BS EN 15721:2013 BS 2000-571:2013 BSI Standards Publication Ethanol as a blending component for petrol — Determination of higher alcohols, methanol and other impurities — Gas chromatographic method BS EN 15721:2013 BS 2000-571:2013 BRITISH STANDARD National foreword This British Standard is the UK implementation of EN 15721:2013 It supersedes BS EN 15721:2009 which is withdrawn The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum Testing and Terminology A list of organizations represented on this committee 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 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 i ndividually Further information is available from: Energy Institute, 61 New Cavendish Street, London, 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 © The British Standards Institution 2013 Published by BSI Standards Limited 2013 ISBN 978 580 77928 ICS 75.160.20 Compliance with a British Standard cannot confer immunity from legal obligations This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2013 Amendments issued since publication Date Text affected EN 15721 EUROPEAN STANDARD BS EN 15721:2013 BS 2000-571:2013 NORME EUROPÉENNE EUROPÄISCHE NORM August 2013 ICS 75.160.20 Supersedes EN 15721:2009 English Version Ethanol as a blending component for petrol - Determination of higher alcohols, methanol and other impurities - Gas chromatographic method Éthanol comme base de mélange l'essence Détermination de la teneur en alcools supérieurs, méthanol et autres impuretés - Méthode par chromatographie en phase gazeuse Ethanol zur Verwendung als Blendkomponente in Ottokraftstoff - Bestimmung von höheren Alkoholen, Methanol und anderen Verunreinigungen Gaschromatographisches Verfahren This European Standard was approved by CEN on 12 July 2013 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 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 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, 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 United Kingdom EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels © 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members Ref No EN 15721:2013: E BS EN 15721:2013 EN 15721:2013 (E) Contents Page Foreword Introduction Scope Normative references Principle Reagents and materials 5 Apparatus .6 Sampling 7 7.1 7.2 7.3 7.4 7.5 Procedure .8 General General considerations for preparation and handling of solutions Preparation of solutions for Procedure A Preparation of solutions for Procedure B Determination 10 8.1 8.2 8.3 Calculation 12 Content of individual compounds 12 Calculation of group contents 12 Expression of results 13 9.1 9.2 9.3 Precision 13 General 13 Repeatability 13 Reproducibility 13 10 Test report 14 Annex A (informative) Examples of chromatograms 15 Bibliography 21 BS EN 15721:2013 EN 15721:2013 (E) Foreword This document (EN 15721:2013) 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 publication of an identical text or by endorsement, at the latest by February 2014, and conflicting national standards shall be withdrawn at the latest by February 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] shall not be held responsible for identifying any or all such patent rights This document supersedes EN 15721:2009 EN 15721:2013 includes the following significant technical changes with respect to EN 15721:2009: the method has been simplified and more tailored towards the determination of the higher alcohols as mentioned in EN 15376 (propan-1-ol, butan-1-ol, butan-2-ol, 2-methylpropan-1-ol (isobutanol), 2-methylbutan-1-ol, 3-methylbutan-1-ol, methanol) All other alcohol compounds are summed as impurities The response factor check and the listed example response factors have been taken out According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, 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, Switzerland, Turkey and the United Kingdom BS EN 15721:2013 EN 15721:2013 (E) Introduction This document specifies a gas chromatographic (GC) test method for the determination of a number of compounds present in ethanol for use as a blending component in petrol according to the CEN ethanol [1] blending component specification EN 15376 The test method comprises of GC identification and analysis of a number of molecules, which are then attributed to several classes ("impurities", "methanol", "higher alcohols"), which are needed