SIST EN ISO 23161:2012
(Main)Soil quality - Determination of selected organotin compounds - Gas-chromatographic method (ISO 23161:2009)
Soil quality - Determination of selected organotin compounds - Gas-chromatographic method (ISO 23161:2009)
ISO 23161:2009 specifies a gas-chromatographic method for the identification and quantification of organotin compounds (OTCs) in soils as specified in Table 1. The method is also applicable to samples from sediments, sludges and wastes (soil-like materials). The working range depends on the detection technique used and the amount of sample taken for analysis. The limit of quantification for each compound is about 10 �g/kg.
Organotin cations can only be determined in accordance with ISO 23161:2009 after derivatization. The anionic part bound to the organotin cation is mainly dependent on the chemical environment and is not determined using this method. The peralkylated organotin compounds behave in a completely different way from their parent compounds. Tetraalkylated organotin compounds which are already peralkylated, such as tetrabutyltin, are determined directly without derivatization.
Bodenbeschaffenheit - Bestimmung ausgewählter Organozinnverbindungen - Gaschromatographisches Verfahren (ISO 23161:2009)
Diese Internationale Norm legt ein Verfahren zur Identifizierung und Quantifizierung von Organozinnverbindungen
(OZV) in Böden, wie in Tabelle 1 angegeben, fest. Das Verfahren ist ebenfalls auf Proben von
Sedimenten, Schlämmen und Abfällen (bodenähnliche Materialien) anwendbar. Der Arbeitsbereich ist von
dem angewendeten Nachweisverfahren und der für die Untersuchung genommenen Probemenge abhängig.
Die Bestimmungsgrenze der Einzelverbindungen ist etwa 10 μg/kg.
ANMERKUNG Wenn dieses Verfahren zur Bestimmung von anderen, nicht in dem Anwendungsbereich festgelegten
Organozinnverbindungen angewendet wird, sollte seine Eignung durch betriebsinterne Validierungsversuche geprüft
werden, z. B. Methylzinnverbindungen (siehe Tabelle 2). Es ist unwahrscheinlich, dass Methylzinnkationen aus wässrigen
Lösemitteln verdunsten, aber peralkylierte Methylzinnverbindungen sind flüchtig und neigen zu Verlusten (siehe C.3).
Deshalb werden zusätzliche Vorsichtsmaßnahmen eingeführt.
Organozinnkationen können nach dieser Internationalen Norm nur nach der Derivatisierung bestimmt werden.
Der an das Organozinnkation gebundene anionische Teil ist vor allem von dem chemischen Umfeld abhängig
und wird mit diesem Verfahren nicht bestimmt. Die peralkylierten Organozinnverbindungen verhalten sich
anders als ihre Ausgangsverbindungen. Tetraalkylierte Organozinnverbindungen, wie z. B. Tetrabutylzinn –
die bereits peralkyliert sind – werden ohne Derivatisierung direkt bestimmt.
Die Eigenschaften, wie z. B. die Korngrößenverteilung, Wassergehalt, Gehalt an organischer Substanz der
mit dieser Internationalen Norm zu untersuchenden Feststoffe, weichen weit voneinander ab. Die
Probenvorbehandlung muss hinsichtlich der Eigenschaften sowohl der Organozinnverbindungen als auch der
zu untersuchenden Matrix angemessen gestaltet werden.
Qualité du sol - Dosage d'une sélection de composés organostanniques - Méthode par chromatographie en phase gazeuse (ISO 23161:2009)
L'ISO 23161:2009 sp�cifie une m�thode d'identification et de quantification des compos�s organostanniques (OTC) dans les sols. Cette m�thode est �galement applicable aux �chantillons de s�diments, de boues et de d�chets (mati�res semblables au sol). La plage de travail d�pend de la technique de d�tection utilis�e et de la quantit� d'�chantillon pr�lev�e pour l'analyse. La limite de quantification applicable � chaque compos� est d'environ 10 �g/kg.
Les cations organostanniques peuvent �tre dos�s conform�ment � l'ISO 23161:2009 uniquement apr�s d�rivation. La partie anionique li�e au cation organostannique d�pend principalement de l'environnement chimique et n'est pas d�termin�e par cette m�thode. Les compos�s organostanniques peralkyl�s se comportent de mani�re totalement diff�rente de leurs compos�s parents. Les compos�s organostanniques t�traalkyl�s comme le t�trabutyl�tain, qui sont d�j� peralkyl�s, sont dos�s directement, sans d�rivation.
Kakovost tal - Določevanje izbranih organokositrovih spojin - Metoda plinske kromatografije (ISO 23161:2009)
Ta mednarodni standard določa metodo plinske kromatografije za ugotavljanje in kvantifikacijo organokositrovih spojin (OTC) v prsteh iz preglednice 1. Metoda se uporablja tudi za vzorce usedlin, blata in odpadkov (prsti podobnih materialov). Delovni razpon je odvisen od uporabljene tehnike za detekcijo in količine odvzetega vzorca za analizo. Meja kvantifikacije spojine znaša približno 10 μg/kg.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 23161:2012
01-februar-2012
.DNRYRVWWDO'RORþHYDQMHL]EUDQLKRUJDQRNRVLWURYLKVSRMLQ0HWRGDSOLQVNH
NURPDWRJUDILMH ,62
Soil quality - Determination of selected organotin compounds - Gas-chromatographic
method (ISO 23161:2009)
Bodenbeschaffenheit - Bestimmung ausgewählter Organozinnverbindungen -
Gaschromatographisches Verfahren (ISO 23161:2009)
Qualité du sol - Dosage d'une sélection de composés organostanniques - Méthode par
chromatographie en phase gazeuse (ISO 23161:2009)
Ta slovenski standard je istoveten z: EN ISO 23161:2011
ICS:
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
SIST EN ISO 23161:2012 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 23161:2012
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SIST EN ISO 23161:2012
EUROPEAN STANDARD
EN ISO 23161
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2011
ICS 13.080.10
English Version
Soil quality - Determination of selected organotin compounds -
Gas-chromatographic method (ISO 23161:2009)
Qualité du sol - Dosage d'une sélection de composés Bodenbeschaffenheit - Bestimmung ausgewählter
organostanniques - Méthode par chromatographie en Organozinnverbindungen - Gaschromatographisches
phase gazeuse (ISO 23161:2009) Verfahren (ISO 23161:2009)
This European Standard was approved by CEN on 14 July 2011.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2011 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 23161:2011: E
worldwide for CEN national Members.
