PUBLISHED DOCUMENT PD CEN/TR

15310-4:2006

Characterization of
waste — Sampling of
waste materials —
Part 4: Guidance on procedures for
sample packaging, storage,
preservation, transport and delivery

ICS 13.030.10; 13.030.20

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PD CEN/TR 15310-4:2006

National foreword

This Published Document was published by BSI. It is the UK implementation

of CEN/TR 15310-4:2006.
The UK participation in its preparation was entrusted by Technical Committee
B/508, Waste management, to Subcommittee B/508/3, Characterization of
waste.
A list of organizations represented on B/508/3 can be obtained on request to its
secretary.
This publication does not purport to include all the necessary provisions of a
contract. Users are responsible for its correct application.

This Published Document was Amendments issued since publication

published under the authority
of the Standards Policy and
Strategy Committee Amd. No. Date Comments
on 29 December 2006

© BSI 2006

ISBN 0 580 49836 0

TECHNICAL REPORT CEN/TR 15310-4
RAPPORT TECHNIQUE
TECHNISCHER BERICHT November 2006

ICS 13.030.10; 13.030.20

English Version

Characterization of waste - Sampling of waste materials - Part 4:

Guidance on procedures for sample packaging, storage,
preservation, transport and delivery

Caractérisation des déchets - Prélèvement des déchets - Charakterisierung von Abfall - Probenahme - Teil 4:
Partie 4: Guide relatif aux procédures d'emballage, de Verpackung, Lagerung, Konservierung, Transport und
stockage, de conservation, de transport et de livraison des Lieferung von Proben
échantillons

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 15310-4:2006: E
worldwide for CEN national Members.
CEN/TR 15310-4:2006

Contents

Foreword..............................................................................................................................................................3
Introduction .........................................................................................................................................................4
1 Scope ......................................................................................................................................................6
2 Normative references ............................................................................................................................6
3 Terms and definitions ...........................................................................................................................6
4 Packing and labelling the sample ........................................................................................................7
4.1 Selecting a sample container ...............................................................................................................7
4.2 Packaging specific types of waste.......................................................................................................9
4.3 Labelling ...............................................................................................................................................10
5 Preserving the sample ........................................................................................................................11
5.1 General..................................................................................................................................................11
5.2 General instructions for sample preservation..................................................................................12
5.3 Preserving specific types of samples ...............................................................................................13
5.4 Preservation methods .........................................................................................................................14
6 Chain of custody forms and sample dispatch..................................................................................16
7 Incorporation in the Sampling Plan ...................................................................................................16
Annex A (informative) Packaging ..................................................................................................................17
Bibliography ......................................................................................................................................................19

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 CEN/TR 15310-4:2006

Foreword
This Technical Report (CEN/TR 15310-4:2006) 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 the boundary conditions and procedures, appropriate for application in the
field, for the packaging, preservation, short-term storage and transport of samples to assist in maintaining their
integrity prior to delivery at the laboratory. The laboratory facility should be consulted in the selection of the
most appropriate procedure to ensure compatibility with the chosen analytical methodology and parameters to
be tested as defined in EN 14899 - Framework standard.
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 15310-4:2006

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 Steps 2 and 3 of the Sampling Plan process map
and elaborates on methods and boundary conditions for preserving, packaging and storing samples to
preserve their integrity, in addition to the transportation and delivery of a sample to the designated analytical
facility.

Sample integrity may be compromised if insufficient attention is paid to correct packaging, preservation, and
storing and transport techniques. This may result in a sample, which is not representative of the sample
population. The selection of the most appropriate procedure should be in collaboration with the laboratory
facility designated to undertake testing to ensure compatibility with the chosen analytical methodology and
parameters to be tested. Specifically this Technical Report supports 4.2.8.3 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, 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 15310-4:2006

1 Scope
This Technical Report describes procedures for the packaging, preservation, short-term storage and transport
of both solid and liquid waste samples, including paste-like substances and sludges. Where available and
appropriate for field application, requirements for specific storage conditions and/or preservation methods
should be selected from the chosen analytical standard and collaboration with the testing 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
analytical laboratory
identified laboratory, which is to undertake the chemical, biological or physical analysis of samples

3.2
constituent
property or attribute of a material that is measured, compared or noted

3.3
delivery
transfer of custody of the sample

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.

