SIST ISO 14507:2019
Soil quality - Pretreatment of samples for determination of organic contaminants
Soil quality - Pretreatment of samples for determination of organic contaminants
ISO 14507:2003 specifies three methods for the pretreatment of soil samples in the laboratory prior to the determination of organic contaminants:
if volatile organic compounds are to be measured;
if moderately volatile to non-volatile organic compounds are to be measured, if the result of the subsequent analysis must be accurate and reproducible, and if the sample contains particles larger than 2 mm and/or the contaminant is heterogeneously distributed;
if non-volatile organic compounds are to be measured and the extraction procedure prescribes a field-moist sample, or if the largest particles of the sample are smaller than 2 mm and the contaminant is homogeneously distributed. This procedure is also applicable if reduced accuracy and repeatability are acceptable.
The pretreatment described in ISO 14507:2003 is used in combination with an extraction procedure in which the contaminant is available for the extraction liquid.
NOTE For the pretreatment of soil samples for the purposes of determining non-volatile inorganic compounds and physico-chemical soil characteristics, see ISO 11464.
Qualité du sol - Prétraitement des échantillons pour la détermination des contaminants organiques
L'ISO 14507:2002 spécifie trois méthodes de prétraitement des échantillons de sol en laboratoire avant détermination des contaminants organiques :
une méthode de prétraitement s'il faut mesurer des composés organiques volatils ;
une méthode de prétraitement s'il faut mesurer des composés organiques peu volatils à non volatils, si le résultat de l'analyse ultérieure doit être précis et reproductible et si l'échantillon contient des particules de taille supérieure à 2 mm et/ou le contaminant est réparti de manière hétérogène ;
une méthode de prétraitement s'il faut mesurer des composés organiques non volatils et si la méthode d'extraction prescrit un échantillon brut prélevé sur le terrain ou encore si les particules les plus grosses de l'échantillon sont inférieures à 2 mm et que le contaminant est réparti de manière homogène. Cette méthode peut également être utilisée si une précision et une répétabilité réduites sont acceptables.
La méthode de prétraitement décrite dans l'ISO 14507:2002 est associée à une méthode d'extraction dans laquelle le contaminant est disponible pour le liquide d'extraction.
NOTE Pour le prétraitement des échantillons de sol en vue de déterminer les composés inorganiques non volatils et les caractéristiques physico-chimiques du sol, se reporter à l'ISO 11464.
Kakovost tal - Priprava vzorcev za določevanje organskih onesnaževal
Ta mednarodni standard določa tri metode za pripravo vzorcev tal v laboratoriju pred določevanjem organskih onesnaževal:
pri merjenju hlapnih organskih spojin;
pri merjenju od slabo hlapnih do nehlapnih organskih spojin, če mora biti rezultat naknadne analize natančen in ponovljiv ter če vzorec vsebuje delce, ki so večji od
2 mm in/ali je onesnaževalo heterogeno porazdeljeno;
pri merjenju nehlapnih organskih spojin, in kadar je za postopek ekstrakcije potreben vzorec vlage na prostem ali če so največji delci v vzorcu manjši od 2 mm in je onesnaževalo heterogeno porazdeljeno. Ta postopek se tudi uporablja, če sta nižji ravni natančnosti in ponovljivosti
sprejemljivi.
Priprava, ki je opisana v tem mednarodnem standardu, se uporablja v kombinaciji s postopkom ekstrakcije, pri kateri je onesnaževalo na voljo za ekstrakcijsko tekočino.
OPOMBA: Za pripravo vzorcev tal za namene določevanja nehlapnih organskih spojin in ugotavljanja fizikalno-kemijskih značilnosti tal glej standard ISO 11464.
General Information
Buy Standard
Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 14507
First edition
2003-03-15
Soil quality — Pretreatment of samples
for determination of organic
contaminants
Qualité du sol — Prétraitement des échantillons pour la détermination
des contaminants organiques
Reference number
ISO 14507:2003(E)
©
ISO 2003
---------------------- Page: 1 ----------------------
ISO 14507:2003(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2003
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 2003 — All rights reserved
---------------------- Page: 2 ----------------------
ISO 14507:2003(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope. 1
2 Normative references . 1
3 Terms and definitions. 1
4 Principle . 2
4.1 Sampling . 2
4.2 Volatile compounds. 2
4.3 Moderately volatile compounds . 2
5 Reagents . 3
6 Apparatus . 3
7 Preservation and storage. 4
8 Procedure . 4
8.1 General. 4
8.2 Volatile compounds (boiling point < 300 °°°°C). 5
8.3 Moderately volatile organic compounds (boiling point > 300 °°°°C) — Grinding necessary . 5
8.4 Moderately volatile organic compounds (boiling point > 300 °°C) — Grinding not possible
°°
or not necessary . 7
8.5 Blank measurements. 8
9 Test report . 8
Annex A (informative) Information concerning vapour pressure, boiling and melting points of
volatile organic compounds . 9
Annex B (informative) Validation . 12
Bibliography . 14
© ISO 2003 — All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 14507:2003(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 14507 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
methods and soil characteristics.
iv © ISO 2003 — All rights reserved
---------------------- Page: 4 ----------------------
ISO 14507:2003(E)
Introduction
The properties of organic micropollutants can differ greatly according to chemical species:
they can range from non-volatile to very volatile compounds (low to high vapour pressure);
they can be labile or reactive at ambient or elevated temperatures;
they can be biodegradable or UV-degradable;
they can have considerably different solubilities in water;
they require different analytical procedures.
Because of these differences, a general pretreatment procedure cannot be proposed. The goal of a
pretreatment procedure is to prepare a test sample in which the concentration of the contaminant is equal to
the concentration in the original soil, provided, however, that this procedure does not alter the chemical
species to be analysed. For instance, if the sample contains only small particles and the contaminant is
homogeneously distributed, it is not necessary to grind the sample. In this International Standard, the size
2 mm is used to distinguish between small and large soil particles.
Consistency among the following aspects is important:
soil diversity;
the aim of the analysis (including its accuracy);
the nature of the chemical species to be analysed.
The particle size distribution of the sample in relation to the mass of sample taken for analysis is also
important to pretreatment. For the analysis of organic contaminants, the sample mass taken in most cases is
about 20 g.
With such a sample mass, and provided that the contaminant is homogeneously distributed and the particles
in the sample are smaller than about 2 mm, further grinding of the sample is not necessary. If the sample
contains large particles or if the contaminant is heterogeneously distributed (as occurs for instance with tar
particles), it is not possible to take a representative test sample of about 20 g without grinding the sample. To
improve the homogeneity, samples are ground to a size smaller than 1 mm. Prior to analysis, very often no
information about the distribution of the contaminant in the soil is known.
Some analytical procedures start with a field-moist sample. Drying of the sample gives lower extraction
results. If the sample is not dried, grinding is not possible.
In a situation in which accurate results are needed, the best available pretreatment procedure should be used.
If it is necessary to establish whether the concentration is above a certain limit and it is already known that the
soil is heavily polluted, the simplest pretreatment procedure may meet the need. In this case however, the
result may not be presented as a representative value for the whole sample.
The choice depends above all on the volatility of the organic compounds under analysis. It also depends on
the soil particle size distribution, the heterogeneity of the sample and the analytical procedure.
© ISO 2003 — All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 14507:2003(E)
Soil quality — Pretreatment of samples for determination of
organic contaminants
1 Scope
This International Standard specifies three methods for the pretreatment of soil samples in the laboratory prior
to the determination of organic contaminants:
if volatile organic compounds are to be measured;
if moderately volatile to non-volatile organic compounds are to be measured, if the result of the
subsequent analysis must be accurate and reproducible, and if the sample contains particles larger than
2 mm and/or the contaminant is heterogeneously distributed;
if non-volatile organic compounds are to be measured and the extraction procedure prescribes a field-
moist sample, or if the largest particles of the sample are smaller than 2 mm and the contaminant is
homogeneously distributed. This procedure is also applicable if reduced accuracy and repeatability are
acceptable.
The pretreatment described in this International Standard is used in combination with an extraction procedure
in which the contaminant is available for the extraction liquid.
NOTE For the pretreatment of soil samples for the purposes of determining non-volatile inorganic compounds and
physico-chemical soil characteristics, see ISO 11464.
