ISO/FDIS 5667-15
(Main)Water quality — Sampling — Part 15: Preservation and handling of samples of sludge, sediment and suspended matter
Water quality — Sampling — Part 15: Preservation and handling of samples of sludge, sediment and suspended matter
ISO 5667-15:2009 provides guidance on procedures for the preservation, handling and storage of samples of sewage and waterworks sludge, suspended matter, saltwater sediments and freshwater sediments, until chemical, physical, radiochemical and/or biological examination can be undertaken in the laboratory. The procedures in ISO 5667-15:2009 are only applicable to wet samples of sludge, sediment and suspended matter.
Qualité de l’eau — Échantillonnage — Partie 15: Conservation et traitement des échantillons de boues, de sédiments et de matières en suspension
L'ISO 5667-15:2009 fournit des lignes directrices relatives aux modes opératoires de conservation, de manipulation et de stockage des échantillons de boues provenant de stations d'épuration et de stations de traitement de l'eau potable, de matières en suspension, de sédiments en eau salée et en eau douce, jusqu'à ce que leur examen chimique, physique, radiochimique et/ou biologique puisse être entrepris en laboratoire. Les modes opératoires fournis dans l'ISO 5667-15:2009 s'appliquent uniquement aux échantillons humides de boues, de sédiments et de matières en suspension.
General Information
- Status
- Not Published
- Technical Committee
- ISO/TC 147/SC 6 - Sampling (general methods)
- Drafting Committee
- ISO/TC 147/SC 6/WG 3 - Preservation and handling of samples
- Current Stage
- 5020 - FDIS ballot initiated: 2 months. Proof sent to secretariat
- Start Date
- 26-Feb-2026
- Completion Date
- 26-Feb-2026
Relations
- Effective Date
- 12-Feb-2026
- Effective Date
- 02-Dec-2023
- Effective Date
- 25-Nov-2023
Overview
ISO/FDIS 5667-15:2026 is part of the ISO 5667 series, establishing internationally recognized procedures for the preservation and handling of wet samples of sludge, sediment, and suspended matter in water quality monitoring. This standard delivers guidance relevant to sewage and waterworks sludge, suspended particulate matter, and both saltwater and freshwater sediments, ensuring sample integrity from collection through transport, storage, and laboratory examination.
The document’s main objective is to maintain representative sample conditions for accurate chemical, physical, radiochemical, hydrobiological, and microbiological analysis. By adhering to ISO/FDIS 5667-15, laboratories, environmental monitoring agencies, and water utilities can optimize reliability and comparability in water quality assessment, while complying with regulatory and best practice requirements.
Key Topics
- Sample Integrity & Chain of Custody: Establishing procedures for documenting and maintaining the integrity of samples from collection to analysis.
- Preservation Techniques: Guidance on sample-specific preservation methods to stabilize chemical, biological, and physical properties until laboratory examination.
- Sample Handling: Best practices for sub-sampling, homogenization, labeling, and minimizing alterations during transport and storage.
- Appropriate Containers & Equipment: Recommendations for container selection and preparation, designed to prevent contamination and analyte loss.
- Sample Collection Volumes: Ensuring enough material for multi-parameter analyses, repeat measurements, and quality control.
- Transport & Storage Conditions: Requirements for cooling, freezing, and monitoring temperatures during transit and storage.
- Identification & Labeling: Reliable methods for labeling and reporting sample data for traceability.
- Safety Precautions: Emphasis on protecting personnel from hazardous substances and pathogens present in sludge and sediments.
- Documentation: Comprehensive recording of sampling and handling details to comply with auditing and traceability standards.
Applications
ISO/FDIS 5667-15 is essential for organizations involved in:
- Water Quality Monitoring: Collecting, preserving, and analyzing sediments and suspended matter from rivers, lakes, estuaries, and marine environments.
- Wastewater Treatment Analysis: Sampling and transport of sewage and waterworks sludge for regulatory compliance and performance evaluation.
- Environmental Impact Assessment: Supporting accurate studies of pollutant transport, accumulation, and ecological risk in aquatic systems.
- Research Laboratories: Preparing and handling wet sediment and sludge samples for advanced analyses, including physical structure, contaminant fate, or biological assemblages.
- Industrial and Municipal Compliance: Demonstrating adherence to environmental regulations concerning water and sediment quality.
By following the standard’s guidelines, users ensure analyses remain accurate and representative, minimizing sample degradation, contamination, or data loss. The procedures facilitate international comparability and reproducibility of water quality data, empowering informed decision-making across sectors.
Related Standards
This standard should be applied together with other documents in the ISO 5667 series and related water quality standards, including:
- ISO 5667-1: Guidance on the design of sampling programs and techniques.
- ISO 5667-3: Guidance on preservation and handling of all types of water samples.
- ISO/TS 5667-25: Validation protocols for new sample storage times and preservation methods.
- ISO 5667-14: Sample containers and contamination control.
- ISO 5667-16: Biotesting with ecotoxicological or biological assays (if such testing is required).
- ISO 5667-27: Specific methodologies for microplastics sampling.
- ISO 18512: Procedures for storage of soil and sediment samples.
Following ISO/FDIS 5667-15 strengthens consistency in environmental sampling, supports regulatory compliance, and advances best practices in water quality assessment worldwide.
Buy Documents
ISO/FDIS 5667-15 - Water quality — Sampling — Part 15: Preservation and handling of samples of sludge, sediment and suspended matter/14/2025
ISO/FDIS 5667-15 - Water quality — Sampling — Part 15: Preservation and handling of samples of sludge, sediment and suspended matter/12/2026
REDLINE ISO/FDIS 5667-15 - Water quality — Sampling — Part 15: Preservation and handling of samples of sludge, sediment and suspended matter/12/2026
ISO/FDIS 5667-15 - Qualité de l’eau — Échantillonnage — Partie 15: Conservation et traitement des échantillons de boues, de sédiments et de matières en suspension/25/2025
Get Certified
Connect with accredited certification bodies for this standard

NSF International
Global independent organization facilitating standards development and certification.
CIS Institut d.o.o.
Personal Protective Equipment (PPE) certification body. Notified Body NB-2890 for EU Regulation 2016/425 PPE.

Kiwa BDA Testing
Building and construction product certification.
Sponsored listings
Frequently Asked Questions
ISO/FDIS 5667-15 is a draft published by the International Organization for Standardization (ISO). Its full title is "Water quality — Sampling — Part 15: Preservation and handling of samples of sludge, sediment and suspended matter". This standard covers: ISO 5667-15:2009 provides guidance on procedures for the preservation, handling and storage of samples of sewage and waterworks sludge, suspended matter, saltwater sediments and freshwater sediments, until chemical, physical, radiochemical and/or biological examination can be undertaken in the laboratory. The procedures in ISO 5667-15:2009 are only applicable to wet samples of sludge, sediment and suspended matter.
ISO 5667-15:2009 provides guidance on procedures for the preservation, handling and storage of samples of sewage and waterworks sludge, suspended matter, saltwater sediments and freshwater sediments, until chemical, physical, radiochemical and/or biological examination can be undertaken in the laboratory. The procedures in ISO 5667-15:2009 are only applicable to wet samples of sludge, sediment and suspended matter.
ISO/FDIS 5667-15 is classified under the following ICS (International Classification for Standards) categories: 13.030.20 - Liquid wastes. Sludge; 13.060.45 - Examination of water in general. The ICS classification helps identify the subject area and facilitates finding related standards.
ISO/FDIS 5667-15 has the following relationships with other standards: It is inter standard links to FprEN ISO 5667-15, ISO 12217-2:2022, ISO 5667-15:2009. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ISO/FDIS 5667-15 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
DRAFT
International
Standard
ISO/DIS 5667-15
ISO/TC 147/SC 6
Water quality — Sampling —
Secretariat: BSI
Part 15:
Voting begins on:
Preservation and handling of 2025-07-09
samples of sludge, sediment and
Voting terminates on:
2025-10-01
suspended matter
ICS: 13.060.45; 13.030.20
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENTS AND APPROVAL. IT
IS THEREFORE SUBJECT TO CHANGE
AND MAY NOT BE REFERRED TO AS AN
INTERNATIONAL STANDARD UNTIL
PUBLISHED AS SUCH.
This document is circulated as received from the committee secretariat.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
ISO/CEN PARALLEL PROCESSING
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS.
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION.
Reference number
ISO/DIS 5667-15:2025(en)
DRAFT
ISO/DIS 5667-15:2025(en)
International
Standard
ISO/DIS 5667-15
ISO/TC 147/SC 6
Water quality — Sampling —
Secretariat: BSI
Part 15:
Voting begins on:
Preservation and handling of
samples of sludge, sediment and
Voting terminates on:
suspended matter
ICS: 13.060.45; 13.030.20
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENTS AND APPROVAL. IT
IS THEREFORE SUBJECT TO CHANGE
AND MAY NOT BE REFERRED TO AS AN
INTERNATIONAL STANDARD UNTIL
PUBLISHED AS SUCH.
This document is circulated as received from the committee secretariat.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
© ISO 2025
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
STANDARDS MAY ON OCCASION HAVE TO
ISO/CEN PARALLEL PROCESSING
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
BE CONSIDERED IN THE LIGHT OF THEIR
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
or ISO’s member body in the country of the requester.
NATIONAL REGULATIONS.
ISO copyright office
RECIPIENTS OF THIS DRAFT ARE INVITED
CP 401 • Ch. de Blandonnet 8
TO SUBMIT, WITH THEIR COMMENTS,
CH-1214 Vernier, Geneva
NOTIFICATION OF ANY RELEVANT PATENT
Phone: +41 22 749 01 11
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION.
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland Reference number
ISO/DIS 5667-15:2025(en)
ii
ISO/DIS 5667-15:2025(en)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms for plastics . 3
5 Sampling and chain of custody . 3
6 Reagents . 3
7 Sample handling and preservation . 4
7.1 General .4
7.2 Sample handling and preservation for chemical analysis .5
7.3 Sample handling and preservation for physical analysis .5
7.4 Sample handling and preservation for radiochemical analysis .5
7.5 Sample handling and preservation for hydrobiological analysis .5
7.6 Sample handling and preservation for microbiological analysis .5
8 Safety precautions. 6
8.1 Staff protection .6
8.2 Sample protection.6
9 Containers . 6
10 Sample collection . 6
11 Identification of samples . 7
12 Sample transport . 7
13 Sample reception . 8
14 Sample storage . 8
Annex A (informative) Techniques for sample preservation .10
Annex B (informative) Container preparation .25
Annex C (informative) Long term storage of wet sediment samples using nitrogen vapour
freezes .27
Bibliography .29
iii
ISO/DIS 5667-15:2025(en)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out through
ISO technical committees. Each member body interested in a subject for which a technical committee
has been established has the right to be represented on that committee. International organizations,
governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely
with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO's adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 147 Water quality, Subcommittee SC 6,
Sampling (general methods).
This third edition cancels and replaces the second edition (ISO 5667-15:2009), which has been technically
revised.
The main changes are as follows:
— ‘suspended matter’ has been added to the title and ‘guidance’ has been deleted from the title;
— ISO/TS 5667-25 has been added as a reference;
— a flow diagram for preservation and storage of samples of sludge, sediment and suspended matter has
been added (in line with ISO 5667-3:2024);
— terms and definitions have been aligned with ISO 5667-3:2024;
— tables from clause 12 have been moved to Annex A;
— references in the previous Tables 1 to 3 have been added;
— the previous Table 3 has been split into Table A.3 ‘Hydrobiological analysis’ and Table A.4 ‘Microbiological
analysis’.
A list of all parts in the ISO 5667 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
ISO/DIS 5667-15:2025(en)
Introduction
[1]
This document is intended to be used in conjunction with ISO 5667-1, which deals with the design
of sampling programmes and sampling techniques.
Where possible, this document has been aligned with current standards. Where new research or validation
results have provided new insights, the latest knowledge has been used.
[6]
Guidance on validation protocols can be found in ISO/TS 5667-25 .
Tables A.1 to A.4 provide the validated preservation times or conditions as well as the descriptions of best
practice. Tables A.1 to A.4 also refer, for each parameter, to references available at the time of publication of
this document (i.e. ISO 5667-15:202x). This is however not an exhaustive list. Other preservation methods
may be used when they have been validated. However, it is strongly recommended that, where a method
validation is not available, the preservation times for the analyte listed in Tables A.1 to A.4 for ISO and CEN
test methods be followed. In case more than one storage time is provided in Tables A.1 to A.4, the order of
preferred use is:
— validated method;
— method provided by reference;
— best practice.
The preservation and storage conditions and maximum storage times per parameter as listed in Tables A.1
to A.4 should be regarded as default conditions to be applied in the absence of any other information.
However, if validation of preservation techniques and holding times has been carried out, relative to specific
circumstances and matrices, by a laboratory, then, provided that it can produce evidence of this validation
where they differ from those set out in Tables A.1 to A.4, these validated preservation and storage conditions
and maximum storage times are deemed acceptable for use by the validating laboratories. A national
standard can contain information on preservation.
NOTE Samples of sludge, sediment and suspended matter that are dried or freeze-dried behave similarly to dried
[37]
soils. For guidance on freeze-drying, see ISO 16720 .
This document and the related analytical references can be used as presented in Figure 1.
v
ISO/DIS 5667-15:2025(en)
WARNING — ‘Method provided by reference’ and ‘validated method’ can be based on previous
[6]
standards and methods and therefore not be in line with ISO/TS 5667-25. This information can be
interpreted by a qualified and experienced person.
Figure 1 — Flow diagram for the selection of a method for the preservation
and storage of samples of sludge, sediment and suspended matter
[6]
Attention is drawn to ISO/TS 5667-25, which contains guidelines and the elaboration of the required
techniques of how to validate new storage times or preservative methods and details of the techniques
described.
vi
DRAFT International Standard ISO/DIS 5667-15:2025(en)
Water quality — Sampling —
Part 15:
Preservation and handling of samples of sludge, sediment and
suspended matter
WARNING — Persons using this document should be familiar with normal laboratory practice. This
document does not purport to address all of the safety problems, if any, associated with its use. It is
the responsibility of the user to establish appropriate safety and health practices.
IMPORTANT — It is absolutely essential that tests conducted in accordance with this document be
carried out by suitably qualified staff.
1 Scope
This part of ISO 5667 specifies the general requirements on procedures for the preservation, handling and
storage of samples of sewage and waterworks sludge, suspended matter, marine sediments and freshwater
sediments for chemical, physical, radiochemical and/or biological examination in the laboratory.
The procedures in this part of ISO 5667 are only applicable to wet samples of sludge, sediment
and suspended matter.
NOTE The storage conditions given do not necessarily apply for derived samples, for example sediment eluates or
extracts.
This document is not applicable to samples intended for biotesting with ecotoxicological or biological assays
[5] [7]
(which is specified in ISO 5667-16 ) nor intended for microplastics (which is specified in ISO 5667-27 ).
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
best practice
method based upon consensus or general use and that can be referred to in literature
Note 1 to entry: Given the differences in conditions and circumstances as well as the impossibility to validate
all parameters from a validated method (3.10) or technique or process, a best practice method based upon the
corresponding properties of a validated parameter can be used.
[2]
[SOURCE: ISO 5667-3:2024, 3.1]
ISO/DIS 5667-15:2025(en)
3.2
integrity
property of the parameter(s) of interest, information or content of a sample stored in a container that has
not been altered or lost in an unauthorized manner or that has been subject to loss of representativeness
[2]
[SOURCE: ISO 5667-3:2024, 3.2]
3.3
method provided by reference
procedure or technique for the preservation of samples taken from the reference to which it refers
Note 1 to entry: It is not in all cases clear whether the preservation procedure provided by the reference was validated
method (3.10), a best practice (3.1) or which procedure was used for its determination or validation. Where available,
the information about the matrices is taken over.
[2]
[SOURCE: ISO 5667-3:2024, 3.3]
3.4
sample preservation
procedure used to stabilize a sample in such a way that the properties under examination are maintained
stable from the collection step until preparation for analysis
Note 1 to entry: Different analytes can require several samples from the same source that are stabilized by different
procedures. More subsamples from one location can be needed as some parameters require a different preservation
procedure.
[10]
[SOURCE: ISO 11074:2025, 3.401, modified — Note 1 to entry has been added.]
3.5
sample storage
process and the result of keeping a sample available under predefined conditions, usually for a specified
time interval between collection and further treatment of a sample
Note 1 to entry: The specified time is the maximum time interval.
[10]
[SOURCE: ISO 11074:2025, 3.407, modified — Note 1 to entry has been added; “soil sample” has been
changed to “sample”.]
3.6
sediment
matter which settles to the bottom of a liquid, often transported in water before settlement occurs
Note 1 to entry: Sediment samples in this document are a part of water quality analysis. The liquid in this case
is therefore water.
[8]
[SOURCE: ISO 6107:2021, 3.505, modified — Note 1 to entry has been added.]
