ISO 5667-15:1999

Water quality — Sampling — Part 15: Guidance on preservation and handling of sludge and sediment samples

Qualité de l'eau — Échantillonnage — Partie 15: Guide général pour la préservation et le traitement des échantillons de boues et de sédiments

Kakovost vode - Vzorčenje - 15. del: Navodilo za konzerviranje in ravnanje z blatom in vzorci sedimenta

General Information

• Status: Withdrawn
• Publication Date: 28-Jul-1999
• Withdrawal Date: 28-Jul-1999
• ICS: 13.060.30 - Sewage water
• ICS: 13.060.45 - Examination of water in general
• Technical Committee: ISO/TC 147/SC 6 - Sampling (general methods)
• Drafting Committee: ISO/TC 147/SC 6 - Sampling (general methods)
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 04-Aug-2009
• Ref Project: SIST ISO 5667-15:2001 - Water quality -- Sampling -- Part 15: Guidance on preservation and handling of sludge and sediment samples

Relations

• Revised: ISO 5667-15:2009 - Water quality — Sampling — Part 15: Guidance on the preservation and handling of sludge and sediment samples
• Effective Date: 15-Apr-2008

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 5667-15
First edition
1999-08-01
Water quality — Sampling —
Part 15:
Guidance on preservation and handling of
sludge and sediment samples
Qualité de l'eau — Échantillonnage —
Partie 15: Guide général pour la préservation et le traitement des
échantillons de boues et de sédiments
A
Reference number
ISO 5667-15:1999(E)

---------------------- Page: 1 ----------------------
ISO 5667-15:1999(E)
Contents
1 Scope .1
2 Normative reference .1
3 Sample storage, preservation and handling.1
3.1 General considerations.1
3.2 Chemical examination.1
3.3 Physical examination .2
3.4 Biological examination.2
3.5 Feasible precautions .2
3.6 Sample handling .3
3.7 Sample preservation.3
3.8 Sample storage .3
4 Sample record and quality assurance .4
Bibliography.7
©  ISO 1999
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic
or mechanical, including photocopying and microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet [e-mail]
Printed in Switzerland
ii

---------------------- Page: 2 ----------------------
© ISO
ISO 5667-15:1999(E)
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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
International Standard ISO 5667-15 was prepared by Technical Committee ISO/TC 147, Water quality,
Subcommittee SC 6, Sampling (general methods).
ISO 5667 consists of the following parts, under the general title Water quality — Sampling:
— Part 1: Guidance on the design of sampling programmes
— Part 2: Guidance on sampling techniques
— Part 3: Guidance on the preservation and handling of samples
— Part 4: Guidance on sampling from lakes
— Part 5: Guidance on sampling of drinking water
— Part 6: Guidance on sampling of rivers and streams
— Part 7: Guidance on sampling of water and steam in boiler plants
— Part 8: Guidance on sampling of wet deposition
— Part 9: Guidance on sampling from marine waters
— Part 10: Guidance on sampling of waste waters
— Part 11: Guidance on sampling of groundwaters
— Part 12: Guidance on sampling of bottom sediments
— Part 13: Guidance on sampling of water, wastewater and related sludges
— Part 14: Guidance on quality assurance of environmental water sampling and handling
— Part 15: Guidance on preservation and handling of sludge and sediment samples
— Part 16: Guidance on biotesting of samples
— Part 17: Guidance on sampling of suspended sediments
— Part 18: Guidance on sampling of groundwater on potentially contaminated sites
iii