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 10381-1, Soil quality — Sampling — Part 1: Guidance on the design of sampling programmes
ISO 11074-2, Soil quality — Vocabulary — Part 2: Terms and definitions relating to sampling
ISO 11465:1993, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric
method
3 Terms and definitions
For the purposes of this document, the terms and definitions in ISO 11074-2 and the following apply:
3.1
volatile compound
organic compound having a boiling point below 300 °C (at a pressure of 101 kPa)
NOTE 1 This includes volatile aromatic and volatile halogenated hydrocarbons as determined in accordance with
ISO 15009. Some mono- and dichlorophenols, for instance, and naphthalene also belong to this group.
© ISO 2003 — All rights reserved 1
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ISO 14507:2003(E)
NOTE 2 The selection of the categories for volatile and moderately volatile compounds can be related in principle to
the vapour pressure. However, as the vapour pressure of only a small number of compounds is known, and in view of the
relationship between vapour pressure and boiling point, the boiling point has been chosen as the criterion for distinction.
See Annex A.
3.2
moderately volatile compound
organic compound having a boiling point above 300 °C (at a pressure of 101 kPa)
NOTE 1 This definition includes:
a) mineral oil (see ISO/TR 11046);
b) most polycyclic aromatic hydrocarbons (PAH) (see ISO 13877);
c) polychlorobiphenyls (PCB) (see ISO 10382);
d) organochlorine pesticides (see ISO 10382).
NOTE 2 In ISO/TR 11046, mineral oil is defined as the group of hydrocarbons which, on chromatography, have
retention times lying between that of n-decane (C H ) and n-tetracontane (C H ). As in this International Standard the
10 22 40 82
limit for volatile compounds lies at a boiling point of 300 °C [approximately hexadecane (C )], this means that mineral oil
16
should be considered as a volatile compound, as part of the compounds to be determined fall within the boiling point range
of volatile compounds. However for practical reasons, it has been decided that the pretreatment for moderately volatile
compounds should be specified for the determination of mineral oil. As a result of cryogenic crushing, an improvement in
the extraction yield occurs for compounds with a boiling point above 300 °C. The possible losses for the lower-boiling
hydrocarbons (C to C ) are assumed to be low, due to the retaining effect of the higher-boiling hydrocarbons present in
10 16
mineral oil and to be compensated by the higher extraction yield of the other hydrocarbons present. As the total yield is
used to determine the mineral oil as a group parameter, it is assumed that pretreatment using the method for moderately
volatile compounds gives the best results at present.
4 Principle
4.1 Sampling
Sampling shall be carried out in accordance with ISO 10381-1. The samples taken shall be kept cool and
processed as soon as possible. The method of pretreatment depends on the volatility of the organic
compound(s) or group(s) of organic compounds to be determined.
When taking a subsample, the quantity of soil should be removed from the sample container in such a way
that this quantity:
a) is a subsample over the full depth of the sample, and
b) can be taken quickly.
4.2 Volatile compounds
For determination of volatile organic compounds, core test samples are taken from the sample and extracted
according to the relevant specific analytical procedure. If composite samples are required, extracts of
individual samples are mixed. It is not possible to obtain composite samples without severe losses of volatiles.
The procedure is described in 8.2.
4.3 Moderately volatile compounds
Samples are chemically dried at a low temperature (− 196 °C, liquid nitrogen). The dried samples are cooled
with liquid nitrogen and ground with a cross-beater mill with a sieve of 1 mm mesh size (cryogenic crushing).
After grinding, suitable test portions are processed according to the relevant specific analytical procedures.
Composite samples can be prepared by mixing the ground samples. This procedure is described in 8.3.
2 © ISO 2003 — All rights reserved
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ISO 14507:2003(E)
If the extraction procedure requires a field-moist sample, drying and grinding are not possible.
If the original sample only contains a small fraction of particles greater than 2 mm and the distribution of
contaminants is likely to be homogeneous, grinding may be omitted. In these two cases, suitable test portions
are taken directly after mixing the sample. This procedure is described in 8.4.
NOTE 1 To distinguish the volatile organic compounds from the moderately volatile organic compounds, boiling points
are used instead of the vapour pressure at ambient temperature. This is explained in Annex A, which also gives boiling
points and vapour pressures of compounds regularly determined in soil investigations.
NOTE 2 For some specific components in the group of moderately volatile organic compounds, freeze-drying may give
good results. In this International Standard freeze-drying is not described.
5 Reagents
Use only reagents of recognized analytical quality. Check samples of each batch of the reagents for the
presence of contaminating compounds.
5.1 Sodium sulfate, anhydrous.
Heat the sodium sulfate before use for at least 6 h at about 550 °C to remove crystalline water and organic
materials. After heating, allow to cool in a desiccator and store in a closed container.
5.2 Magnesium silicate (talcum powder).
5.3 Sand or gravel.
Before use, wash the sand or gravel at least twice with an equivalent mass of demineralized water and then
heat for 6 h at about 550 °C to remove organic materials.
5.4 Liquid nitrogen.
For safety precautions, see warnings in 8.3.2.
6 Apparatus
Usual laboratory glassware and equipment, and in particular:
6.1 Glass containers with a volume of 750 ml to 1 000 ml, with a wide neck and screw cap with a
polytetrafluoroethylene (PTFE) inlay.
6.2 Polyethylene containers with a volume of 750 ml to 1 000 ml, with a wide neck and screw cap. To
prevent a significant headspace being formed, do not use larger containers.
6.3 Refrigerator, capable of maintaining a temperature below 10 °C.
6.4 Dewar vessel(s), capable of holding at least one polyethylene container of about 750 ml.
6.5 Cross-beater mill or mill with comparable qualities, with a sieve of mesh size 1 mm and accessories. A
cross-beater mill as used in most soil laboratories is suitable for milling soil samples cooled with liquid
nitrogen.
6.6 Gloves, suitable for working at low temperatures.
6.7 Oven, suitable for heating to about 550 °C.
© ISO 2003 — All rights reserved 3
---------------------- Page: 8 ----------------------
ISO 14507:2003(E)
6.8 Core cutter or similar instrument, for example apple corer. Depending on the type of soil (sand, clay),
different instruments can be used.
7 Preservation and storage
Do not preserve the samples, but analyse them as soon as possible. Between sampling in the field and
analysis store the samples below 10 °C, if possible in a refrigerator (6.3). The maximum storage time for a
sample kept in the dark below 10 °C depends on the parameter(s) to be determined, but can also depend on
the material used for the container. Details can be obtained from the relevant specific analytical standards.
The storage time also depends on possibilities of volatization and biological degradation. If these processes
are likely to occur, then the storage time should not exceed four days. In cases with no volatization, poorly
biodegradable compounds present and biologically less active soil, longer storage times are possible.
If rapid microbial decomposition of the compounds to be determined can be expected, the sample should be
pretreated immediately after receipt at the laboratory. For samples containing volatile organic compounds in
particular, the storage time should preferably be as short as possible and analysis carried out as soon as
possible, e.g. within 1 day to 2 days.
NOTE Chemically dried and ground samples are generally stable for longer periods if stored in a cool, dark location.
Freezing samples could extend the useful storage time.
8 Procedure
8.1 General
The pretreatment method depends on the volatility of the substance(s) or group(s) of substances to be
determined. Two categories are distinguished here:
a) Volatile compounds: boiling point < 300 °C.
b) Moderately volatile organic compounds: boiling point > 300 °C:
1) grinding necessary;
2) grinding not possible or not necessary.
The method for pretreating samples containing volatile organic compounds is described in 8.2.
The method for pretreating samples containing moderately volatile organic compounds using grinding is
described in 8.3. If grinding is not necessary or the required result is only qualitative, the method described in
8.4 is used.
If the pretreatment methods differ for various parameters to be determined, divide the sample before
pretreatment into subsamples which are as large as possible.
If it is known in advance that both volatile organic compounds and other parameters are to be determined in a
sample, it is essential that a separate sample be taken in the f
...
