1、BRITISH STANDARD BS EN 14039:2004 Characterization of waste Determination of hydrocarbon content in the range of C10 to C40 by gas chromatography The European Standard EN 14039:2004 has the status of a British Standard ICS 13.030.01 BS EN 14039:2004 This British Standard was published under the auth
2、ority of the Standards Policy and Strategy Committee on 29 October 2004 BSI 29 October 2004 ISBN 0 580 44700 6 National foreword This British Standard is the official English language version of EN 14039:2004. The UK participation in its preparation was entrusted by Technical Committee B/508, Waste
3、management, to Subcommittee B/508/3, Waste management Characterisation of waste, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European pub
4、lications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the n
5、ecessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation,
6、 or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 22, an inside back cover and a back cover.
7、 The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN14039 September2004 ICS13.030.01 Englishversion CharacterizationofwasteDeterminationofhydrocarb
8、on contentintherangeofC10toC40bygaschromatography CaractrisationdesdchetsDterminationdelateneur enhydrocarburesparchromatographieenphasegazeuse danslaplageC10C40 CharakterisierungvonAbfllenBestimmungdesGehalts anKohlenwasserstoffenvonC10bisC40mittels Gaschromatographie ThisEuropeanStandardwasapprove
9、dbyCENon9July2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentra
10、lSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationals
11、tandardsbodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COM
12、ITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN14039:2004:EEN 14039:2004 (E) 2 Contents page Foreword 3 Introduction4 1 Scope.5 2 Normative refe
13、rences.5 3 Terms and definitions.5 4 Principle.6 5 Interferences.6 6 Reagents6 7 Hazards8 8 Equipment.8 9 Sample conservation and pretreatment 9 10 Procedure9 11 Performance characteristics12 12 Test report.13 Annex A (informative) Examples of gas chromatograms of hydrocarbon standard and waste samp
14、les 14 Annex B (informative) Determination of the boiling range of mineral oil hydrocarbons from the gas chromatogram.18 Annex C (informative) Flow diagram19 Annex D (informative) Aqueous liquid waste20 Annex E (informative) Summary of general requirements and recommendations 21 Bibliography.22 EN 1
15、4039:2004 (E) 3 Foreword This document (EN 14039:2004) has been prepared by Technical Committee CEN/TC 292 “Characterization of waste”, 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 e
16、ndorsement, at the latest by March 2005, and conflicting national standards shall be withdrawn at the latest by March 2005. Anyone dealing with waste and sludge analysis should be aware of the typical risks of that kind of material irrespective of the parameter to be determined. Waste and sludge sam
17、ples may contain hazardous (e.g. toxic, reactive, flammable, infectious) substances, which can be liable to biological and/or chemical reaction. Consequently these samples should be handled with special care. Gases which may be produced by microbiological or chemical activity are potentially flammab
18、le and will pressurise sealed bottles. Bursting bottles are likely to result in hazardous shrapnel, dust and/or aerosol. National regulations should be followed with respect to all hazards associated with this method. According to the CEN/CENELEC Internal Regulations, the national standards organiza
19、tions of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slove
20、nia, Spain, Sweden, Switzerland and United Kingdom. EN 14039:2004 (E) 4 Introduction Hydrocarbons are important constituents of many types of waste and contaminated soils. They have been determined up to now mainly by infrared spectroscopy after extraction with halogenated solvents such as 1,1,2-tri
21、chloro-1,2,2-trifluoroethane or tetrachloromethane. The objective of this standard is to provide an analytical method for the determination of hydrocarbon content by capillary gas chromatography avoiding the use of such solvents. The user of this document should be aware that the results of this sta
22、ndard might not be comparable with those obtained when using the infrared spectroscopy. A mixture of acetone and n-heptane is the preferred extraction solvent. For waste samples containing large amounts of relatively high boiling hydrocarbons the gravimetric method (see EN 14345) can be used. EN 140
23、39:2004 (E) 5 1 Scope This document specifies a method for the quantitative determination of the hydrocarbon content (C 10to C 40 ) in solid waste by gas chromatography. It is applicable to hydrocarbon content between 100 mg/kg and 10 000 mg/kg expressed as dry matter basis. Using this standard all
24、hydrocarbons with a boiling range of approximately 175 C to 525 C, e.g. n-alkanes from C 10 H 22to C 40 H 82 , isoalkanes, cycloalkanes, alkyl benzenes, alkyl naphthalenes and polycyclic aromatic compounds are determined as hydrocarbons, provided they do not adsorb on the Florisil column during clea
25、n-up. Volatile hydrocarbons cannot be quantitatively determined using this standard. This will affect the determination of some common hydrocarbon fuels, e.g. petrol. NOTE 1 On the basis of the peak pattern of the gas chromatogram (see Annex A) and of the boiling points of the individual n-alkanes l
26、isted in Annex B the approximate boiling range of the hydrocarbons and some qualitative information on the nature of the hydrocarbons can be obtained. NOTE 2 At the moment there is no sufficient information on how to handle organic liquid wastes for the analysis of hydrocarbons. NOTE 3 Aqueous liqui
27、d waste samples can be analysed in accordance with EN ISO 9377-2 or the procedure specified in Annex E. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the
28、latest edition of the referenced document (including any amendments) applies. prEN 14346, Characterization of waste Calculation of dry matter by determination of dry residue and water content EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987) ISO 8466-1