for calculation of the specified values as required in EN 15376 The method described in this document was prepared by CEN/TC 19’s Working Group and is based on two [2] [3] methods ( and ) published from a European Regulation on wine and on other internationally published [4] analytical methods on spirits The method is modified for determinations in ethanol for automotive applications BS EN 15721:2013 EN 15721:2013 (E) Scope This European Standard specifies a gas chromatographic method for ethanol, in which higher alcohols (propan-1-ol, butan-1-ol, butan-2-ol, 2-methylpropan-1-ol (isobutanol), 2-methylbutan-1-ol, and 3-methylbutan-1-ol) from 0,1 % up to 2,5 % (m/m), methanol from 0,1 % up to % (m/m) and other impurities, in the range from 0,1 % up to % (m/m) are determined Impurities are all the compounds not attributed to the groups of higher alcohols or methanol NOTE The European ethanol blending component specification higher alcohols, not the ethanol content itself [1] sets a limit for the combined result of ethanol + Due to possible interferences, the method is not applicable to denatured ethanol samples Water, if present in the sample, is not included in this analysis, because a signal for water is not visible in the chromatogram Therefore, if "alcohol content" is called up in a specification, water needs to be considered separately in the calculations NOTE 2 For the purposes of this European Standard, the term “% (m/m)” is used to represent the mass fraction (ω) Normative references The following 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 3170, Petroleum liquids — Manual sampling (ISO 3170) EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) Principle The compounds specified in the scope are determined by direct injection of a test portion into a gas chromatograph (GC) system An internal standard is added to the sample prior to the injection The compounds are separated with suitable GC equipment using temperature programming with the option to also use flow programming on a suitable column They are detected using a flame ionisation detector (FID) The concentration of each compound is determined from response factors with respect to the internal standard The response factors are obtained during calibration using the same chromatographic conditions as those for the analysis of the ethanol samples Two procedures ("Procedure A" and "Procedure B") are specified which differ mainly in the optional use of a water dilution step prior to the analysis Both variants have been validated to produce identical results and precision in extensive RR tests Reagents and materials All reagents shall be of recognised analytical grade (minimum 99 %) or of higher purity, if commercially available They shall be stored in closed dark glass bottles and can be used for some long time Other internal standards may also be used when there is sufficient proof that their GC signal does not interfere with the other signals in the chromatogram 4.1 Water which, for analytical laboratory use, shall conform to grade of EN ISO 3696 BS EN 15721:2013 EN 15721:2013 (E) 4.2 Compounds The compounds used for calibration and peak identification are listed in Table Table — Compounds for calibration, used as solvents and other related information Compound Attributed to group Calibration compounds Methanol Methanol Propan-1-ol Higher Alcohols Butan-1-ol Higher Alcohols Butan-2-ol Higher Alcohols 2-Methylpropan-1-ol Higher Alcohols 2-Methylbutan-1-ol Higher Alcohols 3-Methylbutan-1-ol Higher Alcohols Internal standards Pentan-3-ol Internal standard for Procedure A 4-Methylpentan-2-ol Internal standard for Procedure B Solvent Ethanol a a Solvent Ethanol is needed in Procedure "A" and "B" as a solvent for the calibration solutions The purity of the ethanol should be taken into account when preparing the mixtures It should not contain any impurities that may interfere with the analysis and the results shall be corrected for the purity of the ethanol Apparatus 5.1 Gas chromatograph, equipped with a Flame Ionisation Detector (FID), a split injector and connected to a PC or other system permitting the recording of chromatograms and execution of quantitative calculations 5.2 Gas chromatographic column 5.2.1 General Bonded capillary column with a suited phase, permitting the complete separation of all requested compounds for the analysis, except for 