Characterization of waste - Sampling of waste materials - Part 3: Guidance on procedures for sub-sampling in the field

This Technical Report describes procedures for reducing the overall size of the waste materials in the field to aid practical transportation of a sample to the laboratory.
NOTE 1   This Technical Report provides a shop shelf of example sampling techniques that can be selected to meet a wide range of sampling situations. For a specific situation one of the presented procedures may be appropriate.
NOTE 2   The procedures listed in this Technical Report reflect current best practice, but these are not exhaustive and other procedures may be equally relevant.

Charakterisierung von Abfall - Probenahme - Teil 3: Verfahren zur Teilprobenahme im Gelände

Caractérisation des déchets - Prélèvement des déchets - Partie 3: Guide relatif aux procédures de sous-échantillonnage sur le terrain

Le présent Rapport Technique décrit des procédures visant à réduire la taille globale des déchets sur le terrain, afin de faciliter le transport de l’échantillon au laboratoire.
NOTE 1   Le présent Rapport Technique fournit plusieurs exemples de techniques d’échantillonnage qui peuvent être utilisées dans de nombreuses situations d’échantillonnage. À chaque situation correspond l’une des procédures présentées.
NOTE 2   Les procédures décrites dans le présent Rapport Technique correspondent aux bonnes pratiques actuelles, mais elles ne sont pas exhaustives et d’autres procédures peuvent être tout aussi appropriées.

Karakterizacija odpadkov - Vzorčenje odpadkov - 3. del: Navodilo o postopkih za zmanjšanje količine vzorca na terenu

General Information

Status
Published
Publication Date
21-Nov-2006
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
22-Nov-2006
Completion Date
22-Nov-2006

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SLOVENSKI STANDARD
SIST-TP CEN/TR 15310-3:2007
01-april-2007
.DUDNWHUL]DFLMDRGSDGNRY9]RUþHQMHRGSDGNRYGHO1DYRGLORRSRVWRSNLK]D
]PDQMãDQMHNROLþLQHY]RUFDQDWHUHQX
Characterization of waste - Sampling of waste materials - Part 3: Guidance on
procedures for sub-sampling in the field

Charakterisierung von Abfall - Probenahme - Teil 3: Verfahren zur Teilprobenahme im

Gelände

Caractérisation des déchets - Prélevement des déchets - Partie 3: Guide relatif aux

procédures de sous-échantillonnage sur le terrain
Ta slovenski standard je istoveten z: CEN/TR 15310-3:2006
ICS:
13.030.10 Trdni odpadki Solid wastes
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
SIST-TP CEN/TR 15310-3:2007 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
TECHNICAL REPORT
CEN/TR 15310-3
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
November 2006
ICS 13.030.10
English Version
Characterization of waste - Sampling of waste materials - Part 3:
Guidance on procedures for sub-sampling in the field

Caractérisation des déchets - Prélèvement des déchets - Charakterisierung von Abfall - Probenahme - Teil 3:

Partie 3: Guide relatif aux procédures de sous- Verfahren zur Teilprobenahme im Gelände

échantillonnage sur le terrain

This Technical Report was approved by CEN on 21 February 2006. It has been drawn up by the Technical Committee CEN/TC 292.

CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,

Germany, 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 STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 15310-3:2006: E

worldwide for CEN national Members.
---------------------- Page: 2 ----------------------
CEN/TR 15310-3:2006 (E)
Contents

Foreword..............................................................................................................................................................3

Introduction.........................................................................................................................................................4

1 Scope ......................................................................................................................................................6

2 Normative references ............................................................................................................................6

3 Terms and definitions ...........................................................................................................................6

4 Principles of sub-sampling in the field................................................................................................8

5 Apparatus ...............................................................................................................................................9

6 Sample preparation ...............................................................................................................................9

6.1 Preparation for granular materials.......................................................................................................9

6.2 Preparation for liquids, sludges and paste like substances...........................................................10

7 Preparing a mixed sample ..................................................................................................................10

7.1 Mixing granular materials ...................................................................................................................10

7.2 Mixing of liquid and sludges ..............................................................................................................10

7.3 Mixing of paste like materials.............................................................................................................11

8 Generic sub-sampling of mobile and viscous liquids .....................................................................11

8.1 General..................................................................................................................................................11

8.2 Single sample method.........................................................................................................................11

8.3 Multiple sample method......................................................................................................................11

9 Generic sub-sampling of liquid and solids rendered mobile by heat ............................................12

9.1 General..................................................................................................................................................12

9.2 Single sample method.........................................................................................................................12

