SIST EN ISO 5667-15:2010
(Main)Water quality - Sampling - Part 15: Guidance on the preservation and handling of sludge and sediment samples (ISO 5667-15:2009)
Water quality - Sampling - Part 15: Guidance on the preservation and handling of sludge and sediment samples (ISO 5667-15:2009)
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.
Wasserbeschaffenheit - Probenahme - Teil 15: Anleitung zur Konservierung und Handhabung von Schlamm- und Sedimentproben (ISO 5667-15:2009)
Dieser Teil von ISO 5667 gibt eine Anleitung zu Verfahren für die Konservierung, Handhabung und Lagerung von Proben von Klärschlämmen, Schlämmen aus Wasserwerken, Schwebstoffen, Salzwassersedimenten und Süßwassersedimenten bis zur chemischen, physikalischen, radiochemischen und/oder biologischen Untersuchung.
Die Verfahren in dieser Norm sind nur auf feuchte Proben von Schlamm, Sediment und Schwebstoffen geeignet.
Proben von Schlamm, Sediment und Schwebstoffen, die getrocknet oder gefriergetrocknet wurden, verhalten sich ähnlich wie getrocknete Böden. Für Hinweise zu einer lang- und kurzfristigen Lagerung von (gefrier )getrockneten Proben siehe ISO/DIS 18512. Für Hinweise zur Gefriertrocknung siehe ISO 16720.
Qualité de l'eau - Échantillonnage - Partie 15: Lignes directrices pour la conservation et le traitement des échantillons de boues et de sédiments (ISO 5667-15:2009)
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.
Kakovost vode - Vzorčenje - 15. del: Navodilo za konzerviranje in ravnanje z blatom in vzorci sedimenta (ISO 5667-15:2009)
Ta del ISO 5667 zagotavlja vodilo za postopke za konzerviranje, ravnanje in shranjevanje vzorcev blata iz čistilnih naprav in naprav za prečiščevanje pitne vode, suspendiranih delcev, slanovodnih in sladkovodnih usedlin, dokler se v laboratoriju ne opravijo kemične, fizikalne, radiokemične in/ali biološke preiskave.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 5667-15:2010
01-februar-2010
1DGRPHãþD
SIST ISO 5667-15:2001
.DNRYRVWYRGH9]RUþHQMHGHO 1DYRGLOR]DNRQ]HUYLUDQMHLQUDYQDQMH]
EODWRPLQY]RUFLVHGLPHQWD ,62
Water quality - Sampling - Part 15: Guidance on the preservation and handling of sludge
and sediment samples (ISO 5667-15:2009)
Wasserbeschaffenheit - Probenahme - Teil 15: Anleitung zur Konservierung und
Handhabung von Schlamm- und Sedimentproben (ISO 5667-15:2009)
Qualité de l'eau - Échantillonnage - Partie 15: Lignes directrices pour la conservation et
le traitement des échantillons de boues et de sédiments (ISO 5667-15:2009)
Ta slovenski standard je istoveten z: EN ISO 5667-15:2009
ICS:
13.060.45 Preiskava vode na splošno Examination of water in
general
SIST EN ISO 5667-15:2010 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 5667-15:2010
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SIST EN ISO 5667-15:2010
EUROPEAN STANDARD
EN ISO 5667-15
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2009
ICS 13.060.45; 13.060.30
English Version
Water quality - Sampling - Part 15: Guidance on the
preservation and handling of sludge and sediment samples (ISO
5667-15:2009)
Qualité de l'eau - Échantillonnage - Partie 15: Lignes Wasserbeschaffenheit - Probenahme - Teil 15: Anleitung
directrices pour la conservation et le traitement des zur Konservierung und Handhabung von Schlamm- und
échantillons de boues et de sédiments (ISO 5667-15:2009) Sedimentproben (ISO 5667-15:2009)
This European Standard was approved by CEN on 24 July 2009.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the
official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 5667-15:2009: E
worldwide for CEN national Members.
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SIST EN ISO 5667-15:2010
EN ISO 5667-15:2009 (E)
Contents Page
Foreword .3
2
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SIST EN ISO 5667-15:2010
EN ISO 5667-15:2009 (E)
Foreword
This document (EN ISO 5667-15:2009) has been prepared by Technical Committee ISO/TC 147 "Water
quality" in collaboration with Technical Committee CEN/TC 308 “Characterization of sludges”, the secretariat
of which is held by AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by February 2010, and conflicting national standards shall be withdrawn
at the latest by February 2010.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 5667-15:2009 has been approved by CEN as a EN ISO 5667-15:2009 without any
modification.
