DIN EN 15492-2012 Ethanol as a blending component for petrol - Determination of inorganic chloride and sulfate content - Ion chromatographic method German version EN 15492 2012《作为汽.pdf

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1、April 2012 Translation by DIN-Sprachendienst.English price group 8No 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!$ae“1886266www.din.deDDIN EN 15492Ethanol as a blending component for petrol Determination of inorganic chloride and sulfate content Ion chromatographic methodEnglish translation of DIN EN 15492:2012-04Ethanol zur Verwendung als Blendkomponente in Ottokraftstoff Bestimmung des Gehaltes an a

3、norganischem Chlor und Sulfat IonenchromatographieEnglische bersetzung von DIN EN 15492:2012-04thanol comme base de mlange lessence Dtermination de la teneur en chlorures minraux et en sulfates Mthode par chromatographie ioniqueTraduction anglaise de DIN EN 15492:2012-04SupersedesDIN EN 15492:2009-0

4、1www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1303.12 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related

5、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 062-06-32-04 UA, Spiegelausschuss zur CEN/TC 19 TF Ana

6、lytik und Spezifikation von Ethanol und E85 of the Fachausschuss Minerall- und Brennstoffnormung (FAM). In the Note to 8.2. Calibration the symbol R is used to denote the correlation coefficient. This should not be confused with “reproducibility”, which is also denoted by the symbol R in this standa

7、rd. Though this is inferred in the Note to 8.2, the correlation coefficient R is not a reliable index of the non-linear behaviour of a calibration curve. Instead, the assessment of non-linearity should be based on systematically ascending or descending deviations of the data points from the regressi

8、on line (i. e. on the absence of normally distributed residuals). Further, non-linear behaviour of a calibration curve does not necessarily mean this cannot be used for the analysis, if the evaluation of signal areas to determine the content uses the correct linear inverse of the calibration. The DI

9、N Standard corresponding to the European Standard referred to in this document is as follows: EN ISO 3696 DIN ISO 3696 Amendments This standard differs from DIN EN 15492:2009-01 as follows: a) the range of application for the chloride content determination has been extended; b) the range of applicat

10、ion for the sulfate content determination has been extended; c) parts of the procedure have been updated according to laboratory practice; d) the results are now to be reported in mg/kg; e) the precision data for chloride and sulfate determination have been revised. Previous editions DIN EN 15492: 2

11、008-03, 2009-01 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods DINEN 15492:2012-04EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15492 January 2012 ICS 71.080.60; 75.160.20 Supersedes EN 15492:2008English Version Et

12、hanol as a blending component for petrol - Determination of inorganic chloride and sulfate content - Ion chromatographic method thanol comme base de mlange lessence - Dtermination de la teneur en chlorures minraux et en sulfates - Mthode par chromatographie ionique Ethanol zur Verwendung als Blendko

13、mponente in Ottokraftstoff - Bestimmung des Gehaltes an anorganischem Chlor und Sulfat - Ionenchromatographie This European Standard was approved by CEN on 26 November 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Europ

14、ean 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 CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions

15、 (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 has the same status as the official versions. CEN members are the national standards bodies of Austria, Bel

16、gium, Bulgaria, Croatia, 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, Turkey and United Kingdom. EURO

17、PEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15492:2012: E2 Contents Page

18、 Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .56 Sampling .67 Preparation of calibration solutions 67.1 Intermediate calibration solutions .67.2 Calibration solutions .68 Preparation of apparatus 78.1 Setting up the instrument .78.2 Calibration 79 Procedure .89.1

19、 Sample preparation .89.2 Sample analysis .810 Calculations 911 Expression of results 912 Precision .912.1 General 912.2 Repeatability, r .912.3 Reproducibility, R . 1013 Test report . 10Bibliography . 11EN 15492:2012 (E) DINEN 15492:2012-043 Foreword This document (EN 15492:2012) has been prepared