9.3 Multiple sample method......................................................................................................................12

10 Generic sub-sampling of sludges......................................................................................................12

10.1 Liquids ..................................................................................................................................................12

10.2 Cakes ....................................................................................................................................................12

10.3 Gelatinous sludges..............................................................................................................................12

11 Generic sub-sampling of paste like substances ..............................................................................13

11.1 General..................................................................................................................................................13

11.2 Single sample method.........................................................................................................................13

11.3 Multiple sample method......................................................................................................................13

12 Generic sub-sampling of powders, granules and small crystals ...................................................13

12.1 General..................................................................................................................................................13

12.2 Aggregate reduction............................................................................................................................14

12.3 Manual and mechanical sub-sampling procedures .........................................................................14

13 Sub-sampling coarse solids and large pieces .................................................................................17

14 Incorporation in the Sampling Plan ...................................................................................................18

15 Undertake field sub-sampling procedures........................................................................................18

Annex A Examples of equipment for sub-sampling .....................................................................................19

A.1 Riffle box...............................................................................................................................................19

A.2 Rotary sample divider .........................................................................................................................19

A.3 Tyler divider .........................................................................................................................................21

A.4 Sheet metal cross ................................................................................................................................21

Bibliography......................................................................................................................................................22

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CEN/TR 15310-3:2006 (E)
Foreword

This Technical Report (CEN/TR 15310-3:2006) has been prepared by Technical Committee CEN/TC 292

“Characterization of waste”, the secretariat of which is held by NEN.

This Technical Report has been prepared under a mandate given to CEN by the European Commission and

the European Free Trade Association.

This Technical Report is one of a series of five, dealing with sampling techniques and procedures, which

provide essential information for the application of the EN-Standard:

EN 14899 Characterisation of waste - Sampling of waste materials - Framework for the preparation and

application of a Sampling Plan

The principal component of the EN Standard is the mandatory requirement to prepare a Sampling Plan. This

EN 14899 standard can be used to:

 produce standardised sampling plans for use in regular or routine circumstances (i.e. the elaboration of

daughter/derived standards dedicated to well defined sampling scenarios);
 incorporate specific sampling requirements into national legislation;
 design and develop a Sampling Plan on a case by case basis.

The Technical Reports display a range of potential approaches and tools to enable the project manager to

tailor his sampling plan to a specific testing scenario (i.e. a ‘shop shelf’ approach to sampling plan

development for waste testing). This approach allows flexibility in the selection of the sampling approach,

sampling point, method of sampling and equipment used.

This Technical Report describes procedures for reducing the overall size of the sample in the field, to aid

practical transportation of a sample to the laboratory. It does not deal with sub-sampling in the laboratory to

provide a test portion or the pre-treatment of samples prior to analysis.

This report does not attempt to provide a definitive procedure for each and every situation that may arise from

sampling a given waste type or specific analytical requirement, rather it aims to expose the factors that

influence the selection of these practical field activities to ensure the most appropriate procedure is selected

for any given sampling scenario. The most appropriate approach, tools, and methodology, in the absence of

an existing recognised Sampling Plan, should be chosen on a scenario-specific basis. However, this does not

present a barrier to technical innovation, and there is no reason why methodologies other than those detailed

in this Technical Report cannot be substituted.
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CEN/TR 15310-3:2006 (E)
Introduction

Wastes are materials, which the holder discards, or intends or is required to discard, and which may be sent

for final disposal, reuse or recovery. Such materials are generally heterogeneous and it will be necessary

therefore to specify in the testing programme the amount of material for which the characteristics of interest

need to be defined. The testing of wastes allows informed decisions to be made on how they should be

treated (or not), recovered or disposed. In order to undertake valid tests, some sampling of the waste is

required.

The principal component of the standard EN 14899 is the mandatory requirement to prepare a Sampling Plan,

within the framework of an overall testing programme as illustrated in Figure 1 of EN 14899:2005. This

standard can be used to:

 produce standardised sampling plans for use in regular or routine circumstances (i.e. the elaboration of

daughter/derived standards dedicated to well defined sampling scenarios);
 incorporate specific sampling requirements into national legislation;
 design and develop a Sampling Plan on a case by case basis.

The development of a Sampling Plan within this framework involves the progression through three steps or

activities.
1) Define the Sampling Plan;
2) Take a field sample in accordance with the Sampling Plan;
3) Transport the laboratory sample to the laboratory.

This Technical Report provides information to support Key Step 2 of the Sampling Plan process map and

elaborates on the range of potential approaches that can be used to reduce the size of a sample in the field to

facilitate the appropriate storage and preservation of the sample and ultimately its transportation to the

designated analytical facility.

