BS EN 15002-2015 Characterization of waste Preparation of test portions from the laboratory sample《废弃物的表征 试验室样本的试验部分准备》.pdf

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1、BSI Standards PublicationBS EN 15002:2015Characterization of waste Preparation of test portionsfrom the laboratory sampleBS EN 15002:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 15002:2015. Itsupersedes BS EN 15002:2006 which is withdrawn.The UK particip

2、ation in its preparation was entrusted to TechnicalCommittee B/508/3, Characterization of waste.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsib

3、le for its correctapplication. The British Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 84521 5ICS 13.030.01Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Poli

4、cy and Strategy Committee on 30 April 2015.Amendments issued since publicationDate Text affectedBS EN 15002:2015EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15002 April 2015 ICS 13.030.01 Supersedes EN 15002:2006English Version Characterization of waste - Preparation of test portions from th

5、e laboratory sample Caractrisation des dchets - Prparation de prises dessai partir de lchantillon pour laboratoire Charakterisierung von Abfllen - Herstellung von Prfmengen aus der Laborprobe This European Standard was approved by CEN on 7 February 2015. CEN members are bound to comply with the CEN/

6、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 Cent

7、re 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

8、 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, Netherl

9、ands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All right

10、s of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15002:2015 EBS EN 15002:2015EN 15002:2015 (E) 2 Contents Page Foreword 4 Introduction .5 1 Scope 6 2 Terms and definitions .6 3 Equipment 8 4 Interferences and sources of error 8 5 Procedure .9 5.

11、1 Key concepts 9 5.2 Sequence of treatment techniques . 10 6 Report 12 Annex A (normative) Guideline for choosing sample treatment techniques . 13 A.1 General . 13 A.2 Homogenization 13 A.2.1 General information 13 A.2.2 Solid samples 13 A.2.3 Liquid samples 14 A.2.4 Homogenization in case of volati

12、le compounds . 15 A.3 Phase/fraction separation 15 A.3.1 General information 15 A.3.2 Solid liquid separation 15 A.3.3 Liquid liquid separation 17 A.3.4 Solid solid separation; separation into different fractions . 18 A.4 Drying . 19 A.4.1 General information 19 A.4.2 Procedures 19 A.5 Particle size

13、 reduction 21 A.5.1 General information 21 A.5.2 Procedures 22 A.6 Sub-sampling 24 A.6.1 General information 24 A.6.2 Manual division of solid samples by coning and quartering . 24 A.6.3 Dry cutting . 25 A.6.4 Mechanical division of solid samples 25 A.6.5 Sub-sampling for volatile compounds . 26 A.6

14、.6 Sub-sampling for moderately volatile organic compounds . 26 BS EN 15002:2015EN 15002:2015 (E) 3 A.6.7 Sub-sampling of sludge and liquid 27 A.6.8 Sub-sampling of monolithic sample 27 Annex B (informative) Relationship between minimum amount of (sub-)sample and particle size. 28 B.1 Formula for the

15、 estimation of the minimum amount of (sub-)sample: 28 B.2 Empirical rule . 29 Annex C (informative) Sample treatment equipment 30 Annex D (informative) Examples for analytical methods 31 Annex E (informative) Examples for preparation of test samples . 37 E.1 Example 1 . 37 E.2 Example 2 . 41 Bibliog

16、raphy 49 BS EN 15002:2015EN 15002:2015 (E) 4 Foreword This document (EN 15002:2015) 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

17、 of an identical text or by endorsement, at the latest by October 2015, and conflicting national standards shall be withdrawn at the latest by October 2015. 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

18、not be held responsible for identifying any or all such patent rights. This document supersedes EN 15002:2006. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. According to the CEN-CENELEC Internal Regulations, the natio

19、nal standards organizations 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, Lith

20、uania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 15002:2015EN 15002:2015 (E) 5 Introduction In laboratory practice, very often different analytical procedures are bound to be applied to the

21、laboratory sample that has been taken according to the sampling plan. For this purpose sub-sampling is bound to be applied in a way, that the different test portions are representative for the original laboratory sample with respect to the compounds of interest and the specific analytical procedures

22、. The representativity of the laboratory sample and of the test portions is of major importance to guarantee the quality and accuracy of analytical results. The representativity of the laboratory sample is specified by the sampling plan. This European Standard specifies the correct sequence of opera

23、tions to ensure the representativity of the test portions. Safety remarks: Anyone dealing with waste and sludge analysis is bound to be aware of the typical risks of that kind of material irrespective of the parameter to be determined. Waste and sludge samples may contain hazardous (e.g. toxic, reac

24、tive, flammable and infectious) substances, which can be liable to biological and/or chemical reaction. Consequently it is recommended that these samples should be handled with special care. The gases that may be produced by microbiological or chemical activity are potentially flammable and will pre

25、ssurize 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. BS EN 15002:2015EN 15002:2015 (E) 6 1 Scope This European Standard is applicable for the preparat

26、ion of representative test portions from the laboratory sample that has been taken according to the sampling plan (EN 14899), prior to physical and/or chemical analysis (e.g. preparation of eluates, extractions, digestion and/or analytical determinations) of solid (including monolithic material) and

27、 liquid samples and sludge. It is also applicable for the preparation of test portions from digests and eluates for the subsequent analyses. This European Standard is intended to find the correct sequence of operations and treatments to be applied to the laboratory sample in order to obtain suitable

28、 test portions in compliance with the specific requirements defined in the corresponding analytical procedures. 2 Terms and definitions For the purposes of this document, the following terms and definitions apply. 2.1 drying process of removing water from a sample Note 1 to entry: For the purpose of