3
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SIST EN ISO 5667-15:2010
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SIST EN ISO 5667-15:2010
INTERNATIONAL ISO
STANDARD 5667-15
Second edition
2009-08-15
Water quality — Sampling —
Part 15:
Guidance on the preservation and
handling of sludge and sediment samples
Qualité de l'eau — Échantillonnage —
Partie 15: Lignes directrices pour la conservation et le traitement des
échantillons de boues et de sédiments
Reference number
ISO 5667-15:2009(E)
©
ISO 2009
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SIST EN ISO 5667-15:2010
ISO 5667-15:2009(E)
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ii © ISO 2009 – All rights reserved
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SIST EN ISO 5667-15:2010
ISO 5667-15:2009(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions. 1
4 Reagents. 2
5 Preservation of samples . 2
5.1 General considerations. 2
5.2 Chemical examination. 3
5.3 Physical examination . 3
5.4 Radiochemical examination . 3
5.5 Biological examination. 4
6 Safety precautions. 4
6.1 Staff protection . 4
6.2 Sample protection. 4
7 Containers . 4
8 Sample collection . 5
9 Identification of samples. 5
10 Transport of samples . 6
11 Reception of samples. 6
12 Sample storage . 6
Annex A (informative) Container preparation. 12
Annex B (informative) Long-term storage of wet sediment samples using nitrogen vapour
freezers . 14
Bibliography . 16
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SIST EN ISO 5667-15:2010
ISO 5667-15:2009(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 2.
The main task of technical committees is to prepare International Standards. 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.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 5667-15 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 6,
Sampling (general methods).
This second edition cancels and replaces the first edition (ISO 5667-15:1999), which has been technically
revised.
ISO 5667 consists of the following parts, under the general title Water quality — Sampling:
⎯ Part 1: Guidance on the design of sampling programmes and sampling techniques
⎯ Part 3: Guidance on the preservation and handling of water samples
⎯ Part 4: Guidance on sampling from lakes, natural and man-made
⎯ Part 5: Guidance on sampling of drinking water from treatment works and piped distribution systems
⎯ 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 the 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
1)
⎯ Part 13: Guidance on sampling of sludges from sewage and water-treatment works
1) In preparation. (Revision of ISO 5667-13:1997)
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SIST EN ISO 5667-15:2010
ISO 5667-15:2009(E)
⎯ Part 14: Guidance on quality assurance of environmental water sampling and handling
⎯ Part 15: Guidance on the preservation and handling of sludge and sediment samples
⎯ Part 16: Guidance on biotesting of samples
⎯ Part 17: Guidance on sampling of bulk suspended solids
⎯ Part 19: Guidance on sampling of marine sediments
⎯ Part 20: Guidance on the use of sampling data for decision making — Compliance with thresholds and
classification systems
⎯ Part 21: Guidance on sampling of drinking water distributed by tankers or means other than distribution
pipes
⎯ Part 22: Guidance on the design and installation of groundwater monitoring points
⎯ Part 23: Determination of priority pollutants in surface water using passive sampling
This part of ISO 5667 may be used in conjunction with the other parts available within the ISO 5667 series.
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SIST EN ISO 5667-15:2010
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SIST EN ISO 5667-15:2010
INTERNATIONAL STANDARD ISO 5667-15:2009(E)
Water quality — Sampling —
Part 15:
Guidance on the preservation and handling of sludge and
sediment samples
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This standard 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 and to
ensure compliance with any national regulatory conditions.
1 Scope
This part of ISO 5667 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 this part of ISO 5667 are only applicable to wet samples of sludge, sediment and
suspended matter.
NOTE Samples of sludge, sediment and suspended matter that are dried or freeze-dried behave similarly to dried
soils. For guidance on long- and short-term storage of (freeze) dried samples, see ISO 18512. For guidance on
freeze-drying, see ISO 16720.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
sample preservation
any 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
[ISO 11074:2005, 4.4.20]
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SIST EN ISO 5667-15:2010
ISO 5667-15:2009(E)
3.2
sample storage
process, and the result, of keeping a sample available under predefined conditions for a (usually) specified
time interval between collection and further treatment of a sample
NOTE Adapted from ISO 11074:2005, 4.4.22.
3.3
storage duration
period of time between sample collection and start of the analysis of the sample in the laboratory, for a sample
stored under pre-defined conditions
4 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 used should be of at least analytical reagent grade.
4.1 Deionized water, Grade 3 quality as specified in ISO 3696.
4.2 Sodium sulfate, Na SO , monohydrate.
2 4
Heat the sodium sulfate before use for at least 6 h at (500 ± 10) °C. Store in an desiccator after heating.