2-methylbutan-1-ol and 3-methylbutan-1-ol, for which a minimum peak resolution of 1,0 (see 5.2.2) is required The internal standard shall be perfectly separated from all other compounds Additional detail, including sample chromatograms, is given in Annex A 5.2.2 Chromatographic resolution The column resolution (as measured for 2-methylbutan-1-ol and 3-methylbutan-1-ol) shall be at least 1,0 Determine the column resolution, CR, with the calibration solutions (7.3) or (7.4) for the 2-methylbutan-1-ol and 3-methylbutan-1-ol peaks using the following Formula (1): CR = 2(t − t ) 1,699(W1 + W ) (1) BS EN 15721:2013 EN 15721:2013 (E) where t1 is the retention time, in seconds, for the 2-methylbutan-1-ol peak; t2 is the retention time, in seconds, for the 3-methylbutan-1-ol peak; W1 is the width, in seconds, at half-height of 2-methylbutan-1-ol peak; W2 is the width, in seconds, at half-height of 3-methylbutan-1-ol peak Figure presents further clarification on the calculation of column resolution, CR, of 2-methylbutan-1-ol and 3-methylbutan-1-ol according to procedure “B” (example: CR = 1,30) Key Pentan-3-ol (retention time 12,292 min) X retention time (min) 2-methylbutan-1-ol 3-methylbutan-1-ol (retention time 13,741 min) (retention time 13,820 min) Y FID signal Figure — Typical chromatogram for calculation of column resolution 5.3 Analytical balance, capable of weighing to the nearest 0,1 mg 5.4 Vials, having seals and used for test portions and calibration solutions Sampling Unless otherwise specified, laboratory samples shall be obtained by the procedures specified in EN ISO 3170 Glass bottles shall be used for taking samples The glass bottles shall be meticulously cleaned and rinsed at least twice with the product to be sampled Special care shall be taken during all further manipulations with the samples to avoid any risk of further contamination, e.g with water BS EN 15721:2013 EN 15721:2013 (E) Procedure 7.1 General Two method variants are defined in this document: a) "Procedure A", using direct injection of a test portion; b) "Procedure B", using injection after one additional preparation step, i.e dilution of the sample with water Which of the two method variants is used is subject to decision in the laboratory It may also depend on a particular request for solution to a specific problem See the examples of chromatograms in Annex A for additional detail 7.2 General considerations for preparation and handling of solutions Several precautions shall be observed in the preparation and handling of stock solutions and calibration solutions to avoid loss of material due to the high volatility of all used compounds Therefore, preparations should always be done starting with the least volatile compound All solutions are prepared gravimetrically Septum caps shall only be removed immediately before adding the next component and replaced immediately after It is strongly recommended to replace a used cap by a new one This change should be done after cooling the sample to about °C The glass vials containing the prepared calibration solutions shall be stored at °C and may be used for six months at maximum 7.3 Preparation of solutions for Procedure A 7.3.1 Calibration stock solution (E) for Procedure A Put a 100 ml septum vial (5.4) on the analytical balance (5.3), close the vial with a cap, and record the mass Open the vial and fill 80 ml of ethanol solvent (see 4.2) in, put the cap on the vial and record the mass of the ethanol added Successively add ml of each of the following compounds through the septum and record the individual added mass to the nearest 0,1 mg: a) 3-methylbutan-1-ol, b) 2-methylbutan-1-ol, c) butan-1-ol, d) 2-methylpropan-1-ol (iso-butanol), e) propan-1-ol, f) butan-2-ol, BS EN 15721:2013 EN 15721:2013 (E) 7.4.2 Internal standard stock solution (ES) for Procedure B In a 20 ml vial add about 16 ml of ethanol solvent and weigh to the nearest 0,1 mg Add 160 µl of the internal standard (4-methylpentan-2-ol) and record the weight to the nearest 0,1 mg 7.4.3 Calibration solution (FS1) for Procedure B Pipette ml of the E solution (7.4.1), transfer the preparation to a 100 ml flask and record the exact mass Add 50 ml of ethanol, record exact mass Add 10 ml of the internal standard solution, (ES, 7.4.2), and weigh to the nearest 0,1 mg Then fill up to 100 ml with water and shake vigorously 7.4.4 Preparation of sample (S) for