29、 test portion preparation, it may be useful to remove just the amount of water that could interfere with other processes involved (e.g. during crushing or milling). In order to minimize the alteration of the sample during test portion preparation, removing the total amount of water present in the sa

30、mple is not necessarily needed. 2.2 fraction sample obtained by procedures from the laboratory sample where the properties of interest may be unequally distributed Note 1 to entry: A fraction may consist of metal pieces, stones, etc. 2.3 granular waste waste that is neither monolithic, liquid, gas n

31、or sludge SOURCE: EN 12457-1:2002, 3.10 2.4 homogenisation process of combining of components, particles, layers or phases into a more homogeneous state of the original sample or pre-treated fractions of the sample in order to ensure equal distribution of substances in and properties of the sample 2

32、.5 laboratory sample sample or sub-samples sent to or received by the laboratory Note 1 to entry: When the laboratory sample is further prepared (reduced) by subdividing, mixing, grinding, or by combinations of these operations, the result is the test sample. When no preparation of the laboratory sa

33、mple is required, the laboratory sample is the test sample. A test portion is removed from the test sample for the performance of the test or for analysis. Note 2 to entry: The laboratory sample is the final sample from the point of view of sample collection but it is the initial sample from the poi

34、nt of view of the laboratory. BS EN 15002:2015EN 15002:2015 (E) 7 Note 3 to entry: Several laboratory samples may be prepared and sent to different laboratories or to the same laboratory for different purposes. When sent to the same laboratory, the set is generally considered as a single laboratory

35、sample and is documented as a single sample. 2.6 moderately volatile compounds sum of semi-volatile organic compounds and moderately volatile inorganic compounds that can be lost during sample preparation Note 1 to entry: Volatile inorganic compounds of e.g. mercury, arsenic cadmium, thallium can be

36、 lost during sample preparation, e.g. heating. 2.7 moderately volatile organic compound; semi volatile organic compound organic compound having a boiling point above 180 C (at a pressure of 101 kPa) Note 1 to entry: This definition includes: a) mineral oil; b) most polycyclic aromatic hydrocarbons (

37、PAH) (see ISO 13877); c) polychlorobiphenyls (PCB) (see ISO 10382); d) organochlorine pesticides (see ISO 10382). 2.8 monolithic waste waste which has certain minimum dimensions and physical and mechanical properties that ensure its integrity over a certain period of time in the considered scenario

38、2.9 particle size reduction mechanical friction of the sample by milling, grinding, crushing or cutting 2.10 phase separation; fraction separation process of dividing components, particles or phases if homogenization of the sample is practically not applicable and/or the analysis of different fracti

39、ons or phases are appropriate 2.11 sample portion of material selected from a larger quantity of material 2.12 sub-sample sample obtained after sample size reduction of a larger sample Note 1 to entry: A sub-sample may be: a) portion of the sample obtained by selection or division; b) the final samp

40、le of multistage sample-preparation; c) in case of monolithic sample, the sample obtained after cutting or coring. BS EN 15002:2015EN 15002:2015 (E) 8 2.13 sub-sampling process of selecting one or more sub-samples from a sample or, in case of monolithic waste, the process of cutting or coring to obt

41、ain a required regular shape 2.14 test portion; analytical portion quantity of material of proper size, for measurement of the concentration or other properties of interest, removed from the test sample Note 1 to entry: The test portion may be taken from the laboratory sample directly if no preparat

42、ion of sample is required (e.g. with liquids or samples of proper homogeneity, size and fineness), but usually it is taken from the prepared test sample. 2.15 test portion of monolithic waste of regular shape test portion of monolithic waste, obtained either by cutting or coring and for which the su

43、rface area can be calculated on the basis of simple geometric formulas 2.16 test sample; analytical sample sample, prepared from the laboratory sample, from which test portions are removed for testing or for analysis 2.17 volatile organic compound compound which is liquid at room temperature (20 C)

44、and which generally has a boiling point below 180 C Note 1 to entry: This includes single-ring aromatic hydrocarbons and other low boiling halogenated hydrocarbons, which are used as solvents or fuels, and some degradation products. SOURCE: ISO 10381-7:2005, 3.23, modified The original term abbrevia

45、tion and example have been retrieved. 3 Equipment For the purpose of preparation of test portions from the laboratory samples appropriate equipment shall be chosen depending on the procedures selected according to Annex A. In the selection of the type of treatment techniques, one should keep in mind

46、 that each of them has some potential impact on analytical results. It can generate loss of the analytes of interest, introduce contamination or alter the physical-chemical properties of the sample. All glassware and devices that come in contact with the sample shall be made out of a suitable materi

47、al, chemically compatible with the sample, selected in order to minimize contamination of samples and adsorption or absorption of the analytes (e.g. plastic materials for inorganic elemental analysis, quartz or glass for volatile and organic analytes). Care shall be taken to ensure a good cleaning,

48、in order to avoid cross-contamination of samples. An informative list of appropriate equipment for the sample treatment procedures is given in Annex C. 4 Interferences and sources of error The (sub)-sample shall be re-homogenized after any particle size reduction operation that may have resulted in

49、segregation of different sized particles. Care should be taken to avoid loss of material and contamination of the sample via the air, by dust, by the use of the apparatus (e.g. from the ambient laboratory atmosphere or between samples stored or processed close to one another). BS EN 15002:2015EN 15002:2015 (E) 9 Three types of contamination could occur from the apparatus: a) abrasion; b) cross-contamination; c) chemical release. It is recommended to perform treatment of waste material in a separate room used only for this purpose, especially crushing or sie