DIN EN 16476-2014 Liquid petroleum products - Determination of Sodium Potassium Calcium Phosphorus Copper and Zinc contents in diesel fuel - Method via Inductively Coupled Plasma O.pdf

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1、July 2014 Translation by DIN-Sprachendienst.English price group 10No 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).ICS 7

2、5.160.20!%7?“2202895www.din.deDDIN EN 16476Liquid petroleum products Determination of Sodium, Potassium, Calcium, Phosphorus, Copper andZinc contents in diesel fuel Method via Inductively Coupled Plasma Optical Emission Spectrometry(ICP OES);English version EN 16476:2014,English translation of DIN E

3、N 16476:2014-07Flssige Minerallerzeugnisse Bestimmung des Gehalts an Natrium, Kalium, Calcium, Phosphor, Kupfer, Zink inDieselkraftstoffen Direkte Bestimmung durch optische Emissionsspektrometrie mit induktiv gekoppeltemPlasma (ICP OES);Englische Fassung EN 16476:2014,Englische bersetzung von DIN EN

4、 16476:2014-07Produits ptroliers liquides Dtermination des concentrations en sodium, potassium, calcium, phosphore, cuivre etzinc dans le gazole Mthode par spectromtrie dmission atomique par plasma couplage inductif(ICP OES);Version anglaise EN 16476:2014,Traduction anglaise de DIN EN 16476:2014-07w

5、ww.beuth.deDocument comprises 16 pagesIn case of doubt, the German-language original shall be considered authoritative.06.14 DIN EN 16476:2014-07 2 A comma is used as the decimal marker. National foreword This document (EN 16476:2014) has been prepared by Technical Committee CEN/TC 19 “Gaseous and l

6、iquid fuels, lubricants and related products of petroleum, synthetic and biological origin” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-06-11 AA Atoms

7、pektrometrie of the Fachausschuss Minerall- und Brennstoffnormung (FAM). EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16476 May 2014 ICS 75.160.20 English Version Liquid petroleum products - Determination of Sodium, Potassium, Calcium, Phosphorus, Copper and Zinc contents in diesel fuel - Me

8、thod via Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) Produits ptroliers liquides - Dtermination des concentrations en sodium, potassium, calcium, phosphore, cuivre et zinc dans le gazole - Mthode par spectromtrie dmission atomique par plasma couplage inductif(ICP OES) Flssige

9、Minerallerzeugnisse - Bestimmung des Gehalts an Natrium, Kalium, Calcium, Phosphor, Kupfer, Zink in Dieselkraftstoffen - Direkte Bestimmung durch optische Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP OES) This European Standard was approved by CEN on 20 March 2014. CEN members are bou

10、nd 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 to the C

11、EN-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 Centre

12、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, Lithuania,

13、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, B-1000 B

14、russels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16476:2014 EEN 16476:2014 (E) 2 Contents Page Foreword 3 Introduction . 4 1 Scope 5 2 Normative references 5 3 Principle 5 4 Reagents . 5 5 Apparatus . 6 6 Sampling . 8 7

15、 Preparation of calibration solutions 8 7.1 General 8 7.2 Internal Standard solution 8 7.3 Calibration solutions . 8 7.4 Calibration check solution 9 8 Calibration 9 8.1 General 9 8.2 Calibration of the ICP OES spectrometer 9 8.3 Procedure A 10 8.4 Procedure B 10 8.5 Check of calibration 10 9 Sample

16、 analysis . 11 9.1 Sample preparation . 11 9.2 Sample measurement 11 10 Calculation 12 11 Expression of result 12 12 Precision . 12 12.1 General 12 12.2 Repeatability . 12 12.3 Reproducibility . 12 13 Test report 13 Bibliography 14 DIN EN 16476:2014-07 EN 16476:2014 (E) 3 Foreword This document (EN

17、16476:2014) 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 Standard shall be given the status of a national standard, either by public