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 CEN/TR 15310-4:2006

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
packaging
act of placing a sample into an appropriate sample container for transport and/or storage
[ISO 11074:2005]

3.7
preservation
any procedure used to stabilise a sample in such a way that the properties under examination are maintained
stable from the collection step until preparation for analysis
[ISO 11074:2005]

3.8
sample
portion of material selected from a larger quantity of material
[ISO 11074:2005]

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.

3.9
storage
process and the result of keeping a sample available under predefined conditions for a usually specified time
interval between collection and further treatment of the sample
[ISO 11074:2005]

3.10
transport
act of transferring a sample from the locality of sampling to the place of subsequent treatment (e.g. laboratory,
soil-specimen bank etc.)
[ISO 11074:2005]

4 Packing and labelling the sample

4.1 Selecting a sample container

4.1.1 General

Sample containers can be made from many different types of materials, some of which may react or
contaminate a specific type of sample. To avoid any accidental contamination by the sample container or
derogation of the sample the project manager should seek scientific advice, usually from the receiving
laboratory, regarding the type and size of sample(s) and container(s), appropriate preservation method(s) if
applicable, maximum storage time prior to analysis, and the labelling system. The maximum storage time prior
to analysis will indicate the period of time available before the sample has to arrive at the laboratory. In general,
this period has to be as short as possible. Once the details have been agreed, the Sampler should follow the
methods detailed in the sampling plan.

The purpose of the sample container is to protect the sample during transport and storage until it is further
treated or analysed. A container should be compatible with the nature of the material sampled and the
components to be analysed. In general:

 collect samples for inorganic analysis in plastic containers;

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CEN/TR 15310-4:2006

NOTE It is common practice to include low-density polyethylene bottles or tubs. Strong polyethylene plastic bags are
useful for bulky solid samples. Samples should be collected for organic analysis in glass containers.

 select a sample container having a size relative to the volume of the required sample;

 select a sample container capable of being sealed. Tamperproof seals are commonly used when
performing regulatory sampling.

Where specialised containers and preservatives are advised the analytical laboratories should be encouraged
to provide containers that conform to the characteristics of the analytical procedure to be used.

Table A.1 details types of containers, preservation and storage conditions for different types of parameters
associated with a particular analysis or test.

4.1.2 Type of container

The following points should be considered when selecting and preparing sample containers:

 adsorption into the walls of the container;

 contamination of the container prior to sampling by improper cleaning;

 contamination of the sample by the material of which the container is made;

 reaction between constituents of the sample and the container;

 resistance to temperature extremes;

 resistance to breakage;

 water and gas tightness;

 ease of reopening;

 size, shape and mass volume;

 availability;

 cost.

4.1.3 Shape and size of container

Consultation should be undertaken with the analytical laboratory regarding type and size of sample containers.
The sample size is a function of the necessary mass required to complete the analytical suite and by any
requirement to store sample for investigation at a later date. The Project Manager should then select the type
and size of container and define this within the Sampling Plan.

 obtain instruction from the analytical laboratory on appropriate headspace above the sample;

 select the shape and size of container such that the volume of headspace does not prevent changes in
the sample. Wide neck rigid containers are useful to aid sample handling;

 either completely fill the container or allow headspace as appropriate for the material being sampled and
determinations to be analysed.

NOTE Some headspace volume is required above samples, which are biologically reactive, or have the potential to
generate gas or to significantly change in volume with relatively small changes of temperature. Air space should be

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minimised, to prevent significant oxidation and/or carbonation reactions, both at the top of the container and for granular
materials between the particles. When freezing is used as a preservation method, some additional space is needed within
the container to allow for expansion. The use of glass is not advisable when freezing aqueous solutions.

4.1.4 Preparation of sample containers

Commonly, instruction on the use of appropriate cleaning protocols can be obtained from the analytical
laboratory.

NOTE The choice of cleaning method will depend on the components to be analysed. Containers may be cleaned
with mixtures of acids followed by rinsing with de-ionised water. Samples that are to be analysed for organic components
may be stored in solvent-rinsed containers and/or calcinations oven. Cleaning procedures may differ depending on the
type of waste to be packed and the components to be analysed. Advice should be sought from the analytical laboratory or
other experts in order to establish the most suitable procedure in each case. In general, the reuse of sample containers is
not advised.

4.2 Packaging specific types of waste

4.2.1 General packaging

Using the guidance given in Table A.1, select a container compatible with the analytical determinants.