SLOVENSKI STANDARD
SIST ISO 14507:2019
01-oktober-2019
Kakovost tal - Priprava vzorcev za določevanje organskih onesnaževal
Soil quality - Pretreatment of samples for determination of organic contaminants
Qualité du sol - Prétraitement des échantillons pour la détermination des contaminants
organiques
Ta slovenski standard je istoveten z: ISO 14507:2003
ICS:
13.080.01 Kakovost tal in pedologija na Soil quality and pedology in
splošno general
SIST ISO 14507:2019 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST ISO 14507:2019
---------------------- Page: 2 ----------------------
SIST ISO 14507:2019
INTERNATIONAL ISO
STANDARD 14507
First edition
2003-03-15
Soil quality — Pretreatment of samples
for determination of organic
contaminants
Qualité du sol — Prétraitement des échantillons pour la détermination
des contaminants organiques
Reference number
ISO 14507:2003(E)
©
ISO 2003
---------------------- Page: 3 ----------------------
SIST ISO 14507:2019
ISO 14507:2003(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2003
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 2003 — All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 14507:2019
ISO 14507:2003(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope. 1
2 Normative references . 1
3 Terms and definitions. 1
4 Principle . 2
4.1 Sampling . 2
4.2 Volatile compounds. 2
4.3 Moderately volatile compounds . 2
5 Reagents . 3
6 Apparatus . 3
7 Preservation and storage. 4
8 Procedure . 4
8.1 General. 4
8.2 Volatile compounds (boiling point < 300 °°°°C). 5
8.3 Moderately volatile organic compounds (boiling point > 300 °°°°C) — Grinding necessary . 5
8.4 Moderately volatile organic compounds (boiling point > 300 °°C) — Grinding not possible
°°
or not necessary . 7
8.5 Blank measurements. 8
9 Test report . 8
Annex A (informative) Information concerning vapour pressure, boiling and melting points of
volatile organic compounds . 9
Annex B (informative) Validation . 12
Bibliography . 14
© ISO 2003 — All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 14507:2019
ISO 14507:2003(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 14507 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
methods and soil characteristics.
iv © ISO 2003 — All rights reserved
---------------------- Page: 6 ----------------------
SIST ISO 14507:2019
ISO 14507:2003(E)
Introduction
The properties of organic micropollutants can differ greatly according to chemical species:
they can range from non-volatile to very volatile compounds (low to high vapour pressure);
they can be labile or reactive at ambient or elevated temperatures;
they can be biodegradable or UV-degradable;
they can have considerably different solubilities in water;
they require different analytical procedures.
Because of these differences, a general pretreatment procedure cannot be proposed. The goal of a
pretreatment procedure is to prepare a test sample in which the concentration of the contaminant is equal to
the concentration in the original soil, provided, however, that this procedure does not alter the chemical
species to be analysed. For instance, if the sample contains only small particles and the contaminant is
homogeneously distributed, it is not necessary to grind the sample. In this International Standard, the size
2 mm is used to distinguish between small and large soil particles.
Consistency among the following aspects is important:
soil diversity;
the aim of the analysis (including its accuracy);
the nature of the chemical species to be analysed.
The particle size distribution of the sample in relation to the mass of sample taken for analysis is also
important to pretreatment. For the analysis of organic contaminants, the sample mass taken in most cases is
about 20 g.
With such a sample mass, and provided that the contaminant is homogeneously distributed and the particles
in the sample are smaller than about 2 mm, further grinding of the sample is not necessary. If the sample
contains large particles or if the contaminant is heterogeneously distributed (as occurs for instance with tar
particles), it is not possible to take a representative test sample of about 20 g without grinding the sample. To
improve the homogeneity, samples are ground to a size smaller than 1 mm. Prior to analysis, very often no
information about the distribution of the contaminant in the soil is known.
Some analytical procedures start with a field-moist sample. Drying of the sample gives lower extraction
results. If the sample is not dried, grinding is not possible.
In a situation in which accurate results are needed, the best available pretreatment procedure should be used.
If it is necessary to establish whether the concentration is above a certain limit and it is already known that the
soil is heavily polluted, the simplest pretreatment procedure may meet the need. In this case however, the
result may not be presented as a representative value for the whole sample.
The choice depends above all on the volatility of the organic compounds under analysis. It also depends on
the soil particle size distribution, the heterogeneity of the sample and the analytical procedure.
© ISO 2003 — All rights reserved v
---------------------- Page: 7 ----------------------
SIST ISO 14507:2019
---------------------- Page: 8 ----------------------
SIST ISO 14507:2019
INTERNATIONAL STANDARD ISO 14507:2003(E)
Soil quality — Pretreatment of samples for determination of
organic contaminants
1 Scope
This International Standard specifies three methods for the pretreatment of soil samples in the laboratory prior
to the determination of organic contaminants:
if volatile organic compounds are to be measured;
if moderately volatile to non-volatile organic compounds are to be measured, if the result of the
subsequent analysis must be accurate and reproducible, and if the sample contains particles larger than
2 mm and/or the contaminant is heterogeneously distributed;
if non-volatile organic compounds are to be measured and the extraction procedure prescribes a field-
moist sample, or if the largest particles of the sample are smaller than 2 mm and the contaminant is
homogeneously distributed. This procedure is also applicable if reduced accuracy and repeatability are
acceptable.
The pretreatment described in this International Standard is used in combination with an extraction procedure
in which the contaminant is available for the extraction liquid.
NOTE For the pretreatment of soil samples for the purposes of determining non-volatile inorganic compounds and
physico-chemical soil characteristics, see ISO 11464.
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 10381-1, Soil quality — Sampling — Part 1: Guidance on the design of sampling programmes
ISO 11074-2, Soil quality — Vocabulary — Part 2: Terms and definitions relating to sampling
ISO 11465:1993, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric
method
3 Terms and definitions
For the purposes of this document, the terms and definitions in ISO 11074-2 and the following apply:
3.1
volatile compound
organic compound having a boiling point below 300 °C (at a pressure of 101 kPa)
NOTE 1 This includes volatile aromatic and volatile halogenated hydrocarbons as determined in accordance with
ISO 15009. Some mono- and dichlorophenols, for instance, and naphthalene also belong to this group.
© ISO 2003 — All rights reserved 1
---------------------- Page: 9 ----------------------
SIST ISO 14507:2019
ISO 14507:2003(E)
NOTE 2 The selection of the categories for volatile and moderately volatile compounds can be related in principle to
the vapour pressure. However, as the vapour pressure of only a small number of compounds is known, and in view of the
relationship between vapour pressure and boiling point, the boiling point has been chosen as the criterion for distinction.
See Annex A.
3.2
moderately volatile compound
organic compound having a boiling point above 300 °C (at a pressure of 101 kPa)
NOTE 1 This definition includes:
a) mineral oil (see ISO/TR 11046);
b) most polycyclic aromatic hydrocarbons (PAH) (see ISO 13877);
c) polychlorobiphenyls (PCB) (see ISO 10382);
d) organochlorine pesticides (see ISO 10382).
NOTE 2 In ISO/TR 11046, mineral oil is defined as the group of hydrocarbons which, on chromatography, have
retention times lying between that of n-decane (C H ) and n-tetracontane (C H ). As in this International Standard the
10 22 40 82
limit for volatile compounds lies at a boiling point of 300 °C [approximately hexadecane (C )], this means that mineral oil
16
should be considered as a volatile compound, as part of the compounds to be determined fall within the boiling point range
of volatile compounds. However for practical reasons, it has been decided that the pretreatment for moderately volatile
compounds should be specified for the determination of mineral oil. As a result of cryogenic crushing, an improvement in
the extraction yield occurs for compounds with a boiling point above 300 °C. The possible losses for the lower-boiling
hydrocarbons (C to C ) are assumed to be low, due to the retaining effect of the higher-boiling hydrocarbons present in
10 16
mineral oil and to be compensated by the higher extraction yield of the other hydrocarbons present. As the total yield is
used to determine the mineral oil as a group parameter, it is assumed that pretreatment using the method for moderately
volatile compounds gives the best results at present.
4 Principle
4.1 Sampling
Sampling shall be carried out in accordance with ISO 10381-1. The samples taken shall be kept cool and
processed as soon as possible. The method of pretreatment depends on the volatility of the organic
compound(s) or group(s) of organic compounds to be determined.
