1、BRITISH STANDARDBS EN 15553:2007 BS 2000-156:2007Petroleum products and related materials Determination of hydrocarbon types Fluorescent indicator adsorption methodThe European Standard EN 15553:2007 has the status of a British StandardICS 75.080g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3
2、g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Licensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontrolled Copy, (c) BSIBS EN 15553:2007This British Standard was published under the a
3、uthority of the Standards Policy and Strategy Committee on 31 May 2007 BSI and Energy Institute 2007ISBN 978 0 580 50782 3National forewordThis British Standard was published by BSI. It is the UK implementation of EN 15553:2007. It supersedes BS 2000-156:2005 which is withdrawn. The UK participation
4、 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 petrol
5、eum 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 individually.Further information is available from: Energy Institute, 61 New Cavendish Street, London W1G 7
6、AR. 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.Compliance with a British Standard cannot confer immunity from legal obligations.Amendments issued since publicationAm
7、d. No. Date CommentsLicensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15553April 2007ICS 75.080English VersionPetroleum products and related materials - Determination ofhydrocarbon types - Fluorescent indicato
8、r adsorption methodProduits ptroliers et produits connexes - Dterminationdes groupes dhydrocarbures - Mthode par adsorption enprsence dindicateur fluorescentMinerallerzeugnisse und verwandte Produkte -Bestimmung der Kohlenwasserstofftypen - Adsorptionsverfahren mit Fluoreszenz-IndikatorThis European
9、 Standard was approved by CEN on 24 February 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concer
10、ning such nationalstandards may be obtained on application to the CEN 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 translationunder the responsibility of a CEN member into its own la
11、nguage and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Lu
12、xembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All righ
13、ts of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15553:2007: ELicensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 15553:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Terms and de
14、finitions .5 4 Principle5 5 Reagents and materials 5 6 Apparatus .6 7 Sampling and sample handling9 8 Apparatus preparation 9 9 Procedure .10 10 Calculation12 11 Expression of results 13 12 Precision.13 12.1 Repeatability, r .13 12.2 Reproducibility, R 13 13 Test report 15 Annex A (normative) Specif
15、ication for silica gel .16 Annex B (informative) Standard adsorption column .17 Bibliography 19 Licensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 15553:2007 (E) 3 Foreword This document (EN 15553:2007) has been prepared by Technical Committee CEN/TC 19 “Ga
16、seous 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 Oct
17、ober 2007, and conflicting national standards shall be withdrawn at the latest by October 2007. This European Standard is based on IP 156/06 1. It is developed as an alternative method to ASTM D1319 2, in which a de-pentanization step is described, which is not used in this European Standard and the
18、 EU environment. 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
19、 Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 15553:2007 (E) 4 1 Scope This Europe
20、an Standard specifies a fluorescent indicator adsorption method for the determination of hydrocarbon types over the concentration ranges from 5 % (V/V) to 99 % (V/V) aromatic hydrocarbons, 0,3 % (V/V) to 55 % (V/V) olefinic hydrocarbons, and 1 % (V/V) to 95 % (V/V) saturated hydrocarbons in petroleu
21、m fractions that distil below 315 C. This method may be applicable to concentrations outside these ranges, but the precision has not been determined. When samples containing oxygenated blending components are analysed, the hydrocarbon type results can be reported on an oxygenate-free basis or, when
22、the oxygenate content is known, the results can be corrected to a total-sample basis. This test method is for use with full boiling range products. Cooperative data have established that the precision statement does not apply to petroleum fractions with narrow boiling ranges near the 315 C limit. Su
23、ch samples are not eluted properly, and results are erratic. Samples containing dark-coloured components that interfere with reading the chromatographic bands cannot be analysed. NOTE 1 The oxygenated blending components methanol, ethanol, tert-butyl methyl ether (MTBE), methyl tert-pentyl ether (TA
24、ME) and tert-butyl ethyl ether (ETBE) do not interfere with the determination of hydrocarbon types at concentrations normally found in commercial blends. These oxygenated compounds are not detected since they elute with the alcohol desorbent. The effects of other oxygenated compounds should be indiv
25、idually verified. NOTE 2 For the purposes of this European Standard, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass fraction and the volume fraction. WARNING The use of this European Standard may involve hazardous materials, operations and equipment. This European Stan
26、dard 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 determine the applicability of regulatory limitations prior to use. 2 Normative references The following
27、 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 1601, Liquid petroleum products Unleaded petrol Determinati
28、on of organic oxygenate compounds and total organically bound oxygen content by gas chromatography (O-FID) EN 13132, Liquid petroleum products Unleaded petrol Determination of organic oxygenate compounds and total organically bound oxygen content by gas chromatography using column switching EN ISO 3
29、170, Petroleum liquids Manual sampling (ISO 3170:2004) EN ISO 3171, Petroleum liquids Automatic pipeline sampling (ISO 3171:1988) EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) Licensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontrol
30、led Copy, (c) BSIEN 15553:2007 (E) 5 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 saturates saturated hydrocarbons volume percentage of alkanes plus cycloalkanes 3.2 olefins olefinic hydrocarbons volume percentage of alkenes plus cycloalke
31、nes plus some alkadienes 3.3 aromatics aromatic hydrocarbons volume percentage of monocyclic and polycyclic aromatic hydrocarbons plus aromatic olefinic hydrocarbons, some dienes, compounds containing sulfur or nitrogen, or higher-boiling oxygenated compounds 4 Principle Approximately 0,75 ml of sam
32、ple is introduced into a special glass adsorption column packed with activated silica gel. A small layer of the silica gel contains a mixture of fluorescent dyes. When all the sample has been adsorbed onto the gel, alcohol is added to desorb the sample down the column. The hydrocarbons are separated
33、, according to their adsorption affinities, into aromatics, olefins and saturates. The fluorescent dyes are also separated selectively with the hydrocarbon types, and render the boundaries of the aromatic, olefin and saturate zones visible under ultraviolet light. The volume percentage of each hydro
34、carbon type is calculated from the length of each zone in the column. 5 Reagents and materials Use only chemicals and reagents of recognised analytical grade and water conforming to grade 3 of EN ISO 3696. 5.1 Silica gel, manufactured to conform to the specifications given in Annex A. NOTE 1 Grace D
35、avison silica gel Grade 923 meets the requirements of this specification. Before use, dry the gel in a shallow vessel at 175 C for at least 3 h. Transfer the dried gel to an airtight container while still hot, and protect it from atmospheric moisture. NOTE 2 Some batches of silica gel that otherwise
36、 meet specifications have been found to produce olefin-boundary fading. The exact reason for this phenomenon is unknown but will affect accuracy and precision. 5.2 Fluorescent indicator-dyed gel, a standard dyed gel, consisting of a mixture of re-crystallized Petrol Red AB4 and purified portions of
37、olefin and aromatic dyes obtained by chromatographic adsorption following a definite, uniform procedure, and deposited on silica gel1). Store the dyed gel in a dark place under an atmosphere of nitrogen. NOTE When stored under these conditions, dyed gel can have a shelf life of at least five years.
38、It is recommended that portions of the dyed gel be transferred as required to a smaller working vial from which the dyed gel is routinely taken for analyses. 1)A list of suppliers is available from the Energy Institute, London. Licensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontr
39、olled Copy, (c) BSIEN 15553:2007 (E) 6 5.3 Propan-2-ol, 99 % (V/V) 5.4 3-methylbutan-1-ol, 99 % (V/V) (optional) 5.5 Acetone, reagent grade 5.6 Pressurizing gas, air (or nitrogen) capable of being delivered to the top of the column at controllable pressures over the range from 0 kPa gauge to 103 kPa
40、 gauge. NOTE A special valve with possibility to regulate this pressure to 2 kPa. (see Error! Reference source not found2) is advised as common valves do not always have this possibility. 6 Apparatus 6.1 Adsorption column, with precision bore tubing conforming to the specification given in Table 1 a
41、nd as shown in Figure 1, part b), made of glass and consisting of a charger section with a capillary neck, a separator section and an analyzer section. NOTE For routine/non-specification compliance analysis adsorption columns with standard wall tubing conforming to the specification given in Annex B
42、 and as shown in Figure 1, part a), may be used. In addition, the length of a thread of liquid approximately 100 mm long, which shall not vary in length by more than 0,3 mm in any part of the analyzer section. Licensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontrolled Copy, (c) BS
43、IEN 15553:2007 (E) 7 Table 1 Precision bore column dimensions and tolerance limits Charger section Inside diameter 12 mm 2 mm Overall length 150 mm 5 mm Neck section Inside diameter 2 mm 0,5 mm Overall length 50 mm 5 mm Separator section Inside diameter 5 mm 0,5 mm Overall length 190 mm 5 mm Analyze
44、r section Inside diameter 1,60 mm to 1,65 mm Overall length 1 200mm 30 mm Tip Overall length 30 mm 5 mm Licensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 15553:2007 (E) 8 Key 1 charger 2 neck 3 separator 4 tip 5 analyzer 6 pressuring gas 7 spherical joint
45、S29 8 pack gel to this level 9 long taper 10 dyed gel 11 zone measuring device (optional) 12 long taper 13 polyvinyl tubing 14 precision bore capillary tubing 15 standard wall tubing 16 spherical joint S13 17 tip drawn out to fine capillary Figure 1 Adsorption columns with a) standard wall and b) pr
46、ecision bore tubing in analyzer section Licensed Copy: Wang Bin, na, Thu Sep 13 03:22:39 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 15553:2007 (E) 9 Glass-sealing of the various sections to each other shall be done with long-taper connections rather than shouldered connections. The silica gel shal
47、l be supported with a small piece of glass wool located between the ball socket of the 12/2 spherical joint and covering the analyzer outlet. The column tip attached to the 12/2 socket shall be approximately 2 mm inside diameter. The ball and socket joints shall be clamped together to ensure that th
48、e tip does not tend to slide from a position in a direct line with the analyzer section during the packing and subsequent use of the column. 6.2 Zone-measuring-device Either a metre rule mounted adjacent to the column, fitted with four movable metal index clips, for measuring the length of each zone
49、, see Figure 1 and 9.9, or glass-writing pencils for marking zone boundaries and metre rule for measuring the length of each zone. 6.3 Ultraviolet light source, with radiation predominantly at wavelength 365 nm. NOTE A convenient arrangement consists of one or two units 915 mm or 1,220 mm in length mounted vertically alongside the apparatus adjusted to give the best fluorescence. 6.4 Electric vibrator, for vibrating the individual columns or for vibrating the frame supporting multiple columns. 6.5 Hypodermic syringe, capacity 1 m