4.2.2 Hazardous Wastes

Advice should always be sought before handling hazardous wastes and all relevant health and safety
regulations should be followed explicitly.

4.2.3 Packaging of mobile liquid waste

Refer to 4.2.1

4.2.4 Packaging of liquid and solids rendered mobile by heat

When packaged after pre-heating, place the sample in the container and allowed to cool before sealing the
container.

Refer to 4.2.1

4.2.5 Packaging of viscous liquids

Place samples with a melting point within the range of anticipated ambient temperature in sealable, wide
necked containers.

Refer to 4.2.1

4.2.6 Packaging of sludges

Refer to 4.2.1

4.2.7 Packaging of paste-like substances

Place samples with a melting point within the range of anticipated ambient temperature in sealable, wide
necked containers.

Refer to 4.2.1

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CEN/TR 15310-4:2006

4.2.8 Packaging of solid waste

Place fine-grained solid wastes containing volatile organic compounds in glass bottles and seal with PTFE
(polytetrafluoroethylene) cap liners. For large particle sizes which cannot be stored in a glass container either:

a) place the sample in any container (with potential loss of volatiles) and analyse as soon as possible;

b) take a small part of the sample and place in the glass container (with the risk that the sample analysed is
not completely representative of the sampled material).

If the sample is stored in such a way that there has been a potential loss of volatiles the sample may no
longer be representative of the sampled population. In these cases the sampler should record the possible
potential loss in the sampling record.

Solid materials, without a liquid phase or volatile constituents may be placed in plastic containers.

NOTE Plastic bags should be thick enough so that the material cannot tear or penetrate the plastic and should be
sealed so that no part of the sample can escape. For additional security it is common practice to place the bagged sample
in a second plastic bag.

Place coarse or very coarse granular materials, in which organic components are to be determined, in plastic
or metal drums. Place samples where metal content or leachability is to be determined in plastic drums.

Place samples with a melting point within the range of anticipated ambient temperature in sealable, wide
necked containers.

Refer to 4.2.1

4.3 Labelling

Apply a clearly legible, unique, unambiguous code to each sample container

either:

a) by writing directly on to the container using a permanent marker pen;

b) by writing on an adhesive label and sticking it to the sample container.

Attach the label to the main body of the container. When labels are attached to the lid, top or cap of the
container, attach an identical label to the container body.

Select a label of a quality capable of remaining firmly attached to the sample container whatever the storage
period and prevailing conditions. Where the possibility exists of the label becoming detached, for example as a
result of condensation caused by cooling, place the container in a plastic bag and seal closed.

Mark the label with all the information necessary for unequivocal identification of the sample.

NOTE 1 Indelible ink should be used and labels should be kept short and simple to avoid mistakes when transcribing
numbers.

NOTE 2 If possible, the use of pre-printed labels and bar-code labels are an advantage.

Laboratory samples for dispatch or transport by third parties and reserved laboratory samples should be
sealed in such a manner that the integrity of the sample is protected. Sealing of the samples may be required
when samples are taken for (potential) regulatory investigations. Any third party should be notified of
hazardous substances.

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 CEN/TR 15310-4:2006

5 Preserving the sample

5.1 General

Ideally, samples should be analysed immediately after collection. However this is seldom possible, and so
preservation techniques are required in the field and during transport to the laboratory. The components to be
determined and the length of time between collection and analysis influence the choice of preservation method.
The chosen method of preservation is often the method for the whole period before analysis even if sample
pre-treatment prior to laboratory analysis is performed. A change of preservation method on arrival at the
laboratory often results in repackaging the sample, which can damage the sample by changing the attributes
to be analysed.

The method of preservation relates to the stability of samples. Preservation methods are considered under the
following broad headings:
 materials that are stable;

 materials that are unstable but where stability can be achieved by a preservation method;

 materials that are unstable and cannot be readily stabilised.

For those components, which are unstable, it is important to minimise loss or change (chemical or biological)
of the constituent. Changes are the result of various environmental factors, including:

 microbiological activity in the waste sample;

 oxidation of compounds by atmospheric oxygen;

 loss of dissolved volatile components due to pressure and/or temperature changes during the sampling
process;

 photochemical reactions;

 changes in the chemical nature of certain substances due to changes of temperature, pressure and loss
of the vapour phase;

 modification of the pH, conductivity, solubility and carbon dioxide by absorption of CO2 from the air;

 reaction with carbon dioxide or water;

 irreversible adsorption on the surface of containers of metals in solution or in colloidal state and certain
organic compounds.