---------------------- Page: 3 ----------------------
INTERNATIONAL STANDARD  © ISO ISO 5667-15:1999(E)
Water quality — Sampling —
Part 15:
Guidance on preservation and handling of sludge and sediment
samples
1 Scope
This part of ISO 5667 provides guidance on the procedures for preservation and handling of sewage and
waterworks sludges, suspended matter, and saltwater and freshwater sediments for subsequent analysis.
2 Normative reference
The following normative document contains provisions which, through reference in this text, constitute provisions of
this part of ISO 5667. For dated references, subsequent amendments to, or revisions of, any of these publications
do not apply. However, parties to agreements based on this part of ISO 5667 are encouraged to investigate the
possibility of applying the most recent edition of the normative documents indicated below. For undated references,
the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of
currently valid International Standards.
ISO 5667-3 :1994, Water quality — Sampling — Part 3: Guidance on the preservation and handling of samples.
3 Sample preservation and handling
3.1 General considerations
Storage begins when the samples are taken. All storage methods will affect the sample to some extent, and the
choice of preservation technique depends mainly on the objective of the sample collection. It is important that the
effects that preservation and storage techniques can have on sample quality and the results of analysis are
understood.
Sludge and sediment samples are subject to chemical, physical and biological changes as soon as they are
collected. If guidance is required on the type of sampling technique to be used, guidance is given in ISO 5667-12
and ISO 5667-13. Sample handling, preservation and storage shall be designed to minimize any changes in
composition of the sample by retarding chemical and/or biological activity and by avoiding contamination. Specific
preservation techniques are often necessary for a representative evaluation of the sludges and sediments, and a
variety of chemical, physical and biological investigations can be performed on the collected samples.
No single preservation method is applicable to all constituents. The objective of the sampling programme and the
nature of the analytical method will determine the handling operation or preservation technique.
3.2 Chemical examination
In this type of investigation, the nature and amounts of the substances which have become absorbed or adsorbed
by the sludges and sediments can be determined. Partition of chemicals between solid phase and water phase is
influenced by several factors, such as particle size, amount of organic matter, pH, redox potential or salinity. The
study of such attributes may be a sampling objective and therefore the preservation needs of the analytical methods
to be employed should be taken into account (see Table 1). The guidance given in this part of ISO 5667 is relevant
1

---------------------- Page: 4 ----------------------
© ISO
ISO 5667-15:1999(E)
to the determination of components in the sum of the separate phases of a sludge or sediment, unless otherwise
indicated. Preservation of samples by fast-freezing can cause mobilization of contaminants by cellular disruption,
whereas not stabilizing samples can permit continued microbial transformation of critical pollutants. In addition to
biodegradation of organics, volatilization is a principal mechanism of loss of volatile compounds during sample
handling.
Anoxic samples require appropriate preservation techniques such as oxygen exclusion during sample handling.
Where refrigeration is not available at the time of collection of liquid sludge samples, particularly in countries with
high ambient temperatures, preservation of the samples for sulfide determination can be achieved by raising the pH
to greater than 10,5. Analysis should still be carried out as soon as possible after collection. 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.
3.3 Physical examination
In this type of examination, the structure, texture and, for sediments, the layer formation, are determined. Sediment
fabric changes are obvious if rapid drainage of pore water occurs. The importance of sludge or sediment 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 sample integrity is important, agitation- and
vibration-free conditions should be maintained during transport; fast-freezing of the sludges and sediments may be
appropriate.
3.4 Biological examination
Biological studies include toxicological, ecotoxicological and ecological examinations. The same factors mentioned
in relation to chemical investigations could alter bioavailability and toxicity of compounds. Chemicals might bio-
degrade, volatilize, oxidize or photolyze during storage. Therefore, careful consideration should be given to these
processes and the storage conditions needed to avoid such alterations. However, the assessment of sludge
contamination by laboratory bioassay testing requires different preservation techniques in comparison to ecological
or microbial investigation. An ecological investigation generally involves classifying the species and numbers of flora
and/or fauna present on and in fixed sludges or sediments. On the other hand, microbial activity may also be of
interest to characterize samples and can only be determined without fixation. Microbial activity may be responsible
for changes in the nitrate-nitrite-ammonia content, for decreases in biochemical oxygen demand, or for reducing
sulfate to sulfide.
To minimize any changes due to microbial activity, samples should be kept as cool as possible, without freezing,
until analysis. For bacteriological examination, sterile glass containers shall be used. Containers should be able to
withstand a sterilization temperature of 175 °C for 1 h and should not produce or release at this temperature any
chemicals that would influence biological activity. It may be possible to use disposable commercial plastics
containers, subject to verification of the absence of interference with the analysis. Manipulation of the samples is
often necessary, and the optimal methods depend on the study objectives.
3.5 Feasible precautions
3.5.1 Safety precautions
It is essential for proper health and safety precautions to be observed at all times when sampling potentially
hazardous sludges or sediments. Human exposure to pathogenic organisms or pollutants should be avoided by
using respirators, safety glasses and appropriate protective gloves. Primary digestion of sludge produces methane,
which presents a risk of fire and explosion if a source of ignition is present. Containers should be wrapped with
waterproof adhesive tape to minimize the fragmentation of the containers if an explosion occurs. Care should be
taken when sampling, transporting and utilizing the sludge, 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.
3.5.2 Other precautions
See ISO 5667-3 for precautions to be taken in the preparation, filling and use of appropriate containers.
Sample containers should be made from materials appropriate for conserving the natural properties of both t
...

