the iron intermediate solution Weigh 3,00 g 0,01 g of iron standard solution (4.3) into a 50 ml HDPE bottle (5.1.3). Add

46、 kerosene solvent (4.1) to 15,00 g 0,01 g. In case iron standard solutions (4.3) with different iron content are used, the mass of standard solution shall be adjusted accordingly to achieve 20 mg/kg iron content. 7.5 Preparation of the calibration solutions The calibration solutions shall be prepare

47、d as indicated in Table 2. Each mass of manganese intermediate solution (7.3) and iron intermediate solution (7.4) shall be weighed to the nearest 0,1 mg into a 20 ml volumetric flask (5.1.2.2). Fill with kerosene (4.1) to the mark. All solutions thus prepared shall be homogenized by shaking. Table

48、2 Concentration of iron and manganese in the calibration solutions Calibration solution Manganese intermediate solution (7.3) g Iron intermediate solution (7.4) g Internal standard solution (7.2) ml Manganese concentration mg/l Iron concentration mg/l Blank 0,00 0,00 10 0,00 0,00 1 0,50 0,50 10 0,50

49、 0,50 2 2,00 2,00 10 2,00 2,00 3 3,50 3,50 10 3,50 3,50 7.6 Preparation of manganese and iron quality control solution A 1,0 mg/l quality control (QC) solution shall be prepared using independent manganese and iron standard solutions. The mass given is based on an element (Fe, Mn) content of 100 mg/kg. In case a standard solution with different element content is used, the mass shall be adjusted accordingly to obtain the specified element content. Weigh 0,5 g of manganese standard solution (4.2) and 0,5 g of iron