When taking a subsample, the quantity of soil should be removed from the sample container in such a way
that this quantity:
a) is a subsample over the full depth of the sample, and
b) can be taken quickly.
4.2 Volatile compounds
For determination of volatile organic compounds, core test samples are taken from the sample and extracted
according to the relevant specific analytical procedure. If composite samples are required, extracts of
individual samples are mixed. It is not possible to obtain composite samples without severe losses of volatiles.
The procedure is described in 8.2.
4.3 Moderately volatile compounds
Samples are chemically dried at a low temperature (− 196 °C, liquid nitrogen). The dried samples are cooled
with liquid nitrogen and ground with a cross-beater mill with a sieve of 1 mm mesh size (cryogenic crushing).
After grinding, suitable test portions are processed according to the relevant specific analytical procedures.
Composite samples can be prepared by mixing the ground samples. This procedure is described in 8.3.
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If the extraction procedure requires a field-moist sample, drying and grinding are not possible.
If the original sample only contains a small fraction of particles greater than 2 mm and the distribution of
contaminants is likely to be homogeneous, grinding may be omitted. In these two cases, suitable test portions
are taken directly after mixing the sample. This procedure is described in 8.4.
NOTE 1 To distinguish the volatile organic compounds from the moderately volatile organic compounds, boiling points
are used instead of the vapour pressure at ambient temperature. This is explained in Annex A, which also gives boiling
points and vapour pressures of compounds regularly determined in soil investigations.
NOTE 2 For some specific components in the group of moderately volatile organic compounds, freeze-drying may give
good results. In this International Standard freeze-drying is not described.
5 Reagents
Use only reagents of recognized analytical quality. Check samples of each batch of the reagents for the
presence of contaminating compounds.
5.1 Sodium sulfate, anhydrous.
Heat the sodium sulfate before use for at least 6 h at about 550 °C to remove crystalline water and organic
materials. After heating, allow to cool in a desiccator and store in a closed container.
5.2 Magnesium silicate (talcum powder).
5.3 Sand or gravel.
Before use, wash the sand or gravel at least twice with an equivalent mass of demineralized water and then
heat for 6 h at about 550 °C to remove organic materials.
5.4 Liquid nitrogen.
For safety precautions, see warnings in 8.3.2.
6 Apparatus
Usual laboratory glassware and equipment, and in particular:
6.1 Glass containers with a volume of 750 ml to 1 000 ml, with a wide neck and screw cap with a
polytetrafluoroethylene (PTFE) inlay.
6.2 Polyethylene containers with a volume of 750 ml to 1 000 ml, with a wide neck and screw cap. To
prevent a significant headspace being formed, do not use larger containers.
6.3 Refrigerator, capable of maintaining a temperature below 10 °C.
6.4 Dewar vessel(s), capable of holding at least one polyethylene container of about 750 ml.
6.5 Cross-beater mill or mill with comparable qualities, with a sieve of mesh size 1 mm and accessories. A
cross-beater mill as used in most soil laboratories is suitable for milling soil samples cooled with liquid
nitrogen.
6.6 Gloves, suitable for working at low temperatures.
6.7 Oven, suitable for heating to about 550 °C.
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6.8 Core cutter or similar instrument, for example apple corer. Depending on the type of soil (sand, clay),
different instruments can be used.
7 Preservation and storage
Do not preserve the samples, but analyse them as soon as possible. Between sampling in the field and
analysis store the samples below 10 °C, if possible in a refrigerator (6.3). The maximum storage time for a
sample kept in the dark below 10 °C depends on the parameter(s) to be determined, but can also depend on
the material used for the container. Details can be obtained from the relevant specific analytical standards.
The storage time also depends on possibilities of volatization and biological degradation. If these processes
are likely to occur, then the storage time should not exceed four days. In cases with no volatization, poorly
biodegradable compounds present and biologically less active soil, longer storage times are possible.
If rapid microbial decomposition of the compounds to be determined can be expected, the sample should be
pretreated immediately after receipt at the laboratory. For samples containing volatile organic compounds in
particular, the storage time should preferably be as short as possible and analysis carried out as soon as
possible, e.g. within 1 day to 2 days.
NOTE Chemically dried and ground samples are generally stable for longer periods if stored in a cool, dark location.
Freezing samples could extend the useful storage time.
8 Procedure
8.1 General
The pretreatment method depends on the volatility of the substance(s) or group(s) of substances to be
determined. Two categories are distinguished here:
a) Volatile compounds: boiling point < 300 °C.
b) Moderately volatile organic compounds: boiling point > 300 °C:
1) grinding necessary;
2) grinding not possible or not necessary.
The method for pretreating samples containing volatile organic compounds is described in 8.2.
The method for pretreating samples containing moderately volatile organic compounds using grinding is
des
...
NORME ISO
INTERNATIONALE 14507
Première édition
2003-03-15
Qualité du sol — Prétraitement des
échantillons pour la détermination des
contaminants organiques
Soil quality — Pretreatment of samples for determination of organic
contaminants
Numéro de référence
ISO 14507:2003(F)
©
ISO 2003
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ISO 14507:2003(F)
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Publié en Suisse
ii © ISO 2003 — Tous droits réservés
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ISO 14507:2003(F)
Sommaire Page
Avant-propos. iv
Introduction . v
1 Domaine d'application. 1
2 Références normatives. 1
3 Termes et définitions. 1
4 Principe . 2
4.1 Échantillonnage . 2
4.2 Composés volatils . 2
4.3 Composés peu volatils. 2
5 Réactifs . 3
6 Appareillage. 3
7 Conservation . 4
8 Mode opératoire . 4
8.1 Généralités. 4
8.2 Composés volatils (point d’ébullition <<<< 300 °C). 5
8.3 Composés peu volatils (point d’ébullition >>>> 300 °C) ― Broyage nécessaire . 5
8.4 Composés organiques peu volatils (point d’ébullition >> 300 °C) ― Broyage impossible ou
>>
inutile. 8
8.5 Essais à blanc . 8
9 Rapport d’essai . 8
Annexe A (informative) Informations concernant la pression de vapeur, les points d'ébullition et
de fusion des composés organiques volatils . 10
Annexe B (informative) Validation . 13
Bibliographie . 15
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ISO 14507:2003(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 (CEI) en ce qui concerne la normalisation électrotechnique.
Les Normes internationales sont rédigées conformément aux règles données dans les Directives ISO/CEI,
Partie 2.
Les projets de Normes internationales adoptés par les comités techniques sont soumis aux comités membres
pour vote. Leur publication comme Normes internationales requiert l'approbation de 75 % au moins des
comités membres votants.
L’attention est appelée sur le fait que certains des éléments de la présente/du présent Norme internationale
peuvent faire l’objet de droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue
pour responsable de ne pas avoir identifié de tels droits de propriété et averti de leur existence.
L’ISO 14507 a été élaborée par le comité technique ISO/TC 190, Qualité du sol, sous-comité SC 3, Méthodes
chimiques et caractéristiques du sol.
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ISO 14507:2003(F)
Introduction
Les caractéristiques des micropolluants organiques peuvent présenter des différences importantes en
fonction de leur espèce chimique:
leur gamme de volatilité peut aller des composants non volatils aux composants très volatils (pression de
vapeur faible à élevée);
ils peuvent être labiles ou réactifs à température ambiante comme à des températures élevées;
ils peuvent être biodégradables ou dégradables aux U.V.;
leur solubilité dans l’eau peut être extrêmement variable;
ils nécessitent différentes méthodes d’analyse.
Ces différences font qu’il n’est pas possible de proposer une méthode générale de prétraitement. Le but d’une
méthode de prétraitement est de préparer un échantillon pour essai dont le contaminant a une concentration
identique à celle du sol d’origine, à condition, toutefois, que cette méthode ne modifie pas l’espèce chimique à
analyser. Par exemple, si l’échantillon contient uniquement des petites particules et que le contaminant est
réparti de façon homogène, il n’est pas nécessaire de broyer l’échantillon. Dans la présente Norme
internationale, la taille de 2 mm est utilisée pour faire la distinction entre petites et grosses particules de sol.
La compatibilité entre les aspects suivants est importante:
la diversité du sol;
le but de l’analyse (y compris sa précision);
la nature de l’espèce chimique à analyser.