20、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 identical text or

21、by endorsement, at the latest by July 2012, and conflicting national standards shall be withdrawn at the latest by July 2012. 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 ide

22、ntifying any or all such patent rights. This document supersedes EN 15492:2008. The method described in this document was originally based on a method from a European Regulation on wine 1. This method has been developed and revised in 2008 to suit the needs as expressed in the ethanol specification

23、(EN 15376:2011 2), also drafted by CEN/TC 19. The precision and range of application for both inorganic chloride and sulfate have again been updated based on a second interlaboratory study done by CEN/TC 19/WG 27 on “Elemental analysis”. Small parts of the procedure have been updated according to la

24、boratory practice and a density correction has been included in order to be able to report the result of the test in mass fraction. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austri

25、a, Belgium, Bulgaria, Croatia, 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, Turkey and United Kingdom

26、. EN 15492:2012 (E) DINEN 15492:2012-044 1 Scope This European Standard specifies an ion chromatographic (IC) method for the determination of inorganic chloride content in ethanol from about 1 mg/kg to about 30 mg/kg and of sulfate content in ethanol from about 1 mg/kg to about 20 mg/kg. NOTE Sulfat

27、e content can be determined from 0,5 mg/kg to 1,0 mg/kg. However, the precision was not established as no samples with sulfate content in this range were included in the interlaboratory test. WARNING Use of this method may involve hazardous equipment, materials and operations. This method does not p

28、urport to address to all of the safety problems associated with its use, but it is the responsibility of the user to search and establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2 Normative references The following referenced do

29、cuments 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 15486:2007, Ethanol as a blending component for petrol Determination of s

30、ulfur content Ultraviolet fluorescence method EN ISO 1042, Laboratory glassware One-mark volumetric flasks (ISO 1042) EN ISO 3170, Petroleum liquids Manual sampling (ISO 3170) EN ISO 3675, Crude petroleum and liquid petroleum products Laboratory determination of density Hydrometer method (ISO 3675)

31、EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) EN ISO 12185, Crude petroleum and petroleum products Determination of density Oscillating U-tube method (ISO 12185) 3 Principle A test portion of ethanol sample is evaporated on a water bath. The dry residue i

32、s dissolved in water. The chloride and sulfate ion contents are determined by comparing the peak area in the chromatogram of the aqueous solution of the test portion with the curve of the calibration standards. The calibration standards are prepared from suitable compounds in aqueous solution. 4 Rea

33、gents Use only reagents of recognized analytical grade, such as “Ionic Chromatography grade”, unless otherwise specified. 4.1 Sodium chloride (NaCl), molar mass 58,44 g/mol. 4.2 Sulfuric acid (H2SO4), aqueous solution at 0,1 mol/l. The concentration of sulfuric acid shall be verified by titration, o

34、r shall be certified in case of commercially available product. EN 15492:2012 (E) DINEN 15492:2012-045 4.3 Water, for analytical laboratory use, conforming to grade 2 of EN ISO 3696. 4.4 Eluent compounds 4.4.1 Sodium carbonate (Na2CO3), molar mass 105,99 g/mol. 4.4.2 Sodium hydrogen carbonate (NaHCO

35、3), molar mass 84,01 g/mol. 4.4.3 Potassium hydroxide (KOH), molar mass 56,11 g/mol. 4.5 Nitric acid (HNO3) aqueous solution, c(HNO3) 0,75 mol/l. Cautiously add 50 ml 2 ml of nitric acid ( = 1,40 g/ml) to 500 ml 10 ml water (4.3). Mix and allow to cool to room temperature. Make up to 1 000 ml in a v

36、olumetric flask (5.3) with water (4.3). 5 Apparatus Before use, wash glassware (5.3) and evaporating dish (5.6) with nitric acid solution (4.5) and rinse thoroughly with water (4.3). 5.1 Ion chromatograph equipped with the following components. 5.1.1 Injection system, manual or automatic, with a sam