The choice of preservation method depends on the material to be preserved and the material properties and/or
constituent concentrations to be determined.

The time between sampling and analysis is particularly important for samples in which biological degradation is
likely to occur or in which (semi-) volatile organic components are to be determined. For these types of
samples extended delays between sampling and analysis can result in significant loss of biodegradable,
volatile and (semi-) volatile components eradicating the representative value of the sample. It is advisable that
the time between sampling and analysis is kept to a minimum, not exceeding 7 days.

Common methods of preservation include:

 air tight storage;

 dark storage;

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CEN/TR 15310-4:2006

 cooled storage (< 4 ± 2 °C) (but may result in precipitation);

 nitrogen atmosphere;

 freezing (may change properties by segregation);

 drying (may change properties by loss of volatiles);

 chemical preservation.

These methods are further explained in 5.3

5.2 General instructions for sample preservation

Consultation should be undertaken with the analytical laboratory, or other experts, to obtain advice on the type
of preservation methods required for the identified parameters.

It is common practice that action is taken to:

 avoid the introduction of unacceptable contamination through the preservation method(s);

 incorporate the selected method(s) of preservation into the sampling plan - see Part 1;

 arrange for the samples to be analysed within a time frame agreed with the analytical laboratory, and
specified this in the sampling plan - see Part 1.

Examples of minimum preservation measures are listed in Table 1.

NOTE Additional measures may be applied (e.g. storage for analysis of non-volatile inorganic compounds in a cool
environment).

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Table 1 – Example minimum preservation measures for different types of components

Volatile Semi-volatile Non-volatile Reducing or
components components inorganic rapidly oxidised
components wastes
e
Air tight storage + + - +
Dark storage + + - -
Cooled storage (< 4 ± 2 °C) + + - +
Nitrogen atmosphere - - - +
Freezing - - - -
d
Drying - - + -
f f
Chemical preservation + + - -
a b c
Maximum period of storage <7 7 7 <7
a
When stored with the appropriate preservation method
b
No maximum period when dried prior to storage
c
Maximum storage period depended on the air tightness of the sample container, but maximum of 7 days
d
Only necessary for prolonged storage (>> 7 days)
e
Leaving an appropriate amount of headspace
f
By adding the correct solvent of analytical quality

NOTE The maximum period of 7 days is not validated, but based on laboratory practice. Volatile components are
organic and inorganic components with a boiling point less than 300 °C. All organic components with a boiling point above
300 °C are here to be considered as semi-volatile.

The selected analytical method may specify the most appropriate preservation technique that may not correspond to the
technique detail in the above table. Guidance on preservation techniques should be sought from the chosen analytical
laboratory.

5.3 Preserving specific types of samples

5.3.1 Preservation of mobile liquids

 store mobile liquids under refrigeration and in the dark at (4 ± 2) °C;

 see Table 1

5.3.2 Preservation of liquid and solids rendered mobile by heat

 store liquid and solids rendered mobile by heat under refrigeration and in the dark at (4 ± 2) °C;

 see Table 1

5.3.3 Preservation of viscous liquids

 store viscous liquids under refrigeration and in the dark at (4 ± 2) °C;

 see Table 1

5.3.4 Preservation of sludges

Either:

Store sludges under refrigeration and in the dark at (4 ± 2) °C;

(See Table 1)

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Where there has been considerable bacterial activity prior to sampling (e.g. sludges from water treatment
plants), biological degradation can occur within days of sampling. In these cases analysis should be carried
out as soon as possible after sampling or the samples should be dried immediately after sampling.

5.3.5 Preservation of paste-like substances

Store paste-like substances under refrigeration and in the dark at (4 ± 2) °C.

Where the sample is to be stored for more than seven days drying the sample should be considered.

(See Table 1)

NOTE Drying is only advisable for certain types of paste. For example drying would not be appropriate where the
material is a paste with an organic constituent / solvent. Drying is appropriate where the material has high water content
and analysis does not require the physical properties to be maintained.

5.3.6 Preservation of solids

Store solid samples under refrigeration and in the dark at (4 ± 2) °C.

If it is suspected that bacterial activity may change the concentration of any of the parameters of interest,
drying of the sample should be considered.