Procedure B The purity of the ethanol should be taken into account when preparing the samples, it should not contain any impurities that may interfere with the analysis and the results shall be corrected for the purity of the ethanol Reduce alcoholic strength of the sample to about 40 g/100 g of ethanol with pure water If it is necessary to dilute sample, use pure ethanol (4.2) as dilution solution before reducing the alcoholic strength EXAMPLE ml of water with ml of sample in a 20 ml vial, cap the vial, shake vigorously Record exact mass of sample and diluted sample solution Add ml of ES solution (7.4.2) to 10 ml sample, record exact mass of internal standard solution added 7.5 7.5.1 Determination Gas chromatograph analysis conditions Typical gas chromatography conditions are given in Table in case of using a CPWax 57 CB column (25 m (length) x 250 µm (diameter) x 0,2 µm (film thickness)) and a DB 1701 column (60 m x 250 µm x 1,0 µm) See Annex A for further detail Relative retention times shall be determined and recorded for each signal in the calibration solution and saved for further reference Examples of typical retention times are given in Annex A 10 BS EN 15721:2013 EN 15721:2013 (E) Table — Chromatographic conditions for two different column systems Column A Part of GC a Column B a Value Unit Value Unit Split injector temperature 200 °C 200 °C Split ratio 90 — 50 — FID temperature 200 °C 260 °C FID air flow 400 ml/min 300 ml/min FID hydrogen flow 35 ml/min 30 ml/min FID makeup flow 30 ml/min 30 Carrier gas Mean linear velocity Flow program He b 21 He cm/s ml/min b 22 (0,8 to 1) ml/min from to 20 min, then (1 to 1,5) ml/min for 10 cm/s 1,4 ml/min Injection volume Procedure A µl µl Injection volume Procedure B µl µl Oven temperature profile 35 °C during 10 min, then by °C/min to 80 °C, then by 15 °C/min to 200 °C (8 min) 40 °C during min, then °C/min to 250 °C, then hold a Column A is a CPwax 57 and column B is a DB 1701 1) b Hydrogen or nitrogen is also possible, however may result in slightly different retention times, relative retention times (RRT) and peak resolutions 7.5.2 Determination of response factors Response factors are calculated for each compound in the mixture from the chromatogram of the calibration solution FS1 (7.3.3 for Procedure A; 7.4.3 for Procedure B) using Formula (2): FA = SEI ⋅ C A S A ⋅ CEI (2) where FA is the response factor for compound A; CA is the concentration of compound A in mg/100 g; CEI is the internal standard concentration in mg/100 g; SA is the peak area of compound A; SEI is the peak area of internal standard 1) CPWax and DB 1701 are examples of suitable commercially available products This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of these products 11 BS EN 15721:2013 EN 15721:2013 (E) If the concentrations in the sample are a multiple of the concentration in the calibration solution, adjust the concentration in the calibration solution to an appropriate level 7.5.3 Recording the chromatogram The chromatogram is recorded following the instructions of the apparatus manufacturer by injecting the sample (S) (7.3.4 for Procedure A, 7.4.4 for Procedure B) using the injection volumes and recommended operation parameters given in Table (see also Annex A) Before execution of the final calculations, the chromatogram shall be checked for correct peak identification by comparison (e.g relative retention times) with those from the calibration chromatograms 7.5.4 Performance checks The apparatus shall be checked in regular intervals to make sure that it is in perfect working condition This may be done with a calibration solution, a sample solution containing higher alcohols and methanol or with a consensus sample from a round robin study Checking shall be done using exactly the same operation settings as for the analysis Attention should be paid to: base line, signal form(s), relative retention times and response factors Calculation 8.1 Content of individual compounds The content (CA) of each compound (A) is calculated according to Formula (3) The compounds as specified in Table will use the response factor as calculated in 7.5.2, all other components shall be calculated using a response factor of 2, relative to that of the internal standard Care shall be taken to apply the dilution factor correctly when the sample has been diluted with water in Procedure B Calculated results