DIN EN 15944-2011 Liquid petroleum products - Determination of nickel and vanadium content - Inductively coupled plasma optical emission spectrometry method (ICP OES) German versio.pdf

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1、February 2011 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 75.100!$mpR“1747747www.din.deDDIN EN 15944Liquid petroleum products Determination of nickel and vanadium content Inductively coupled plasma optical emission spectrometry method English translation of DIN EN 15944:2011-02Flssige Minerallerzeugnisse Bestimmung des Gehaltes an Nickel und Vanadium Opt

3、ische Emissionsspektralanalyse mit induktiv gekopppeltem Plasma (ICP OES)Englische bersetzung von DIN EN 15944:2011-02Produits ptroliers liquides Dtermination de la teneur en nickel et vanadium Mthode directement par spectromtrie dmission atomique couplage inductif parplasma (SOD-PCI)Traduction angl

4、aise de DIN EN 15944:2011-02SupersedesDIN 51790-6:2007-11www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.13(ICP OES)02.11 DIN EN 15944:2011-02 2 A comma is used as the decimal marker. National foreword This standard has been prepar

5、ed 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 involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards C

6、ommittee), Working Committee NA 062-06-11 AA Atomspektrometrie of the Fachausschuss Minerall- und Brennstoffnormung. Amendments This standard differs from DIN 51790-6:2007-11 as follows: a) the content of DIN 51790-6:2007-11 has been included in EN 15944. Previous editions DIN 51790-6: 1994-07, 2007

7、-11 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15944 November 2010 ICS 75.100 English Version Liquid petroleum products - Determination of nickel and vanadium content - Inductively coupled plasma optical emission spectrometry method (ICP OES) Produits ptroliers liquides - Dtermination de l

8、a teneur en nickel et vanadium - Mthode directement par spectromtrie dmission atomique couplage inductif par plasma (SOD-PCI) Flssige Minerallerzeugnisse - Bestimmung des Gehaltes an Nickel und Vanadium - Optische Emissionsspektralanalyse mit induktiv gekopppeltem Plasma (ICP OES) This European Stan

9、dard was approved by CEN on 9 October 2010. CEN members 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

10、such national standards may be obtained on application 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

11、own language and notified to the CEN-CENELEC Management 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, France, Germany, Greece, Hungary, Iceland, Ireland, It

12、aly, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-10

13、00 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15944:2010: EEN 15944:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .56 Sampling .67 Preparation of calibr

14、ation solutions 67.1 General 67.2 Calibration solutions .67.3 Internal standard solution .77.4 Working solutions78 Calibration 78.1 General 78.2 Calibration of the ICP OES spectrometer 78.3 Procedure A 78.4 Procedure B 88.5 Check of calibration 89 Sample analysis .89.1 Sample preparation .89.2 Sampl

15、e measurement 910 Calculation 910.1 Procedure A 910.2 Procedure B 911 Expression of results . 1012 Precision 1012.1 General . 1012.2 Repeatability, r 1012.3 Reproducibility, R . 1013 Test report . 10Bibliography . 11DIN EN 15944:2011-02 EN 15944:2010 (E) 3 Foreword This document (EN 15944:2010) has

16、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 publication of an iden

17、tical text or by endorsement, at the latest by May 2011, and conflicting national standards shall be withdrawn at the latest by May 2011. 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 respons

18、ible for identifying any or all such patent rights. The method described in this document is based on DIN 51790-6 1. It has been developed originally as an alternative to (second part of) EN 13131 2, but as the method enables the use of an instrumental technique more and more employed in analytical

19、laboratories, it was decided to have it as a stand-alone method. 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, Denmark, Est

20、onia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15944:2011-02 EN 15944:2010 (E) 4 1 Scope This European Standa

21、rd specifies an inductively coupled plasma optical emission spectrometry (ICP OES) method for the determination of nickel content in the range 4 mg/kg to 55 mg/kg and of vanadium content in the range 4 mg/kg to 150 mg/kg in fuel oils and residual fuel oils. NOTE 1 Nickel content can be determined fr

22、om 2 mg/kg to 4 mg/kg and vanadium content can be determined from 1 mg/kg to 4 mg/kg. However, the precision was not established as no samples with nickel and vanadium contents in these ranges were included in the interlaboratory test. Nickel and vanadium contents higher than those reported can be d

23、etermined after sample dilution. However, the precision was not established for diluted samples. NOTE 2 For the purposes of this European Standard, the term “% (V/V)” is used to represent the volume fraction (). WARNING The use of this standard may involve hazardous materials, operations and equipme

24、nt. 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 the applicability of regulatory limitations prior to use. 2 Normative referenc

25、es 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 (including any amendments) applies. EN ISO 1042, Laboratory glassware One-mark vol

26、umetric flasks (ISO 1042:1998) EN ISO 3170, Petroleum liquids Manual sampling (ISO 3170:2004) EN ISO 3171, Petroleum liquids Automatic pipeline sampling (ISO 3171:1988) 3 Principle The sample is diluted with an organic solvent. The solution is then introduced directly into the ICP OES spectrometer.