18、ation of an identical text or by endorsement, at the latest by November 2014 and conflicting national standards shall be withdrawn at the latest by November 2014. 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

19、shall not be held responsible for identifying any or all such patent rights. 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, Croatia, Cyprus, Czech Republic,

20、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, Switzerland, Turkey and the United Kingdom. DIN EN 164

21、76:2014-07 EN 16476:2014 (E) 4 Introduction This document specifies a method for determining concentration of the six most essential ash forming elements. The number of six was chosen in order to limit the complexity of the test and to be able to determine a decent method precision. The six elements

22、 were specified by the vehicle manufacturers. The test provides additional information to the more common ash concentration determination methods which do aim towards filter problems. Metals have more impact on the durability of modern DPF exhaust gas after-treatment systems in diesel vehicles than

23、ash in general. DIN EN 16476:2014-07 EN 16476:2014 (E) 5 1 Scope This European Standard specifies an inductively coupled plasma optical emission spectrometry (ICP OES) method for the determination of sodium, potassium, calcium, phosphorus, copper and zinc concentrations of diesel fuels, including th

24、ose containing up to 30 % (V/V) fatty acid methyl ester (FAME), in the range detailed in Table 1. These six elements are considered as the most essential ash forming elements. Table 1 Application ranges for ash forming elements Element Range mg/kg Sodium 1,2 to 2,5 Potassium 0,9 to 2,5 Calcium 0,3 t

25、o 2,5 Phosphorus 0,9 to 2,5 Copper 0,2 to 2,5 Zinc 0,2 to 2,5 NOTE For the purposes of this European Standard, the term “% (V/V)” is used to represent the volume fraction, . WARNING The use of this European Standard may involve hazardous materials, operations and equipment. This European Standard do

26、es not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this European Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2 Normative references The followi

27、ng documents, in whole 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, Labor

28、atory glassware - One-mark volumetric flasks (ISO 1042) EN ISO 3170, Petroleum liquids - Manual sampling (ISO 3170) EN ISO 3171, Petroleum liquids - Automatic pipeline sampling (ISO 3171) 3 Principle A weighed amount of diesel fuel sample is diluted with an organic solvent. The solution is then intr

29、oduced directly into an ICP OES spectrometer. Sodium, potassium, calcium, phosphorous, copper and zinc concentrations are determined by comparison with calibration solutions. An Internal Standard is employed to correct viscosity effects. 4 Reagents If not specified otherwise, only chemicals of a kno

30、wn high degree of purity shall be used. DIN EN 16476:2014-07 EN 16476:2014 (E) 6 4.1 Kerosene, boiling range between 175 C and 250 C, elements free. The solvent shall contain less than 0,1 mg/kg of each of the element under test. NOTE In case of unstable plasma or in case of special laboratory requi

31、rements, kerosene can be substituted by other suitable solvents, provided that they are free of analytes. 4.2 Sodium Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg sodium. 4.3 Potassium Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg pot

32、assium. 4.4 Calcium Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg calcium. 4.5 Phosphorus Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg phosphorus. 4.6 Copper Standard solution, commercially available in oil, containing, e.g. 1 000 mg

33、/kg copper. 4.7 Zinc Standard solution, commercially available in oil, containing, e.g. 1 000 mg/kg zinc. 4.8 Sodium, potassium, calcium, phosphorus, copper and zinc intermediate working Standard (50 mg/kg each). Weigh (1,00 g 0,01) g of each element Standard solution (4.2), (4.3), (4.4), (4.5), (4.