NOTE1 Drying would be appropriate where the material has a high water content and analysis does not require the
physical property of the waste to be maintained. It is not appropriate where volatile or semi-volatile parameters require
quantification. For additional information on suitability of drying refer to Table 1.

NOTE 2 Preservation by addition of acid, as carried out on aqueous samples to prevent precipitation of metals, is not
suitable for solid waste materials. Matrix changes can result from this method of preservation.

NOTE 3 This method of preservation may induce segregation of water for wet solids.

5.4 Preservation methods

5.4.1 Airtight storage

When airtight storage is required, store liquid, paste-like and fine-grained materials in glass bottles sealed with
PTFE cap liners.

NOTE 1 Plastics are not considered airtight.

NOTE 2 Airtight storage will prevent volatilisation of components and will reduce biological degradation. However, for
granular materials the air volume within the sample is always large; irrespective of tight filling of the sample container.
Airtight storage for these types of samples is therefore never a guarantee for keeping the characteristics of the sample
constant during the storage period.

NOTE 3 In some cases, inert gas flushing (for example using nitrogen) can be used to limit chemical reactions
(oxidation, carbonation). Inert gas flushing may result in losses of volatile/semi-volatile compounds and advice on the
necessity and potential detrimental effects on the sample of undertaking such procedures should be sought from the
analytical laboratory.

5.4.2 Dark storage

Dark storage is achieved by using dark coloured sample containers or by storing the containers in a dark
place. A cool box with frozen chill packs can provide a cool and dark environment, for example. It is common
practice to store all samples in the dark.

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 CEN/TR 15310-4:2006

5.4.3 Cooled storage

When cooling is required, use a mobile refrigerator, or a refrigeration vehicle. It is common practice to cool all
samples to a temperature of (4 ± 2) °C.

It is common practice to keep the time between sampling and cooling to a minimum, not exceeding 12 h.

NOTE 1 Biological activity can be slowed sufficiently by refrigeration (4 ± 2) °C to maintain sample integrity for up to at
least 24 h.

NOTE 2 For liquid samples, cooling may result in physical changes (crystallisation, precipitation, segregation) possibly
irreversible when re-heating to room temperature. This may induce problems for sub-sampling if required.

5.4.4 Nitrogen atmosphere

When the reducing character of the sample is to be preserved, limit exposure to oxygen after sampling. It is
common practice to flush both the sample container and the sample, in the field, with nitrogen gas (technical
quality is acceptable). Airtight packaging is then sufficient for short-term storage.

When in-field nitrogen flushing is not feasible it is common practice that the time between sampling and
flushing with nitrogen after arrival at the laboratory, is kept to a minimum not exceeding 24 h.

Place the sample in a gas-tight container.

NOTE 1 A suitable container is one, which easily allows flushing to take place, for example, a container with gas
inlet/outlet connectors on it.

 pass nitrogen gas through the container, applying a volume at least 10 times that of the container;

 flush the sample again after an interval of 24 h (to remove any oxygen still diffusing from the sample).

NOTE 2 Long-term storage using nitrogen is possible only in containers with a hermetic gas-tight seal such as a glass
sample container welded shut. Other containers, particularly plastic containers, are insufficiently gas tight and would
expose the sample to oxygen on storage.

Inert gas flushing may result in losses of volatile/semi-volatile compounds.

5.4.5 Freezing

Use liquid nitrogen for immediate deep freezing of samples.

NOTE This method of freezing is difficult to conduct in the field.

 for on-site freezing, either seal samples in plastic bags and store in ice, or pack in insulated cool boxes with frozen
chill packs immediately following collection.

 it is common practice to ensure that samples are transferred to a freezer as soon as possible upon return from
fieldwork.

5.4.6 Chemical preservation

 chemical preservation is pertinent in only a limited number of situations;

 consultation should be undertaken with the analytical laboratory, or other experts, to obtain advice on the
type of preservation methods required for the identified parameters. For liquid samples it is now common
practice for laboratories to provide sample containers with the appropriate chemical preservative added.

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CEN/TR 15310-4:2006

NOTE 1 No one method of chemical preservation will be compatible with the range of parameters, which may be
required for a single sample. For such a range of parameters it may be necessary to collect a number of sub-samples,
each preserved using a different method.

NOTE 2 Care should be taken to avoid unquantifiable reactions that can occur between the sample and additives
during sample preparation (e.g. drying or milling). It is common to obtain this information from the analytical laboratory.