37、pling loop with minimum capacity of 25 l. 5.1.2 Pumping system, capable of delivering mobile phase flows between 0,5 ml/min and 1,5 ml/min with a precision better than 5 %. 5.1.3 Chromatographic column, of which the following conditions have been found satisfactory: Column Type anion exchange resin

38、Dimension 4,0 mm 250 mm Mesh size 9,0 m Eluent Composition 1 mmol/l Na2CO3+ 4 mmol/l NaHCO3 Flow rate 1,0 ml/min NOTE A 25 mmol/l KOH eluent may be used instead of the carbonate eluent. It is also possible to use a precolumn (4,0 mm 50,0 mm) with the same anion exchange resin and, if necessary, equi

39、pped with suppressors to remove interference from eluent. The thermal regulation of the system is not required, as the acceptable temperature of the column is in the range from 15 C to 30 C. 5.1.4 Conductivity detector, if necessary equipped with suppressor. 5.1.5 Integrator or computer, capable of

40、measuring peak areas and retention times and correct the data according to the baseline of the chromatogram. 5.2 Balance, capable of weighing with an accuracy of 0,01 mg. 5.3 Glassware: 25 ml, 50 ml, 100 ml and 1 000 ml volumetric flasks, according to EN ISO 1042, and 25 ml and 50 ml graduated cylin

41、ders. 5.4 Graduated pipettes, of 1 ml and 5 ml capacity or variable volume automatic pipettes fitted with disposable polypropylene tips. EN 15492:2012 (E) DINEN 15492:2012-046 5.5 Warm water bath NOTE In order to avoid potential external contamination, the warm water bath should be exempt of chlorid

42、e and sulfates, as during the evaporation process water can potentially be mixed into a certain extent with the ethanol samples. 5.6 Evaporating dish, capacity 100 ml to 250 ml. 5.7 Desiccator, containing freshly activated silica gel (or equivalent desiccant) with moisture content indicator. 5.8 Ove

43、n, thermostatically controlled at (105 2) C. 6 Sampling Unless otherwise specified, obtain samples in accordance with the procedures given in EN ISO 3170 and/or in accordance with the requirements of national standards or regulations for the sampling of the product under test. High-density polyethyl

44、ene containers shall be used. The containers shall be carefully cleaned and rinsed with water (4.3) to avoid contamination. Samples should be analysed as soon as possible after removal from bulk supplies to prevent loss of ethanol. 7 Preparation of calibration solutions 7.1 Intermediate calibration

45、solutions 7.1.1 Approximately 50 mg/l chloride solution. Weigh 82,4 mg of sodium chloride (4.1) in a 100 ml volumetric flask (5.3). Bring to the mark with water (4.3) and homogenise. Dilute this solution 1:10 with water (4.3) and homogenise. 7.1.2 Approximately 150 mg/l sulfate solution. Add 1,5 ml

46、of sulfuric acid (4.2) in a 100 ml flask (5.3). Bring to the mark with water (4.3) and homogenise. 7.1.3 The actual concentration of chloride and sulfate used shall be known to calculate the concentration of each ion in the solution, as 50 mg/l and 150 mg/l only represent target concentrations. NOTE

47、 Alternatively, commercially available stock calibration solutions may be used, provided that the solutions are traceable to primary stock solutions or Certified Reference Materials and are free from other analytes if single ion solutions are employed. 7.2 Calibration solutions Dilute the intermedia

48、te calibration solutions (7.1) with water (4.3) in five volumetric flasks to obtain calibration solutions having the ion contents as given in Table 1. Fresh solutions shall be prepared daily. EN 15492:2012 (E) DINEN 15492:2012-047 Table 1 Ion contents for calibration solutions Solution Sulfate Chloride mg/l mg/l1 (blank) 0 0 2 1,0 2,0 3 2,0 5,04 5,0 10,0 5 10,0 20,08 Preparation of apparatus 8.1 Setting up the instrument Since instruments from