3.7
sludge
mixture of water and solids originating from various types of water during natural and artificial treatment
[43]
[SOURCE: ISO 19698:2020, 3.23, modified — The word “wastewater” has been replaced by “water”.]
3.8
storage time
period of time between filling of the sample container and further treatment of the sample in the laboratory,
if stored under predefined conditions
Note 1 to entry: Sampling finishes as soon as the sample container has been filled with the sample. Storage time ends
when the sample is taken by the analyst to start sample preparation prior to analysis.
Note 2 to entry: Further treatment is, for most analytes, a solvent extraction or acid destruction. The initial steps
of sample preparation can be steps complementary to the storage conditions for the maintenance of analyte
concentrations.
ISO/DIS 5667-15:2025(en)
[2]
[SOURCE: ISO 5667-3:2024, 3.6]
3.9
suspended matter
solids remaining in suspension in water which can be removed by sedimentation, filtration or centrifugation
[8]
[SOURCE: ISO 6107:2021, 3.554]
3.10
validated method
method for which the validity of correctness has been checked by verification or qualification against
a number of predefined requirements
Note 1 to entry: A validated method indicates that a preservation method is capable of delivering the intended results
with an acceptable degree of uncertainty for the parameter or group of parameters and sample type.
[2]
[SOURCE: ISO 5667-3:2024, 3.7]
4 Abbreviated terms for plastics
FEP perfluoro(ethylene/propylene)
PE polyethylene
PE-HD high density polyethylene
PET polyethylene terephthalate
PFA perfluoroalkoxy (polymer)
PP polypropylene
PTFE polytetrafluoroethylene
PVC poly(vinyl chloride)
5 Sampling and chain of custody
If there is a need to take samples, this is done according to a sampling programme. The first step is to design
[1]
a sampling programme. Guidance on this topic is given in ISO 5667-1 .
Depending on the sample type and matrix, instructions are given in the relevant part(s) of the ISO 5667 series.
The process of preservation and handling of samples consists of several steps. During this process, the
responsibility for the samples can change. To ensure the integrity of the samples, all steps involving the
sample shall be documented.
6 Reagents
WARNING — Sampling personnel should be warned of potential dangers and appropriate safety
procedures should be available. Beware of formaldehyde vapours. Do not store large numbers of
samples in small working areas.
All reagents and waters used shall be of at least analytical grade.
6.1 Deionized water.
ISO/DIS 5667-15:2025(en)
6.2 Sodium sulfate Na SO .
2 4
Heat the sodium sulfate before use for at least 3 h at 500 °C. Store in an desiccator after heating.
6.3 Zinc acetate solution (CH COO) Zn·2H O (100 g/l).
3 2 2
Dissolve 10,0 g of zinc acetate dihydrate in approximately 90 ml of water. Dilute to 100 ml with water.
6.4 Methanol CH OH.
6.5 Ethanol C H OH (volume fraction of 96 %).
2 5
6.6 Formaldehyde solution (formalin), CH O, φ(CH O) = 37 % (freshly prepared).
2 2
WARNING — Beware of formaldehyde vapours. Do not store large numbers of samples in small
working areas.
6.7 Sodium tetraborate (Na B O ·10H O).
2 4 7 2
6.8 Hexamethylenetetramine [(CH ) N ]
2 6 4
6.9 Neutralized formaldehyde solution formaldehyde solution (6.6) neutralized with sodium
tetraborate (6.7) or hexamethylenetetramine (6.8).
Formalin solution at 100 g/l gives a final solution of φ(CH O) = 3,7 %.
WARNING — Beware of formaldehyde vapours. Do not store large numbers of samples in small
working areas.
7 Sample handling and preservation
7.1 General
Sample handling is specific for each determination to be conducted. Manipulation of samples is often
required to yield consistent material for analysis. Homogenization, by mixing or sieving, dilution to obtain
a suitable concentration and addition of chemical preservatives all complicate interpretations of in situ
comparisons.
Any large individuals of macrofauna should be removed from the samples immediately after collecting
samples taken for the chemical, physical, radiochemical and/or biological examinations.
The purpose of preservation is to retain the integrity of the collected material as it was on site in relation
to the parameters to be analyzed. Analytes might be subject to biotransformation, volatilization and
chemical transformation (e.g. oxidation, reduction, hydrolysis, photolysis) during storage. Therefore, careful
consideration should be given to these processes and the storage conditions needed to avoid such alterations.
The need to preserve sludge, sediment and suspended matter begins immediately after a sample has been
taken. The most critical changes to the sample can occur in the first few hours after sampling. Therefore,
where possible, preservation steps should be taken immediately upon sample collection.
The choice of preservation technique depends mainly on the objective of the sample collection and the
analysis being determined. It is important to understand the effects that preservation and storage can have
on the sample quality and the analysis results.
No other general recommendations can be given for a preservation or storage method. A preservation
method suitable for one group of parameters can interfere with the analysis of other groups of parameters.
To overcome this problem, a number of sub-samples should be collected; each sub-sample should be
preserved using a suitable method such that the specific demands of each analytical parameter are met.
ISO/DIS 5667-15:2025(en)
7.2 Sample handling and preservation for chemical analysis
Chemical analysis can be performed to determine the nature and amounts of the substances that are
contained in the whole sample, dissolved in the aqueous phase and absorbed by sludge, sediment or
suspended matter.
Partition of chemical components between the solid phase and the water phase is influenced by several
factors, such as particle size, amount of organic matter, pH, redox potential and salinity. The study of such
attributes can be a sampling objective. Therefore, the preservation needs for the analytical methods to be
employed should be taken into account (see Table A.1). The guidance given in this part of ISO 5667 is relevant
to the determination of components in the sum of the separate phases of sludge, sediment or suspended
matter, unless otherwise indicated.
Preservation of samples by freezing can cause mobilization of contaminants by cellular disruption, whereas
not stabilizing samples can permit continued microbial transformation of critical parameters of interest. In
addition to biodegradation of organics, volatilization is a principal mechanism of loss of volatile compounds
during sample handling. Microbial activity can be responsible for changes in the nitrate-nitrite-ammonia
content, for decrease in biochemical oxygen demand, or for reducing sulfate to sulfide. Anoxic samples
require appropriate preservation techniques such as oxygen exclusion during sample handling. Drying,
freezing and freeze-drying of anoxic samples alter the binding sites of, for example, heavy metals, making
more differentiated investigation of binding forms virtually impossible.
Details of the sample preservation are given in Table A.1.
7.3 Sample handling and preservation for physical analysis
The structure, texture and, for sediments, the layer formation should be determined.
NOTE Sediment matrix changes are obvious if rapid drainage of pore water occurs.
The importance of sludge, sediment or suspended matter integrity to the investigation objectives should be
evaluated as it can influence the preservation and handling techniques. In general, any disturbance of the
samples should be minimized. Where the physical structure of the material sampled is important for the
measurement of parameters (e.g. resistance to filtration), agitation and vibration during transport should
be reduced to a minimum. Freezing of the sludge, sediments or suspended matter may be appropriate. In
some cases, thermal techniques should be avoided as they strongly modify sludge structure, thus affecting
physical characteristics (e.g. de-waterability, settleability, flowability).
Details of the sample preservation are given in Table A.1.
7.4 Sample handling and preservation for radiochemical analysis
Some sampling sites can have measurable radiochemical activity, e.g. in the soil or air. Some items of domestic
equipment within the laboratory can also be a source of radioactive material. Contamination of the sample
by its environment should therefore be avoided, especially if the sample activity is likely to be very low.
Details of the sample preservation are given in Table A.2.
7.5 Sample handling and preservation for hydrobiological analysis
Hydrobiological analysis generally involves classifying the species and numbers of flora and/or fauna
present on and in fixed sludge or sediments.
Details of the sample preservation are given in Table A.3.
7.6 Sample handling and preservation for microbiological analysis
Microbial activity may also be used to characterize samples and can only be determined without fixation.
Details of the sample preservation are given in Table A.4.
ISO/DIS 5667-15:2025(en)
8 Safety precautions
8.1 Staff protection
Health and safety precautions should be observed at all times when sampling potentially hazardous sludge,
sediments or suspended matter.
Human exposure to pathogenic organisms or pollutants should be avoided by using appropriate protective
equipment such as respiratory protective masks, safety glasses, safety boots and protective gloves.
The hazard due to pathogenic organisms in sludge can be very high. It is vital that all sampling personnel
should receive thorough training and be provided with appropriate medical inoculations.
Degradation of sludge produces methane, which presents a risk of fire and explosion if a source of ignition
is present. Containers should be appropriately packed to minimize the fragmentation of the containers if an
excessive pressure build-up of methane occurs.
If sludge samples are to be taken in locations where there is restricted ventilation, staff should take safety
precautions to protect themselves against sulfide, carbon dioxide and methane.
8.2 Sample protection
When sampling, transporting and utilizing sludge, care should be taken to prevent a build-up of gas pressure
in the sample container. Manual release of pressure during and after transport may be necessary if prolonged
storage is required.
Samples collected for the analysis of volatile organic or sulfide compounds should not be homogenized
because many of these compounds could be lost while compositing.
9 Containers
Sample containers should be made of a material appropriate for preserving the natural properties of both
the sample and the expected range of contaminants. Suitable types of containers for each analyte to be
measured are given in Tables A.1 to A.4.
[1]
The choice of sample container is of major importance and ISO 5667-1 provides guidance on this subject.
Although certain container materials are generally favourable for certain analytes, the use of other materials
might be technically correct.
The applicability of the specific sample containers should be verified for contaminations and analyte loss
before usage with samples to avoid the loss of samples.
If the samples are to be frozen, suitable material such as polyethylene (PE), polypropylene (PP) or
polytetrafluoroethylene (PTFE) should be used to minimize the risk of breakage.
Careful consideration should also be given to the suitability of the container for cleaning/decontamination
or disposal and appropriate action taken. Recommendations for the preparation of containers are given in
Annex B.
[4]
In 11.3 of ISO 5667-14:2014, guidance is given on measuring the contamination impact of the container. The
analyte level in the blank should be negligible compared to the analyte level to be measured in the sample.
NOTE Regular container volumes are 500 g to 1 000 g.
10 Sample collection
Samples should be collected in sufficient volumes to allow:
a) separation of sub-samples to be preserved for each type of analysis or examination to be undertaken;
ISO/DIS 5667-15:2025(en)
b) repetition of the analysis in the event of error checking or the routine quality control requirements
of duplicate analysis;
c) preparation of time-dependent composites; for example, a daily aliquot of sewage works sludge
(preserved as appropriate) may be retained to produce a composite for monthly analysis.
For sludge samples, it is recommended that the container is filled completely as far as possible, especially if
biological activity is expected, in order to reduce the risk of overpressurization and explosion.
If analysis of volatile compounds is required, containers should be completely filled with sample from the
first grab, prior to sample homogenization. No headspace should remain in either container.
If the sample is to be frozen, enough headspace should be allowed for expansion to take place.
Where samples are collected for the purpose of microscopic examination, for example of activated sludges,
it is recommended to fill the container to no more than 5 % of its capacity to ensure an oxygen supply to the
sludge prior to examination.
The temperature of the sample, especially of sludge samples, can influence the properties of the sample.
Therefore, the initial temperature of the sludge samples should be measured on site and recorded.
11 Identification of samples
Container labels should withstand wetting, drying and freezing without detaching or becoming illegible.
The labelling system shall be waterproof to allow use on site.
The exact information given in the sampling report and on the sample labels depends on the objectives of the
particular measurement programme. In all cases, an indelible label shall be secured to the sample container.
For each sample, at least the following information shall be available:
— Identification of sampling personnel;
— A unique identifier, traceable to sample date, location and sample number shall appear on the label of the
sample container.
All other information is supplementary and should be detailed in the sampling report.
12 Sample transport
Cooling or freezing procedures shall be applied to samples to increase the time period available for transport
and storage (and if required, by Tables A.1 to A.4). When transport takes place, the sampling plan (e.g.
[1]
ISO 5667-1 ) shall consider:
— the time between sampling (end of filling the sample container intended for the laboratory) and start of
transport;
— the transport time;
— the time before further treatment in the laboratory.
The sum of these three periods is limited to the maximum storage times according to Tables A.1 to A.4.
If the maximum storage time cannot be met, then the sampling plan shall be reformulated to allow these
requirements to be accommodated.
[6]
In case the requirements cannot be met, instructions given in ISO/TS 5667-25 can be used to validate the
preservation time of specific water samples or sample types.
Containers holding samples shall be protected and sealed during transport in such a way that the samples
do not deteriorate or lose any part of their content. Container packaging shall protect the containers
ISO/DIS 5667-15:2025(en)
from possible external contamination, particularly near the opening, and should not itself be a source of
contamination.
Glass containers shall be protected from potential breakage during transport by appropriate packaging.
Samples shall be transported as soon as possible after sampling and with cooling (if necessary, according to
Tables A.1 to A.4).
Laboratory samples for dispatch or transport by third parties and preserved laboratory samples should be
sealed in such manner that the integrity of the sample can be maintained.
During transportation to the laboratory, samples shall be stored in a cooling device capable of maintaining
a temperature of 5 °C ± 3 °C. Samples intended for radiochemical analysis can be placed under room
temperature. For proper evaluation of the conditions during transport, a device capable of recording the
(maximum) temperature of the air surrounding the sample can be used. The temperature sensor should
then be placed in a small container (e.g. 50 ml to 100 ml) filled with a fluid in order to avoid short time
fluctuations in temperature.
Cooling and freezing procedures applied shall be in line with instructions from the analytical laboratory.
Freezing especially requires detailed control of the freezing and thawing process in order to return
the sample to its initial equilibrium after thawing.
Samples should not be in direct contact with the ice packs.
NOTE 1 Devices capable of logging of the temperature during the transportation are available.
NOTE 2 For the transport of samples from the field to the laboratory, the preferred fluid for measuring
the temperature is glycerol. If samples are transported in the field (e.g. on large locations), the fluid can also be, for
example, water.
13 Sample reception
All relevant information regarding the sample identification in accordance with Clause 11 and the sample
transport in accordance with Clause 12 shall be recorded.
The laboratory shall receive and check information on sample preservation and sample transport conditions.
If at least one of the conditions is not met, a disclaimer should be reported along with the results.
In all cases, and especially when a “chain of custody” process needs to be established, the number of sample
containers received in the laboratory and the integrity shall be verified against the number of sample
containers submitted.
14 Sample storage
The storage time of samples of sludge, sediment and suspended matter within the laboratory is specific to
the analyte(s) to be analyzed. Samples should be stored no longer than the maximum storage times given in
Tables A.1 to A.4, with the exception of wet sediments that may be stored for longer periods when samples
are preserved using a nitrogen vapour freezer.
NOTE 1 For guidance on long-term storage of wet sediment samples using nitrogen vapour freezers, see Annex C.
[41]
NOTE 2 For further information on long- and short-term storage of dried samples, see ISO 18512 .
The refrigeration conditions within the laboratory shall be 3 °C ± 2 °C. Samples for microbiological analysis
shall be stored at 5 °C ± 3 °C. The temperature of samples frozen for preservation shall be maintained below
–18 °C, unless otherwise specified. Exceptions to these refrigeration conditions are listed in Tables A.1 to A.5.
When thawing frozen samples, it is recommended that each sample container be placed in a separate
secondary container to minimize the risk of liquid loss, should a split become apparent during the thawing
process or a rupture occur during initial freezing and storage. A mild impact can cause splitting of some
plastics at low temperatures. With respect to thawing, it is recommended that this be done under ambient
conditions.
ISO/DIS 5667-15:2025(en)
Be aware of the fact that the cooling conditions within the laboratory (1 °C to 5 °C) are different from the
cooling conditions during transport (2 °C to 8 °C).
ISO/DIS 5667-15:2025(en)
Annex A
(informative)
Techniques for sample preservation
A.1 General
This document and the analytical International Standards listed in this annex are complementary.
In some cases, the alternative preservation techniques listed contradict each other. It is intended that
where an existing analytical standard is used, the preservation technique described in that method applies.
However, alternative preservation techniques given in this document can also be appropriate. Where no
preservation method is described in the analytical International Standard, or no analytical International
Standard is used, the technique(s) listed in this document shall be used.
The information presented by line in each table comes from the international reference standard cited in the
first cell of the line and the source column (best practice, validated method, method provided by reference)
applies to the entire line.
[6]
A validation protocol used for validation studies can be found in ISO/TS 5667-25
A.2 Physicochemical and chemical analysis
The following general remarks should be noted in relation to the use of Table A.1.
— A preservation time of 1 d means that if 24 h is exceeded, this should be stated in the report.
— The types of containers are identical to those in the analytical International Standards. In some cases,
the type of container in the standard is very specific, e.g. PTFE. This can be essential when very low
concentrations of inorganic parameters have to be measured. In other cases, when the specific type of
plastic is not important, the term plastics is sufficient. Plastics used for containers in the laboratory are
for instance PE, PTFE, PET, PP, PFA and FEP.