34、6), (4.7) into a 50 ml bottle (5.2). Add kerosene (4.1) to (20,00 0,20) g. Each mass shall be weighed to the nearest 0,001 g. In the case of using several mono-element Standard solutions, attention-shall be paid to ensure that they are free of other analyte elements. Some commercial element Standard

35、 solutions are furnished with higher concentration on the market. Those solutions may be used instead of the required solutions, but in this case an initial mass to mass dilution shall be done according to recommendations given in 7.1. Ready-made commercial multi-element Standard solutions may be us

36、ed instead of the single element Standard solutions (4.2, 4.3, 4.4, 4.5, 4.6 and 4.7) as the method is designed to avoid interference at the wavelengths specified. 4.9 Internal Standard solution (cobalt, scandium, yttrium), commercially available in oil (analyte free), for example with 1 000 mg/kg p

37、er element, available as single element Standard. NOTE The internal Standard solutions are commonly available as single element Standards with various element concentrations. 4.10 Argon, with a mass fraction w (Ar) 99,996 %. Small amounts of oxygen may be added to the argon gas stream using a meteri

38、ng valve (for example 30 ml/min to 100 ml/min) to prevent carbon deposits in the area of the plasma torch. 5 Apparatus 5.1 Volumetric flasks, 25 ml and 250 ml, according to EN ISO 1042, with taper sleeve and plug. To avoid contamination of the test samples, all solutions shall be prepared in plastic

39、 containers. Surfaces which can come in contact with the solutions shall not be touched by hand. DIN EN 16476:2014-07 EN 16476:2014 (E) 7 To avoid phosphorus contamination due to the phosphates contained in the detergents used for washing the flasks, rinse the latter at least twice with an approxima

40、te 5 mol/l solution of nitric acid. Then rinse with distilled water and dry. The use of borosilicate glass containers is not recommended due to the risk of sodium contamination. 5.2 Bottles, 50 ml, with screw caps, polyethylene PE. To avoid phosphorus contamination due to the phosphates contained in

41、 the detergents used for washing the bottles, rinse the latter at least twice with an approximate 5 mol/l solution of nitric acid. Then rinse with distilled water and dry. 5.3 Analytical balance, capable of weighing to the nearest 0,000 1 g. 5.4 ICP OES spectrometer 5.4.1 General ICP OES spectromete

42、r equipped for the analysis of organic liquids. The use of a feed pump for sample introduction into the nebuliser is required. Pump tubing shall be suitable for organic use. Both setup and operation of the ICP OES spectrometer shall be done in accordance with operating instructions of the manufactur

43、er. The use of vertically oriented plasma, radially observed ICP OES is recommended to avoid carbon residue formation and minimize matrix interference due to the presence of carbon in the plasma. 5.4.2 Recommended wavelengths The recommended wavelengths of sodium, potassium, calcium, phosphorus, cop

44、per and zinc, cobalt, scandium and yttrium are given in Table 2. Table 2 Recommended wavelengths Element Wavelength anm Sodium 589,592 588,995 Potassium 766,491 769,897 Calcium 317,933 184,006 (183,944) 315,887 396,847 393,366 Phosphorus 177,499 (177,434) 178,287 (178,222) 213,618b214,914 Copper 324

45、,754 327,396 224,700 Zinc 206,200 213,856 202,548 bCobalt 238,892 258,033 Scandium 361,383 Yttrium 224,306 371,029 360,073 aWavelengths are expressed as vacuum lines or as air lines (in brackets) according to the expression of the different manufacturers of ICP OES spectrometers. bCan be slightly in

46、terfered by Cu at the same wavelength. DIN EN 16476:2014-07 EN 16476:2014 (E) 8 6 Sampling 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

47、of the product under test. Collect and store samples in sample bottles made of plastic material (HDPE, FEP, PP, or PFA) or metallic epoxy coated containers. 7 Preparation of calibration solutions 7.1 General In order to avoid inhomogeneity, the intermediate working Standard (4.8) shall be thoroughly

48、 shaken before use. The masses given correspond to a nominal element concentration of 1 000 mg/kg in the single element solutions (4.2, 4.3, .4.4, 4.5, 4.6 and 4.7) and the element Internal Standard solution (4.9). If solutions with other element concentrations are used, these masses shall be adjusted accordingly in order to establish the given nominal concentrations as closely as possible. Calculate the exact concentrations of the calibration solutions, taking into account the exact masses. It is strongly