SIST EN ISO 5667-3:2013

SLOVENSKI STANDARD
SIST EN ISO 5667-3:2013
01-januar-2013
1DGRPHãþD
SIST EN ISO 5667-3:2004
SIST EN ISO 5667-3:2004/AC:2007
.DNRYRVWYRGH9]RUþHQMHGHO6KUDQMHYDQMHLQUDYQDQMH]Y]RUFLYRGH,62

Water quality - Sampling - Part 3: Preservation and handling of water samples (ISO 5667
-3:2012)
Wasserbeschaffenheit - Probenahme - Teil 3: Konservierung und Handhabung von
Wasserproben (ISO 5667-3:2012)
Qualité de l'eau - Échantillonnage - Partie 3: Conservation et manipulation des
échantillons d'eau (ISO 5667-3:2012)
Ta slovenski standard je istoveten z: EN ISO 5667-3:2012
ICS:
13.060.45 Preiskava vode na splošno Examination of water in
general
SIST EN ISO 5667-3:2013 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 5667-3:2013

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SIST EN ISO 5667-3:2013


EUROPEAN STANDARD
EN ISO 5667-3

NORME EUROPÉENNE

EUROPÄISCHE NORM
November 2012
ICS 13.060.45 Supersedes EN ISO 5667-3:2003
English Version
Water quality - Sampling - Part 3: Preservation and handling of
water samples (ISO 5667-3:2012)
Qualité de l'eau - Échantillonnage - Partie 3: Conservation Wasserbeschaffenheit - Probenahme - Teil 3:
et manipulation des échantillons d'eau (ISO 5667-3:2012) Konservierung und Handhabung von Wasserproben (ISO
5667-3:2012)
This European Standard was approved by CEN on 14 November 2012.

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-CENELEC 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-CENELEC Management Centre has the same
status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 5667-3:2012: E
worldwide for CEN national Members.

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SIST EN ISO 5667-3:2013
EN ISO 5667-3:2012 (E)
Contents Page
Foreword .3

2

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SIST EN ISO 5667-3:2013
EN ISO 5667-3:2012 (E)
Foreword
This document (EN ISO 5667-3:2012) has been prepared by Technical Committee ISO/TC 147 "Water
quality" in collaboration with Technical Committee CEN/TC 230 “Water analysis” the secretariat of which is
held by DIN.
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 May 2013, and conflicting national standards shall be withdrawn at the
latest by May 2013.
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.
This document supersedes EN ISO 5667-3:2003.
According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech
Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
Endorsement notice
The text of ISO 5667-3:2012 has been approved by CEN as a EN ISO 5667-3:2012 without any modification.
3

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SIST EN ISO 5667-3:2013

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SIST EN ISO 5667-3:2013
INTERNATIONAL ISO
STANDARD 5667-3
Fourth edition
2012-11-15
Water quality — Sampling —
Part 3:
Preservation and handling of water
samples
Qualité de l’eau — Ėchantillonnage —
Partie 3: Conservation et la manipulation des échantillions d’eau
Reference number
ISO 5667-3:2012(E)
©
ISO 2012

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SIST EN ISO 5667-3:2013
ISO 5667-3:2012(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2012
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 either ISO at the
address below or ISO’s member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2012 – All rights reserved

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SIST EN ISO 5667-3:2013
ISO 5667-3:2012(E)

Contents Page
Foreword .iv
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Sampling and chain of custody . 2
5 Reagents and materials . 2
5.1 Solids . 3
5.2 Solutions . 3
5.3 Materials . 4
6 Containers . 4
6.1 Container selection and preparation . 4
6.2 Filtration on site . 5
6.3 Filling the container . 5
7 Sample handling and preservation . 5
7.1 Sample handling and preservation for physical and chemical examination . 5
7.2 Sample handling and preservation for biological examination . 6
7.3 Sample handling and preservation for radiochemical analysis . 6
8 Sample transport . 7
9 Identification of samples . 7
10 Sample reception . 8
11 Sample storage . 8
Annex A (informative) Techniques for sample preservation . 9
Annex B (informative) Container preparation .35
Annex C (informative) Protocol as used in Dutch validation studies .36
Bibliography .38
© ISO 2012 – All rights reserved iii

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SIST EN ISO 5667-3:2013
ISO 5667-3:2012(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 5667-3 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 6,
Sampling (general methods).
This fourth edition cancels and replaces the third edition (ISO 5667-3:2003), 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: 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
— Part 13: Guidance on sampling of sludges
— 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
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SIST EN ISO 5667-3:2013
ISO 5667-3:2012(E)

