1、BS EN 15527:2008ICS 13.030.01NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDCharacterization ofwaste Determinationof polycyclic aromatichydrocarbons (PAH)in waste using gaschromatography massspectrometry (GC/MS)This British Standardwas published under theauthor
2、ity of the StandardsPolicy and StrategyCommittee on 31 March2009 BSI 2009ISBN 978 0 580 55486 5Amendments/corrigenda issued since publicationDate CommentsBS EN 15527:2008National forewordThis British Standard is the UK implementation of EN 15527:2008.The UK participation in its preparation was entru
3、sted to TechnicalCommittee B/508/3, Characterization of waste.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Com
4、pliance with a British Standard cannot confer immunityfrom legal obligations.BS EN 15527:2008EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15527July 2008ICS 13.030.01; 71.040.50English VersionCharacterization of waste - Determination of polycyclic aromatichydrocarbons (PAH) in waste using gas ch
5、romatography massspectrometry (GC/MS)Caractrisation des dchets - Dosage des hydrocarburesaromatiques polycycliques (HAP) dans les dchets parchromatographie en phase gazeuse/spectromtrie demasse (CG/SM)Charakterisierung von Abfllen - Bestimmung vonpolycyclischen aromatischen Kohlenwasserstoffen (PAK)
6、 inAbfall mittels Gaschromatographie-Massenspektrometrie(GC/MS)This European Standard was approved by CEN on 29 May 2008.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
7、 any alteration. Up-to-date lists and bibliographical references concerning 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
8、 by translationunder the responsibility of a CEN member into its own language 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, G
9、ermany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGM
10、anagement Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15527:2008: EBS EN 15527:2008EN 15527:2008 (E) 2 Contents Page Foreword3 Introduction .4 1 Scope 5 2 Normative references 5 3
11、Terms and definitions .5 4 Principle6 5 Reagents.6 5.1 General6 5.2 Reagents for extraction procedures6 5.3 Reagents for clean-up procedures 6 5.4 Reagents for gas chromatographic analysis7 5.5 Standards .7 6 Apparatus .8 6.1 Extraction and clean-up procedures .8 6.2 Gas chromatograph.9 6.3 Capillar
12、y columns9 6.4 Preparation of standard solutions .10 7 Hazards .11 8 Interference 12 8.1 Interference during sampling, storage and extraction 12 8.2 Interference due to co-elution 12 9 Sample conservation.12 10 Pretreatment.12 10.1 General12 10.2 Drying13 10.3 Particle size reduction.13 11 Procedure
13、 .13 11.1 Blank .13 11.2 Extraction .13 11.3 Addition of the internal standard solution 14 11.4 Concentration or dilution14 11.5 Clean up of the extract 14 11.6 Addition of the injection standard .15 11.7 Gas chromatographic analysis with mass spectrometric detection15 12 Performance characteristics
14、 19 13 Test report 22 Annex A (informative) Representative chromatograms23 Annex B (informative) Additional validation data 32 Annex C (informative) Summary of general requirements and recommendations36 Bibliography 37 BS EN 15527:2008EN 15527:2008 (E) 3 Foreword This document (EN 15527:2008) has be
15、en 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 endorsement, at the latest by January 2009, and conflicting na
16、tional standards shall be withdrawn at the latest by January 2009. 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. According to the CE
17、N/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, Ireland, Italy, Latvia, Lithuania,
18、Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 15527:2008EN 15527:2008 (E) 4 Introduction Polynuclear aromatic hydrocarbons (PAH) are ubiquitous because of the fact that they are released in appreciable
19、quantities every year into the environment through the combustion of organic materials such as coal, fuel oils, petrol, wood, refuse and plant materials. Since some of these PAH compounds are carcinogenic or mutagenic, their presence in the environment (air, water, soil, sediment and waste) are regu
20、larly monitored and controlled. At present, the determination of PAH is carried out in these matrices in most of the routine laboratories following the preceding steps for sampling, pre-treatment, extraction, clean-up by measurement of specific PAH by means of gas chromatography in combination with