A.3 Radiochemical analysis
The following general remarks should be noted in relation to the use of Table A.2.
WARNING — Radioprotection, such as shielding, can be necessary, depending on the activity
of the sample.
— Acidification is carried out to avoid algal growth, biological spoilage and adsorption of metal ions to the
inner wall of the sample container.
— Contamination of the sample should be avoided, especially if the sample activity is very low. Some
sample sites can have measurable activity in the soil of air, or in waters other than those being sampled.
Laboratories, as well as some items of domestic equipment, can contain radioactive material. When
sampling precipitation, any special requirements in Table A.2 are additional to those given in ISO 5667-8.
[3]
As the collection of sufficient samples can require a period of days, both the starting and finishing
times and dates should be recorded. A record of precipitation collection for the sample station for the
appropriate period should be appended. A stabilizer or carrier may be added if appropriate for the
analytes being measured.
— Plastics used for containers in the laboratory are for instance PE, PTFE, PET, PP, PFA and FEP.
ISO/DIS 5667-15:2025(en)
NOTE Some plastic bottles slowly concentrate samples over a period of many months by being very slightly
permeable to water.
A.4 Hydrobiological analysis
The following general remarks should be noted in relation to the use of Table A.3.
— Plastics used for containers in the laboratory are for instance PE, PTFE, PET, PP, PFA and FEP.
— If a preservation method is not specified, it is generally unimportant. The indication “1 month” represents
preservations without particular difficulty.
A.5 Microbiological analysis
The following general remark should be noted in relation to the use of Table A.4.
— Plastics used for containers in the laboratory are for instance PE, PTFE, PVC and PET.
ISO/DIS 5667-15:2025(en)
Table A.1 — Techniques for sample preservation — Physicochemical and chemical analysis of organic and inorganic analytes
Preservation and
Analyte/parameter Type of contain- storage condi- Maximum stor-
Reference Source Types
a b
to be studied er tions additional to age times
Clauses 8 and 11
Sediment, sludge, sus-
Acidity and alkalinity ISO 5667-15 P or G Dark and airtight 14 d Best practice
pended matter
Ammonia ISO 5667-15 P or G Dark and airtight 1 d Best practice Sludge
Analyze as soon
Not provided Method provided
as possible after sam- 1 d Sludge
by reference by reference
[14]
pling.
EN 14671:2006
No reference
If prolonged stor-
to ISO 5667-15
Not provided age is unavoidable, Method provided
28 d Sludge
by reference then store the sam- by reference
Ammonia (extracta-
ples ≤ -18 °C.
ble)
Analyze the nitrogen
[31]
CEN/TS 16177:2012 fractions as soon
Not provided Not provided by ref- Method provided
as possible.
Sludge
No reference
by reference erence by reference
to ISO 5667-15 Cool the filtrates
when stored.
Anions Sediment, sludge, sus-
ISO 5667-15 P or G Dark and airtight 1 month Best practice
(Cl, Br, F and SO ) pended matter
Dark
Sample pretreatment
Method provided
fo
...
FINAL DRAFT
International
Standard
ISO/TC 147/SC 6
Water quality — Sampling —
Secretariat: BSI
Part 15:
Voting begins on:
2026-02-26
Preservation and handling of
samples of sludge, sediment and
Voting terminates on:
2026-04-23
suspended matter
Qualité de l’eau — Échantillonnage —
Partie 15: Conservation et traitement des échantillons de boues,
de sédiments et de matières en suspension
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
WITH THEIR COMMENTS, NOTIFICATION OF ANY
RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE
AND TO PROVIDE SUPPOR TING DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/CEN PARALLEL PROCESSING LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
Reference number
FINAL DRAFT
International
Standard
ISO/TC 147/SC 6
Water quality — Sampling —
Secretariat: BSI
Part 15:
Voting begins on:
Preservation and handling of
samples of sludge, sediment and
Voting terminates on:
suspended matter
Qualité de l’eau — Échantillonnage —
Partie 15: Conservation et traitement des échantillons de boues,
de sédiments et de matières en suspension
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
WITH THEIR COMMENTS, NOTIFICATION OF ANY
RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE
AND TO PROVIDE SUPPOR TING DOCUMENTATION.
© ISO 2026
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
ISO/CEN PARALLEL PROCESSING
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
or ISO’s member body in the country of the requester.
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland Reference number
ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 3
4.1 Plastics .3
4.2 Analytical chemistry techniques .3
5 Sampling and chain of custody . 4
6 Reagents . 4
7 Sample handling and preservation . 5
7.1 General .5
7.2 Sample handling and preservation for chemical analysis .5
7.3 Sample handling and preservation for physical analysis .6
7.4 Sample handling and preservation for radiochemical analysis .6
7.5 Sample handling and preservation for hydrobiological analysis .6
7.6 Sample handling and preservation for microbiological analysis .6
8 Safety precautions. 7
8.1 Staff protection .7
8.2 Sample protection.7
9 Containers . 7
10 Sample collection . 7
11 Identification of samples . 8
12 Sample transport . 8
13 Sample reception . 9
14 Sample storage . 9
Annex A (informative) Techniques for sample preservation .11
Annex B (informative) Container preparation .26
Annex C (informative) Long term storage of wet sediment samples using nitrogen vapour
freezes .28
Bibliography .30
iii
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out through
ISO technical committees. Each member body interested in a subject for which a technical committee
has been established has the right to be represented on that committee. International organizations,
governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely
with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO's adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 6,
Sampling (general methods), in collaboration with the European Committee for Standardization (CEN)
Technical Committee CEN/TC 308, Characterization and management of sludge,in accordance with the
Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
This third edition cancels and replaces the second edition (ISO 5667-15:2009), which has been technically
revised.
The main changes are as follows:
— ‘suspended matter’ has been added to the title and ‘guidance’ has been deleted from the title;
— ISO/TS 5667-25 has been added as an informative reference;
— a flow diagram for preservation and storage of samples of sludge, sediment and suspended matter has
been added (in line with ISO 5667-3);
— terms and definitions have been aligned with ISO 5667-3;
— tables from Clause 12 have been moved to Annex A;
— references in the previous Tables 1 to 3 have been added;
— the previous Table 3 has been split into Table A.3 ‘Hydrobiological analysis’ and Table A.4 ‘Microbiological
analysis’.
A list of all parts in the ISO 5667 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
Introduction
[1]
This document is intended to be used in conjunction with ISO 5667-1 , which deals with the design
of sampling programmes and sampling techniques.
Where possible, this document has been aligned with current standards. Where new research or validation
results have provided new insights, the latest knowledge has been used.
[6]
Guidance on validation protocols can be found in ISO/TS 5667-25 .
Tables A.1 to A.4 provide the validated preservation times or conditions as well as the descriptions of best
practice. Tables A.1 to A.4 also refer, for each parameter, to references available at the time of publication of
this document (i.e. ISO 5667-15:2026). This is however not an exhaustive list. Other preservation methods
may be used when they have been validated. However, it is strongly recommended that, where a method
validation is not available, the preservation times for the analyte listed in Tables A.1 to A.4 for ISO and CEN
test methods be followed. In case more than one storage time is provided in Tables A.1 to A.4, the order of
preferred use is:
— validated method;
— method provided by reference;
— best practice.
The preservation and storage conditions and maximum storage times per parameter as listed in Tables A.1
to A.4 should be regarded as default conditions to be applied in the absence of any other information.
However, if validation of preservation techniques and holding times has been carried out, relative to specific
circumstances and matrices, by a laboratory, then, provided that it can produce evidence of this validation
where they differ from those set out in Tables A.1 to A.4, these validated preservation and storage conditions
and maximum storage times are deemed acceptable for use by the validating laboratories. A national
standard can contain information on preservation.
NOTE Samples of sludge, sediment and suspended matter that are dried or freeze-dried behave similarly to dried
[39]
soils. For guidance on freeze-drying, see ISO 16720 .
This document and the related analytical references can be used as presented in Figure 1.
v
WARNING — ‘Method provided by reference’ and ‘validated method’ can be based on previous standards
[6]
and methods and therefore not be in line with ISO/TS 5667-25 . This information can be interpreted
by a qualified and experienced person.
Figure 1 — Flow diagram for the selection of a method for the preservation
and storage of samples of sludge, sediment and suspended matter
[6]
Attention is drawn to ISO/TS 5667-25 , which contains guidelines and the elaboration of the required
techniques of how to validate new storage times or preservative methods and details of the techniques
described.
vi
FINAL DRAFT International Standard ISO/FDIS 5667-15:2026(en)
Water quality — Sampling —
Part 15:
Preservation and handling of samples of sludge, sediment and
suspended matter
WARNING — Persons using this document should be familiar with normal laboratory practice. This
document does not purport to address all of the safety problems, if any, associated with its use. It is
the responsibility of the user to establish appropriate safety and health practices.
IMPORTANT — It is absolutely essential that tests conducted in accordance with this document be
carried out by suitably qualified staff.
1 Scope
This document specifies the general requirements on procedures for the preservation, handling and
storage of samples of sewage and waterworks sludge, suspended matter, marine sediments and freshwater
sediments for either chemical, physical, radiochemical, hydrobiological or microbiological examination, or
all, in the laboratory.
The procedures in this document are not applicable to dried samples of sludge, sediment and suspended
matter.
NOTE The storage conditions given do not necessarily apply for derived samples, e.g. sediment eluates or extracts.
This document is not applicable to samples intended for biotesting with ecotoxicological or biological assays
[5] [7]
(which is specified in ISO 5667-16 ) nor intended for microplastics (which is specified in ISO 5667-27 ).
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
best practice
method based upon consensus or general use and that can be referred to in literature
Note 1 to entry: Given the differences in conditions and circumstances as well as the impossibility to validate
all parameters from a validated method (3.10) or technique or process, a best practice method based upon the
corresponding properties of a validated parameter can be used.
[2]
[SOURCE: ISO 5667-3:2024, 3.1 ]
3.2
integrity
property of the parameter(s) of interest, information or content of a sample stored in a container that has
not been altered or lost in an unauthorized manner or that has been subject to loss of representativeness
[2]
[SOURCE: ISO 5667-3:2024, 3.2 ]
3.3
method provided by reference
procedure or technique for the preservation of samples taken from the reference to which it refers
Note 1 to entry: It is not in all cases clear whether the preservation procedure provided by the reference was validated
method (3.10), a best practice (3.1) or which procedure was used for its determination or validation. Where available,
the information about the matrices is taken over.
[2]
[SOURCE: ISO 5667-3:2024, 3.3 ]
3.4
sample preservation
procedure used to stabilize a sample in such a way that the properties under examination are maintained
stable from the collection step until preparation for analysis
Note 1 to entry: Different analytes can require several samples from the same source that are stabilized by different
procedures. More subsamples from one location can be needed as some parameters require a different preservation
procedure.
[10]
[SOURCE: ISO 11074:2025, 3.401, modified — Note 1 to entry has been added.]
3.5
sample storage
process and the result of keeping a sample available under predefined conditions, usually for a specified
time interval between collection and further treatment of a sample
Note 1 to entry: The specified time is the maximum time interval.
[10]
[SOURCE: ISO 11074:2025, 3.407, modified — Note 1 to entry has been added; “soil sample” has been
changed to “sample”.]
3.6
sediment
matter which settles to the bottom of a liquid, often transported in water before settlement occurs
Note 1 to entry: Sediment samples in this document are a part of water quality analysis. The liquid in this case
is therefore water.
[8]
[SOURCE: ISO 6107:2021, 3.505, modified — Note 1 to entry has been added.]
3.7
sludge
accumulated settled solids separated from various types of water as a result of natural or artificial processes
[48]
[SOURCE: ISO/DIS 23880:2025, 3.1.2 ]
3.8
storage time
period of time between filling of the sample container and further treatment of the sample in the laboratory,
if stored under predefined conditions
Note 1 to entry: Sampling finishes as soon as the sample container has been filled with the sample. Storage time ends
when the sample is taken by the analyst to start sample preparation prior to analysis.
Note 2 to entry: Further treatment is, for most analytes, a solvent extraction or acid destruction. Initial sample
preparation steps may be considered as an extension of the storage conditions for maintaining analyte stability.
[2]
[SOURCE: ISO 5667-3:2024, 3.6, modified — Note 2 to entry has been adjusted.]
3.9
suspended matter
solids remaining in suspension in water which can be removed by sedimentation, filtration or centrifugation
[8]
[SOURCE: ISO 6107:2021, 3.554 ]
3.10
validated method
method for which the validity of correctness has been checked by verification or qualification against
a number of predefined requirements
Note 1 to entry: A validated method indicates that a preservation method is capable of delivering the intended results
with an acceptable degree of uncertainty for the parameter or group of parameters and sample type.
[2]
[SOURCE: ISO 5667-3:2024, 3.7 ]
4 Abbreviated terms
4.1 Plastics
FEP perfluoro(ethylene/propylene)
PE polyethylene
PE-HD high density polyethylene
PET polyethylene terephthalate
PFA perfluoroalkoxy (polymer)
PP polypropylene
PTFE polytetrafluoroethylene
PVC poly(vinyl chloride)
4.2 Analytical chemistry techniques
AAS atomic absorption spectroscopy
AFS atomic fluorescence spectroscopy
AMP amperometric method
CAL calometric method
CLM coulometric method
DIG digestion method
FRZ freeze-drying
GC-ECD gas chromatography - electron capture detector
GC-MS gas chromatography - mass spectrometry
GRA gravimetric method
IC ion chromatography
ICP-MS inductively coupled plasma - mass spectrometry
ICP-OES inductively coupled plasma - optical emission spectroscopy
LC liquid chromatography
LC-FD liquid chromatography - fluorometric detection
LC-MS liquid chromatography - mass spectrometry
LC-UV liquid chromatography - ultraviolet detection
MB microbiological method
MIC microscopy
POT potentiometry
SP spectroscopy
TIT titrimetric method
VAR various methods
VM visual method
5 Sampling and chain of custody
Before samples can be taken, a sampling programme shall be designed. Guidance on this topic is given in
[1]
ISO 5667-1 .
Depending on the sample type and matrix, instructions are given in the relevant part(s) of the ISO 5667 series.
The process of preservation and handling of samples consists of several steps. During this process, the
responsibility for the samples can change. To ensure the integrity of the samples, all steps involving the
sample shall be documented.
6 Reagents
WARNING — Sampling personnel should be warned of potential dangers and appropriate safety
procedures should be available. Beware of formaldehyde vapours. Do not store large numbers of
samples in small working areas.
All reagents and waters used shall be at least of analytical grade.
6.1 Deionized water.
6.2 Sodium sulfate (Na SO ).
2 4
Heat the sodium sulfate before use for at least 3 h at 500 °C. Store in a desiccator after heating.
6.3 Zinc acetate solution (CH COO) Zn·2H O (100 g/l).
3 2 2
Dissolve 10,0 g of zinc acetate dihydrate in approximately 90 ml of water. Dilute to 100 ml with water.
6.4 Methanol (CH OH).
6.5 Ethanol (C H OH), volume fraction of 96 %.
2 5
6.6 Formaldehyde solution (formalin; CH O), w(CH O) = 37 % (mass fraction) (freshly prepared).
2 2
WARNING — Beware of formaldehyde vapours. Do not store large numbers of samples in small
working areas.
6.7 Sodium tetraborate (Na B O ·10H O).
2 4 7 2
6.8 Hexamethylenetetramine [(CH ) N ].
2 6 4
6.9 Neutralized formaldehyde solution formaldehyde solution (6.6) neutralized with sodium
tetraborate (6.7) or hexamethylenetetramine (6.8).
Formalin solution at 100 g/l gives a final solution of w(CH O) = 3,7 % (mass fraction).
WARNING — Beware of formaldehyde vapours. Do not store large numbers of samples in small
working areas.
6.10 Glycerol (glycerin, glycerine), C H (OH) .
3 5 3
7 Sample handling and preservation
7.1 General
Sample handling is specific for each determination to be conducted. Manipulation of samples is often
required to yield consistent material for analysis. Homogenization, by mixing or sieving, dilution to obtain
a suitable concentration and addition of chemical preservatives all complicate interpretations of in situ
comparisons.
Any large individuals of macrofauna should be removed from the samples immediately after collecting
samples taken for either chemical, physical, radiochemical or biological examination, or all.
The purpose of preservation is to retain the integrity of the collected material as it was on site in relation
to the parameters to be analysed. Analytes can be subject to biotransformation, volatilization and chemical
transformation (e.g. oxidation, reduction, hydrolysis, photolysis) during storage. Therefore, careful
consideration should be given to these processes and the storage conditions needed to avoid such alterations.
The need to preserve sludge, sediment and suspended matter begins immediately after a sample has been
taken. The most critical changes to the sample can occur in the first few hours after sampling. Therefore,
where possible, preservation steps should be taken immediately upon sample collection.