La répartition granulométrique de l’échantillon par rapport à la masse d’échantillon prélevée pour l’analyse est
importante pour le prétraitement. Pour l’analyse des contaminants organiques, la masse prélevée pour
analyse est d’environ 20 g dans la plupart des cas.
Avec cette masse d’échantillon et à condition que la répartition du contaminant soit homogène et que la taille
des particules soit inférieure à 2 mm environ dans l’échantillon, il n’est pas nécessaire de procéder à un
nouveau broyage de l’échantillon. Si l’échantillon contient de grosses particules ou si la répartition du
contaminant est hétérogène (comme c’est le cas, par exemple, avec les particules de goudron), il est
impossible de prélever un échantillon pour essai représentatif de 20 g environ sans broyer l’échantillon. Pour
améliorer l’homogénéité, les échantillons sont broyés à moins de 1 mm. Avant l’analyse, on ne dispose très
souvent d’aucune information sur la répartition du contaminant dans le sol.
Certaines méthodes d’analyse démarrent avec un échantillon brut prélevé sur le terrain. Le séchage de
l’échantillon donnera des résultats d’extraction inférieurs. Si l’échantillon n’est pas séché, le broyage est
impossible.
Dans une situation nécessitant des résultats précis, il convient d’utiliser la meilleure méthode de prétraitement
disponible. Le prétraitement le plus simple peut répondre aux besoins si les analyses ont pour objectif de
contrôler le dépassement de certaines limites et si l’on sait déjà que le sol est fortement pollué. Dans ce cas,
le résultat ne peut pas être présenté comme une valeur représentative de la totalité de l’échantillon.
Le choix dépend avant tout de la volatilité des composés organiques soumis à l’analyse. Il dépend également
de la répartition granulométrique du sol, de l’hétérogénéité de l’échantillon et de la méthode d’analyse qui suit.
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NORME INTERNATIONALE ISO 14507:2003(F)
Qualité du sol — Prétraitement des échantillons pour la
détermination des contaminants organiques
1 Domaine d'application
La présente Norme internationale spécifie trois méthodes de prétraitement des échantillons de sol en
laboratoire avant détermination des contaminants organiques:
une méthode de prétraitement s’il faut mesurer des composés organiques volatils;
une méthode de prétraitement s’il faut mesurer des composés organiques peu volatils à non volatils, si le
résultat de l’analyse ultérieure doit être précis et reproductible et si l’échantillon contient des particules de
taille supérieure à 2 mm et/ou le contaminant est réparti de manière hétérogène;
une méthode de prétraitement s’il faut mesurer des composés organiques non volatils et si la méthode
d’extraction prescrit un échantillon brut prélevé sur le terrain ou encore si les particules les plus grosses
de l’échantillon sont inférieures à 2 mm et que le contaminant est réparti de manière homogène. Cette
méthode peut également être utilisée si une précision et une répétabilité réduites sont acceptables.
La méthode de prétraitement décrite dans la présente Norme internationale est associée à une méthode
d’extraction dans laquelle le contaminant est disponible pour le liquide d’extraction.
NOTE Pour le prétraitement des échantillons de sol en vue de déterminer les composés inorganiques non volatils et
les caractéristiques physico-chimiques du sol, se reporter à l’ISO 11464.
2 Références normatives
Les documents de référence suivants sont indispensables pour l'application du présent document. Pour les
références datées, seule l'édition citée s'applique. Pour les références non datées, la dernière édition du
document de référence s'applique (y compris les éventuels amendements).
ISO 10381-1, Qualité du sol — Échantillonnage — Partie 1: Lignes directrices pour l'établissement des
programmes d'échantillonnage
ISO 11074-2, Qualité du sol — Vocabulaire — Partie 2: Termes et définitions relatifs à l’échantillonnage
ISO 11465:1993, Qualité du sol — Détermination de la teneur pondérale en matière sèche et en eau —
Méthode gravimétrique
3 Termes et définitions
Pour les besoins du présent document, les termes et définitions donnés dans l’ISO 11074-2 ainsi que les
suivants s'appliquent.
3.1
composé volatil
composé organique ayant un point d’ébullition inférieur à 300 °C (pour une pression de 101 kPa)
NOTE 1 Il englobe les hydrocarbures volatils aromatiques et halogénés déterminés conformément à l’ISO 15009.
Certains mono- et dichlorophénols, par exemple, et le naphtalène appartiennent également à ce groupe.
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ISO 14507:2003(F)
NOTE 2 La sélection des catégories de composés volatils et peu volatils peut être liée en principe à la pression de
vapeur. Toutefois, la pression de vapeur d’un petit nombre seulement de composés étant connue et étant donné la
relation entre pression de vapeur et point d’ébullition, cette dernière caractéristique a été choisie comme critère de
distinction. Voir Annexe A.
3.2
composé peu volatil
composé organique ayant un point d’ébullition supérieur à 300 °C (pour une pression de 101 kPa)
NOTE 1 Cette définition comprend:
a) les huiles minérales (voir l’ISO/TR 11046);
b) les hydrocarbures aromatiques polycycliques (HAP) (voir l’ISO 13877);
c) les polychlorobiphényls (voir l’ISO 10382);
d) les pesticides organo-chlorés (voir l’ISO 10382).
NOTE 2 L’ISO/TR 11046 définit les huiles minérales comme étant le groupe des hydrocarbures dont les temps de
rétention en chromatographie se situent entre ceux du n-décane (C H ) et ceux du n-tétracontane (C H ). La limite
10 22 40 82
des composés volatils se situant dans la présente Norme internationale à un point d’ébullition de 300 °C
[approximativement l’hexadécane (C )], cela signifie qu’il convient de considérer les huiles minérales, comme composés
16
volatils, car une partie des composés à déterminer ont des points d’ébullition entrant dans la plage définie pour la
classification des composés volatils. Toutefois, il a été décidé, pour des raisons pratiques, qu’il convient de prescrire le
prétraitement des composés peu volatils en vue du dosage des huiles minérales. Le concassage cryogénique entraîne
une amélioration du rendement d’extraction pour les composés dont le point d’ébullition est supérieur à 300 °C. Les pertes
éventuelles pour les hydrocarbures à point d’ébullition inférieur (C à C ) sont supposées faibles du fait de l’effet de
10 16
rétention des hydrocarbures à point d’ébullition élevé présents dans les huiles minérales et compensées par le rendement
d’extraction plus élevé des autres hydrocarbures présents. Le rendement total servant à déterminer l’huile minérale
comme paramètre de groupe, on suppose que le prétraitement utilisant la méthode applicable aux composés peu volatils
donne actuellement les meilleurs résultats.
4 Principe
4.1 Échantillonnage
L’échantillonnage doit être effectué selon l’ISO 10381-1. Une fois prélevés, les échantillons doivent être
conservés au froid et traités dès que possible. La méthode de prétraitement dépend de la volatilité du (des)
composé(s) organique(s) ou du (des) groupe(s) de composés organiques à déterminer.
Lors du prélèvement d’un sous-échantillon, il convient de retirer la quantité de sol du récipient pour échantillon
de manière que cette quantité:
a) soit un sous-échantillon de la profondeur totale de l’échantillon; et
b) puisse être prélevée rapidement.
4.2 Composés volatils
Pour la détermination des composés organiques volatils, les carottes pour essai sont prélevées sur
l’échantillon et extraites selon la méthode d’analyse spécifique. S’il faut des échantillons composites, des
extraits d’échantillons individuels sont mélangés. Il est impossible d’obtenir des échantillons composites sans
pertes sévères en produits volatils. La méthode est décrite en 8.2.
4.3 Composés peu volatils
Les échantillons font l’objet d’un séchage chimique à basse température (− 196 °C, azote liquide). Les
échantillons séchés sont refroidis à l’azote liquide et broyés à l’aide d’un broyeur à fléaux muni d’un tamis de
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ISO 14507:2003(F)
1 mm (concassage cryogénique). Après broyage, des prises d’essai appropriées sont traitées selon les
méthodes d’analyse spécifiques. Des échantillons composites peuvent être préparés en mélangeant les
échantillons broyés. Cette méthode est décrite en 8.3.
Si la méthode d’extraction prescrit un échantillon brut prélevé sur le terrain, le séchage et le broyage ne sont
pas possibles.