This Technical report describes procedures for reducing the overall size of the sample in the field, to aid

practical transportation of a sample to the laboratory. It does not deal with sub-sampling in the laboratory to

provide a test portion, or the pre-treatment of samples prior to analysis. Samples dispatched to the laboratory

may require additional sub-sampling and/or pre-treatment steps prior to analysis. Some samples may be

analysed without additional treatment. Field sub-sampling should be carried out in such a way as to obtain, at

all stages, a sample that is representative of the field sample. Specifically this Technical Report supports

4.2.8.2 (Procedures for sub-sampling in the field) of the Framework Standard.

This Technical Report should be read in conjunction with the Framework Standard for the preparation and

application of a Sampling Plan as well as the other Technical Reports that contain essential information to

support the Framework Standard. The full series comprises:

EN 14899, Characterization of waste - Sampling of waste materials - Framework for the preparation and

application of a Sampling Plan.

CEN/TR 15310-1, Characterization of waste – Sampling of waste materials - Part 1: Guidance on selection

and application of criteria for sampling under various conditions.

CEN/TR 15310 -2, Characterization of waste – Sampling of waste materials - Part 2 - Guidance on sampling

techniques.
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CEN/TR 15310-3:2006 (E)

CEN/TR 15310 -3, Characterization of waste – Sampling of waste materials – Part 3: Guidance on procedures

for sub-sampling in the field.

CEN/TR 15310 -4, Characterization of waste – Sampling of waste materials – Part 4: Guidance on

procedures for sample packaging, storage, preservation, transport and delivery.

CEN/TR 15310 -5, Characterization of waste – Sampling of waste materials – Part 5: Guidance on the

process of defining the Sampling Plan.

The Technical Reports contain procedural options (as detailed in Figure 2 of EN 14899:2005) that can be

selected to match the sampling requirements of any testing programme.
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CEN/TR 15310-3:2006 (E)
1 Scope

This Technical Report describes procedures for reducing the overall size of the waste materials

in the field to aid practical transportation of a sample to the laboratory.

NOTE 1 This Technical Report provides a shop shelf of example sampling techniques that can be

selected to meet a wide range of sampling situations. For a specific situation one of the presented

procedures may be appropriate.

NOTE 2 The procedures listed in this Technical Report reflect current best practice, but these are not

exhaustive and other procedures may be equally relevant.
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 latest edition of the referenced

document (including any amendments) applies.

EN 13965-1:2004, Characterization of waste - Terminology - Part 1: Material related terms and definitions

EN 13965-2:2004, Characterization of waste - Terminology - Part 2: Management related terms and

definitions
3 Terms and definitions

For the purposes of this Technical Report the terms and definitions given in EN 13965-1:2004 and

EN 13965-2:2004 and the following apply
3.1
aliquot

known amount of a homogeneous material, assumed to be taken with negligible sampling error

[ISO 11074-2]
NOTE This term is usually applied to a liquid.
3.2
composite sample

two or more increments/sub-samples mixed together in appropriate proportions, either discretely

or continuously (blended composite sample), from which the average value of a desired

characteristic may be obtained
[ISO 11074-2]
3.3
increment

individual portion of material collected by a single operation of a sampling device which will not be analysed /

investigated as a single entity, but will be mixed with other increments in a composite sample

NOTE 1 Whenever the portion of material collected by a single operation of a sampling device is analysed individually,

the obtained material is called a sample. In such a situation it is essential that the quantity of material fulfils both the

criteria for the size of an increment as well as for a sample.

NOTE 2 In some languages the term 'increment' is used without the condition that an increment will never be analysed

on its own. For this Technical Report this is however an essential condition in the definition of the term ‘increment’.

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CEN/TR 15310-3:2006 (E)
3.4
field sample

quantity (mass or volume) of material obtained through sampling without any sub-sampling

3.5
laboratory sample
sample(s) or sub-sample(s) sent to or received by the laboratory.
[IUPAC, definition 2.5.5]

NOTE 1 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 sample is required, the laboratory

sample is the test sample.