NOTE 3 When samples are required for the determination of extractable levels (e.g. using leaching tests), the addition
of chemical stabilising agents can affect the leachability of other components and, if not chosen advisedly, can make it
difficult to quantify the true concentrations of those parameters within the waste.

NOTE 4 It is very difficult to keep a solvent of analytical quality free from any contamination. The use of solvents in the
field for sample preservation will therefore be limited.

5.4.7 Drying

Ideally samples requiring a measure of biological activity should be tested as soon as is possible after
collection to minimize any changes in the sample. However, if this is not possible and where either the
biological activity of the sample must be preserved or it is suspected that bacterial activity may change the
concentration of any of the parameters of interest, drying of the sample should be considered. Drying should
not be undertaken above 30 °C to minimize loss of any volatile components in the sample. If drying is
undertaken a dry matter content should be calculated by weighing the loss in moisture loss by weighing the
sample before and after drying.

NOTE Drying would be appropriate where the material has a high water content and analysis does not require the
physical property of the waste to be maintained. It is not appropriate where volatile or semi-volatile parameters require
quantification. For additional information on suitability of drying refer to Table 1. Consultation should be undertaken with
the analytical laboratory, or other expert, to obtain advice whether potential compounds of interest may be affected by the
drying. Higher drying temperature than 30 °C may be used, if an assurance can be obtained that there will be no adverse
effects on the potential components and that the temperature will not influence the matrix itself, i.e. influence
characteristics to be determined (such as leaching behaviour).

6 Chain of custody forms and sample dispatch

Samples should be accompanied by a chain of custody form (see EN 14899).

The chain of custody form should be checked and signed at each transfer of the samples.

The packaging should meet the requirements of the authorities or other organisation(s) concerned with the
transport of the sample - see 4.2.

7 Incorporation in the Sampling Plan

The storage, preservation and transport procedure(s) and necessary equipment, should be specified by the
Project Manager in the Sampling Plan; see EN 14899, prior to commencing sampling.

16
 CEN/TR 15310-4:2006

Annex A
(informative)

Packaging

Table A.1 – Sample containers, preservation and storage conditions for different parameters measured
in sediments and sludges and liquids.
Analysis or test Container Preservation Storage Storage International
Conditions duration Standard
)
Acidity Polyethylene/ Refrigerate (2 to 5 °C & 14 days
Glass dark & airtight
Alkalinity Polyethylene/ Refrigerate (2 to 5) °C & 14 days
Glass dark &airtight
pH Sampling Wet Determined None
Device Undisturbed In the field
pH Polyethylene Refrigerate (2 to 5) °C & 24 h
(with /Glass dark & airtight
temperature
correction)
Conductivity Polyethylene Refrigerate (2 to 5) °C & 24 h
/Glass dark & airtight
Dry Weight Glass Refrigerate (2 to 5) °C & 1 month
dark & airtight
Anions Polyethylene Refrigerate (2 to 5) °C & 28 days ISO 11048
(e.g. sulfate) /Glass dark & airtight
Nitrate Polyethylene Refrigerate (2 to 5) °C & 2 days
/Glass dark & airtight
Nitrite Polyethylene Refrigerate (2 to 5) °C & As short as
/Glass dark & airtight possible
Sulfide Polyethylene Refrigerate (2 to 5) °C & As short as
/Glass dark & airtight Possible
Phosphorus Glass Refrigerate (2 to 5) °C & 1 month
dark & airtight
Orthophosphate Glass Refrigerate (2 to 5) °C & 2 days
dark & airtight
Cyanides Polyethylene Freeze <-20 °C & 1 month
dark & airtight
Metals Polyethylene Refrigerate 2-5 °C & 8 days
/Glass dark & airtight
C
Freeze <-20 ° & 6 months
dark & airtight

Dry (30°C) ambient 6 months

temperature
dark & airtight
Chromium (V1) Polyethylene Refrigerate (2 to 5) °C & 2 days
/Glass dark & airtight
Mercury Glass/PTFE Refrigerate (2 to 5) °C & 8 days
dark & airtight