for each compound are given in % (m/m) and are recorded without rounding for later group assignment and summation CA = S A ⋅ CEI ⋅ F ⋅D F S EI (3) where 8.2 CA is the content of compound A; F is the calculated response factor from calibration of compound A; SA is the peak area for compound A; CEI is the internal standard concentration in g/100 g; SEI is the area of internal standard peak; DF is the sample dilution factor Calculation of group contents Calculation of group contents is the same for Procedure A and Procedure B and is carried out by summation of the corresponding individual compound determined as in (8.1), respecting the group assignments from Table 12 BS EN 15721:2013 EN 15721:2013 (E) Water, if present in the sample, is not included in this analysis, because a signal for water is not visible in the chromatogram Therefore, if "alcohol content" is called up in a specification, water shall be analysed and considered separately in calculations Individual compounds for which the calculated content according to (8.1) is less than 0,001 % (m/m) are not included in the summation 8.3 Expression of results Results for the following group contents shall be calculated, and reported after rounding to the nearest 0,001 % (m/m): Impurities (Ci) = sum of content of all peaks not belonging to those of Table Methanol (Cm) = methanol content Higher alcohols (Ch) = sum of content of higher alcohols as specified in Table Ethanol, including higher alcohols (Ce) = 100,000 – Ci – Cm 9.1 (4) Precision General The precision has been determined by statistical examination of inter-laboratory test results using [5] EN ISO 4259 procedures Since extensive round robin testing has shown that precision estimators for Procedure A and Procedure B not show visible differences, only one precision statement is given which is valid for Procedure A and Procedure B 9.2 Repeatability The difference between two test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material, would in the long run, in the normal and correct operation of the test method, exceed the values calculated from the formulae given in Table only in one case in twenty 9.3 Reproducibility The difference between two single and independent test results, obtained by different operators working in different laboratories on identical test material, would in the long run, in the normal and correct operation of the test method, exceed the values calculated from the formulae given in Table only in one case in twenty 13 BS EN 15721:2013 EN 15721:2013 (E) Table — Precision prediction formulae Determination Repeatability, r % (m/m) a Reproducibility, R a % (m/m) Cm r = 0,101 X - 0,007 R = 0,334 X - 0,006 Ch r = 0,012 X + 0,025 R = 0,295 X - 0,003 Ce r = -0,025 X + 2,572 R = -0,302 X + 30,261 X a is the mean of the two results being compared Results calculated for r and R shall be rounded to the nearest 0,001 % (m/m) 10 Test report The test report shall specify: a) reference to this European Standard, i.e EN 15721; b) type and complete identification of the product tested; c) procedure used, i.e Procedure A or Procedure B; d) result of the test (see 8.3); e) any deviation, by agreement or otherwise, from the procedure specified; f) date of the test 14 BS EN 15721:2013 EN 15721:2013 (E) Annex A (informative) Examples of chromatograms This annex shows additional detail from sample chromatograms using a CPWax 57 2) CB column (25 m, 250 µm, 0,2 µm stationary phase) and a DB 17012) column (60 m, 250 μm, 1,0 μm stationary phase) The figures show the specific peaks and retention times for those individual compounds that may be present in ethanol Figure A.1 shows a chromatogram of a bioethanol calibration mixture produced on a DB 1701 column using procedure A Figure A.2 shows a chromatogram of a bioethanol sample produced on a similar column using the same procedure For details concerning compounds and retention times as indicated in the two figures, see Table A.1 Key X retention time (min) Y FID signal Figure A.1 — Calibration mixture on a DB 1701 column 2) CPWax and DB 1701 are examples of suitable commercially available products This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of these products 15 BS EN 15721:2013 EN 15721:2013 (E) Key X retention time (min) Y FID signal Figure A.2 — Sample on a DB 1701 column Table A.1 — Compounds and retentions times for Column DB 1701 Peak no Figure