— 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: Guidance on passive sampling in surface waters
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SIST EN ISO 5667-3:2013
ISO 5667-3:2012(E)

Introduction
This part of ISO 5667 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 part of ISO 5667 has been brought into line with current standards. Where new
research or validation results have provided new insights, the latest knowledge has been used.
[63]
Guidance on validation protocols can be found in ISO Guide 34.
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SIST EN ISO 5667-3:2013
INTERNATIONAL STANDARD ISO 5667-3:2012(E)
Water quality — Sampling —
Part 3:
Preservation and handling of water samples
NOTICE — This part of ISO 5667 and the analytical International Standards listed in Annex A
are complementary. Where no analytical International Standard is applicable, the technique(s)
described in Tables A.1 to A.3 take(s) normative status.
When new or revised analytical standards are developed with storage times or preservative
techniques differing from those in Tables A.1 to A.3, then the storage times or preservative
techniques should be validated and presented to ISO/TC 147/SC 6/WG 3 for incorporation into
the next revision of this part of ISO 5667.
1 Scope
This part of ISO 5667 establishes general requirements for sampling, preservation, handling, transport
and storage of all water samples including those for biological analyses. It is not applicable to water
samples intended for microbiological analyses as specified in ISO 19458, ecotoxicological assays,
biological assays, and passive sampling as specified in the scope of ISO 5667-23.
This part of ISO 5667 is particularly appropriate when spot or composite samples cannot be analysed on
site and have to be transported to a laboratory for analysis.
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
ISO 5667 (all parts), Water quality — Sampling
ISO 19458, Water quality — Sampling for microbiological analysis
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
integrity
property that the parameter(s) of interest, information or content of the sample container has not been
altered or lost in an unauthorized manner or subject to loss of representativeness
3.2
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
[29]
[ISO 11074:2005, 4.4.20]
NOTE Different analytes may require several samples from the same source that are stabilized by
different procedures.
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SIST EN ISO 5667-3:2013
ISO 5667-3:2012(E)

3.3
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
[29]
NOTE 1 Adapted from ISO 11074:2005, 4.4.22.
NOTE 2 Specified time is the maximum time interval.
3.4
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 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 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.
4 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 a sampling programme. Guidance on this topic is given in ISO 5667-1.
Depending on the sample type and matrix, the guidelines found in the relevant part(s) of ISO 5667 and
ISO 19458 shall be consulted.
The process of preservation and handling of water samples consists of several steps. During this
process, the responsibility for the samples might change. To ensure the integrity of the samples, all steps
involving the sample shall be documented.
All preparation procedures shall be checked to ensure positive or negative interferences do not occur.
As a minimum, this shall include the analysis of blanks (e.g. field blank or sample container) or samples
containing known levels of relevant analytes as specified in ISO 5667-14.
5 Reagents and materials
WARNING — Certain preservatives (e.g. acids, alkalis, formaldehyde) need to be used with
caution. Sampling personnel should be warned of potential dangers, and appropriate safety
procedures should be followed.
The following reagents are used for the sample preservation and shall only be prepared according to
individual sampling requirements. All reagents used shall be of at least analytical reagent grade and
water shall be of at least ISO 3696, grade 2. Acids referred to in this part of ISO 5667 are commercially
available “concentrated” acids.
All reagents shall be labelled with a “shelf-life”. The shelf-life represents the period for which the reagent
is suitable for use, if stored correctly. This shelf-life shall not be exceeded. Any reagents that are not
completely used by the expiry of the shelf-life date shall be discarded.
NOTE Often the shelf-life of reagents is supplied by the receiving laboratory.
Check reagents periodically, e.g. by field blanks, and discard any reagent found to be unsuitable.
Between on-site visits, reagents shall be stored separately from sample containers and other equipment
in a clean, secure cabinet in order to prevent contamination.
Each sample shall be labelled accordingly, after the addition of the preservative. Otherwise, there could
be no visible indication as to which samples have been preserved, and which have not.
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SIST EN ISO 5667-3:2013
ISO 5667-3:2012(E)