The choice of preservation technique depends mainly on the objective of the sample collection and the
analysis being determined. It is important to understand the effects that preservation and storage can have
on the sample quality and the analysis results.
No other general recommendations can be given for a preservation or storage method. A preservation
method suitable for one group of parameters can interfere with the analysis of other groups of parameters.
To overcome this problem, a number of sub-samples should be collected; each sub-sample should be
preserved using a suitable method such that the specific demands of each analytical parameter are met.
Annex A provides techniques for sample preservation accompanied by the information in Tables A.1 to A.4.
7.2 Sample handling and preservation for chemical analysis
Chemical analysis can be performed to determine the nature and amounts of the substances that are
contained in the whole sample, dissolved in the aqueous phase and absorbed by sludge, sediment or
suspended matter.
Partition of chemical components between the solid phase and the water phase is influenced by several
factors, such as particle size, amount of organic matter, pH, redox potential and salinity. The study of such
attributes can be a sampling objective. Therefore, the preservation needs for the analytical methods to be
employed should be taken into account (see Table A.1). The guidance given in this document is relevant to
the determination of components in the sum of the separate phases of sludge, sediment or suspended matter,
unless otherwise indicated.
Preservation of samples by freezing can cause mobilization of contaminants by cellular disruption, whereas
not stabilizing samples can permit continued microbial transformation of critical parameters of interest. In
addition to biodegradation of organics, volatilization is a principal mechanism of loss of volatile compounds
during sample handling. Microbial activity can be responsible for changes in the nitrate-nitrite-ammonia
content, for decrease in biochemical oxygen demand or for reducing sulfate to sulfide. Anoxic samples
require appropriate preservation techniques such as oxygen exclusion during sample handling. Drying,
freezing and freeze-drying of anoxic samples alter the binding sites of, for example, heavy metals, making
more differentiated investigation of binding forms virtually impossible.
Details of the sample preservation are given in Table A.1.
7.3 Sample handling and preservation for physical analysis
The structure, texture and, for sediments, the layer formation should be determined.
NOTE Sediment matrix changes are obvious if rapid drainage of pore water occurs.
The importance of sludge, sediment or suspended matter integrity to the investigation objectives should be
evaluated as it can influence the preservation and handling techniques. In general, any disturbance of the
samples should be minimized. Where the physical structure of the material sampled is important for the
measurement of parameters (e.g. resistance to filtration), agitation and vibration during transport should
be reduced to a minimum. Freezing of the sludge, sediments or suspended matter should be avoided, but
can be appropriate. In some cases, thermal techniques can strongly modify sludge structure, thus affecting
physical characteristics (e.g. de-waterability, settleability, flowability).
Details of the sample preservation are given in Table A.1.
7.4 Sample handling and preservation for radiochemical analysis
Some sampling sites can have measurable radiochemical activity, e.g. in the soil or air. Some items of domestic
equipment within the laboratory can also be a source of radioactive material. Contamination of the sample
by its environment should therefore be avoided, especially if the sample activity is likely to be very low.
Details of the sample preservation are given in Table A.2.
7.5 Sample handling and preservation for hydrobiological analysis
Hydrobiological analysis generally involves classifying the species and numbers of either flora or fauna, or
both, present on and in fixed sludge or sediments.
Details of the sample preservation are given in Table A.3.
7.6 Sample handling and preservation for microbiological analysis
Microbial activity may also be used to characterize samples and can only be determined without fixation.
Details of the sample preservation are given in Table A.4.
8 Safety precautions
8.1 Staff protection
Health and safety precautions should be observed at all times when sampling potentially hazardous sludge,
sediments or suspended matter.
Human exposure to pathogenic organisms or pollutants should be avoided by using appropriate protective
equipment such as respiratory protective masks, safety glasses, safety boots and protective gloves.
The hazard due to pathogenic organisms in sludge can be very high. It is vital that all sampling personnel
should receive thorough training and be provided with appropriate medical inoculations.
Degradation of sludge produces methane, which presents a risk of fire and explosion if a source of ignition
is present. Containers should be appropriately packed to minimize the fragmentation of the containers if an
excessive pressure build-up of methane occurs.
If sludge samples are to be taken in locations where there is restricted ventilation, staff should take safety
precautions to protect themselves against sulfide, carbon dioxide and methane.
8.2 Sample protection
When sampling, transporting and utilizing sludge, care should be taken to prevent a build-up of gas pressure
in the sample container. Manual release of pressure during and after transport can be necessary if prolonged
storage is required.
Samples collected for the analysis of volatile organic or sulfide compounds should not be homogenized
because many of these compounds can be lost while compositing.
9 Containers
Sample containers should be made of a material appropriate for preserving the natural properties of both
the sample and the expected range of contaminants. Suitable types of containers for each analyte to be
measured are given in Annex A.
[1]
The choice of sample container is of major importance and ISO 5667-1 provides guidance on this subject.
Although certain container materials are generally favourable for certain analytes, the use of other materials
can be technically correct.
The applicability of the specific sample containers should be verified for contaminations and analyte loss
before usage with samples to avoid the loss of samples.
If the samples are to be frozen, suitable material such as PE, PP or PTFE should be used to minimize the risk
of breakage.
Careful consideration should also be given to the suitability of the container for cleaning or decontamination
or disposal and appropriate action taken. Recommendations for the preparation of containers are given in
Annex B.
[4]
In ISO 5667-14:2014, 11.3, guidance is given on measuring the contamination impact of the container. The
analyte level in the blank should be negligible compared to the analyte level to be measured in the sample.
NOTE Regular container volumes are suitable for samples of 500 g to 1 000 g.
10 Sample collection
Samples should be collected in sufficient volumes to allow:
a) separation of sub-samples to be preserved for each type of analysis or examination to be undertaken;
b) repetition of the analysis in the event of error checking or the routine quality control requirements
of duplicate analysis;
c) preparation of time-dependent composites; for example, a daily aliquot of sewage works sludge
(preserved as appropriate) may be retained to produce a composite for monthly analysis.
For sludge samples, the container should be filled completely as far as possible, especially if biological
activity is expected, in order to reduce the risk of overpressurization and explosion.
If analysis of volatile compounds is required, containers should be completely filled with sample from the
first grab, prior to sample homogenization. No headspace should remain in either container.
If the sample is to be frozen, enough headspace should be allowed for expansion to take place.
Where samples are collected for the purpose of microscopic examination (e.g. activated sludges), the
container should be filled to no more than 5 % of its capacity to ensure an oxygen supply to the sludge prior
to examination.
The temperature of the sample, especially of sludge samples, can influence the properties of the sample.
Therefore, the initial temperature of the sludge samples should be measured on site and recorded.
11 Identification of samples
Container labels should withstand wetting, drying and freezing without detaching or becoming illegible.
The labelling system shall be waterproof to allow use on site.
The exact information given in the sampling report and on the sample labels depends on the objectives of the
particular measurement programme. In all cases, an indelible label shall be secured to the sample container.
For each sample, at least the following information shall be available:
— identification of sampling personnel;
— a unique identifier, traceable to sample date, location and sample number shall appear on the label of the
sample container.
All other information is supplementary and should be detailed in the sampling report.
12 Sample transport
Cooling or freezing procedures shall be applied to samples to increase the time period available for transport
and storage (and if required, by Tables A.1 to A.4). When transport takes place, the sampling plan (e.g.
[1]
ISO 5667-1 ) shall consider:
— the time between sampling (end of filling the sample container intended for the laboratory) and start of
transport;
— the transport time;
— the time before further treatment in the laboratory.
The sum of these three periods is limited to the maximum storage times according to Tables A.1 to A.4.
If the maximum storage time cannot be met, then the sampling plan shall be reformulated to allow these
requirements to be accommodated.
[6]
In case the requirements cannot be met, instructions given in ISO/TS 5667-25 can be used to validate the
preservation time of specific water samples or sample types.
Containers holding samples shall be protected and sealed during transport in such a way that the samples
do not deteriorate or lose any part of their content. Container packaging shall protect the containers
from possible external contamination, particularly near the opening, and should not itself be a source of
contamination.
Glass containers shall be protected from potential breakage during transport by appropriate packaging.
Samples shall be transported as soon as possible after sampling and with cooling (if necessary, according to
Tables A.1 to A.4).
Laboratory samples for dispatch or transport by third parties and preserved laboratory samples should be
sealed in such manner that the integrity of the sample can be maintained.
During transportation to the laboratory, samples shall be stored in a cooling device capable of maintaining
a temperature of 5 °C ± 3 °C. Samples intended for radiochemical analysis can be placed under room
temperature. For proper evaluation of the conditions during transport, a device capable of recording the
(maximum) temperature of the air surrounding the sample can be used. The temperature sensor should
then be placed in a small container (e.g. 50 ml to 100 ml) filled with a fluid in order to avoid short time
fluctuations in temperature.
Cooling and freezing procedures applied shall be in line with instructions from the analytical laboratory.
Freezing especially requires detailed control of the freezing and thawing process in order to return
the sample to its initial equilibrium after thawing.
Samples should not be in direct contact with the ice packs.
NOTE 1 Devices capable of logging of the temperature during the transportation are available.
NOTE 2 For the transport of samples from the field to the laboratory, glycerol (6.10) is used for measuring
the temperature. The fluid can also be, for example, water.
13 Sample reception
All relevant information regarding the sample identification in accordance with Clause 11 and the sample
transport in accordance with Clause 12 shall be recorded.
The laboratory shall receive and check information on sample preservation and sample transport conditions.
If at least one of the conditions is not met, a disclaimer should be reported along with the results.
In all cases, and especially when a “chain of custody” process needs to be established, the number of sample
containers received in the laboratory and the integrity shall be verified against the number of sample
containers submitted.
14 Sample storage
The storage time of samples of sludge, sediment and suspended matter within the laboratory is specific to
the analyte(s) to be analysed. Samples should be stored no longer than the maximum storage times given in
Tables A.1 to A.4, with the exception of wet sediments that may be stored for longer periods when samples
are preserved using a nitrogen vapour freezer.
NOTE 1 For guidance on long-term storage of wet sediment samples using nitrogen vapour freezers, see Annex C.
[45]
NOTE 2 For further information on long- and short-term storage of dried samples, see ISO 18512 .
The refrigeration conditions within the laboratory shall be 3 °C ± 2 °C. Samples for microbiological analysis
shall be stored at 5 °C ± 3 °C. The temperature of samples frozen for preservation shall be maintained below
–18 °C, unless otherwise specified. Exceptions to these refrigeration conditions are listed in Tables A.1 to
A.4.
When thawing frozen samples, each sample container should be placed in a separate secondary container to
minimize the risk of liquid loss, should a split become apparent during the thawing process or a rupture occur
during initial freezing and storage. A mild impact can cause splitting of some plastics at low temperatures.
With respect to thawing, this should be done under ambient conditions.
NOTE 3 The cooling conditions within the laboratory (1 °C to 5 °C) are different from the cooling conditions during
transport (2 °C to 8 °C).
Annex A
(informative)
Techniques for sample preservation
A.1 General
This document and the analytical International Standards listed in this annex are complementary.
In some cases, the alternative preservation techniques listed contradict each other. It is intended that
where an existing analytical standard is used, the preservation technique described in that method applies.
However, alternative preservation techniques given in this document can also be appropriate. Where no
preservation method is described in the analytical International Standard, or no analytical International
Standard is used, the technique(s) listed in this document shall be used.
The information presented by line in each table comes from the international reference standard cited in the
first cell of the line and the source column (best practice, validated method, method provided by reference)
applies to the entire line.
[6]
A validation protocol used for validation studies can be found in ISO/TS 5667-25 .
A.2 Physicochemical and chemical analysis
The following general remarks should be noted in relation to the use of Table A.1.
— A preservation time of 1 d means that if 24 h is exceeded, this should be stated in the report.
— The types of containers are identical to those in the analytical International Standards. In some cases,
the type of container in the standard is very specific, e.g. PTFE. This can be essential when very low
concentrations of inorganic parameters have to be measured. In other cases, when the specific type of
plastic is not important, the term plastics is sufficient. Plastics used for containers in the laboratory are
for instance PE, PTFE, PET, PP, PFA and FEP.
A.3 Radiochemical analysis
The following general remarks should be noted in relation to the use of Table A.2.
WARNING — Radioprotection, such as shielding, can be necessary, depending on the activity
of the sample.
— Acidification is carried out to avoid algal growth, biological spoilage and adsorption of metal ions to the
inner wall of the sample container.
— Contamination of the sample should be avoided, especially if the sample activity is very low. Some
sample sites can have measurable activity in the soil of air, or in waters other than those being
sampled. Laboratories, as well as some items of domestic equipment, can contain radioactive material.
When sampling precipitation, any special requirements in Table A.2 are additional to those given in
[3]
ISO 5667-8 . As the collection of sufficient samples can require a period of days, both the starting and
finishing times and dates should be recorded. A record of precipitation collection for the sample station
for the appropriate period should be appended. A stabilizer or carrier may be added if appropriate for the
analytes being measured.
— Plastics used for containers in the laboratory are for instance PE, PTFE, PET, PP, PFA and FEP.
NOTE Depending of the plastic material some plastic bottles slowly concentrate samples over a period of many
months by being very slightly permeable to water.
A.4 Hydrobiological analysis
The following general remarks should be noted in relation to the use of Table A.3.
— Plastics used for containers in the laboratory are for instance PE, PTFE, PET, PP, PFA and FEP.
— If a preservation method is not specified, it is generally unimportant. The indication “1 month” represents
preservations without particular difficulty.
A.5 Microbiological analysis
The following general remark should be noted in relation to the use of Table A.4.
— Plastics used for containers in the laboratory are for instance PE, PTFE, PVC and PET.
...
ReResstrtriicctetedd
ISO/DISFDIS 5667-15:2025(en)
ISO/TC 147/SC 6
Secretariat: BSI
Date: 2026-02-10
Water quality — Sampling — —
Part 15:
Preservation and handling of samples of sludge, sediment and
suspended matter
Qualité de l’eau — Échantillonnage — —
Partie 15: Conservation et le traitement des échantillons de boues, de sédiments et de matières en
suspension
Third edition
Date: 2025-09-25
TTTTTThhhhhhiiiiiissssss dr dr dr dr dr draaaaaafffffftttttt i i i i i issssss s s s s s suuuuuubbbbbbmmmmmmiiiiiitttttttttttteeeeeed td td td td td toooooo a a a a a a p p p p p paaaaaarrrrrraaaaaalllllllllllleeeeeellllll v v v v vvooooootttttteeeeee i i i i i innnnnn I I I I I ISSSSSSO,O,O,O,O,O, C C C C C CEEEEEENN.N.N.N.N.
ReResstrtriicctetedd
FDIS stage
Restricted
ISO/DISFDIS 5667-15:20252026(en)
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication
may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying,
or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO
at the address below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: + 41 22 749 01 11
Email: E-mail: copyright@iso.org
Website: www.iso.org
Published in Switzerland
iii
Restricted
ISO #####-#:####(X/FDIS 5667-15:2026(en)
Contents
Foreword . v
Introduction . vii
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Abbreviated terms . 3
4.1 Plastics . 3
4.2 Analytical chemistry techniques . 3
5 Sampling and chain of custody . 4
6 Reagents . 4
7 Sample handling and preservation . 5
7.1 General . 5
7.2 Sample handling and preservation for chemical analysis . 6
7.3 Sample handling and preservation for physical analysis . 6
7.4 Sample handling and preservation for radiochemical analysis . 6
7.5 Sample handling and preservation for hydrobiological analysis . 6
7.6 Sample handling and preservation for microbiological analysis . 7
8 Safety precautions . 7
8.1 Staff protection . 7
8.2 Sample protection . 7
9 Containers . 7
10 Sample collection . 8
11 Identification of samples . 8
12 Sample transport . 8
13 Sample reception . 9
14 Sample storage . 10
Annex A (informative) Techniques for sample preservation . 11
Annex B (informative) Container preparation . 31
Annex C (informative) Long term storage of wet sediment samples using nitrogen vapour
freezes . 33
Bibliography . 35
© ISO #### 2026 – All rights reserved
iv
Restricted
ISO/DISFDIS 5667-15:20252026(en)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out through
ISO technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types of
ISO documents should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Field Code Changed
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent rights
in respect thereof. As of the date of publication of this document, ISO had not received notice of (a) patent(s)
which may be required to implement this document. However, implementers are cautioned that this may not
represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO's adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www.iso.org/iso/foreword.html.
Field Code Changed
This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 6,
Sampling (general methods). 6, Sampling (general methods), in collaboration with the European Committee for
Standardization (CEN) Technical Committee CEN/TC 308, Characterization and management of sludge,in
accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).
This third edition cancels and replaces the second edition (ISO 5667-15:2009), which has been technically
revised.