27、Vanadium and nickel contents are determined by comparison with calibration solutions. An internal standard is employed to correct viscosity effects. 4 Reagents 4.1 Paraffin oil, with viscosity between 1,5 mm2/s and 6,0 mm2/s, Pharmacopeia (EUPHARM EP5), e.g. Merck 107174 1). 4.2 Kerosene, boiling ra

28、nge included between 150 C and 325 C, e.g. Aldrich 32.946-0 1). 4.3 Xylene, analytical reagent grade. 4.4 2-Ethyl hexanoic acid, analytical reagent grade or other suitable stabilizer for element standard solution. 1) This information is given for the convenience of the users of this European Standar

29、d and does not constitute an endorsement by CEN of these products. Equivalent products may be used if they can be shown to lead to the same results. DIN EN 15944:2011-02 EN 15944:2010 (E) 5 4.5 Element standard solutions, dissolved in oil, for example with 500 mg/kg per element, available as single

30、element standards, or at least partially as multi-element standards. NOTE Some commercial element standard solutions on the market are furnished with higher content. Those solutions may be used instead of the required solutions, but an initial mass to mass dilution should be done according to recomm

31、endations given in 7.1. 4.6 Argon, with minimum purity (Ar) = 99,996 % (V/V). NOTE Small amounts of oxygen (minimum purity (O2) 99,995 % (V/V) may be added 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

32、 5.1 Laboratory equipment All glassware shall be cleaned carefully before use to remove soluble constituents. Fill new glass vessels with xylene (4.3) and allow to stand for at least two days. 5.1.1 Glassware 5.1.1.1 Beakers, tall type, 150 ml. 5.1.1.2 Erlenmeyer flasks with wide neck and plug, 50 m

33、l. 5.1.1.3 Volumetric flasks, 500 ml, according to EN ISO 1042, with narrow neck and plug. 5.1.2 Sample containers, storage bottles with screw cap, brown glass. 5.1.3 Graduated pipettes or variable volume automatic pipettes, fitted with disposable polypropylene tips. 5.2 Balance, capable of weighing

34、 to the nearest 0,001 g. 5.3 ICP OES spectrometer, equipped with organic sample introduction system. 5.3.1 General Simultaneous and equally suitable sequential ICP OES spectrometer equipped for the analysis of organic liquids, with a high-frequency generator and a nebulizer suitable for organic solv

35、ents. 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 Recommended wavelengths The recommended wavelengths for nickel, vanadium and in

36、ternal standard element are reported in Table 1. Organometallic yttrium has performed well as an internal standard for this test method and is recommended. DIN EN 15944:2011-02 EN 15944:2010 (E) 6 Table 1 Recommended wavelengths Element Wavelength nm Nickel 216,555 231,604 221,647 Vanadium 292,401 3

37、09,310 Cobalt Scandium Yttrium 238,892 361,383 224,306 371,029 360,073 NOTE The line at 227,021 nm may be used for nickel, but this line suffers from interference with tungsten. Lines at 268,796 nm and 311,070 nm may be used for vanadium, but these lines suffer from interference with molybdenum and

38、manganese respectively. 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 the product under consideration. The samples shall be filled into clean containers. The containers

39、shall be rinsed with xylene (4.3) at least twice and then dried before use. 7 Preparation of calibration solutions 7.1 General In order to avoid inhomogeneity, the standard solutions (4.5) shall be shaken vigorously before use. The masses given correspond to a nominal element content of 500 mg/kg pe

40、r element in the multi-element solutions (4.5). If solutions with other element contents or single element standards 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 calibrati

41、on solutions, taking into account the exact masses. 7.2 Calibration solutions For each calibration solution, weigh stock standard solution (4.5), stabiliser (4.4), and paraffin oil (4.1) to the nearest 0,001 g in 50 ml Erlenmeyer flasks (5.1.1.2) as indicated in Table 2. All solutions shall be homog

42、enized by vigorous shaking. Table 2 Calibration solutions Calibration solutionElement contentmg/kg Standard solutiong Stabilizerg Paraffin oil g 1 0 (blank) - 0,15 24,85 2 5 0,25 0,15 24,603 10 0,50 0,15 24,35 4 20 1,00 0,15 23,855 100 5,00 0,15 19,85 6 200 10,00 0,15 14,85DIN EN 15944:2011-02 EN 15

43、944:2010 (E) 7 7.3 Internal standard solution Weigh 5 g of cobalt, scandium or yttrium stock solution (4.5) with a precision of 0,001 g in a 500 ml volumetric flask (5.1.1.3). Add 3 g of stabilizer (4.4) and fill up to 500 ml with a mixture of kerosene/xylene solvent having a volume ratio of 2:1 (4.

44、2 and 4.3). The solution shall be homogenized before use by vigorous shaking. NOTE 1 The use of a mixture of xylene and kerosene is necessary to avoid precipitation of asphaltene fractions occurring when kerosene only is employed, and to reduce the build-up of carbon on the tip of the torch. NOTE 2

45、Experience from daily practice with yttrium used as internal standard has shown that internal standard solutions can be used for about two weeks. 7.4 Working solutions For each calibration solution (7.2), weigh (1,0 0,001) g in a 50 ml Erlenmeyer flask (5.1.1.2). Add 10 ml of internal standard solut

46、ion (7.3). All prepared solutions shall be homogenized by vigorous shaking. 8 Calibration 8.1 General The ICP OES spectrometer setup with organic solutions and the instrument check are performed according to the instructions of the manufacturer. The choice of the instrumental parameters is made to o

47、btain the best signal/background ratio for all elements. Net intensity of analytical lines shall be calculated by subtracting the intensity measured at appropriate background wavelengths. Some instruments are equipped with software which allows the automatic correction of the background. A separate

48、calibration function for each element under investigation shall be established. 8.2 Calibration of the ICP OES spectrometer The calibration of the ICP OES spectrometer shall be done by the measurement of the blank solution and of the working solutions (7.4) using three replicates. For the determinat

49、ion of the elements, the wavelengths recommended in Table 1 shall be used. The background subtraction shall be performed at wavelengths not affected by other lines. IMPORTANT Ensure that the wavelengths used in calibration also match exactly the ones used in the sample measurement. Depending on the spectrometer software, follow either procedure A or B. 8.3 Procedure A For each element under invest