5.1 Solids
5.1.1 Sodium thiosulfate pentahydrate, Na S O ·5H O, w(Na S O ·5H O) > 99 %.
2 2 3 2 2 2 3 2
5.1.2 Ascorbic acid, C H O , w(C H O ) > 99 %.
6 8 6 6 8 6
5.1.3 Sodium hydroxide, NaOH, w(NaOH) > 99 %.
5.1.4 Sodium tetraborate decahydrate, Na B O ·10H O, w(Na B O ·10H O), > 99 %.
2 4 7 2 2 4 7 2
CAUTION Sodium tetraborate decahydrate is known to be a carcinogen, mutagen and
reproductive toxin (CMR).
5.1.5 Hexamethylenetetramine (hexamine, urotropine), C H N , w(C H N ) > 99 %.
6 12 4 6 12 4
5.1.6 Potassium iodide, KI, w(KI) > 99 %.
5.1.7 Iodine, I , w(I ) > 99 %.
2 2
5.1.8 Sodium acetate, C H NaO , w(C H NaO ) > 99 %.
2 3 2 2 3 2
5.1.9 Ethylenediamine, C H N , w(C H N ) > 99 %.
2 8 2 2 8 2
5.2 Solutions
5.2.1 Zinc acetate solution C H O Zn (10 g/l).
4 6 4
Dissolve 10,0 g of zinc acetate in ∼100 ml of water . Dilute to 100 ml with water. Store the solution in a
polypropylene or glass bottle for a maximum period of 1 a.
5.2.2 Orthophosphoric acid (ρ ≈ 1,7 g/ml), H PO , w(H PO ) > 85 %, c(H PO ) = 15 mol/l.
3 4 3 4 3 4
5.2.3 Hydrochloric acid (ρ ≈ 1,2 g/ml), HCl, w(HCl) > 36 %, c(HCl) = 12,0 mol/l.
5.2.4 Nitric acid (ρ ≈ 1,42 g/ml), HNO , w(HNO ) > 65 %, c(HNO ) = 15,8 mol/l.
3 3 3
5.2.5 Sulfuric acid (ρ ≈ 1,84 g/ml), H SO (freshly prepared).
2 4
Dilute concentrated sulfuric acid (H SO ), ρ ≈ 1,84 g/ml, w(H SO ) ≈ 98 % 1 + 1 by carefully adding the
2 4 2 4
concentrated acid to an equal volume of water and mix.
WARNING — Adding the concentrated acid to the water can give violent reactions because of an
exothermic reaction.
5.2.6 Sodium hydroxide solution (ρ ≈ 0,40 g/ml), NaOH.
5.2.7 Formaldehyde solution (formalin), CH O, ϕ(CH O) = 37 % to 40 % (freshly prepared),
2 2
WARNING — Beware of formaldehyde vapours. Do not store large numbers of samples in
small work areas.
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SIST EN ISO 5667-3:2013
ISO 5667-3:2012(E)

5.2.8 Disodium salt of ethylenediaminetetraacetic acid (EDTA) (ρ ≈ 0,025 g/ml),
C H N Na O ⋅2H O, w(C H N Na O ⋅2H O) > 99 %.
10 14 2 2 8 2 10 14 2 2 8 2
Dissolve 25 g EDTA in 1 000 ml of water.
5.2.9 Ethanol C H OH, ϕ(C H OH) = 96 %.
2 5 2 5
5.2.10 Alkaline Lugol’s solution, 100 g potassium iodide (5.1.6), 50 g iodine (5.1.7), and 250 g sodium
acetate (5.1.8) in 1 000 ml water to pH 10.
5.2.11 Acidic Lugol’s solution, 100 g potassium iodide (5.1.6), 50 g iodine (5.1.7) and 100 ml glacial
acetic acid (5.2.17) in 1 000 ml water to pH 2.
5.2.12 Neutralized formaldehyde solution, formaldehyde solution (5.2.7) neutralized with sodium
tetraborate (5.1.4) or hexamethylenetetramine (5.1.5). Formalin solution at 100 g/l gives a final solution
of ϕ(CH O) = 3,7 % to 4,0 %.
2
WARNING — Beware of formaldehyde vapours. Do not store large numbers of samples in
small work areas.
5.2.13 Ethanol preservative solution.
Ethanol (5.2.9), formaldehyde solution (5.2.7) and glycerol (5.2.18) (100 + 2 + 1 parts by volume,
respectively).
5.2.14 Sodium hypochlorite NaOCl, w(NaOCl) = 10 %. Dissolve 100 g sodium hypochlorite (NaOCl) in
1 000 ml of water.
5.2.15 Potassium iodate KIO , w(KIO ) = 10 %. Dissolve 100 g potassium iodate (KIO ) in 1 000 ml of water.
3 3 3
5.2.16 Methanoic acid (formic acid) CH O , ϕ(CH O ) > 98 %.
2 2 2 2
5.2.17 Glacial acetic acid C H O , w(C H O ) > 99 %.
2 4 2 2 4 2
5.2.18 Glycerol (glycerin, glycerine) C H (OH) .
3 5 3
5.3 Materials
5.3.1 Container and cap, types as specified in Tables A.1 to A.3.
5.3.2 Filter, pore size 0,40 µm to 0,45 µm, unless a different filter size is specified in the analytical
International Standard.
6 Containers
6.1 Container selection and preparation
The choice of sample container (5.3.1) is of major importance and ISO 5667-1 provides some guidance
on this subject.
Details of the type of container used for the collection and storage of samples are given in Tables A.1 to
A.3. The same considerations given to this selection of suitable container material shall also be given to
the selection of cap liner materials.
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SIST EN ISO 5667-3:2013
ISO 5667-3:2012(E)