Si les échantillons d’origine ne contiennent qu’une petite fraction de particules de plus de 2 mm et si la
répartition des contaminants est normalement homogène, on peut renoncer au broyage. Dans ces deux cas,
des prises d’essai appropriées sont prélevées directement après broyage de l’échantillon. Cette méthode est
décrite en 8.4.
NOTE 1 On utilise les points d’ébullition au lieu de la pression de vapeur à température ambiante pour distinguer les
composés organiques volatils des composés organiques peu volatils. L’explication est donnée en Annexe A qui indique
également les points d’ébullition et la pression de vapeur des composés régulièrement déterminés lors des investigations
de sol.
NOTE 2 Pour certains composés spécifiques du groupe des composés organiques peu volatils, la lyophilisation peut
donner de bons résultats. La lyophilisation n’est pas décrite dans la présente Norme internationale.
5 Réactifs
Utiliser uniquement des réactifs de qualité analytique reconnue. Vérifier les échantillons de chaque lot de
réactifs pour déterminer la présence de composés contaminants.
5.1 Sulfate de sodium anhydre.
Traiter le sulfate de sodium pendant au moins 6 h à 550 °C environ pour retirer l’eau de cristallisation et les
matières organiques. Après chauffage, le laisser refroidir dans un dessiccateur et le conserver dans un
récipient fermé.
5.2 Silicate de magnésium (poudre de talc).
5.3 Sable ou gravier.
Avant utilisation, laver le sable ou le gravier au moins deux fois avec une quantité équivalente (même masse)
d’eau déminéralisée, puis le chauffer pendant 6 h à 550 °C environ, afin de retirer les matières organiques.
5.4 Azote liquide.
Pour les précautions de sécurité, voir les avertissements en 8.3.2.
6 Appareillage
Verrerie et matériel courants de laboratoire et en particulier:
6.1 Fioles en verre, d’un volume compris entre 750 ml et 1 000 ml, à large col et couvercle vissé, avec
joint à face en polytétrafluoréthylène (PTFE).
6.2 Récipients en polyéthylène, d’un volume compris entre 750 ml et 1 000 ml, à large col et couvercle
vissé. Ne pas utiliser de récipients plus grands afin d’éviter de créer un espace de tête important.
6.3 Réfrigérateur, pouvant maintenir une température inférieure à 10 °C.
6.4 Vase(s) de Dewar, capable(s) de contenir au moins un récipient en polyéthylène de 750 ml environ.
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ISO 14507:2003(F)
6.5 Broyeur à fléaux, muni d’un tamis ayant une ouverture de maille de 1 mm et d’accessoires. Le broyeur
à fléaux utilisé dans la plupart des laboratoires de sol convient pour moudre des échantillons de sol refroidis à
l’azote liquide.
6.6 Gants, convenant pour travailler à basses températures.
6.7 Étuve, convenant pour chauffer à 550 °C environ.
6.8 Carotteuse ou instrument analogue, par exemple un évideur à pomme. Différents instruments peuvent
être utilisés en fonction du type de sol (sable, argile).
7 Conservation
Ne pas conserver les échantillons mais les analyser dès que possible. Entre le prélèvement sur le terrain et
l’analyse, entreposer les échantillons à une température inférieure à 10 °C, si possible dans un réfrigérateur
(6.3). La durée de stockage maximum d’un échantillon conservé dans l’obscurité à une température inférieure
à 10 °C dépend du ou des paramètres à déterminer; toutefois, elle peut également dépendre du matériau
utilisé pour le récipient. Les normes d’analyses spécifiques peuvent fournir de plus amples détails.
La durée de stockage dépend aussi des possibilités de volatilisation et de dégradation biologique. Si ces
processus sont susceptibles de se produire, il convient alors de ne pas dépasser quatre jours de stockage. En
cas d’absence de volatilisation, de composés faiblement biodégradables et d’un sol moins actif, des durées
de stockage plus longues sont possibles.
Si l’on peut s’attendre à une décomposition microbienne rapide des composés à déterminer, il convient de
prétraiter l’échantillon dès réception au laboratoire. Pour le groupe des composés organiques volatils en
particulier, il est préférable que la durée de conservation soit aussi brève que possible et que l’analyse soit
effectuée dès que possible, par exemple au bout de 1 jour ou 2 jours.
NOTE Les échantillons séchés chimiquement et broyés sont généralement stables plus longtemps s’ils sont
conservés au froid et dans l’obscurité. La congélation des échantillons pourrait prolonger la durée de stockage utile.
8 Mode opératoire
8.1 Généralités
La méthode de prétraitement dépend de la volatilité de la ou des substances ou du ou des groupes de
substances à déterminer. On distingue ici deux catégories:
a) Composés organiques volatils: point d’ébullition < 300 °C.
b) Composés organiques peu volatils: point d’ébullition > 300 °C:
1) broyage nécessaire;
2) broyage impossible ou inutile.
La méthode concernant les composés organiques volatils est décrite en 8.2.
La méthode applicable aux composés organiques peu volatils et comportant un broyage est décrite en 8.3. Si
le broyage est inutile ou si le résultat exigé est uniquement qualitatif, la méthode décrite en 8.4 est utilisée.
Si les méthodes de prétraitement diffèrent pour les divers paramètres à déterminer, diviser l’échantillon avant
prétraitement en sous-échantillons aussi importants que possible.
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ISO 14507:2003(F)
Si l’on doit déterminer simultanément les composés organiques volatils ainsi que d’autres paramètres sur un
même échantillon, il est indispensable de prélever un échantillon séparé sur le terrain pour les composés
volatils conformément à la Norme internationale appropriée.
Pour les besoins du calcul de la teneur en composés organiques volatils et peu volatils à partir d’une matière
sèche, la teneur en matière sèche doit être déterminée conformément à l’ISO 11465 sur un sous-échantillon
de l’échantillon d’origine (brut).
8.2 Composés volatils (point d’ébullition <<<< 300 °C)
8.2.1 Généralités
Il n’est effectué aucun prétraitement des échantillons sur lesquels il faut analyser les composés volatils.
Prélever les échantillons pour essai dès que possible pour éviter les pertes.
Les échantillons pour essai peuvent être prélevés et extraits sur le terrain. Il convient de prendre des
précautions pour éviter toute contamination du liquide d’extraction. Il convient de vérifier ce point en utilisant
des blancs prélevés sur le terrain et soumis aux mêmes méthodes que les échantillons. Sinon, il convient de
recouvrir l’échantillon de solution d’extraction, de fermer hermétiquement le récipient et de le transporter au
froid jusqu’au laboratoire afin de procéder à l’extraction.
8.2.2 Échantillons individuels
Conserver les échantillons dans le réfrigérateur (6.3) avant traitement. À l’aide d’une carotteuse (6.8), prélever
une ou plusieurs carottes de sol dans le récipient de manière à ce que la masse combinée des carottes
corresponde à la taille requise de l’échantillon pour essai (voir Article 2 et la Bibliographie pour les Normes
internationales correspondantes).
En cas de prélèvement d’un plus grand nombre de carottes de sol et/ou de prélèvement d’un plus grand
nombre d’échantillons pour essai dans le même récipient, prélever si possible les carottes en différents points
du récipient.
8.2.3 Échantillons composites
Il n’est pas possible de constituer des échantillons composites pour l’analyse de composés organiques
volatils. Si la méthode d’analyse fait intervenir un extrait liquide, un extrait composite peut être préparé en
mélangeant des volumes équivalents d’extraits des différents échantillons.
8.3 Composés peu volatils (point d’ébullition >>>> 300 °C) ― Broyage nécessaire
8.3.1 Généralités
Retirer tous les éléments qui ne sont pas représentatifs du sol, par exemple tous les éléments métalliques
visibles.
Le rapport d’analyse doit comporter une note à cet effet.
8.3.2 Échantillons individuels
8.3.2.1 Séchage chimique
Pour chaque échantillon à analyser, ajouter environ 200 g de sulfate de sodium (5.1) et environ 50 g de
silicate de magnésium (5.2) dans une fiole en verre (6.1). Déterminer la masse totale de ces substances avec
une précision de 0,1 g. Après avoir hermétiquement fermé la fiole, agiter les deux substances pour les
mélanger et refroidir à une température inférieure à 10 °C.