Freeze <-20 °C & 1 month

dark & airtight
Particle size Polyethylene Refrigerate (2 to 5) °C &

17
CEN/TR 15310-4:2006

Analysis or test Container Preservation Storage Storage International

Conditions duration Standard
/Glass/Metal dark & airtight
TOC Glass with Refrigerate (2 to 5)°C & 1 month
PTFE-lined dark & airtight
cap
Freeze <-20 °C & dark 6 months
& airtight
Semi- and non- Glass with Refrigerate (2 to 5) °C& 1 month
Volatile organic PTFE-lined dark & airtight
Compounds cap
Freeze <-20 °C &
dark & airtight 6 months

(PCBs, PAHs, Glass with Refrigerate (2 to 5) °C & 1 month

pesticides, high Aluminium foil dark & airtight
molecular cap
weight Freeze <-20 °C & 6 months
hydrocarbons) dark & airtight
Mineral oil Glass with Refrigerate (2 to 5) °C & 1 month
PTFE-lined dark & airtight
cap
Volatile organics Glass/metal Refrigerate/ (2 to 5) °C & As short as
as received rings with Addition of Dark & airtight possible
PTFE-lined methanol
cap
Freeze <-20 °C & 1 month
dark & airtight
Ecotoxicological Polyethylene Refrigerate (2 to 5) °C & 14 days EN 14735
tests /Glass dark & airtight
Bacteriological Sterile Glass Refrigerate (2 to 5) °C & 6h
Examination dark & airtight
Microbial activity Sterile Glass None None None
Ecological Polyethylene 70% (v/v) (2 to 5) °C & 1 year ISO 5667-3
Examination /Glass ethanol dark & airtight

4% (v/v) 1 year
formalin

(taken from BS 6068-6. 15: 1999, ISO 5667-15:1999 Water quality – Sampling - Part 15: Guidance on
preservation and handling of sludge and sediment samples)

18
 CEN/TR 15310-4:2006

Bibliography

EN 14899:2005, Characterization of waste - Sampling of waste materials - Framework for the

preparation and application of a Sampling Plan

CEN/TR 15310-1:2006, Characterization of waste – Sampling of waste materials - Part 1: Guidance on

selection and application of criteria for sampling under various conditions

CEN/TR 15310-2:2006, Characterization of waste – Sampling of waste materials – Part 2: Guidance

on sampling techniques

CEN/TR 15310 –3:2006, Characterization of waste – Sampling of waste materials – Part 3: Guidance
on procedures for sub-sampling in the field

CEN/TR 15310 –5:2006, Characterization of waste – Sampling of waste materials – Part 5: Guidance on the
process of defining the Sampling Plan

EN 14735:2005, Characterisation of waste – Preparation of waste samples for ecotoxicity tests

Nordtest method NT ENVIR 001, Solid waste, municipal: sampling and characterisation, 1995.

Nordtest method NT ENVIR 004, Solid waste, particulate materials: sampling, 1996

NVN 5870:1998, Waste – Analysis of waste – Sample pretreatment for determination of organic and inorganic
parameters

NVN 7310:1995, Leaching characteristics of solid earth and stony building and waste materials - Sample pre-
treatment - General instructions

NVN 7311:1995, Leaching characteristics of solid earth and stony building and waste materials - Sample pre-
treatment - Sample storage and preservation

NVN 7312:1995, Leaching characteristics of solid earthy and stony building and waste materials - Sample
pretreatment - Sample pretreatment for leaching tests and the analysis of inorganic components

NVN 7313:1995, Leaching characteristics of solid earthy and stony building and waste materials - Sample
pretreatment - Sample pretreatment for leaching tests and the analysis of organic components

EN 932-1:1996, Tests for general properties of aggregates - Part 1: Methods for sampling

EN 932-2:1999, Tests for general properties of aggregates - Part 2: Methods for reducing laboratory samples

BS 7755-2.6:1994, ISO 10381-6: 1993, Soil quality – Sampling - Part 6: Guidance on the collection, handling
and storage of soil for the assessment of aerobic microbial processes in the laboratory

EPA, 1994, Waste analysis at facilities that generate, treat, store, and dispose of hazardous wastes – a
guidance manual

EN 1097-5:1999, Tests for mechanical and physical properties of aggregates - Part 5: Determination of the
water content by drying in a ventilated oven

19
CEN/TR 15310-4:2006

BS 6068-6. 15:1999, ISO 5667-15:1999, Water quality – Sampling - Part 15: Guidance on preservation
and handling of sludge and sediment samples

IUPAC (1990), Nomenclature for sampling in analytical chemistry. Pure Appl Chem, 62: 1193-1208.

20
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PD CEN/TR
15310-4:2006
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