The main changes are as follows:
— — ‘suspended matter’ has been added to the title and ‘guidance’ has been deleted from the title;
— — ISO/TS 5667-25 has been added as an informative reference;
— — a flow diagram for preservation and storage of samples of sludge, sediment and suspended matter has
been added (in line with ISO 5667-3:2024);
— — terms and definitions have been aligned with ISO 5667-3:2024;
— — tables from Clause 12Clause 12 have been moved to Annex AAnnex A;;
— — references in the previous Tables 1 to 3 have been added;
— — the previous Table 3 has been split into Table A.3Table A.3 ‘Hydrobiological analysis’ and
Table A.4Table A.4 ‘Microbiological analysis’.
A list of all parts in the ISO 5667 series can be found on the ISO website.
v
Restricted
ISO #####-#:####(X/FDIS 5667-15:2026(en)
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
© ISO #### 2026 – All rights reserved
vi
Restricted
ISO/DISFDIS 5667-15:20252026(en)
Introduction
[1 [1] [1]]
This document is intended to be used in conjunction with ISO 5667-1 , , which deals with the design
of sampling programmes and sampling techniques.
Where possible, this document has been aligned with current standards. Where new research or validation
results have provided new insights, the latest knowledge has been used.
[6 [6][6] ]
Guidance on validation protocols can be found in ISO/TS 5667-25 . .
Tables A.1Tables A.1 to A.4A.4 provide the validated preservation times or conditions as well as the
descriptions of best practice. Tables A.1Tables A.1 to A.4A.4 also refer, for each parameter, to references
available at the time of publication of this document (i.e. ISO 5667-15:202x2026). This is however not an
exhaustive list. Other preservation methods may be used when they have been validated. However, it is
strongly recommended that, where a method validation is not available, the preservation times for the analyte
listed in Tables A.1Tables A.1 to A.4A.4 for ISO and CEN test methods be followed. In case more than one
storage time is provided in Tables A.1Tables A.1 to A.4A.4,, the order of preferred use is:
— — validated method;
— — method provided by reference;
— — best practice.
The preservation and storage conditions and maximum storage times per parameter as listed in
Tables A.1Tables A.1 to A.4A.4 should be regarded as default conditions to be applied in the absence of any
other information.
However, if validation of preservation techniques and holding times has been carried out, relative to specific
circumstances and matrices, by a laboratory, then, provided that it can produce evidence of this validation
where they differ from those set out in Tables A.1Tables A.1 to A.4A.4,, these validated preservation and
storage conditions and maximum storage times are deemed acceptable for use by the validating laboratories.
A national standard can contain information on preservation.
NOTE Samples of sludge, sediment and suspended matter that are dried or freeze-dried behave similarly to dried
[39 [39] [39] ]
soils. For guidance on freeze-drying, see ISO 16720 :2005 . .
This document and the related analytical references can be used as presented in Figure 1Figure 1.
vii
Restricted
ISO #####-#:####(X/FDIS 5667-15:2026(en)
© ISO #### 2026 – All rights reserved
viii
Restricted
ISO/DISFDIS 5667-15:20252026(en)
WARNING — ‘Method provided by reference’ and ‘validated method’ can be based on previous standards and methods and
[6 [6] [6]]
therefore not be in line with ISO/TS 5667-25 . . This information can be interpreted by a qualified and experienced
person.
Figure 1 — Flow diagram for the selection of a method for the preservation
and storage of samples of sludge, sediment and suspended matter
[6 [6] [6]]
Attention is drawn to ISO/TS 5667-25 , , which contains guidelines and the elaboration of the required
techniques of how to validate new storage times or preservative methods and details of the techniques
described.
ix
DRAFT International Standard ISO/DIS 5667-15:2025(en)
Restricted
Water quality — Sampling — —
Part 15:
Preservation and handling of samples of sludge, sediment and
suspended matter
WARNING — Persons using this document should be familiar with normal laboratory practice. This
document does not purport to address all of the safety problems, if any, associated with its use. It is
the responsibility of the user to establish appropriate safety and health practices.
IMPORTANT — It is absolutely essential that tests conducted in accordance with this document be
carried out by suitably qualified staff.
1 Scope
This document specifies the general requirements on procedures for the preservation, handling and storage
of samples of sewage and waterworks sludge, suspended matter, marine sediments and freshwater sediments
for either chemical, physical, radiochemical, hydrobiological or microbiological examination, or all, in the
laboratory.
The procedures in this document are not applicable to dried samples of sludge, sediment and suspended
matter.
NOTE The storage conditions given do not necessarily apply for derived samples, for examplee.g. sediment eluates
or extracts.
This document is not applicable to samples intended for biotesting with ecotoxicological or biological assays
[5 [5][5] ]
(which is specified in ISO 5667-16 ) ) nor intended for microplastics (which is specified in ISO 5667-
[7 [7][7] ]
27 ). ).
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— — ISO Online browsing platform: available at https://www.iso.org/obp
— — IEC Electropedia: available at https://www.electropedia.org/
3.1 3.1
best practice
method based upon consensus or general use and that can be referred to in literature
Note 1 to entry: Given the differences in conditions and circumstances as well as the impossibility to validate
all parameters from a validated method (3.10(3.10)) or technique or process, a best practice method based upon the
corresponding properties of a validated parameter can be used.
[2 [2][2] ]
[SOURCE: ISO 5667-3:2024, 3.1 ] ]
3.2 3.2
integrity
property of the parameter(s) of interest, information or content of a sample stored in a container that has not
been altered or lost in an unauthorized manner or that has been subject to loss of representativeness
[2 [2][2] ]
[SOURCE: ISO 5667-3:2024, 3.2 ] ]
3.3 3.3
method provided by reference
procedure or technique for the preservation of samples taken from the reference to which it refers
Note 1 to entry: It is not in all cases clear whether the preservation procedure provided by the reference was validated
method (3.10(3.10),), a best practice (3.1(3.1)) or which procedure was used for its determination or validation. Where
available, the information about the matrices is taken over.
[2 [2][2] ]
[SOURCE: ISO 5667-3:2024, 3.3 ] ]
3.4 3.4
sample preservation
procedure used to stabilize a sample in such a way that the properties under examination are maintained
stable from the collection step until preparation for analysis
Note 1 to entry: Different analytes can require several samples from the same source that are stabilized by different
procedures. More subsamples from one location can be needed as some parameters require a different preservation
procedure.
[10 [10][10] ]
[SOURCE: ISO 11074:2025, 3.401, , modified — Note 1 to entry has been added.]
3.5 3.5
sample storage
process and the result of keeping a sample available under predefined conditions, usually for a specified time
interval between collection and further treatment of a sample
Note 1 to entry: The specified time is the maximum time interval.
[10 [10][10] ]
[SOURCE: ISO 11074:2025, 3.407, , modified — Note 1 to entry has been added; “soil sample” has been
changed to “sample”.]
3.6 3.6
sediment
matter which settles to the bottom of a liquid, often transported in water before settlement occurs
Note 1 to entry: Sediment samples in this document are a part of water quality analysis. The liquid in this case is therefore
water.
[8 [8][8] ]
[SOURCE: ISO 6107:2021, 3.505, , modified — Note 1 to entry has been added.]
3.7 3.7
sludge
accumulated settled solids separated from various types of water as a result of natural or artificial processes
© ISO #### 2026 – All rights reserved
Restricted
ISO/DISFDIS 5667-15:20252026(en)
[48 [48][48] ]
[SOURCE: ISO/DIS 23880:2025, 3.1.2 ] ]
3.8 3.8
storage time
period of time between filling of the sample container and further treatment of the sample in the laboratory,
if stored under predefined conditions
Note 1 to entry: Sampling finishes as soon as the sample container has been filled with the sample. Storage time ends
when the sample is taken by the analyst to start sample preparation prior to analysis.
Note 2 to entry: Further treatment is, for most analytes, a solvent extraction or acid destruction. Initial sample
preparation steps may be considered as an extension of the storage conditions for maintaining analyte stability.
[2 [2][2] ]
[SOURCE: ISO 5667-3:2024, 3.6, , modified — Note 2 to entry has been adjusted.]
3.9 3.9
suspended matter
solids remaining in suspension in water which can be removed by sedimentation, filtration or centrifugation
[8 [8][8] ]
[SOURCE: ISO 6107:2021, 3.554 ] ]
3.10 3.10
validated method
method for which the validity of correctness has been checked by verification or qualification against
a number of predefined requirements
Note 1 to entry: A validated method indicates that a preservation method is capable of delivering the intended results
with an acceptable degree of uncertainty for the parameter or group of parameters and sample type.
[2 [2][2] ]
[SOURCE: ISO 5667-3:2024, 3.7 ] ]
4 Abbreviated terms
4.1 Plastics
FEP perfluoro(ethylene/propylene)
PE polyethylene
PE-HD high density polyethylene
PET polyethylene terephthalate
PFA perfluoroalkoxy (polymer)
PP polypropylene
PTFE polytetrafluoroethylene
PVC poly(vinyl chloride)
4.2 Analytical chemistry techniques
AAS atomic absorption spectroscopy
AFS atomic fluorescence spectroscopy
AMP amperometric method
CAL calometric method
CLM coulometric method
DIG digestion method
FRZ freeze-drying
GC-ECD gas chromatography - electron capture detector
GC-MS gas chromatography - mass spectrometry
GRA gravimetric method
IC ion chromatography
ICP-MS inductively coupled plasma - mass spectrometry
ICP-OES inductively coupled plasma - optical emission spectroscopy
LC liquid chromatography
LC-FD liquid chromatography - fluorometric detection
LC-MS liquid chromatography - mass spectrometry
LC-UV liquid chromatography - ultraviolet detection
MB microbiological method
MIC microscopy
POT potentiometry
SP spectroscopy
TIT titrimetric method
VAR various methods
VM visual method
5 Sampling and chain of custody
Before samples can be taken, a sampling programme shall be designed. Guidance on this topic is given in ISO
[1 [1][1] ]
5667-1 . .
Depending on the sample type and matrix, instructions are given in the relevant part(s) of the ISO 5667 series.
The process of preservation and handling of samples consists of several steps. During this process, the
responsibility for the samples can change. To ensure the integrity of the samples, all steps involving the sample
shall be documented.
6 Reagents
WARNING — Sampling personnel should be warned of potential dangers and appropriate safety
procedures should be available. Beware of formaldehyde vapours. Do not store large numbers of
samples in small working areas.
All reagents and waters used shall be at least of analytical grade.
6.1 6.1 Deionized water.
6.2 6.2 Sodium sulfate (Na SO ).
2 4
Heat the sodium sulfate before use for at least 3 h at 500 °C. Store in a desiccator after heating.
© ISO #### 2026 – All rights reserved
Restricted
ISO/DISFDIS 5667-15:20252026(en)
6.3 6.3 Zinc acetate solution (CH3COO)2Zn·2H2O (100 g/l).
Dissolve 10,0 g of zinc acetate dihydrate in approximately 90 ml of water. Dilute to 100 ml with water.
6.4 6.4 Methanol (CH3OH).
6.5 6.5 Ethanol (C H OH), volume fraction of 96 %.
2 5
6.6 6.6 Formaldehyde solution (formalin; CH O), w(CH O) = 37 % (mass fraction) (freshly
2 2
prepared).
WARNING — Beware of formaldehyde vapours. Do not store large numbers of samples in small
working areas.
6.7 6.7 Sodium tetraborate (Na2B4O7·10H2O).
6.8 6.8 Hexamethylenetetramine [(CH ) N ].
2 6 4
6.9 6.9 Neutralized formaldehyde solution formaldehyde solution (6.6(6.6)) neutralized with
sodium tetraborate (6.7(6.7)) or hexamethylenetetramine (6.8(6.8).).
Formalin solution at 100 g/l gives a final solution of w(CH O) = 3,7 % (mass fraction).
WARNING — Beware of formaldehyde vapours. Do not store large numbers of samples in small
working areas.
6.10 6.10 Glycerol (glycerin, glycerine), C3H5(OH)3.
7 Sample handling and preservation
7.1 General
Sample handling is specific for each determination to be conducted. Manipulation of samples is often required
to yield consistent material for analysis. Homogenization, by mixing or sieving, dilution to obtain a suitable
concentration and addition of chemical preservatives all complicate interpretations of in situ comparisons.
Any large individuals of macrofauna should be removed from the samples immediately after collecting
samples taken for either chemical, physical, radiochemical or biological examination, or all.
The purpose of preservation is to retain the integrity of the collected material as it was on site in relation to
the parameters to be analyzedanalysed. Analytes can be subject to biotransformation, volatilization and
chemical transformation (e.g. oxidation, reduction, hydrolysis, photolysis) during storage. Therefore, careful
consideration should be given to these processes and the storage conditions needed to avoid such alterations.
The need to preserve sludge, sediment and suspended matter begins immediately after a sample has been
taken. The most critical changes to the sample can occur in the first few hours after sampling. Therefore, where
possible, preservation steps should be taken immediately upon sample collection.
The choice of preservation technique depends mainly on the objective of the sample collection and the analysis
being determined. It is important to understand the effects that preservation and storage can have on the
sample quality and the analysis results.
No other general recommendations can be given for a preservation or storage method. A preservation method
suitable for one group of parameters can interfere with the analysis of other groups of parameters. To
overcome this problem, a number of sub-samples should be collected; each sub-sample should be preserved
using a suitable method such that the specific demands of each analytical parameter are met.
Annex AAnnex A provides techniques for sample preservation accompanied by the information in
Tables A.1Tables A.1 to A.4A.4. .
7.2 Sample handling and preservation for chemical analysis
Chemical analysis can be performed to determine the nature and amounts of the substances that are contained
in the whole sample, dissolved in the aqueous phase and absorbed by sludge, sediment or suspended matter.
Partition of chemical components between the solid phase and the water phase is influenced by several
factors, such as particle size, amount of organic matter, pH, redox potential and salinity. The study of such
attributes can be a sampling objective. Therefore, the preservation needs for the analytical methods to be
employed should be taken into account (see Table A.1Table A.1).). The guidance given in this document is
relevant to the determination of components in the sum of the separate phases of sludge, sediment or
suspended matter, unless otherwise indicated.
Preservation of samples by freezing can cause mobilization of contaminants by cellular disruption, whereas
not stabilizing samples can permit continued microbial transformation of critical parameters of interest. In
addition to biodegradation of organics, volatilization is a principal mechanism of loss of volatile compounds
during sample handling. Microbial activity can be responsible for changes in the nitrate-nitrite-ammonia
content, for decrease in biochemical oxygen demand or for reducing sulfate to sulfide. Anoxic samples require
appropriate preservation techniques such as oxygen exclusion during sample handling. Drying, freezing and
freeze-drying of anoxic samples alter the binding sites of, for example, heavy metals, making more
differentiated investigation of binding forms virtually impossible.
Details of the sample preservation are given in Table A.1Table A.1.
7.3 Sample handling and preservation for physical analysis
The structure, texture and, for sediments, the layer formation should be determined.
NOTE Sediment matrix changes are obvious if rapid drainage of pore water occurs.
The importance of sludge, sediment or suspended matter integrity to the investigation objectives should be
evaluated as it can influence the preservation and handling techniques. In general, any disturbance of the
samples should be minimized. Where the physical structure of the material sampled is important for the
measurement of parameters (e.g. resistance to filtration), agitation and vibration during transport should be
reduced to a minimum. Freezing of the sludge, sediments or suspended matter should be avoided, but can be
appropriate. In some cases, thermal techniques can strongly modify sludge structure, thus affecting physical
characteristics (e.g. de-waterability, settleability, flowability).
Details of the sample preservation are given in Table A.1Table A.1.
7.4 Sample handling and preservation for radiochemical analysis
Some sampling sites can have measurable radiochemical activity, e.g. in the soil or air. Some items of domestic
equipment within the laboratory can also be a source of radioactive material. Contamination of the sample by
its environment should therefore be avoided, especially if the sample activity is likely to be very low.
Details of the sample preservation are given in Table A.2Table A.2.
7.5 Sample handling and preservation for hydrobiological analysis
Hydrobiological analysis generally involves classifying the species and numbers of either flora or fauna, or
both, present on and in fixed sludge or sediments.
Details of the sample preservation are given in Table A.3Table A.3.
© ISO #### 2026 – All rights reserved
Restricted
ISO/DISFDIS 5667-15:20252026(en)
7.6 Sample handling and preservation for microbiological analysis
Microbial activity may also be used to characterize samples and can only be determined without fixation.
Details of the sample preservation are given in Table A.4Table A.4.
8 Safety precautions
8.1 Staff protection
Health and safety precautions should be observed at all times when sampling potentially hazardous sludge,
sediments or suspended matter.
Human exposure to pathogenic organisms or pollutants should be avoided by using appropriate protective
equipment such as respiratory protective masks, safety glasses, safety boots and protective gloves. The hazard
due to pathogenic organisms in sludge can be very high. It is vital that all sampling personnel should receive
thorough training and be provided with appropriate medical inoculations.