29、, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration function 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 hydrocarbon conte
30、nt by gas chromatography sum of compounds that are extractable with with acetone/n-heptane (2+1), provided that they do not adsorb on Florisil; they can be chromatographed on a non-polar capillary column with retention times between those of n-decane (C 10 H 22 ) and n-tetracontane (C 40 H 82 ) NOTE
31、 1 Substances that comply with this definition are mainly non-polar long chain or branched aliphatic, alicyclic, alkyl substituted aromatic or polycyclic aromatic compounds. NOTE 2 This definition differs from that given in EN 14345. EN 14039:2004 (E) 6 4 Principle A known amount of the homogenised
32、waste sample is extracted by mechanical shaking or sonication with acetone/n-heptane. The organic layer is separated and washed twice with water. Polar compounds are removed by chromatography on Florisil. An aliquot of the purified extract is analysed by capillary gas chromatography with flame ionis
33、ation detection. The total peak area between the retention time window standards n-decane and n-tetracontane is measured and the amount of hydrocarbons in the sample is quantified against an external standard consisting of equal amounts of two different types of mineral oil. NOTE Instead of heptane,
34、 other non-polar solvent (e.g. petroleum ether, cyclohexane, n-hexane) can be used, however its suitability for the extraction of hydrocarbons from waste has to be proven. 5 Interferences High concentration of more polar compounds, e.g. animal and vegetable fats and oils, may exceed the adsorption c
35、apacity of the Florisil used. A mass concentration of up to 10 000 mg/kg of such compounds will not interfere with the determination of hydrocarbon content. 6 Reagents 6.1 In general all reagents shall be of recognized analytical grade and suitable for their specific purposes. Use water complying wi
36、th at least EN ISO 3696, grade 3. 6.2 Acetone, (CH 3 ) 2 CO; 6.3 n-Heptane, C 7 H 16 ; 6.4 Florisil 1for the preparation of clean-up column, particle size 150 m to 250 m (mesh 100 to 60), heated for at least 16 h at 140 C and stored in a desiccator over a molecular sieve. Alternatively, commercially
37、 available Florisil cartridges can be used. 6.5 Anhydrous sodium sulfate, Na 2 SO 4 ; 6.6 Test solution of n-octadecanoic acid octadecyl ester, C 36 H 72 O 2 ; Dissolve about (100 1) mg of n-octadecanoic acid octadecyl ester in 100 ml n-heptane 6.3. The solution is stable for 6 months when stored in
38、 a refrigerator between 1 C and 5 C. 6.7 Retention time window (RTW) standard solution containing n-tetracontane and n-decane Weigh (30 1) mg of n-tetracontane into a 1 l volumetric flask, dissolve completely in an appropriate volume of n-heptane 6.3, add 30 l of n-decane (about 21 mg), mix well, fi
39、ll up to volume with n-heptane and homogenise. This solution shall be used for all dilution steps of the hydrocarbon standard 6.8 and be stored at room temperature. NOTE n-tetracontane is only moderately soluble in n-heptane. Slight warm-up and/or sonication accelerates the dissolution process. 6.8
40、Hydrocarbon standard solution for calibration 21Florisil is a trade name for a prepared diatomaceous substance, mainly consisting of anhydrous magnesium silicate. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of this product. Eq
41、uivalent products may be used if it can be shown to lead to comparable results. EN 14039:2004 (E) 7 Mix approximately equal masses of two different types of mineral oil. Weigh to the nearest 0,1 g this mixture and dissolve in the RTW standard solution 6.7 to give a hydrocarbon content of about 8 g/l
42、. Preparation of the calibration solutions can be done by diluting an aliquot of this standard solution 6.8 with the RTW standard solution 6.7. The first oil type should show discrete peaks in the gas chromatogram as can be seen in Figure A.1 (left part of the chromatogram) of Annex A. A suitable oi
43、l of this type is a diesel fuel without any additives. The second type should have a boiling range higher than the first one and should show a “hump“ in the gas chromatogram, as can be seen in Annex A, in Figure A.1 (right part of the chromatogram). A suitable oil of this type is a lubricating oil w
44、ithout any additives. 6.9 Control solution Prepare an independent control solution in accordance with 6.8 with a hydrocarbon concentration of about in the middle of the working range. 6.10 System performance standard solution Prepare a mixture of equal amounts, on a mass basis, of the n-alkanes with
45、 even carbon numbers from C 10to C 40 , dissolved in n-heptane 6.3, to give a concentration of about 50 mg/l of each n-alkane. Store at room temperature. NOTE 1 This solution is used to verify the suitability of the gas chromatographic system for the resolution of n-alkanes as well as for the detect
46、or response. NOTE 2 This solution is used to give information of the retention times of the n-alkanes to characterize the hydrocarbons in the samples. 2General purpose hydrocarbon standards for calibration can be obtained from many commercial organisations. Calibration standards specific to this Eur
47、opean Standard can be purchased from Bundesanstalt fr Materialforschung und -prfung, Fachgruppe I.2, Richard-Willsttter-Strasse 11 D-12489 Berlin, Germany. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product.
48、EN 14039:2004 (E) 8 6.11 Preparation of the clean-up column A plug of pre-washed glass wool or a PTFE frit is pushed down into the column 8.9. Then, successively 2 g Florisil 6.4 and 2 g sodium sulfate 6.5 are added. The column shall be prepared immediately before use. 7 Hazards Acetone and n-heptane are highly flammable solvents and shall therefore be handled with caution. Special care is required during centrifugation. During extraction substantial pressure can built-up in the extraction vessel. This pressure shall
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