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ISO 14507:2003(F)
Pour chaque échantillon, ajouter environ 250 g de sol (pesés à 0,1 g près) dans la fiole en verre contenant le
sulfate de sodium et le silicate de magnésium.
Fermer la fiole et agiter le sol avec les substances additives pour les mélanger. Placer la fiole dans un
réfrigérateur (6.3) et la laisser reposer au froid pendant 12 h à 16 h. Agiter vigoureusement la fiole toutes les
heures pendant les 4 premières heures pour éviter la formation de mottes. Agiter à nouveau vigoureusement
les échantillons avant la fin du temps de séchage.
Les grosses mottes de plus de 3 cm, par exemple, qui se forment éventuellement en phase initiale, peuvent
être écrasées en les coupant avec une spatule dans le récipient. Cette opération peut s’avérer tout
particulièrement nécessaire avec un sol d’argile lourd.
Si l’humidité est supérieure à 60 %, il faut rajouter du sulfate de sodium au lieu de réduire la quantité
d’échantillon. Si l’échantillon a un faible taux d’humidité et n’a pas formé de mottes, il est possible de le laisser
sécher pendant moins de 12 h. Il convient d’assurer un temps de séchage suffisant.
Il convient de conserver l’échantillon aussi longtemps que possible dans un milieu froid avant et après pesée.
NOTE 1 Cette méthode convient moins pour la détermination de composés organiques peu volatils dans les boues ou
les sédiments ayant une teneur en eau élevée. Le séchage chimique d’un tel échantillon avant broyage peut provoquer
des problèmes dus à un séchage insuffisant et à la formation de mottes.
NOTE 2 Si le sol n’est pas correctement mélangé aux additifs dans la phase initiale, il peut se former de grosses
mottes qui ne sécheront plus.
NOTE 3 Si un échantillon n’est pas complètement sec avant le concassage cryogénique, il peut se produire une
contamination considérable du broyeur à fléaux. En particulier des mottes (qui peuvent ne pas être entièrement sèches à
l’intérieur à l’issue d’un temps de séchage trop court) ont une rétention relativement longue dans les mâchoires du
concasseur. Cela provoque un échauffement de la motte et la matière humide est étalée à l’intérieur du concasseur. Cette
contamination est très difficile à éliminer et peut entraîner une contamination sérieuse des échantillons suivants.
8.3.2.2 Broyage
Remplir les vases de Dewar (6.4) avec une quantité suffisante d’azote liquide pour recouvrir entièrement les
récipients en polyéthylène (6.2) placés dans les vases. Transférer rapidement dans un récipient en
polyéthylène le contenu de chaque fiole en verre, y compris le sol et les additifs (voir 8.3.2.1). Fermer
hermétiquement le récipient en polyéthylène et l’immerger complètement dans l’azote liquide. Laisser reposer
le récipient jusqu’à ce que l’azote liquide ne soit plus en forte ébullition. Laisser refroidir pendant environ
10 min. Après refroidissement complet, retirer le récipient de l’azote liquide et en transférer le contenu dans le
broyeur à fléaux (6.5).
Placer le broyeur à fléaux dans une zone bien ventilée. Après chaque échantillon, il convient de nettoyer le
désintégrateur pour éviter de contaminer les échantillons suivants. Une méthode efficace consiste à
concasser une certaine quantité de gravier (5.4) propre (non contaminé) puis à nettoyer le moulin à croisillon
avec un aspirateur.
Après broyage, retirer soigneusement la plateau collecteur se trouvant sous le broyeur à fléaux et prélever les
échantillons pour essai dans le sol concassé. Lors du retrait du plateau collecteur, tenir compte du
dégagement de poussière fine. En conséquence, attendre quelques minutes après l’arrêt du moteur pour
retirer le plateau, mais pas trop longtemps pour éviter le réchauffement de l’échantillon. Il convient de prélever
...
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.YDOQualité du sol - Prétraitement des échantillons pour la détermination des contaminants organiquesSoil quality - Pretreatment of samples for determination of organic contaminants13.080.01Kakovost tal in pedologija na splošnoSoil quality and pedology in generalICS:Ta slovenski standard je istoveten z:ISO 14507:2003oSIST ISO 14507:2019en01-maj-2019oSIST ISO 14507:2019SLOVENSKI
STANDARD
oSIST ISO 14507:2019
Reference numberISO 14507:2003(E)© ISO 2003
INTERNATIONAL STANDARD ISO14507First edition2003-03-15Soil quality — Pretreatment of samples for determination of organic contaminants Qualité du sol — Prétraitement des échantillons pour la détermination des contaminants organiques
oSIST ISO 14507:2019
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oSIST ISO 14507:2019
ISO 14507:2003(E) © ISO 2003 — All rights reserved iii Contents Page Foreword.iv Introduction.v 1 Scope.1 2 Normative references.1 3 Terms and definitions.1 4 Principle.2 4.1 Sampling.2 4.2 Volatile compounds.2 4.3 Moderately volatile compounds.2 5 Reagents.3 6 Apparatus.3 7 Preservation and storage.4 8 Procedure.4 8.1 General.4 8.2 Volatile compounds (boiling point < 300 °°°°C).5 8.3 Moderately volatile organic compounds (boiling point > 300 °°°°C) — Grinding necessary.5 8.4 Moderately volatile organic compounds (boiling point > 300 °°°°C) — Grinding not possible or not necessary.7 8.5 Blank measurements.8 9 Test report.8 Annex A (informative)
Information concerning vapour pressure, boiling and melting points of volatile organic compounds.9 Annex B (informative)
Validation.12 Bibliography.14
oSIST ISO 14507:2019
ISO 14507:2003(E) iv © ISO 2003 — All rights reserved 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 14507 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. oSIST ISO 14507:2019
ISO 14507:2003(E) © ISO 2003 — All rights reserved v Introduction The properties of organic micropollutants can differ greatly according to chemical species: =they can range from non-volatile to very volatile compounds (low to high vapour pressure); =they can be labile or reactive at ambient or elevated temperatures; =they can be biodegradable or UV-degradable; =they can have considerably different solubilities in water; =they require different analytical procedures. Because of these differences, a general pretreatment procedure cannot be proposed. The goal of a pretreatment procedure is to prepare a test sample in which the concentration of the contaminant is equal to the concentration in the original soil, provided, however, that this procedure does not alter the chemical species to be analysed. For instance, if the sample contains only small particles and the contaminant is homogeneously distributed, it is not necessary to grind the sample. In this International Standard, the size 2 mm is used to distinguish between small and large soil particles.
Consistency among the following aspects is important: =soil diversity; =the aim of the analysis (including its accuracy); =the nature of the chemical species to be analysed. The particle size distribution of the sample in relation to the mass of sample taken for analysis is also important to pretreatment. For the analysis of organic contaminants, the sample mass taken in most cases is about 20 g. With such a sample mass, and provided that the contaminant is homogeneously distributed and the particles in the sample are smaller than about 2 mm, further grinding of the sample is not necessary. If the sample contains large particles or if the contaminant is heterogeneously distributed (as occurs for instance with tar particles), it is not possible to take a representative test sample of about 20 g without grinding the sample. To improve the homogeneity, samples are ground to a size smaller than 1 mm. Prior to analysis, very often no information about the distribution of the contaminant in the soil is known. Some analytical procedures start with a field-moist sample. Drying of the sample gives lower extraction results. If the sample is not dried, grinding is not possible. In a situation in which accurate results are needed, the best available pretreatment procedure should be used. If it is necessary to establish whether the concentration is above a certain limit and it is already known that the soil is heavily polluted, the simplest pretreatment procedure may meet the need. In this case however, the result may not be presented as a representative value for the whole sample. The choice depends above all on the volatility of the organic compounds under analysis. It also depends on the soil particle size distribution, the heterogeneity of the sample and the analytical procedure.