Sample containers shall 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.3.
NOTE For very low concentrations of metals, containers prescribed can be different from those used for
higher concentrations. Details can be found in Table A.1 or in the analytical International Standards.
If the samples are to be frozen, suitable containers, such as polyethylene (PE) or polytetrafluoroethylene
(PTFE), shall be used to prevent breakage.
The use of disposables is preferred. Some manufacturers supply containers with a certificate of
cleanliness. If such a certificate of cleanliness is supplied, it is not necessary to clean or rinse the
containers before use.
6.2 Filtration on site
Filtration on site is required in some cases.
— Groundwaters shall be filtered on site if dissolved metals need to be analysed.
— Waters shall be filtered (5.3.2) on site, if this is required according to Annex A. Unless specified
otherwise, a filter pore size 0,40 µm to 0,45 µm shall be used.
If immediate filtration on site is impossible, then the reason and the time between sampling and filtration
shall be added to the test report.
6.3 Filling the container
The container (5.3.1) shall be filled completely unless prescribed differently in Tables A.1 to A.3 or the
analytical International Standard used. If the samples are to be frozen as part of their preservation,
sample containers shall not be completely filled. This is in order to prevent breakage which may arise
from expansion of ice during the freezing and thawing process.
If no preservatives are present in the bottle, then prerinsing the bottle may be advisable. Guidance on
prerinsing can be found in ISO 5667-14.
7 Sample handling and preservation
7.1 Sample handling and preservation for physical and chemical examination
Waters, particularly fresh waters, waste waters and groundwaters, are susceptible to changes as a result
of physical, chemical or biological reactions which may take place between the time of sampling and the
commencement of analysis. The nature and rate of these reactions are often such that, if precautions are
not taken during sampling, transport and storage (for specific analytes), the concentrations determined
are different to those existing at the time of sampling.
The extent of these changes is dependent on the chemical and biological nature of the sample, its
temperature, its exposure to light, the type of the container in which it is placed, the time between
sampling and analysis, and the conditions to which it is subjected, e.g. agitation during transport.
Further specific causes of variation are listed in a) to f).
a) The presence of bacteria, algae and other organisms can consume certain constituents of the samples.
These organisms can also modify the nature of the constituents to produce new constituents. This
biological activity affects, for example, the concentrations of dissolved oxygen, carbon dioxide,
compounds of nitrogen, phosphorus and, sometimes, silicon.
b) Certain compounds can be oxidized either by dissolved oxygen present in the samples, or by
atmospheric oxygen [e.g. organic compounds, Fe(II) and sulfides].
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SIST EN ISO 5667-3:2013
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c) Certain substances can precipitate out of solution, e.g. calcium carbonate, metals, and metallic
compounds such as Al(OH) , or can be lost to the vapour phase (e.g. oxygen, cyanides, and mercury).
3
d) Absorption of carbon dioxide from air can modify pH, conductivity, and the concentration of
dissolved carbon dioxide. Passage of compounds like ammonia and silicon fluoride through some
types of plastics may also affect pH or conductivity.
e) Dissolved metals or metals in a colloidal state, as well as certain organic compounds, can be
irreversibly adsorbed on to the surface of the containers or solid materials in the samples.
f) Polymerized products can depolymerize, and conversely, simple compounds can polymerize.
Changes to particular constituents vary both in degree and rate, not only as a function of the type of
water, but also, for the same water type, as a function of seasonal conditions.
These changes are often sufficiently rapid to modify the sample considerably in a short time. In all cases,
it is essential to take precautions to minimize these reactions and, in the case of many analytes, to
analyse the sample with a minimum of delay. If the required precaution for changes is filtration on site,
then a filter (5.3.2) shall be used.
Details of the sample preservation are given in Table A.1.
7.2 Sample handling and preservation for biological examination
The handling of samp
...