SLOVENSKI STANDARD
SIST ISO 5667-15:2001
01-december-2001
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EODWRPLQY]RUFLVHGLPHQWD
Water quality -- Sampling -- Part 15: Guidance on preservation and handling of sludge
and sediment samples
Qualité de l'eau -- Échantillonnage -- Partie 15: Guide général pour la préservation et le
traitement des échantillons de boues et de sédiments
Ta slovenski standard je istoveten z: ISO 5667-15:1999
ICS:
13.060.45 Preiskava vode na splošno Examination of water in
general
SIST ISO 5667-15:2001 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------

SIST ISO 5667-15:2001

---------------------- Page: 2 ----------------------

SIST ISO 5667-15:2001
INTERNATIONAL ISO
STANDARD 5667-15
First edition
1999-08-01
Water quality — Sampling —
Part 15:
Guidance on preservation and handling of
sludge and sediment samples
Qualité de l'eau — Échantillonnage —
Partie 15: Guide général pour la préservation et le traitement des
échantillons de boues et de sédiments
A
Reference number
ISO 5667-15:1999(E)

---------------------- Page: 3 ----------------------

SIST ISO 5667-15:2001
ISO 5667-15:1999(E)
Contents
1 Scope .1
2 Normative reference .1
3 Sample storage, preservation and handling.1
3.1 General considerations.1
3.2 Chemical examination.1
3.3 Physical examination .2
3.4 Biological examination.2
3.5 Feasible precautions .2
3.6 Sample handling .3
3.7 Sample preservation.3
3.8 Sample storage .3
4 Sample record and quality assurance .4
Bibliography.7
©  ISO 1999
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic
or mechanical, including photocopying and microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet [e-mail]
Printed in Switzerland
ii

---------------------- Page: 4 ----------------------

SIST ISO 5667-15:2001
© ISO
ISO 5667-15:1999(E)
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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
International Standard ISO 5667-15 was prepared by Technical Committee ISO/TC 147, Water quality,
Subcommittee SC 6, Sampling (general methods).
ISO 5667 consists of the following parts, under the general title Water quality — Sampling:
— Part 1: Guidance on the design of sampling programmes
— Part 2: Guidance on sampling techniques
— Part 3: Guidance on the preservation and handling of samples
— Part 4: Guidance on sampling from lakes
— Part 5: Guidance on sampling of drinking water
— Part 6: Guidance on sampling of rivers and streams
— Part 7: Guidance on sampling of water and steam in boiler plants
— Part 8: Guidance on sampling of wet deposition
— Part 9: Guidance on sampling from marine waters
— Part 10: Guidance on sampling of waste waters
— Part 11: Guidance on sampling of groundwaters
— Part 12: Guidance on sampling of bottom sediments
— Part 13: Guidance on sampling of water, wastewater and related sludges
— Part 14: Guidance on quality assurance of environmental water sampling and handling
— Part 15: Guidance on preservation and handling of sludge and sediment samples
— Part 16: Guidance on biotesting of samples
— Part 17: Guidance on sampling of suspended sediments
— Part 18: Guidance on sampling of groundwater on potentially contaminated sites
iii