NOTE 2 The laboratory sample is the final sample from the point of view of sample collection but it is the initial sample

from the point of view of the laboratory.
3.6
mixing
combining of components, particles or layers into a more homogeneous state
[ISO 11074]
3.7
particle size reduction

crushing or cutting the sample in order to reduce the particle size of the whole (sub-)sample

without reducing the sample size (mass)
3.8
portion

wach of the discrete, identifiable portions of a material suitable for removal from a population as a

sample or as a portion of a sample, and which can be individually considered, examined, tested

or combined
[ISO 11074]
3.9
representative sample

sample in which the characteristic(s) of interest is (are) present with a reliability appropriate for the purposes

of the testing programme
3.10
riffling

separation of a free-flowing sample into (usually) equal parts by means of a mechanical device

composed of diverter chutes
[ISO 11074]
3.11
sample
portion of material selected from a larger quantity of material
[ISO 11074]

NOTE 1 The manner of selection of the sample should be described in a sampling plan.

NOTE 2 The use of the term ‘sample’ should be supported with a preface as far as possible as it does not indicate to

which step of the total sampling procedure it is related when used alone e.g. field sample, laboratory sample.

3.12
Sampling Plan
all the information pertinent to a particular sampling activity
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CEN/TR 15310-3:2006 (E)

NOTE Predetermined procedure for the selection, withdrawal, preservation, transportation and

preparation of the portions to be removed from a population as a sample. (ISO 11074:2005)

3.13
sample division
process of selecting one or more sub-samples from a sample of population
[ISO 11074]
3.14
stratum/ Strata

strata are mutually exclusive and exhaustive parts of a population. They are identified either, because they are

believed to be different from each other or for the purposes of sampling
3.15
sub-sample

quantity (mass or volume) of material obtained by procedures in which the characteristics of

interest are randomly distributed in parts of equal or unequal size
NOTE 1 A sub-sample may be:
a) a portion of the sample obtained by selection or division; or
b) an individual unit of the stratum taken as part of the sample; or
c) the final unit of multi-stage sampling.

NOTE 2 The term ‘sub-sample’ is used either in the sense of a ‘sample of a sample’ or as a synonym for ‘unit’. In

practice, the meaning is usually apparent from the context or is defined.
3.16
sub-sampling
process of selecting one or more sub-samples from a sample of a population
[ISO 11074:2005]
4 Principles of sub-sampling in the field

A method of sub-sampling should be selected that minimises possible change in the physical and chemical

composition of the sample. The ultimate selection of a procedure will depend on the stated objectives of the

sampling programme, detailed in the Sampling Plan, and the tests to be carried out on the sample.

Sub-sampling should be carried out in the field only if it is necessary to reduce the sample size for

transportation and where the integrity of a sample and sub-samples can be assured, that is in an environment

that protects the loss of moisture and volatile components due to evaporation, or cross contamination of

samples. Sub-sampling activities should ideally be carried out in an appropriately equipped mobile or field

laboratory to safeguard sample integrity.

Sub-sampling can be achieved with or without particle size reduction. Particle size reduction consists of

crushing or grinding the sample in order to reduce the particle size of the whole or sub-sample without

reducing the sample size (mass). Such reduction procedures are particularly susceptible to the loss of fine

particles due to air entrainment in a field environment and such procedures should only be undertaken at the

analytical facility. The procedures in this Technical Report are restricted to methods that exclude particle size

reduction by grinding.

If a heterogeneous bulk sample cannot be adequately mixed in the field or field laboratory to produce a

homogeneous sample it should be returned to the laboratory for sub-sampling.
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CEN/TR 15310-3:2006 (E)

When two or more laboratory samples are required from a bulk sample, the sub-sampling process should be

defined in such a way that two or more sub-samples of equal size and expected equal composition are

generated. In most cases, multiple equal laboratory samples are obtained from the last sub-sampling stage (if

the sub-sampling process consists of more than one stage) to ensure that multiple laboratory samples are as

comparable as possible
5 Apparatus
Examples of sub-sampling apparatus are given in Annex A.
Suitable apparatus may include:
 large heavy-duty plastic sheeting;
 scoop;
 spade;
 sledge hammer;
 mechanical shovel;
 sheet metal cross;
 balance;
 riffle box;
 Tyler divider;
 mechanised turntable / Rotating dividers .

NOTE In all cases, alternative designs may be used as long as the devices can be used to fulfil the sub-sampling

procedures described in Clauses 7 to 12.
6 Sample preparation
6.1 Preparation for granular materials

The following procedure should be followed, where possible, prior to all sample pre-treatment

activities.

 identify an area within the a covered area or of hard standing sheltered from the effects of wind and rain,

preferably flat and large enough to allow ease of access around the whole sample when spread on the

surface;

 place a clean protective floor covering, preferable heavy-duty plastic sheeting, on the floor of the

laboratory or on the ground to protect the sample from contamination by the floor surface;

 all apparatus and tools should be clean in order to reduce the risk of cross-contamination.