4.3 Zinc acetate, (CH COO) Zn⋅2H O (10 % mass fraction).
3 2 2
4.4 Methanol, CH OH.
3
4.5 Ethanol, C H OH (volume fraction of 96 %).
2 5
4.6 Sodium tetraborate (Na B O⋅10H O), sodium phosphate (Na P O⋅10H O) or hexamethylene-
2 4 7 2 4 2 7 2
tetramine [(CH ) N ].
2 6 4
4.7 Formaldehyde solution, CH O (volume fraction of 3,7 %).
2
Add 37 % formaldehyde neutralized to pH 7 with sodium tetraborate, sodium phosphate or
hexamethylenetetramine (100 g/l formalin solution) to give a final solution of 3,7 % formaldehyde
(corresponding to a 1 to 10 dilution of formalin solution).
NOTE 37 % formaldehyde is 100 % formalin.
5 Preservation of samples
5.1 General considerations
Sample handling is specific for each determination to be conducted. Manipulation of samples is often required
to yield consistent material for toxicity testing and laboratory experiments. Homogenization, by mixing or
sieving, dilution to obtain a suitable concentration and addition of chemical preservatives all complicate
interpretations of in situ comparisons.
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 might biodegrade, volatilize, oxidize, be reduced or photolyse during
storage. Therefore, careful consideration should be given to these processes and the storage conditions
needed to avoid such alterations.
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ISO 5667-15:2009(E)
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 recommendations can be given for a universal preservation or storage method. A preservation method
used 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
different method such that the full range of required analyses is represented.
5.2 Chemical examination
Chemical analysis can be performed to determine the nature and amounts of the substances that have
become absorbed or adsorbed by sludge, sediment and 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 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 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 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.
5.3 Physical examination
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 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 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. Fast-freezing of the sludge and sediments 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).
Samples should be stored and preserved in accordance with the conditions given in Table 1.
5.4 Radiochemical examination
Some sample sites can have measurable radiochemical activity in the soil or air. Some items of domestic
equipment within the laboratory can also be a source of radioactive material. Infection of the sample by its
environment should therefore be avoided, especially if the sample activity is likely to be very low.
Samples should be stored and preserved in accordance with the conditions given in Table 2.
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ISO 5667-15:2009(E)
5.5 Biological examination
Biological studies include toxicological, ecotoxicological and ecological examinations. The same factors
mentioned in relation to chemical examination (see 5.2) can alter the bioavailability and toxicity of compounds.
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 sludge or
sediments.
Microbial activity may also be used to characterize samples and can only be determined without fixation.
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.
Samples should be stored and preserved in accordance with the conditions given in Tables 1 and 3.
6 Safety precautions
6.1 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 and protective gloves. The hazard due to
pathogenic organisms 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 wrapped to minimize the fragmentation of the containers if an
explosion 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.
6.2 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.
7 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 container for each analyte to be measured
are given in Tables 1, 2 and 3.
If the samples are to be frozen, suitable material such as polyethylene or polytetrafluoroethylene (PTFE)
should be used to minimize the risk of breakage.
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ISO 5667-15:2009(E)
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 A.
The choice of sample container is of major importance and ISO 5667-1 provides guidance on this subject.
In 5.3 of ISO 5667-14:1998, 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.
8 Sample collection
Samples should be collected in sufficient volumes to allow:
a) separate sub-samples to be preserved for each type of analysis or examination to be undertaken;
b) repeat the analysis in the event of error checking or the routine quality control requirements of duplicate
analysis;
c) prepare 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 to a maximum of 80 % of its capacity,
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 sediment 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.
9 Identification of samples
Container labels should withstand wetting, drying and freezing without detaching or becoming illegible. The
labelling system should be waterproof to allow use in the field.
The exact information given in the sampling report and on the sample labels will depend on the objectives of
the particular measurement programme. In all cases, an indelible label should be secured to the sample
container.
For each sample, the following information should be provided as a minimum:
⎯ a unique identifier, traceable to the date, time and location of sampling;
⎯ a description and disposition of sample;
⎯ the name of the individual sampler;
⎯ details of preservation used;
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SIST EN ISO 5667-15:2010
ISO 5667-15:2009(E)
⎯ details of sample storage used;
⎯ any information regarding integrity and manipulation of the sample;
⎯ other information as necessary.
The unique identifier should be on the label of the sample container. The remaining information can be
provided in the sample report.
10 Transport of samples
During transportation, samples should be stored in a cooling device capable of maintaining a temperature
between 2 °C and 8 °C. It is recognized that not all sample locations allow for immediate storage under such
conditions for practical and safety reasons. Where this arises appropriate facts should be recorded in the
sample report.
However, samples that need to be frozen for preservation purposes (see Tables 1, 2 and 3) should be frozen
on site and transported at a temperature below −18 °C.
The temperature of the cooling device, refrigerator and/or freezing device should be recorded and the
information provided in the sample report.
NOTE In circumstances where
...
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