---------------------- Page: 5 ----------------------

SIST ISO 5667-15:2001

---------------------- Page: 6 ----------------------

SIST ISO 5667-15:2001
INTERNATIONAL STANDARD  © ISO ISO 5667-15:1999(E)
Water quality — Sampling —
Part 15:
Guidance on preservation and handling of sludge and sediment
samples
1 Scope
This part of ISO 5667 provides guidance on the procedures for preservation and handling of sewage and
waterworks sludges, suspended matter, and saltwater and freshwater sediments for subsequent analysis.
2 Normative reference
The following normative document contains provisions which, through reference in this text, constitute provisions of
this part of ISO 5667. For dated references, subsequent amendments to, or revisions of, any of these publications
do not apply. However, parties to agreements based on this part of ISO 5667 are encouraged to investigate the
possibility of applying the most recent edition of the normative documents indicated below. For undated references,
the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of
currently valid International Standards.
ISO 5667-3 :1994, Water quality — Sampling — Part 3: Guidance on the preservation and handling of samples.
3 Sample preservation and handling
3.1 General considerations
Storage begins when the samples are taken. All storage methods will affect the sample to some extent, and the
choice of preservation technique depends mainly on the objective of the sample collection. It is important that the
effects that preservation and storage techniques can have on sample quality and the results of analysis are
understood.
Sludge and sediment samples are subject to chemical, physical and biological changes as soon as they are
collected. If guidance is required on the type of sampling technique to be used, guidance is given in ISO 5667-12
and ISO 5667-13. Sample handling, preservation and storage shall be designed to minimize any changes in
composition of the sample by retarding chemical and/or biological activity and by avoiding contamination. Specific
preservation techniques are often necessary for a representative evaluation of the sludges and sediments, and a
variety of chemical, physical and biological investigations can be performed on the collected samples.
No single preservation method is applicable to all constituents. The objective of the sampling programme and the
nature of the analytical method will determine the handling operation or preservation technique.
3.2 Chemical examination
In this type of investigation, the nature and amounts of the substances which have become absorbed or adsorbed
by the sludges and sediments can be determined. Partition of chemicals between solid phase and water phase is
influenced by several factors, such as particle size, amount of organic matter, pH, redox potential or salinity. The
study of such attributes may be a sampling objective and therefore the preservation needs of the analytical methods
to be employed should be taken into account (see Table 1). The guidance given in this part of ISO 5667 is relevant
1

---------------------- Page: 7 ----------------------

SIST ISO 5667-15:2001
© ISO
ISO 5667-15:1999(E)
to the determination of components in the sum of the separate phases of a sludge or sediment, unless otherwise
indicated. Preservation of samples by fast-freezing can cause mobilization of contaminants by cellular disruption,
whereas not stabilizing samples can permit continued microbial transformation of critical pollutants. In addition to
biodegradation of organics, volatilization is a principal mechanism of loss of volatile compounds during sample
handling.
Anoxic samples require appropriate preservation techniques such as oxygen exclusion during sample handling.
Where refrigeration is not available at the time of collection of liquid sludge samples, particularly in countries with
high ambient temperatures, preservation of the samples for sulfide determination can be achieved by raising the pH
to greater than 10,5. Analysis should still be carried out as soon as possible after collection. 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.
3.3 Physical examination
In this type of examination, the structure, texture and, for sediments, the layer formation, are determined. Sediment
fabric changes are obvious if rapid drainage of pore water occurs. The importance of sludge or sediment 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 sample integrity is important, agitation- and
vibration-free conditions should be maintained during transport; fast-freezing of the sludges and sediments may be
appropriate.
3.4 Biological examination
Biological studies include toxicological, ecotoxicological and ecological examinations. The same factors mentioned
in relation to chemical investigations could alter bioavailability and toxicity of compounds. Chemicals might bio-
degrade, volatilize, oxidize or photolyze during storage. Therefore, careful consideration should be given to these
processes and the storage conditions needed to avoid such alterations. However, the assessment of sludge
contamination by laboratory bioassay testing requires different preservation techniques in comparison to ecological
or microbial investigation. An ecological investigation generally involves classifying the species and numbers of flora
and/or fauna present on and in fixed sludges or sediments. On the other hand, microbial activity may also be of
interest to characterize samples and can only be determined without fixation. Microbial activity may be responsible
for changes in the nitrate-nitrite-ammonia content, for decreases in biochemical oxygen demand, or for reducing
sulfate to sulfide.
To minimize any changes due to microbial activity, samples should be kept as cool as possible, without freezing,
until analysis. For bacteriological examination, sterile glass containers shall be used. Containers should be able to
withstand a sterilization temperature of 175 °C for 1 h and should not produce or release at this temperature any
chemicals that would influence biological activity. It may be possible to use disposable commercial plastics
containers, subject to verification of the absence of interference with the analysis. Manipulation of the samples is
often necessary, and the optimal methods depend on the study objectives.
3.5 Feasible precautions
3.5.1 Safety precautions
It is essential for proper health and safety precautions to be observed at all times when sampling potentially
hazardous sludges or sediments. Human exposure to pathogenic organisms or pollutants should be avoided by
using respirators, safety glasses and appropriate protective gloves. Primary digestion of sludge produces methane,
which presents a risk of fire and explosion if a source of ignition is present. Containers should be wrapped with
waterproof adhesive tape to minimize the fragmentation of the contai
...