21、mass spectrometric detection(GC-MS) or by HPLC in combination with UV-DAD- or Fluorescence-detection (HPLC-UV-DAD/FLD). However, the different matrices covered in this standard may contain a lot of contaminants. For this reason, the GC-MS method seems to be most appropriate for waste analysis. BS EN
22、 15527:2008EN 15527:2008 (E) 5 1 Scope This European Standard specifies the quantitative determination of 16 polynuclear aromatic hydrocarbons (PAH) according to the priority list of the Environmental Protection Agency (EPA, 1982). This European Standard is applicable for wastes such as contaminated
23、 soil, sludge and rubble, bitumen or waste containing bitumen. This European Standard describes a gas chromatographic method with mass spectrometric detection (GC-MS). Under the conditions specified in this document, a typical lower limit of application of 0,1 mg/kg for each individual PAH can be ac
24、hieved. NOTE 1 This method may be applied to the analysis of other PAH compounds not specified in the scope provided its applicability has been proven by proper in-house validation experiments. NOTE 2 For some materials, e. g. bitumen, the lower limit of application of 0,1 mg/kg cannot be achieved d
25、ue to interferences. NOTE 3 Under certain circumstances the method may be applicable to PAH concentrations lower than 0,1 mg/kg but it is in the responsibility of the laboratory to provide proper validation data for such low concentrations. 2 Normative references The following referenced documents a
26、re 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 14346, Characterization of waste Calculation of dry matter by determination of dry
27、 residue or water content EN 15002, Characterization of waste Preparation of test portions from the laboratory sample ISO 14507, Soil quality Pretreatment of samples for determination of organic contaminants 3 Terms and definitions For the purposes of this document, the following terms and definitio
28、ns apply. 3.1 analyte selected polynuclear aromatic hydrocarbons (PAH) with 2 to 6 condensed aromatic rings (see Table 1) 3.2 calibration standard solution of PAH prepared from a secondary standard and/or stock solutions of native PAH and deuterated PAH used to calibrate the response of the instrume
29、nt 3.3 extraction standard deuterated PAH or native (unlabeled) PAH of medium volatility that are unlikely to be present in waste added to the sample before extraction and used for control of the extraction efficiency BS EN 15527:2008EN 15527:2008 (E) 6 3.4 internal standard deuterated PAH added to
30、the sample after extraction and used for quantification of the concentrations of PAH in the sample 3.5 injection standard deuterated or native PAH that are unlikely to be present in waste samples added to the sample extract before injection into the GC, to monitor variability of instrument response
31、and the recovery of the internal/extraction standards 4 Principle The PAH are extracted from the sample by use of acetone and a hexane-like solvent. If appropriate, the obtained extract is purified by adsorption column chromatography. The extract is analysed by gas chromatography with mass spectrome
32、tric detection (GC-MS) using capillary columns of low polarity. Concentrations of PAH are quantified using an internal-standard-method. 5 Reagents 5.1 General All reagents shall be of recognised analytical grade. The suitability of the reagents shall be checked by running a blank determination as de
33、scribed in 11.1. 5.2 Reagents for extraction procedures 5.2.1 Reagents for extraction by shaking/sonication 5.2.1.1 Acetone. 5.2.1.2 Petroleum ether (Boiling range 40 C to 60 C) or n-hexane or iso-hexane or cyclohexane (hexane-like solvents with a boiling range between 30 C and 68 C are allowed). 5.
34、2.1.3 Sodium chloride, anhydrous. 5.2.1.4 Distilled water or water of equivalent quality. 5.2.1.5 Anhydrous sodium sulphate, heated for at least 6 h to 550 C 20 C, cooled to about 200 C in the furnace and then to ambient temperature in a desiccator containing magnesium perchlorate or a suitable alte
35、rnative. The anhydrous sodium sulphate shall be kept carefully sealed. Commercial available anhydrous sodium sulphate is also applicable. 5.2.2 Reagents for Soxhlet extraction 1:1 (v/v) mixtures of acetone/petroleum ether (boiling range 40 C to 60 C) or acetone/ n-hexane or acetone/iso-hexane or ace