oSIST ISO 14507:2019
oSIST ISO 14507:2019
INTERNATIONAL STANDARD ISO 14507:2003(E) © ISO 2003 — All rights reserved 1 Soil quality — Pretreatment of samples for determination of organic contaminants 1 Scope This International Standard specifies three methods for the pretreatment of soil samples in the laboratory prior to the determination of organic contaminants: =if volatile organic compounds are to be measured; =if moderately volatile to non-volatile organic compounds are to be measured, if the result of the subsequent analysis must be accurate and reproducible, and if the sample contains particles larger than 2 mm and/or the contaminant is heterogeneously distributed; =if non-volatile organic compounds are to be measured and the extraction procedure prescribes a field-moist sample, or if the largest particles of the sample are smaller than 2 mm and the contaminant is homogeneously distributed. This procedure is also applicable if reduced accuracy and repeatability are acceptable. The pretreatment described in this International Standard is used in combination with an extraction procedure in which the contaminant is available for the extraction liquid. NOTE For the pretreatment of soil samples for the purposes of determining non-volatile inorganic compounds and physico-chemical soil characteristics, see ISO 11464. 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 10381-1, Soil quality — Sampling — Part 1: Guidance on the design of sampling programmes ISO 11074-2, Soil quality — Vocabulary — Part 2: Terms and definitions relating to sampling ISO 11465:1993, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric method 3 Terms and definitions For the purposes of this document, the terms and definitions in ISO 11074-2 and the following apply: 3.1 volatile compound organic compound having a boiling point below 300 °C (at a pressure of 101 kPa) NOTE 1 This includes volatile aromatic and volatile halogenated hydrocarbons as determined in accordance with ISO 15009. Some mono- and dichlorophenols, for instance, and naphthalene also belong to this group. oSIST ISO 14507:2019
ISO 14507:2003(E) 2 © ISO 2003 — All rights reserved NOTE 2 The selection of the categories for volatile and moderately volatile compounds can be related in principle to the vapour pressure. However, as the vapour pressure of only a small number of compounds is known, and in view of the relationship between vapour pressure and boiling point, the boiling point has been chosen as the criterion for distinction. See Annex A. 3.2 moderately volatile compound organic compound having a boiling point above 300 °C (at a pressure of 101 kPa) NOTE 1 This definition includes: a) mineral oil (see ISO/TR 11046); b) most polycyclic aromatic hydrocarbons (PAH) (see ISO 13877); c) polychlorobiphenyls (PCB) (see ISO 10382); d) organochlorine pesticides (see ISO 10382). NOTE 2 In ISO/TR 11046, mineral oil is defined as the group of hydrocarbons which, on chromatography, have retention times lying between that of n-decane (C10H22) and n-tetracontane (C40H82). As in this International Standard the limit for volatile compounds lies at a boiling point of 300 °C [approximately hexadecane (C16)], this means that mineral oil should be considered as a volatile compound, as part of the compounds to be determined fall within the boiling point range of volatile compounds. However for practical reasons, it has been decided that the pretreatment for moderately volatile compounds should be specified for the determination of mineral oil. As a result of cryogenic crushing, an improvement in the extraction yield occurs for compounds with a boiling point above 300 °C. The possible losses for the lower-boiling hydrocarbons (C10 to C16) are assumed to be low, due to the retaining effect of the higher-boiling hydrocarbons present in mineral oil and to be compensated by the higher extraction yield of the other hydrocarbons present. As the total yield is used to determine the mineral oil as a group parameter, it is assumed that pretreatment using the method for moderately volatile compounds gives the best results at present. 4 Principle 4.1 Sampling Sampling shall be carried out in accordance with ISO 10381-1. The samples taken shall be kept cool and processed as soon as possible. The method of pretreatment depends on the volatility of the organic compound(s) or group(s) of organic compounds to be determined.
When taking a subsample, the quantity of soil should be removed from the sample container in such a way that this quantity: a) is a subsample over the full depth of the sample, and b) can be taken quickly. 4.2 Volatile compounds For determination of volatile organic compounds, core test samples are taken from the sample and extracted according to the relevant specific analytical procedure. If composite samples are required, extracts of individual samples are mixed. It is not possible to obtain composite samples without severe losses of volatiles. The procedure is described in 8.2. 4.3 Moderately volatile compounds Samples are chemically dried at a low temperature (− 196 °C, liquid nitrogen). The dried samples are cooled with liquid nitrogen and ground with a cross-beater mill with a sieve of 1 mm mesh size (cryogenic crushing). After grinding, suitable test portions are processed according to the relevant specific analytical procedures. Composite samples can be prepared by mixing the ground samples. This procedure is described in 8.3. oSIST ISO 14507:2019
ISO 14507:2003(E) © ISO 2003 — All rights reserved 3 If the extraction procedure requires a field-moist sample, drying and grinding are not possible. If the original sample only contains a small fraction of particles greater than 2 mm and the distribution of contaminants is likely to be homogeneous, grinding may be omitted. In these two cases, suitable test portions are taken directly after mixing the sample. This procedure is described in 8.4. NOTE 1 To distinguish the volatile organic compounds from the moderately volatile organic compounds, boiling points are used instead of the vapour pressure at ambient temperature. This is explained in Annex A, which also gives boiling points and vapour pressures of compounds regularly determined in soil investigations. NOTE 2 For some specific components in the group of moderately volatile organic compounds, freeze-drying may give good results. In this International Standard freeze-drying is not described. 5 Reagents Use only reagents of recognized analytical quality. Check samples of each batch of the reagents for the presence of contaminating compounds. 5.1 Sodium sulfate, anhydrous. Heat the sodium sulfate before use for at least 6 h at about 550 °C to remove crystalline water and organic materials. After heating, allow to cool in a desiccator and store in a closed container. 5.2 Magnesium silicate (talcum powder). 5.3 Sand or gravel. Before use, wash the sand or gravel at least twice with an equivalent mass of demineralized water and then heat for 6 h at about 550 °C to remove organic materials. 5.4 Liquid nitrogen. For safety precautions, see warnings in 8.3.2. 6 Apparatus Usual laboratory glassware and equipment, and in particular: 6.1 Glass containers with a volume of 750 ml to 1 000 ml, with a wide neck and screw cap with a polytetrafluoroethylene (PTFE) inlay. 6.2 Polyethylene containers with a volume of 750 ml to 1 000 ml, with a wide neck and screw cap. To prevent a significant headspace being formed, do not use larger containers. 6.3 Refrigerator, capable of maintaining a temperature below 10 °C. 6.4 Dewar vessel(s), capable of holding at least one polyethylene container of about 750 ml. 6.5 Cross-beater mill or mill with comparable qualities, with a sieve of mesh size 1 mm and accessories. A cross-beater mill as used in most soil laboratories is suitable for milling soil samples cooled with liquid nitrogen. 6.6 Gloves, suitable for working at low temperatures. 6.7 Oven, suitable for heating to about 550 °C. oSIST ISO 14507:2019
ISO 14507:2003(E) 4 © ISO 2003 — All rights reserved 6.8 Core cutter or similar instrument, for example apple corer. Depending on the type of soil (sand, clay), different instruments can be used. 7 Preservation and storage Do not preserve the samples, but analyse them as soon as possible. Between sampling in the field and analysis store the samples below 10 °C, if possible in a refrigerator (6.3). The maximum storage time for a sample kept in the dark below 10 °C depends on the parameter(s) to be determined, but can also depend on the material used for the container. Details can be obtained from the relevant specific analytical standards. The storage time also depends on possibilities of volatization and biological degradation. If these processes are likely to occur, then the storage time should not exceed four days. In cases with no volatization, poorly biodegradable compounds present and biologically less active soil, longer storage times are possible. If rapid microbial decomposition of the compounds to be determined can be expected, the sample should be pretreated immediately after receipt at the laboratory. For samples containing volatile organic compounds in particular, the storage time should preferably be as short as possible and analysis carried out as soon as possible, e.g. within 1 day to 2 days. NOTE Chemically dried and ground samples are generally stable for longer periods if stored in a cool, dark location. Freezing samples could extend the useful storage time.
8 Procedure 8.1 General The pretreatment method depends on the volatility of the substance(s) or group(s) of substances to be determined. Two categories are distinguished here: a) Volatile compounds: boiling point < 300 °C. b) Moderately volatile organic compounds: boiling point > 300 °C: 1) grinding necessary; 2) grinding not possible or not necessary. The method for pretreating samples containing volatile organic compounds is described in 8.2. The method for pretreating samples contain
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