Degradation of sludge produces methane, which presents a risk of fire and explosion if a source of ignition is
present. Containers should be appropriately packed to minimize the fragmentation of the containers if an
excessive pressure build-up of methane occurs.
If sludge samples are to be taken in locations where there is restricted ventilation, staff should take safety
precautions to protect themselves against sulfide, carbon dioxide and methane.
8.2 Sample protection
When sampling, transporting and utilizing sludge, care should be taken to prevent a build-up of gas pressure
in the sample container. Manual release of pressure during and after transport can be necessary if prolonged
storage is required.
Samples collected for the analysis of volatile organic or sulfide compounds should not be homogenized
because many of these compounds can be lost while compositing.
9 Containers
Sample containers should be made of a material appropriate for preserving the natural properties of both the
sample and the expected range of contaminants. Suitable types of containers for each analyte to be measured
are given in Annex AAnnex A.
[1 [1][1]]
The choice of sample container is of major importance and ISO 5667-1 provides guidance on this subject.
Although certain container materials are generally favourable for certain analytes, the use of other materials
can be technically correct.
The applicability of the specific sample containers should be verified for contaminations and analyte loss
before usage with samples to avoid the loss of samples.
If the samples are to be frozen, suitable material such as PE, PP or PTFE should be used to minimize the risk
of breakage.
Careful consideration should also be given to the suitability of the container for cleaning or decontamination
or disposal and appropriate action taken. Recommendations for the preparation of containers are given in
Annex BAnnex B.
[4 [4][4] ]
In ISO 5667-14:2014, 11.3, , guidance is given on measuring the contamination impact of the container.
The analyte level in the blank should be negligible compared to the analyte level to be measured in the sample.
NOTE Regular container volumes are suitable for samples of 500 g to 1 000 g.
10 Sample collection
Samples should be collected in sufficient volumes to allow:
a) a) separation of sub-samples to be preserved for each type of analysis or examination to be
undertaken;
b) b) repetition of the analysis in the event of error checking or the routine quality control
requirements of duplicate analysis;
c) c) preparation of time-dependent composites; for example, a daily aliquot of sewage works
sludge (preserved as appropriate) may be retained to produce a composite for monthly analysis.
For sludge samples, the container should be filled completely as far as possible, especially if biological activity
is expected, in order to reduce the risk of overpressurization and explosion.
If analysis of volatile compounds is required, containers should be completely filled with sample from the first
grab, prior to sample homogenization. No headspace should remain in either container.
If the sample is to be frozen, enough headspace should be allowed for expansion to take place.
Where samples are collected for the purpose of microscopic examination (e.g. activated sludges), the container
should be filled to no more than 5 % of its capacity to ensure an oxygen supply to the sludge prior to
examination.
The temperature of the sample, especially of sludge samples, can influence the properties of the sample.
Therefore, the initial temperature of the sludge samples should be measured on site and recorded.
11 Identification of samples
Container labels should withstand wetting, drying and freezing without detaching or becoming illegible. The
labelling system shall be waterproof to allow use on site.
The exact information given in the sampling report and on the sample labels depends on the objectives of the
particular measurement programme. In all cases, an indelible label shall be secured to the sample container.
For each sample, at least the following information shall be available:
— — identification of sampling personnel;
— — a unique identifier, traceable to sample date, location and sample number shall appear on the label of
the sample container.
All other information is supplementary and should be detailed in the sampling report.
12 Sample transport
Cooling or freezing procedures shall be applied to samples to increase the time period available for transport
and storage (and if required, by Tables A.1Tables A.1 to A.4A.4).). When transport takes place, the sampling
[1 [1][1] ]
plan (e.g. ISO 5667-1 ) ) shall consider:
© ISO #### 2026 – All rights reserved
Restricted
ISO/DISFDIS 5667-15:20252026(en)
— — the time between sampling (end of filling the sample container intended for the laboratory)
and start of transport;
— — the transport time;
— — the time before further treatment in the laboratory.
The sum of these three periods is limited to the maximum storage times according to Tables A.1Tables A.1 to
A.4A.4.
If the maximum storage time cannot be met, then the sampling plan shall be reformulated to allow these
requirements to be accommodated.
[6 [6][6]]
In case the requirements cannot be met, instructions given in ISO/TS 5667-25 can be used to validate
the preservation time of specific water samples or sample types.
Containers holding samples shall be protected and sealed during transport in such a way that the samples do
not deteriorate or lose any part of their content. Container packaging shall protect the containers from
possible external contamination, particularly near the opening, and should not itself be a source of
contamination.
Glass containers shall be protected from potential breakage during transport by appropriate packaging.
Samples shall be transported as soon as possible after sampling and with cooling (if necessary, according to
Tables A.1Tables A.1 to A.4A.4).).
Laboratory samples for dispatch or transport by third parties and preserved laboratory samples should be
sealed in such manner that the integrity of the sample can be maintained.
During transportation to the laboratory, samples shall be stored in a cooling device capable of maintaining a
temperature of 5 °C ± 3 °C. Samples intended for radiochemical analysis can be placed under room
temperature. For proper evaluation of the conditions during transport, a device capable of recording the
(maximum) temperature of the air surrounding the sample can be used. The temperature sensor should then
be placed in a small container (e.g. 50 ml to 100 ml) filled with a fluid in order to avoid short time fluctuations
in temperature.
Cooling and freezing procedures applied shall be in line with instructions from the analytical laboratory.
Freezing especially requires detailed control of the freezing and thawing process in order to return the sample
to its initial equilibrium after thawing.
Samples should not be in direct contact with the ice packs.
NOTE 1 Devices capable of logging of the temperature during the transportation are available.
NOTE 2 For the transport of samples from the field to the laboratory, glycerol (6.10(6.1.10)) is used for measuring
the temperature. The fluid can also be, for example, water.
13 Sample reception
All relevant information regarding the sample identification in accordance with Clause 11Clause 11 and the
sample transport in accordance with Clause 12Clause 12 shall be recorded.
The laboratory shall receive and check information on sample preservation and sample transport conditions.
If at least one of the conditions is not met, a disclaimer should be reported along with the results.
In all cases, and especially when a “chain of custody” process needs to be established, the number of sample
containers received in the laboratory and the integrity shall be verified against the number of sample
containers submitted.
14 Sample storage
The storage time of samples of sludge, sediment and suspended matter within the laboratory is specific to the
analyte(s) to be analyzedanalysed. Samples should be stored no longer than the maximum storage times given
in Tables A.1Tables A.1 to A.4A.4,, with the exception of wet sediments that may be stored for longer periods
when samples are preserved using a nitrogen vapour freezer.
NOTE 1 For guidance on long-term storage of wet sediment samples using nitrogen vapour freezers, see
Annex CAnnex C.
[45 [45][45] ]
NOTE 2 For further information on long- and short-term storage of dried samples, see ISO 18512 . .
The refrigeration conditions within the laboratory shall be 3 °C ± 2 °C. Samples for microbiological analysis
shall be stored at 5 °C ± 3 °C. The temperature of samples frozen for preservation shall be maintained below
–18 °C, unless otherwise specified. Exceptions to these refrigeration conditions are listed in
Tables A.1Tables A.1 to A.4A.4.
When thawing frozen samples, each sample container should be placed in a separate secondary container to
minimize the risk of liquid loss, should a split become apparent during the thawing process or a rupture occur
during initial freezing and storage. A mild impact can cause splitting of some plastics at low temperatures.
With respect to thawing, this should be done under ambient conditions.
NOTE 3 The cooling conditions within the laboratory (1 °C to 5 °C) are different from the cooling conditions during
transport (2 °C to 8 °C).
© ISO #### 2026 – All rights reserved
Restricted
ISO/DISFDIS 5667-15:20252026(en)
Annex A
(informative)
Techniques for sample preservation
A.1 General
This document and the analytical International Standards listed in this annex are complementary.
In some cases, the alternative preservation techniques listed contradict each other. It is intended that where
an existing analytical standard is used, the preservation technique described in that method applies. However,
alternative preservation techniques given in this document can also be appropriate. Where no preservation
method is described in the analytical International Standard, or no analytical International Standard is used,
the technique(s) listed in this document shall be used.
The information presented by line in each table comes from the international reference standard cited in the
first cell of the line and the source column (best practice, validated method, method provided by reference)
applies to the entire line.
[6 [6][6] ]
A validation protocol used for validation studies can be found in ISO/TS 5667-25 . .
A.2 Physicochemical and chemical analysis
The following general remarks should be noted in relation to the use of Table A.1Table A.1.
— — A preservation time of 1 d means that if 24 h is exceeded, this should be stated in the report.
— — The types of containers are identical to those in the analytical International Standards. In some cases,
the type of container in the standard is very specific, e.g. PTFE. This can be essential when very low
concentrations of inorganic parameters have to be measured. In other cases, when the specific type of
plastic is not important, the term plastics is sufficient. Plastics used for containers in the laboratory are for
instance PE, PTFE, PET, PP, PFA and FEP.
A.3 Radiochemical analysis
The following general remarks should be noted in relation to the use of Table A.2Table A.2.
WARNING — Radioprotection, such as shielding, can be necessary, depending on the activity
of the sample.
— — Acidification is carried out to avoid algal growth, biological spoilage and adsorption of metal ions to
the inner wall of the sample container.
— — Contamination of the sample should be avoided, especially if the sample activity is very low. Some
sample sites can have measurable activity in the soil of air, or in waters other than those being sampled.
Laboratories, as well as some items of domestic equipment, can contain radioactive material. When
sampling precipitation, any special requirements in Table A.2Table A.2 are additional to those given in ISO
[3 [3] [3]]
5667-8 . . As the collection of sufficient samples can require a period of days, both the starting and
finishing times and dates should be recorded. A record of precipitation collection for the sample station
for the appropriate period should be appended. A stabilizer or carrier may be added if appropriate for the
analytes being measured.
— — Plastics used for containers in the laboratory are for instance PE, PTFE, PET, PP, PFA and FEP.
NOTE Depending of the plastic material some plastic bottles slowly concentrate samples over a period of many
months by being very slightly permeable to water.
A.4 Hydrobiological analysis
The following general remarks should be noted in relation to the use of Table A.3Table A.3.
— — Plastics used for containers in the laboratory are for instance PE, PTFE, PET, PP, PFA and FEP.
— — If a preservation method is not specified, it is generally unimportant. The indication “1 month”
represents preservations without particular difficulty.
A.5 Microbiological analysis
The following general remark should be noted in relation to the use of Table A.4Table A.4.
— — Plastics used for containers in the laboratory are for instance PE, PTFE, PVC and PET.
© ISO #### 2026 – All rights reserved
DRAFT International Standard ISO/DIS 5667-15:2025(en)
Restricted
Table A.1 — Techniques for sample preservation — Physicochemical and chemical analysis of organic and inorganic analytes
Preservation
Type of and storage
Maximum
Analyte or parameter Technique container conditions
b
Reference storage times Source Types
to be studied (see 4.24.2)) (see 4.14.1) additional to
b
times
a
) Clauses 7Clause
s 7 and 1414
Sediment, sludge,
Acidity and alkalinity ISO 5667-15 - P or G Dark and airtight 14 d Best practice
suspended matter
Ammonia ISO 5667-15 - P or G Dark and airtight 1 d Best practice Sludge
AnalyzeAnalyse as
Method provided
soon as possible
1 d Sludge
by reference
[16 [16] [16]] after sampling.
EN 14671 :2006
Not provided
VAR
No reference
If prolonged storage
by reference
to ISO 5667-15
is unavoidable, Method provided
28 d Sludge
then store the by reference
Ammonia (extractable)
sampl
...
PROJET
Norme
internationale
ISO/DIS 5667-15
ISO/TC 147/SC 6
Qualité de l’eau —
Secrétariat: BSI
Échantillonnage —
Début de vote:
Partie 15: 2025-07-09
Conservation et traitement des
Vote clos le:
2025-10-01
échantillons de boues, de sédiments
et de matières en suspension
Water quality — Sampling —
Part 15: Preservation and handling of samples of sludge,
sediment and suspended matter
ICS: 13.060.45; 13.030.20
CE DOCUMENT EST UN PROJET DIFFUSÉ
POUR OBSERVATIONS ET APPROBATION. IL
EST DONC SUSCEPTIBLE DE MODIFICATION
ET NE PEUT ÊTRE CITÉ COMME NORME
INTERNATIONALE AVANT SA PUBLICATION EN
TANT QUE TELLE.
Le présent document est distribué tel qu’il est parvenu du secrétariat
du comité. OUTRE LE FAIT D’ÊTRE EXAMINÉS POUR
ÉTABLIR S’ILS SONT ACCEPTABLES À DES
FINS INDUSTRIELLES, TECHNOLOGIQUES ET
COMMERCIALES, AINSI QUE DU POINT DE VUE
DES UTILISATEURS, LES PROJETS DE NORMES
INTERNATIONALES DOIVENT PARFOIS ÊTRE
TRAITEMENT PARALLÈLE ISO/CEN
CONSIDÉRÉS DU POINT DE VUE DE LEUR
POSSIBILITÉ DE DEVENIR DES NORMES
POUVANT SERVIR DE RÉFÉRENCE DANS LA
RÉGLEMENTATION NATIONALE.
LES DESTINATAIRES DU PRÉSENT PROJET
SONT INVITÉS À PRÉSENTER, AVEC LEURS
OBSERVATIONS, NOTIFICATION DES DROITS
DE PROPRIÉTÉ DONT ILS AURAIENT
ÉVENTUELLEMENT CONNAISSANCE
ET À FOURNIR UNE DOCUMENTATION
EXPLICATIVE.
Numéro de référence
ISO/DIS 5667-15:2025(fr)
ISO/DIS 5667-15:2025(fr)
ISO/TC 147/SC 6
Date : 2025-10-01
ISO/DIS 5667-15:2025(F)
ISO/TC 147/SC 6
Secrétariat : BSI
Qualité de l’eau — Échantillonnage — Partie 15 : Conservation et
traitement des échantillons de boues, de sédiments et de matières
en suspension
Water quality — Sampling — Part 15: Preservation and handling of samples of sludge, sediment and
suspended matter
Avertissement
Ce document n’est pas une Norme internationale de l’ISO. Il est distribué pour examen et observations.
Il est susceptible de modification sans préavis et ne peut être cité comme Norme internationale.
Les destinataires du présent projet sont invités à présenter, avec leurs observations, notification des
droits de propriété dont ils auraient éventuellement connaissance et à fournir une documentation
explicative.
ICS : 13.060.45 ; 13.030.20
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2025
Tous droits réservés. Sauf prescription différente ou nécessité dans le contexte de sa mise en œuvre, aucune partie de cette
publication ne peut être reproduite ni utilisée sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique,
y compris la photocopie, ou la diffusion sur l’internet ou sur un intranet, sans autorisation écrite préalable. Une autorisation peut
être demandée à l’ISO à l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
ISO copyright office
Case postale 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Genève
Tél.: +41 22 749 01 11
E-mail: copyright@iso.org Type du document : Norme internationale
Web: www.iso.org
Sous-type du document :
Publié en Suisse Stade du document : (40) Enquête
Langue du document : F
ii
ISO/DIS 5667-15:2025(F)
Sommaire Page
Avant-propos . iv
Introduction . vi
1 Domaine d’application .1
2 Références normatives .1
3 Termes et définitions .1
4 Abréviations relatives aux plastiques .3
5 Échantillonnage et chaîne de traçabilité .4
6 Réactifs .4
7 Manipulation et conservation des échantillons .5
7.1 Généralités .5
7.2 Manipulation et conservation pour l’analyse chimique .5
7.3 Manipulation et conservation pour l’analyse physique .6
7.4 Manipulation et conservation pour l’analyse radiochimique .6
7.5 Manipulation et conservation pour l’analyse hydrobiologique .6
7.6 Manipulation et conservation pour l’analyse microbiologique .6
8 Précautions de sécurité .7
8.1 Protection du personnel .7
8.2 Protection de l’échantillon .7
9 Récipients .7
10 Prélèvement de l’échantillon .8
11 Identification des échantillons .8
12 Transport des échantillons .9
13 Réception des échantillons . 10
14 Stockage des échantillons . 10
Annexe A (informative) Techniques de conservation des échantillons. 11
Annexe B (informative) Préparation des récipients . 29
Annexe C (informative) Stockage à long terme d’échantillons de sédiments humides à l’aide
de congélateurs à azote liquide . 31
Bibliographie . 33
iii
ISO/DIS 5667-15:2025(F)
Avant-propos
L’ISO (Organisation internationale de normalisation) est une fédération mondiale d’organismes
nationaux de normalisation (comités membres de l’ISO). L’élaboration des Normes internationales est
en général confiée aux comités techniques de l’ISO. Chaque comité membre intéressé par une étude a le
droit de faire partie du comité technique créé à cet effet. Les organisations internationales,
gouvernementales et non gouvernementales, en liaison avec l’ISO participent également aux travaux.
L’ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui
concerne la normalisation électrotechnique.
Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier de prendre note des différents
critères d’approbation requis pour les différents types de documents ISO. Le présent document a été
rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2
(voir www.iso.org/directives).
L’ISO attire l’attention sur le fait que la mise en application du présent document peut entraîner
l’utilisation d’un ou de plusieurs brevets. L’ISO ne prend pas position quant à la preuve, à la validité et à
l’applicabilité de tout droit de brevet revendiqué à cet égard. À la date de publication du présent
document, l’ISO n’avait pas reçu notification qu’un ou plusieurs brevets pouvaient être nécessaires à sa
mise en application. Toutefois, il y a lieu d’avertir les responsables de la mise en application du présent
document que des informations plus récentes sont susceptibles de figurer dans la base de données de
brevets, disponible à l’adresse www.iso.org/brevets. L’ISO ne saurait être tenue pour responsable de ne
pas avoir identifié de tels droits de propriété.
Les appellations commerciales éventuellement mentionnées dans le présent document sont données
pour information, par souci de commodité, à l’intention des utilisateurs et ne sauraient constituer un
engagement.
Pour une explication de la nature volontaire des normes, la signification des termes et expressions
spécifiques de l’ISO liés à l’évaluation de la conformité, ou pour toute information au sujet de l’adhésion
de l’ISO aux principes de l’Organisation mondiale du commerce (OMC) concernant les obstacles
techniques au commerce (OTC), voir www.iso.org/avant-propos.
Le présent document a été élaboré par le comité technique ISO/TC 147, Qualité de l’eau, sous-comité
SC 6, Échantillonnage (méthodes générales).
Cette troisième édition annule et remplace la deuxième édition (ISO 5667-15:2009), qui a fait l’objet
d’une révision technique.
Les principales modifications sont les suivantes :
— « matières en suspension » a été ajouté au titre et « lignes directrices » a été supprimé du titre ;
— l’ISO/TS 5667-25 a été ajoutée en tant que référence ;
— un logigramme pour la conservation et le stockage des échantillons de boues, de sédiments et de
matières en suspension a été ajouté (conformément à l’ISO 5667-3:2024) ;
iv
ISO/DIS 5667-15:2025(F)
— les termes et définitions ont été harmonisés par rapport à l’ISO 5667-3:2024 ;
— les tableaux de l’Article 12 ont été déplacés dans l’Annexe A ;
— des références dans les Tableaux 1 à 3 précédents ont été ajoutées ;
— le précédent Tableau 3 a été divisé en deux : Tableau A.3 « Analyse hydrobiologique » et
Tableau A.4 « Analyse microbiologique ».
Une liste de toutes les parties de la série ISO 5667 se trouve sur le site web de l’ISO.
Il convient que l’utilisateur adresse tout retour d’information ou toute question concernant le présent
document à l’organisme national de normalisation de son pays. Une liste exhaustive desdits organismes
se trouve à l’adresse www.iso.org/fr/members.html.
v
ISO/DIS 5667-15:2025(F)
Introduction
[1]
Le présent document est destiné à être utilisé conjointement avec l’ISO 5667-1, qui traite de la
conception des programmes d’échantillonnage et des techniques d’échantillonnage.
Le présent document a été aligné sur les normes actuelles lorsque cela était possible. Lorsque de
nouveaux résultats de recherche ou de validation ont ouvert de nouvelles perspectives,
les connaissances les plus récentes ont été utilisées.
Des recommandations relatives aux protocoles de validation peuvent être obtenues dans
[6]
l’ISO/TS 5667-25 .
Les Tableaux A.1 à A.4 fournissent des durées ou des conditions de conservation validées ainsi que des
descriptions de pratique recommandée. Les Tableaux A.1 à A.4 intègrent également, pour chaque
paramètre, des références disponibles à la date de publication du présent document (à savoir
l’ISO 5667-15:202x). Toutefois, il ne s’agit pas d’une liste exhaustive. D’autres méthodes de
conservation peuvent être utilisées si elles ont été validées. Par contre, pour une méthode dont les
données de validation ne sont pas disponibles, il est vivement conseillé de respecter les durées de
conservation des méthodes d’essai ISO et CEN correspondant à l’analyte qui sont répertoriées dans les
Tableaux A.1 à A.4. Si plusieurs durées de stockage sont indiquées dans les Tableaux A.1 à A.4,
l’ordre de préférence est le suivant :
— méthode validée ;
— méthode indiquée par une référence ;
— pratique recommandée.
Il convient d’envisager les conditions de conservation et de stockage et les durées maximales de
stockage répertoriées par paramètre dans les Tableaux A.1 à A.4 comme des conditions par défaut à
appliquer en l’absence d’autres informations.
Toutefois, l’utilisation de conditions de conservation et de stockage et de durées maximales de stockage
différentes de celles indiquées dans les Tableaux A.1 à A.4 est jugée acceptable, si le laboratoire qui les
utilise a soumis à validation et validé ces techniques de conservation et durées de stockage, par rapport
aux circonstances et matrices particulières, et qu’il peut en apporter la preuve. Une norme nationale
peut contenir des informations sur la conservation.
NOTE Les échantillons de boues, de sédiments et de matières en suspension séchés ou lyophilisés se
[37]
comportent comme des sols séchés. L’ISO 16720 fournit des recommandations relatives à la lyophilisation.
Le présent document et les références d’analyse connexes peuvent être utilisés tel que présenté à la
Figure 1.
vi
ISO/DIS 5667-15:2025(F)
AVERTISSEMENT — « Méthode indiquée par une référence » et « méthode validée » peuvent
faire référence à des normes et méthodes antérieures et par conséquent ne pas concorder avec
[6]
l’ISO/TS 5667-25 . Une personne qualifiée et expérimentée peut apprécier cette information.
Figure 1 — Logigramme concernant la sélection d’une méthode pour la conservation et
le stockage des échantillons de boues, sédiments et matières en suspension
[6]
L’attention est appelée sur le fait que l’ISO/TS 5667-25 , donne des lignes directrices sur la façon de
valider de nouvelles durées de stockage ou méthodes de conservation et décrit en détail les techniques
de validation.
vii
PROJET DE NORME INTERNATIONALE ISO/DIS 5667-15:2025(F)
Qualité de l’eau — Échantillonnage — Partie 15 :
Conservation et traitement des échantillons de boues,
de sédiments et de matières en suspension
AVERTISSEMENT — Il convient que les utilisateurs du présent document soient familiarisés avec
les pratiques courantes de laboratoire. Le présent document n’a pas pour but de traiter tous les
problèmes de sécurité qui sont, le cas échéant, liés à son utilisation. Il incombe à l’utilisateur
d’établir des pratiques appropriées en matière d’hygiène et de sécurité.
IMPORTANT — Il est absolument essentiel que les essais conduits conformément au présent
document soient exécutés par du personnel ayant reçu une formation adéquate.
1 Domaine d’application
La présente partie de l’ISO 5667 spécifie des exigences générales relatives aux modes opératoires de
conservation, de manipulation et de stockage des échantillons de boues provenant de stations
d’épuration et de stations de traitement de l’eau potable, de matières en suspension, de sédiments
marins et en eau douce pour examen chimique, physique, radiochimique et/ou biologique en
laboratoire.
Les modes opératoires fournis dans la présente partie de l’ISO 5667 s’appliquent uniquement aux
échantillons humides de boues, de sédiments et de matières en suspension.
NOTE Les conditions de stockage données ne s’appliquent pas nécessairement aux échantillons dérivés,
par exemple, les éluats ou les extraits de sédiments.
Le présent document ne s’applique pas aux échantillons destinés aux bioessais à l’aide d’essais
[5]
écotoxicologiques ou biologiques (qui sont spécifiés dans l’ISO 5667-16 ) ni aux microplastiques
[7]
(qui sont spécifiés dans l’ISO 5667-27 ).
2 Références normatives
Le présent document ne contient aucune référence normative.
3 Termes et définitions
Pour les besoins du présent document, les termes et définitions suivants s’appliquent.
L’ISO et l’IEC tiennent à jour des bases de données terminologiques destinées à être utilisées en
normalisation, consultables aux adresses suivantes :
— ISO Online browsing platform : disponible à l’adresse https://www.iso.org/obp
— IEC Electropedia : disponible à l’adresse https://www.electropedia.org/
ISO/DIS 5667-15:2025(F)
3.1
pratique recommandée
méthode fondée sur un consensus ou un usage général et qui peut être citée dans la littérature
Note 1 à l’article : Compte tenu des différences de conditions et de circonstances et compte tenu de l’impossibilité
de valider tous les paramètres d’une méthode, technique ou procédure validée (3.10), une méthode de pratique
recommandée sur la base des propriétés correspondantes d’un paramètre validé peut être utilisée.
[2]
[SOURCE : ISO 5667-3:2024 , 3.1.]
3.2
intégrité
état d’un échantillon stocké dans un récipient dont le ou les paramètres étudiés, les informations ou la
propriété n’ont pas été altérés ou perdus d’une manière non autorisée et qui est toujours représentatif
[2]
[SOURCE : ISO 5667-3:2024 , 3.2]
3.3
méthode indiquée par une référence
procédure ou technique de conservation d’échantillons issue de la référence à laquelle elle se rapporte
Note 1 à l’article : Il n’est pas toujours facile de savoir si la procédure de conservation indiquée par une référence
correspond à une méthode validée (3.10), s’il s’agit d’une pratique recommandée (3.1) ou de savoir quelle
procédure a été utilisée pour sa détermination ou sa validation. Les informations concernant la matrice,
si elles sont disponibles, prévalent.
[2]
[SOURCE : ISO 5667-3:2024 , 3.3]
3.4
conservation d’un échantillon
procédure visant à stabiliser un échantillon, c’est-à-dire à stabiliser les propriétés à étudier,
depuis l’étape du prélèvement jusqu’à celle de la préparation pour analyse
Note 1 à l’article : Différents analytes peuvent nécessiter plusieurs échantillons provenant de la même source qui
sont stabilisés par différentes procédures. Un plus grand nombre de sous-échantillons d’un même endroit peut
être nécessaire, car certains paramètres exigent un mode opératoire de conservation différent.
[10]
[SOURCE : ISO 11074:2025 , 3.401, modifié — La Note 1 à l’article a été ajoutée.]
3.5
stockage d’un échantillon
processus, et son résultat, consistant à garder un échantillon disponible dans des conditions
prédéfinies, en général pour un laps de temps déterminé, entre le prélèvement et le traitement de cet
échantillon
Note 1 à l’article : Le temps déterminé est le laps de temps maximal.
[10]
[SOURCE : ISO 11074:2025 , 3.407, modifié — La Note 1 à l’article a été ajoutée ; « échantillon de sol »
a été remplacé par « échantillon ».]
3.6
sédiment
matière qui se dépose au fond d’un liquide, souvent transportée dans l’eau avant décantation
Note 1 à l’article : Les échantillons de sédiments dans le présent document représentent une partie de l’analyse de
la qualité de l’eau. Dans ce contexte, le liquide est donc l’eau.
[8]
[SOURCE : ISO 6107:2021 , 3.505, modifié — La Note 1 à l’article a été ajoutée.]
ISO/DIS 5667-15:2025(F)
3.7
boue
mélange d’eau et de solides provenant de différents types d’eaux par des traitements naturels et artificiels
[43]
[SOURCE : ISO 19698:2020 , 3.23, modifié — Le terme « effluents de stations d’épuration » a été
remplacé par « boue » ; « eaux usées » a été remplacé par « eaux ».]
3.8
durée de stockage
période entre le remplissage du récipient et le traitement ultérieur de l’échantillon au laboratoire,
si l’échantillon est conservé dans des conditions prédéfinies
Note 1 à l’article : L’échantillonnage prend fin dès que le récipient a été rempli avec l’échantillon. La durée de
stockage prend fin lorsque l’échantillon est prélevé par l’analyste pour commencer la préparation de l’échantillon
avant l’analyse.
Note 2 à l’article : Pour la plupart des analytes, le traitement ultérieur est une extraction au solvant ou une
minéralisation à l’acide. Les étapes initiales de préparation de l’échantillon peuvent être des étapes
complémentaires aux conditions de stockage visant à stabiliser les concentrations en analytes.
[2]
[SOURCE : ISO 5667-3:2024 , 3.6]
3.9
matière en suspension
matière solide restant en suspension dans l’eau, qui peut être éliminée par sédimentation, filtration ou
centrifugation
[8]
[SOURCE : ISO 6107:2021 , 3.554]
3.10
méthode validée
méthode dont la validité ou la justesse a été vérifiée par vérification ou qualification vis-à-vis d’un
certain nombre d’exigences prédéfinies
Note 1 à l’article : Une méthode validée indique que la méthode de conservation est en mesure de délivrer les résultats
attendus avec un degré d’incertitude acceptable pour le paramètre ou le groupe de paramètres et le type d’eau.
[2]
[SOURCE : ISO 5667-3:2024 , 3.7]
4 Abréviations relatives aux plastiques
FEP perfluoro(éthylène/propylène)
PE polyéthylène
PE-HD polyéthylène haute densité
PET polyéthylène téréphtalate
PFA perfluoroalkoxy (polymère)
PP polypropylène
PTFE polytétrafluoroéthylène
PVC polychlorure de vinyle
ISO/DIS 5667-15:2025(F)
5 Échantillonnage et chaîne de traçabilité
Lorsqu’il est nécessaire de prélever des échantillons, cette opération est réalisée conformément à un
programme d’échantillonnage. La première étape consiste à concevoir un programme
[1]
d’échantillonnage. Des recommandations relatives à cet aspect sont données dans l’ISO 5667-1 .
Selon le type d’échantillon et la matrice, des instructions sont données dans la ou les parties concernées
de la série ISO 5667.
Le processus de conservation et de manipulation des échantillons comporte plusieurs étapes. Durant ce
processus, la responsabilité des échantillons peut changer. Pour assurer l’intégrité des échantillons,
toutes les étapes impliquant l’échantillon doivent être documentées.
6 Réactifs
AVERTISSEMENT — Il convient que le personnel réalisant l’échantillonnage soit averti des
dangers potentiels et que des procédures de sécurité appropriées soient disponibles.
Prendre garde aux vapeurs de formaldéhyde. Ne pas stocker un grand nombre d’échantillons
dans une petite zone de travail.
Tous les réactifs et eaux utilisés doivent être au minimum de qualité analytique.
6.1 Eau désionisée
6.2 Sulfate de sodium Na SO .
2 4
Chauffer le sulfate de sodium pendant au moins 3 h à 500 °C avant de l’utiliser. Stocker dans un
dessiccateur après le chauffage.
6.3 Solution d’acétate de zinc (CH COO) Zn·2H O (100 g/l).
3 2 2
Dissoudre 10,0 g d’acétate de zinc dihydraté dans approximativement 90 ml d’eau. Compléter avec de
l’eau jusqu’à 100 ml.
6.4 Méthanol CH OH.
6.5 Éthanol C H OH (96 % fraction volumique).
2 5
6.6 Solution de formaldéhyde (formol), CH O, φ(CH O) = 37 % (préparée extemporanément).
2 2
AVERTISSEMENT — Prendre garde aux vapeurs de formaldéhyde. Ne pas stocker un grand
nombre d’échantillons dans une petite zone de travail.
6.7 Tétraborate de sodium (Na B O ·10H O).
2 4 7 2
6.8 Hexaméthylène tétramine [(CH ) N ].
2 6 4
6.9 Solution de formaldéhyde neutralisé, solution de formaldéhyde (6.6) neutralisé au tétraborate
de sodium (6.7) ou à l’hexaméthylènetétramine (6.8).
Une solution de formol à 100 g/l donne une solution finale de φ(CH O) = 3,7 %.
AVERTISSEMENT — Prendre garde aux vapeurs de formaldéhyde. Ne pas stocker un grand
nombre d’échantillons dans une petite zone de travail.
ISO/DIS 5667-15:2025(F)
7 Manipulation et conservation des échantillons
7.1 Généralités
La manipulation des échantillons est spécifique selon les déterminations à réaliser. Elle est souvent
requise pour fournir un matériau cohérent en vue d’une analyse. L’homogénéisation, par mélange ou
tamisage, la dilution pour l’obtention d’une concentration appropriée et l’ajout de conservateurs
chimiques compliquent les interprétations des comparaisons in situ.
Il convient de retirer tous les grands individus de la macrofaune des échantillons immédiatement après
les prélèvements destinés aux examens chimique, physique, radiochimique et/ou biologique.
L’objectif de la conservation est de garder l’intégrité du matériau prélevé tel qu’il était sur site
par rapport aux paramètres à analyser. Les analytes peuvent être soumis à une biotransformation,
à une volatilisation et à une transformation chimique (par exemple oxydation, réduction, hydrolyse,
photolyse) pendant le stockage. Par conséquent, il convient qu’une attention particulière soit apportée à
ces processus et aux conditions de stockage nécessaires pour éviter toute altération.