36、tone/cyclohexane. 5.3 Reagents for clean-up procedures 5.3.1 Clean-up A Aluminium oxide 5.3.1.1 Aluminium oxide basic or neutral, specific surface 200 m2/g, activity Super I. BS EN 15527:2008EN 15527:2008 (E) 7 5.3.1.2 Preparation of deactivated aluminium oxide. Add 10 g of water to 90 g of aluminiu
37、m oxide (5.3.1.1). Shake until all lumps have disappeared. Allow the aluminium oxide to equilibrate before use for some 16 h, sealed from air. Use it for a maximum of 2 weeks. 5.3.2 Clean up B- Silica gel 60 5.3.2.1 Silica gel 60, particle size 63 m to 200 m. 5.3.2.2 Preparation of silica gel 60 wit
38、h a water content of 10 % (w/w). Silica gel 60, heated for at least 3 h at 450 C, cooled down and stored in a desiccator containing magnesium perchlorate or another suitable drying agent. Before use, heat it once again at least for 5 h at 130 C in a drying oven. Then allow to cool in a desiccator to
39、 ambient temperature. Transfer the silica gel to a flask and add 10 % water (w/w). Shake for 5 min intensively by hand until all lumps have disappeared and then for 2 h in a shaking machine. Store the deactivated silica gel sealed from air and use it for maximum of one week. 5.4 Reagents for gas chr
40、omatographic analysis Carrier gas for gas chromatography, e. g. helium of suitable purity. 5.5 Standards 5.5.1 Calibration standards, extraction standards and internal standards Choose internal/extraction standard substances whose physical and chemical properties (such as extraction behaviour, reten
41、tion time) are similar to those of the compounds to be analysed. Deuterated PAH should be used as internal standards for the GC-MS method for evaluation of results. Verify the stability of the internal/extraction standards regularly. Table 1 contains native and a minimum number of deuterated PAH to
42、be used for calibration of specific analytes. The use of isotope dilution (each native PAH is quantified with respect to his labelled analogue) is recommended. NOTE Certified solutions of PAH and single solid PAH substances with certified purity are commercially available. BS EN 15527:2008EN 15527:2
43、008 (E) 8 Table 1 Native PAH and deuterated PAH PAH reference substances for calibration Internal/extraction standard substances: (deuterated PAH) Naphthalene (CAS No. 91-20-3) Naphthalene- D8Acenaphthene (CAS No.83-32-9) Acenaphthene-D10Acenaphthylene (CAS No.208-96-8) Fluorene (CAS No.86-73-7) Ant
44、hracene (CAS No.120-12-7) Phenanthrene (CAS No. 85-01-8) Phenanthrene-D10 (extraction standard) Fluoranthene (CAS No.206-44-0) Pyrene (CAS No.129-00-0) Benzo(a)anthracene (CAS No.56-55-3) Benzo(a)anthracene-D12Chrysene (CAS.No.218-01-9) Benzo(b)fluoranthene (CAS No. 205-99-2) Benzo(k)fluoranthene (C
45、AS No.207-08-9) Benzo(a)pyrene (CAS No.50-32-8) Benzo(a)pyrene-D12Indeno(1,2,3-cd)pyrene (CAS No.193-39-5) Dibenzo(ah)anthracene (CAS No.53-70-3) Benzo(ghi)perylene (CAS No.191-24-2) Perylene-D125.5.2 Injection standards A deuterated PAH is added to the final extract before GC-MS injection to check
46、the recovery of the deuterated internal/extraction standards. Suitable injection standards are 1-methylnaphthalene-D10, benzo(e)pyrene-D10and triphenylene-D12. 6 Apparatus 6.1 Extraction and clean-up procedures Customary laboratory glassware. All glassware and material that comes into contact with t
47、he sample or extract shall be free of PAH and any interfering compounds. 6.1.1 Extraction procedures 6.1.1.1 Glass sample bottles of appropriate size with glass stopper or screw top and polytetrafluorethene seal (PTFE). BS EN 15527:2008EN 15527:2008 (E) 9 6.1.1.2 Shaking device, with horizontal move
48、ment (200 to 300 strokes per minute). 6.1.1.3 Ultrasonic bath. 6.1.1.4 Water bath, adjustable up to 100 C. 6.1.1.5 Separatory funnels with a capacity of 1 l. 6.1.1.6 Conical flasks with a capacity of 500 ml. 6.1.1.7 Soxhlet extraction apparatus, consisting of: round bottom flask, e. g.100 ml, Soxhle
49、t extractors and soxhlet thimbles, e. g. 27 mm x 100 mm, vertical condensers, e. g. 300 mm, water-bath or heating mantle as heating apparatus. 6.1.1.8 Evaporator, Kuderna Danish or other evaporators, e. g. a rotary evaporator, if found to be equally suitable. 6.1.1.9 5 ml volumetric flask. 6.1.2 Clean-up procedures 6.1.2.1 Quartz wool or silanized glass wool NOTE Working with quartz wool imposes a risk to health through the release of fine quartz particles. Inhalation of these should be prevented . 6.1.2.2 Boiling chips glass or porc
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