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CEN/TR 15310-3:2006 (E)
6.2 Preparation for liquids, sludges and paste like substances

The following procedure should be followed, where possible, prior to all sample pre-treatment

activities.

 identify an area within the a covered area or of hard standing sheltered from the effects of wind and rain,

preferably flat and large enough to allow ease of access around the whole sample container(s);

 all apparatus and tools should be clean in order to reduce the risk of cross-contamination.

7 Preparing a mixed sample
7.1 Mixing granular materials
7.1.1 General
Mixing of homogenous samples and small volumes of heterogeneous material may be

undertaken in the field. If a heterogeneous sample cannot be mixed in the field to produce a

homogeneous sample the sample(s) should be returned to the laboratory for mechanical mixing.

 prepare a mixed sample containing equivalent quantities (m/m or v/v) of the individual increments;

 determine the quantities of the increments to be mixed together by dry weight:

NOTE It is possible for the moisture content of multiple sample increments from a single volume or mass of waste to

vary considerably. In this situation mixing of the waste increments by equal weight or volume would result in a bulk sample

that is biased due to under or over sampling of the individual increments. Mixing of increments with variable moisture

content should therefore, where possible, be carried out in the laboratory following determination of the dry matter content

of each increment. In most cases where increments are taken from the same stratum, the moisture content of individual

increments should be approximately the same and increments can be mixed in the field on an equal volume or weight

basis.
7.1.2 Methodology
 undertake preparations for sample pre-treatment (see 6.1);

 mix the material by forming a conical heap. Take a spade or scoopful of the material and put it on the top

of the preceding one. The size of the scoop or spade should be of such size that this action should be

repeated on at least 20 occasions in order to transfer the full amount of material;

The Project Manager should document the selected mixing method in the Sampling Plan.

7.2 Mixing of liquid and sludges
7.2.1 General

All samples should be returned to the laboratory without field mixing if they cannot be adequately

mixed in the field to produce a homogeneous sample. Mixing of stratified samples, where the

stratification must be maintained, should be undertaken in the laboratory.
7.2.2 Methodology
If mixing of liquids and sludges is required:
 undertake preparations for sample pre-treatment (see 6.2);
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CEN/TR 15310-3:2006 (E)

 the receptacle into which all samples are placed for mixing should be large enough so that there is no

loss of sample during mixing;

 determine the quantities of the increments to be mixed together by volume, place in the mixing container

and mix by rolling, shaking or stirring.

NOTE Mixing in containers open to the air is not appropriate for material with volatile or semi-volatile components. It

is advisable that materials with such constituents are returned to the laboratory for mixing.

The Project Manager should document the selected mixing method in the Sampling Plan.

7.3 Mixing of paste like materials
7.3.1 General
Mixing of homogenous samples and small volumes of heterogeneous material may be

undertaken in the field. If a heterogeneous sample cannot be mixed in the field to produce a

homogeneous sample the sample(s) should be returned to the laboratory for mechanical mixing.

7.3.2 Methodology
If mixing of paste like materials is required:
 undertake preparations for sample pre-treatment (see 6.2);

 the receptacle into which all samples are placed for mixing should be large enough so that there is no

loss of sample during mixing;

 determine the quantities of the increments to be mixed together by volume, place in the mixing container

and mix by stirring.

NOTE Mixing in containers open to the air is not appropriate for material with volatile or semi-volatile components. It

is advisable that materials with such constituents are returned to the laboratory for mixing.

8 Generic sub-sampling of mobile and viscous liquids
8.1 General

All samples should be returned to the laboratory without field sub-sampling if they cannot be

adequately mixed in the field to produce a homogeneous sample. Sub-sampling of stratified

samples, where the stratification must be maintained, should be undertaken in the laboratory.

8.2 Single sample method
 mix the primary sample thoroughly (by shaking, stirring or rolling);

 transfer the required quantity or quantities to a smaller container by pouring, taking care to minimise the

loss of volatile components.

The Project Manager should document the selected sub-sampling method in the Sampling Plan.

8.3 Multiple sample method
 mix each sample thoroughly (see 7.2);
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CEN/TR 15310-3:2006 (E)

 pour a volume from each sample, as specified in the sampling plan, into a separate sample container,

taking care to minimise loss of volatile components;

 mix the combined portions thoroughly by shaking, stirring or rolling (see 7.2).

The Project Manager should document the selected sub-sampling procedure in the Sampling Plan.

9 Generic sub-sampling of liquid and solids rendered mobile by heat
9.1 General

All samples should be returned to the laboratory without field sub-sampling if they cannot be

adequate
...

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