A.2 Retention time Retention time Ethanal (Acetic aldehyde) 4,968 4,971 Methanol 5,215 5,221 Ethanol Propan-1-ol 8,616 8,617 Ethyl-ethanoate (Ethyl acetate) 8,992 8,997 Butan-2-ol 9,489 2-Methylpropan-1-ol (Isobutanol) 10,456 10,457 Acetal (1,1-Diethoxyethane) 11,523 11,525 Butan-1-ol 11,584 10 Pentan-3-ol a 12,292 11 3-Methylbutan-1-ol 13,741 12 2-Methylbutan-1-ol 13,820 a 16 Compound Figure A.1 Internal standard 12,293 BS EN 15721:2013 EN 15721:2013 (E) Figure A.3 shows a chromatogram of a bioethanol calibration mixture produced on a CPWax column using procedure A, whereas Figure A.4 shows one of a bioethanol sample using the similar procedure For details concerning compounds and retention times, see Table A.2 Key X retention time (min) Y FID signal Figure A.3 — Calibration mixture on a CPWax column Key X retention time (min) Y FID signal Figure A.4 — Sample on a CPWax column 17 BS EN 15721:2013 EN 15721:2013 (E) Table A.2 — Compounds and retentions times for Column CPWax Peak No 18 Figure A.3 Figure A.4 Retention time Retention time 2,908 Compound Ethanal (Acetic aldehyde) 2,900 2-Methylpropanal (Isobutyric aldehyde) 3,601 Propan-2-on (acetone) 3,652 3,657 Ethyl-ethanoate (Ethyl-acetate) 4,600 4,581 Acetal (1,1-Diethoxyethane) 4,770 4,750 3-Methylbutanal (Isovaleric aldehyde) 5,100 5,109 Methanol 5,170 tert-Butanol 5,490 Propan-2-ol (Isopropanol) a 6,000 10 Pentanal (Valeric aldehyde) a 7,100 11 Ethyl-butyrate (Butanoic acid ethyl ester) 9,742 9,735 12 Butan-2-ol 10,200 10,190 13 Propan-1-ol 10,900 10,897 14 2-Methylpropan-1-ol (Isobutanol) 13,530 13,543 14,420 14,390 16,011 b 15 Pentan-3-ol 16 Butan-1-ol 16,000 17 3-Methylbutan-1-ol 18,360 18 2-Methylbutan-1-ol 18,440 a Co-elution with ethanol b Co-elution with 3-methyl-1-butyl acetate (isoamyl acetate) BS EN 15721:2013 EN 15721:2013 (E) Figure A.5 shows a chromatogram of a bioethanol calibration mixture produced on a CPWax column using procedure B For peak assignments, see Table A.3 Exact data towards the signal assignments are not available Key X retention time (min) Y FID signal Figure A.5 — Calibration mixture on a CPWax column using procedure B 19 BS EN 15721:2013 EN 15721:2013 (E) Table A.3 — Compounds for chromatogram A.5 (Column CPWax, Procedure B) Peak No Ethanal (Acetic aldehyde) Ethyl-ethanoate (Ethyl-acetate) Acetal (1,1-Diethoxyethane) Methanol Butan-2-ol Propan-1-ol 2-Methylpropan-1-ol (Isobutanol) Pentan-3-ol Pentan-2-ol 10 Butan-1-ol 11 4-Methylpentan-2-ol 12 3-Methylbutan-1-ol 13 2-Methylbutan-1-ol 14 Pentan-1-ol a 20 Compound = Internal Standard a BS EN 15721:2013 EN 15721:2013 (E) Bibliography [1] EN 15376, Automotive fuels — Ethanol as a blending component for petrol — Requirements and test methods [2] Determination of real alcoholic strength by volume of spirit drinks – Measurement by electronic densimetry (based on the resonant frequency oscillation of a sample in an oscillation cell), Appendix 2, method B of Regulation EC/2870/2000 of 19 December 2000 laying down Community reference methods for the analysis of spirits drinks [3] Determination of volatile substances and methanol of spirit drinks, Method III of EC/2870/2000 of 19 December 2000 laying down Community reference methods for the analysis of spirits drinks [4] International Spirits analytical methods, OIV, 1994 [5] EN ISO 4259, Petroleum products — Determination and application of precision data in relation to methods of test (ISO 4259) 21 BS 2000 Series Energy Institute Buying Parts of BS 2000 Orders for BS 2000 publications should be addressed to either: Energy Institute – Library and Information Service 61 New Cavendish Street London W1G 7AR Tel: +44 (0)20 7467 7100 Fax: +44 (0)20 7255 1472 www.energyinst.org.uk Order standards securely via: www.energyinstpubs.org.uk or: British Standards Institution – Customer Services 389 Chiswick High Road London W4 4AL Tel: +44 (0)20 8996 9001 Fax: +44 (0)20 8996 7001 www.bsi-global.com Order hard copy standards securely via: www.bsi-global.com/bsonline Copyright Copyright exists in all BS 2000 publications No part of this publication may be reproduced in any form without the prior permission in writing of BSI and the Energy Institute Enquiries about copyright should be made to the Secretary of PTI/13 at the Energy Institute PTI/13 This page deliberately left blank NO COPYING WITHOUT BSI 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