Il est nécessaire de conserver les boues, les sédiments et les matières en suspension juste après le
prélèvement de l’échantillon. Les modifications les plus critiques de l’échantillon ont lieu pendant les
premières heures après l’échantillonnage. Par conséquent, dans la mesure du possible, il convient que
l’étape de conservation débute immédiatement après le prélèvement des échantillons.
Le choix de la technique de conservation dépend principalement de l’objectif du prélèvement et de
l’analyse à réaliser. Il est important de comprendre les effets de la conservation et du stockage sur la
qualité de l’échantillon et sur les résultats des analyses.
Aucune autre recommandation générale ne peut être fournie pour une méthode de conservation et de
stockage. Une méthode de conservation adaptée à un groupe de paramètres peut interférer avec les
analyses des autres groupes de paramètres. Pour surmonter ce problème, il convient de prélever un certain
nombre de sous-échantillons ; il convient de conserver chaque sous-échantillon à l’aide d’une méthode
adaptée de manière à ce que les impératifs spécifiques de chaque paramètre analytique soient satisfaits.
7.2 Manipulation et conservation pour l’analyse chimique
L’analyse chimique peut être réalisée pour déterminer la nature et la quantité des substances contenues
dans l’ensemble de l’échantillon, dissoutes en phase aqueuse et absorbées par les boues, les sédiments
ou les matières en suspension.
La répartition des composants chimiques entre la phase solide et la phase liquide dépend de plusieurs
facteurs, tels que la granulométrie, la quantité de matière organique, le pH, le potentiel redox et la
salinité. L’étude de ces paramètres peut faire l’objet d’un échantillonnage. Par conséquent, il convient de
prendre en considération la nécessité de conservation pour les méthodes d’analyse à utiliser
(voir le Tableau A.1). Les recommandations fournies dans la présente partie de l’ISO 5667 s’appliquent
à la détermination de composants pour l’ensemble des phases séparées de boues, de sédiments ou de
matières en suspension, sauf spécification contraire.
La conservation des échantillons par congélation peut provoquer la mobilisation des polluants par
perturbations cellulaires, tandis que la non-stabilisation des échantillons peut permettre la transformation
microbienne continue des paramètres critiques d’intérêt. Outre la biodégradation des éléments organiques,
la volatilisation est le mécanisme principal de perte de composés volatils pendant la manipulation des
échantillons. L’activité microbienne peut être responsable des modifications dans la teneur en nitrate,
en nitrites et en ammoniac, de la diminution de la demande biochimique en oxygène ou de la réduction du
sulfate en sulfure. Les échantillons anoxiques nécessitent des techniques de conservation appropriées
telles que l’isolement de l’oxygène pendant la manipulation. Le séchage, la congélation et la lyophilisation
des échantillons anoxiques altèrent les sites de liaison des métaux lourds, par exemple, et il est donc
quasiment impossible de réaliser une différenciation plus poussée des formes de liaison.
ISO/DIS 5667-15:2025(F)
Les informations détaillées relatives à la conservation des échantillons sont données dans le
Tableau A.1.
7.3 Manipulation et conservation pour l’analyse physique
Il convient de déterminer la structure et la texture, et pour les sédiments, la formation des strates.
NOTE Les modifications de la matrice du sédiment deviennent visibles lorsqu’un écoulement rapide de l’eau
interstitielle se produit.
Il convient d’évaluer l’importance de l’intégrité des boues, des sédiments ou des matières en suspension
pour les analyses, puisqu’elle peut avoir une influence sur les techniques de conservation et de
manipulation. En général, il convient de réduire le plus possible toute perturbation des échantillons.
Lorsque la structure physique du matériau échantillonné est importante pour le mesurage des
paramètres (par exemple la résistance à la filtration), il convient que l’agitation et la vibration pendant
le transport soient réduites au minimum. La congélation des boues, des sédiments ou des matières en
suspension peut être appropriée. Dans certains cas, il convient d’éviter les techniques thermiques,
car elles modifient considérablement la structure des boues, altérant ainsi ses caractéristiques
physiques (par exemple déshydratation, décantation ou fluidité).
Les informations détaillées relatives à la conservation des échantillons sont données dans le
Tableau A.1.
7.4 Manipulation et conservation pour l’analyse radiochimique
Certains sites de prélèvement peuvent avoir une activité radiochimique mesurable, par exemple dans le
sol ou dans l’air. Certains articles d’équipement domestique dans le laboratoire peuvent également
contenir de la matière radioactive. Par conséquent, il convient d’éviter la contamination de l’échantillon
par son environnement, en particulier si l’activité de l’échantillon semble être très faible.
Les informations détaillées relatives à la conservation des échantillons sont données dans le
Tableau A.2.
7.5 Manipulation et conservation pour l’analyse hydrobiologique
Une analyse hydrobiologique implique généralement la classification des espèces et l’énumération de la
flore et/ou de la faune présentes sur et dans les boues ou les sédiments fixes.
Les informations détaillées relatives à la conservation des échantillons sont données dans le
Tableau A.3.
7.6 Manipulation et conservation pour l’analyse microbiologique
L’activité microbienne peut également être utilisée pour la caractérisation des échantillons et peut
uniquement être déterminée sans fixation.
Les informations détaillées relatives à la conservation des échantillons sont données dans le
Tableau A.4.
ISO/DIS 5667-15:2025(F)
8 Précautions de sécurité
8.1 Protection du personnel
Il convient de toujours respecter les mesures de sécurité et d’hygiène lors de l’échantillonnage de
boues, de sédiments ou de matières en suspension potentiellement dangereux.
Il convient d’éviter toute exposition humaine à des organismes pathogènes ou à des contaminants à
l’aide d’un équipement de protection approprié, tel que des masques de protection respiratoire,
des lunettes de sécurité, des bottes de sécurité et des gants de protection. Les risques engendrés par les
organismes pathogènes présents dans les boues sont très importants. Il convient que tout le personnel
d’échantillonnage soit bien formé et soit vacciné.
La dégradation des boues produit du méthane, qui présente un risque d’incendie ou d’explosion en
présence d’une flamme. Il convient de bien envelopper les récipients de manière à réduire leur
fragmentation en cas d’accumulation excessive de pression due au méthane.
Lorsque des échantillons de boues doivent être prélevés sur des sites présentant une aération limitée,
il convient que le personnel respecte les mesures de sécurité en se protégeant du sulfure, du dioxyde de
carbone et du méthane.
8.2 Protection de l’échantillon
Lors de l’échantillonnage, du transport et de la manipulation des boues, il convient d’empêcher la
formation de pression gazeuse dans le récipient de l’échantillon. Si un stockage prolongé est requis,
une dépressurisation manuelle pendant et après le transport peut être nécessaire.
Il convient que les échantillons prélevés pour l’analyse de composés organiques volatils ou sulfurés ne
soient pas homogénéisés, car un grand nombre de ces composés peuvent être perdus pendant la
manipulation de l’échantillon.
9 Récipients
Il convient que les récipients pour échantillons soient fabriqués avec un matériau approprié afin de
conserver les propriétés naturelles de l’échantillon et de la gamme de contaminants prévue. Les types
de récipients adaptés à chaque analyte à mesurer sont indiqués dans les Tableaux A.1 à A.4.
[1]
Le choix du récipient est d’une importance capitale et l’ISO 5667-1 donne des recommandations à ce sujet.
Bien que certains matériaux de récipient soient généralement favorables à certains analytes,
l’utilisation d’autres matériaux peut être techniquement correcte.
Il convient de vérifier l’applicabilité des récipients d’échantillons spécifiques pour les contaminations et
la perte d’analyte avant utilisation avec les échantillons afin d’éviter la perte d’échantillons.
Lorsque les échantillons doivent être congelés, il convient d’utiliser un matériau tel que le polyéthylène
(PE), le polypropylène (PP) ou le polytétrafluoroéthylène (PTFE) pour réduire le plus possible tout
risque de rupture.
Il convient de faire attention à l’aptitude du récipient au nettoyage/à la décontamination ou il convient
de prendre les dispositions les plus appropriées. Les recommandations relatives à la préparation des
récipients sont données à l’Annexe B.
Des recommandations sur la mesure de l’impact de la contamination du récipient sont données dans le
[4]
paragraphe 11.3 de l’ISO 5667-14:2014, . Il convient que le niveau de concentration d’analyte dans le
blanc soit négligeable comparativement au niveau d’analyte à mesurer dans l’échantillon.
NOTE Les contenances des récipients généralement utilisés sont de 500 g à 1 000 g.
ISO/DIS 5667-15:2025(F)
10 Prélèvement de l’échantillon
Il convient de prélever des volumes d’échantillon suffisants afin de permettre :
a) la séparation des sous-échantillons à conserver pour chaque type d’analyse ou examen à réaliser ;
b) la répétition de l’analyse en vue de vérifier les éventuelles erreurs ou conformément aux exigences
de contrôle qualité de routine comme des analyses en double ;
c) la préparation des composés en fonction du temps ; par exemple, une aliquote quotidienne de
boues de stations d’épuration (conservée comme il convient) peut être gardée pour produire un
composé destiné à une analyse mensuelle.
Dans le cas des échantillons de boues, il est recommandé de remplir le récipient le plus possible,
en particulier si une activité biologique est supposée, afin de réduire les risques de surpression et
d’explosion.
Lorsqu’une analyse des composés volatils est requise, il convient de remplir complètement les
récipients avec l’échantillon provenant de la première benne, avant l’homogénéisation de l’échantillon.
Il convient que les récipients ne présentent aucun reste d’espace de tête.
Lorsque la congélation de l’échantillon est nécessaire, il convient de laisser assez d’espace de tête pour
la dilatation.
Lorsque les prélèvements sont destinés à l’examen microscopique des boues activées, par exemple,
il est recommandé de remplir le récipient à moins de 5 % de sa capacité pour assurer un
approvisionnement en oxygène aux boues avant examen.
La température de l’échantillon, en particulier les échantillons de boues, peut avoir une influence sur les
propriétés de l’échantillon. Par conséquent, il convient que la température initiale des échantillons de
boues soit mesurée sur site et enregistrée.
11 Identification des échantillons
Il convient que les étiquettes apposées sur les récipients résistent à l’humidité, au séchage et à la
réfrigération, sans se détacher ni devenir illisibles. Le système d’étiquetage doit être étanche pour
permettre son utilisation sur site.
Les informations exactes fournies dans le rapport d’échantillonnage et sur les étiquettes dépendent des
objectifs du programme de mesure concerné. Dans tous les cas, une étiquette indélébile doit être
apposée sur le récipient.
Pour chaque échantillon, les informations suivantes doivent au minimum être fournies :
— identification du personnel ayant réalisé le prélèvement ;
— un identifiant unique pouvant être relié à la date, au lieu de l’échantillonnage et au numéro de
l’échantillon doit figurer sur l’étiquette apposée sur le récipient.
Toutes les autres informations sont complémentaires, et il convient de les consigner dans le rapport
d’échantillonnage.
ISO/DIS 5667-15:2025(F)
12 Transport des échantillons
Les procédures de réfrigération ou de congélation doivent être appliquées aux échantillons
pour augmenter le temps disponible pour le transport et le stockage (et lorsque cela est exigé dans
les Tableaux A.1 à A.4). Lorsqu’un transport a lieu, la stratégie d’échantillonnage (par exemple
[1]
ISO 5667-1 ) doit tenir compte :
— du temps entre l’échantillonnage (fin du remplissage du récipient destiné au laboratoire) et le
début du transport ;
— de la durée du transport ;
— du laps de temps avant le traitement ultérieur au laboratoire.
La somme de ces trois périodes est limitée par les durées maximales de stockage conformément aux
Tableaux A.1 à A.4.
Si la durée maximale de stockage ne peut être tenue, la stratégie d’échantillonnage doit être reformulée
pour permettre de respecter ces exigences.
[6]
Si les exigences ne peuvent pas être respectées, les recommandations données dans l’ISO/TS 5667-25
peuvent être utilisées pour valider la durée de conservation des échantillons d’eau ou des types
d’échantillons donnés.
Les récipients contenant les échantillons doivent être protégés et bouchés de sorte que les échantillons
ne se détériorent pas ou qu’ils ne perdent aucun de leurs constituants durant le transport. L’emballage
des récipients doit les protéger contre toute contamination extérieure éventuelle, notamment près de
l’ouverture du récipient, et il convient qu’il ne soit pas lui-même une source de contamination.
Les récipients en verre doivent être protégés des risques de bris durant le transport au moyen d’un
emballage approprié. Les échantillons doivent être transportés le plus tôt possible après
l’échantillonnage et être réfrigérés (si cela est spécifié dans les Tableaux A.1 à A.4).
Il convient que les échantillons pour laboratoire destinés à être acheminés ou transportés par des
tierces parties, ainsi que les échantillons de laboratoire conservés, soient scellés de manière à pouvoir
préserver leur intégrité.
Pendant le transport jusqu’au laboratoire, les échantillons doivent être stockés dans un dispositif de
refroidissement capable de maintenir une température de 5 °C ± 3 °C. Les échantillons destinés à une
analyse radiochimique peuvent être placés à température ambiante. Pour une évaluation correcte des
conditions pendant le transport, un dispositif capable d’enregistrer la température (maximale) de l’air
entourant l’échantillon peut être utilisé. Il convient alors de positionner le capteur de température dans
un petit récipient (par exemple de 50 ml à 100 ml) rempli d’un fluide afin d’éviter de relever les brèves
fluctuations de température.
Les méthodes de réfrigération et de congélation appliquées doivent être conformes aux instructions
données par le laboratoire d’analyse. La congélation en particulier nécessite un contrôle détaillé des
modalités de congélation et de décongélation pour que l’échantillon retrouve son équilibre initial après
la décongélation.
Il convient que les échantillons ne soient pas en contact direct avec les blocs de glace.
NOTE 1 Des dispositifs capables d’enregistrer la température de l’air pendant le transport sont disponibles.
NOTE 2 Pour le transport d’échantillons du site jusqu’au laboratoire, le fluide conseillé pour mesurer la
température est le glycérol. Si les échantillons sont transportés au sein du site (par exemple, au sein d’un site
vaste), le fluide peut également être de l’eau, par exemple.
ISO/DIS 5667-15:2025(F)
13 Réception des échantillons
Toutes les informations pertinentes concernant l’identification de l’échantillon conformément à
l’Article 11 et le transport de l’échantillon conformément à l’Article 12 doivent être enregistrées.
Le laboratoire doit réceptionner et vérifier les informations relatives aux conditions de conservation et
de transport de l’échantillon. Si au moins une des conditions n’est pas remplie, il convient de consigner
une clause d’exonération de responsabilité avec les résultats.
Dans tous les cas, et particulièrement lorsqu’une traçabilité doit être établie, il doit être vérifié que le
nombre de récipients reçus au laboratoire correspond au nombre de flacons fournis pour chaque
échantillon, ainsi que leur intégrité.
14 Stockage des échantillons
La durée de stockage des échantillons de boues, de sédiments et de matières en suspension en
laboratoire dépend du ou des analytes à analyser. Il convient que les durées de stockage des
échantillons ne dépassent pas les durées maximales indiquées dans les Tableaux A.1 à A.4, excepté pour
les sédiments humides qui peuvent être stockés plus longuement lorsque les échantillons sont
conservés au moyen d’un congélateur à azote liquide.
NOTE 1 Pour des recommandations sur le stockage à long terme d’échantillons de sédiments humides au
moyen de congélateurs à azote liquide, voir l’Annexe C.
NOTE 2 Pour plus d’informations sur le stockage à long terme et à court terme d’échantillons séchés,
[41]
voir l’ISO 18512 .
Les conditions de réfrigération à l’intérieur du laboratoire doivent être de 3 °C ± 2 °C. Les échantillons
destinés à une analyse microbiologique doivent être conservés à 5 °C ± 3 °C. La température des
échantillons congelés en vue de leur conservation doit être maintenue à une température inférieure
à -18 °C, sauf spécification contraire. Les exceptions à ces conditions de réfrigération sont répertoriées
dans les Tableaux A.1 à A.5.
Pour décongeler les échantillons, il est recommandé de placer chaque récipient dans un contenant
secondaire distinct afin de réduire au minimum le risque de perte de liquide en cas de casse lors de la
décongélation, ou en cas de casse survenue au préalable lors de la congélation et du stockage initial,
qui peut se produire en cas d’impact léger pouvant provoquer une cassure de certains plastiques à
basse température. En ce qui concerne la décongélation, il est recommandé de le faire dans les
conditions ambiantes.
Il faut savoir que les conditions de refroidissement en laboratoire (1 °C – 5 °C) diffèrent de celles
présentes pendant le transport (2 °C – 8 °C).
ISO/DIS 5667-15:2025(F)
Annexe A
(informative)
Techniques de conservation des échantillons
A.1 Généralités
Le présent document et les Normes internationales d’analyse é
...
















Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.
Loading comments...