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SIST EN ISO 23161:2012
EN ISO 23161:2011 (E)
Contents Page
Foreword .3
2
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SIST EN ISO 23161:2012
EN ISO 23161:2011 (E)
Foreword
The text of ISO 23161:2009 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the
International Organization for Standardization (ISO) and has been taken over as EN ISO 23161:2011 by
Technical Committee CEN/TC 308 “Characterization of sludges” the secretariat of which is held by AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by February 2012, and conflicting national standards shall be withdrawn
at the latest by February 2012.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 23161:2009 has been approved by CEN as a EN ISO 23161:2011 without any modification.
3
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SIST EN ISO 23161:2012
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SIST EN ISO 23161:2012
INTERNATIONAL ISO
STANDARD 23161
First edition
2009-09-01
Soil quality — Determination of selected
organotin compounds — Gas-
chromatographic method
Qualité du sol — Dosage d'une sélection de composés
organostanniques — Méthode par chromatographie en phase gazeuse
Reference number
ISO 23161:2009(E)
©
ISO 2009
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
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Published in Switzerland
ii © ISO 2009 – All rights reserved
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
Contents Page
Foreword .iv
Introduction.v
1 Scope.1
2 Normative references.2
3 Terms and definitions .2
4 Principle.2
5 Reagents.4
5.1 General .4
5.2 Chemicals.4
5.3 Standards .5
5.4 Preparation of reagents and solutions.6
5.5 Clean-up .7
6 Apparatus.7
6.1 Requirements for glassware .7
6.2 Sampling apparatus .8
6.3 Additional apparatus.8
7 Procedure.8
7.1 Sampling and sample pretreatment .8
7.2 Sample extraction.9
7.3 Clean-up of the extract.10
7.4 Determination of dry mass .11
7.5 Measurement .11
8 Calibration.12
9 Recovery rates of the internal standard compounds .12
10 Quantification .13
11 Expression of results.14
12 Precision.14
13 Test report.14
Annex A (informative) Information about the procedure .15
Annex B (informative) Additional clean-up procedures.17
Annex C (informative) Information about typical instrumental conditions .20
Annex D (informative) Information about GC/MS identification.31
Annex E (informative) Validation data .33
Bibliography.37
© ISO 2009 – All rights reserved iii
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 23161 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
methods and soil characteristics.
iv © ISO 2009 – All rights reserved
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
Introduction
It is absolutely essential that tests conducted in accordance with this International Standard be carried out by
suitably qualified staff.
It can be noted whether, and to what extent, particular problems will require the specification of additional
boundary conditions.
© ISO 2009 – All rights reserved v
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SIST EN ISO 23161:2012
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SIST EN ISO 23161:2012
INTERNATIONAL STANDARD ISO 23161:2009(E)
Soil quality — Determination of selected organotin
compounds — Gas-chromatographic method
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This International Standard does not purport to address all of the safety problems, if any,
associated with its use. It is the responsibility of the user to establish appropriate safety and health
practices and to ensure compliance with any national regulatory conditions.
1 Scope
This International Standard specifies a gas-chromatographic method for the identification and quantification of
organotin compounds (OTCs) in soils as specified in Table 1. The method is also applicable to samples from
sediments, sludges and wastes (soil-like materials). The working range depends on the detection technique
used and the amount of sample taken for analysis. The limit of quantification for each compound is about
10 µg/kg.
Table 1 — Organotin compound, which can be determined in accordance with this International
Standard
(4−n)+
R Sn R n Name Acronym
n
a
Organotin cations
3+
BuSn Butyl 1 Monobutyltin cation MBT
2+
Bu Sn Butyl 2 Dibutyltin cation DBT
2
+
Bu Sn Butyl 3 Tributyltin cation TBT
3
3+
OcSn Octyl 1 Monooctyltin cation MOT
2+
Oc Sn Octyl 2 Dioctyltin cation DOT
2
+
Ph Sn Phenyl 3 Triphenyltin cation TPhT
3
+
Cy Sn Cyclohexyl 3 Tricyclohexyltin cation TCyT
3
Peralkylated organotin
Bu Sn Butyl 4 Tetrabutyltin TTBT
4
a
Organotin compounds are measured after derivatization.
NOTE When applying this method to the determination of other organotin compounds not specified in the scope, its
suitability is proven by proper in-house validation experiments, e.g. methyltin compounds. See Table 2. Methyltin cations
are unlikely to evaporate from aqueous solvents, but peralkylated methyltin compounds are volatile and subject to losses
(see C.3). Therefore, additional precautions are established.
Table 2 — Methyltin compounds
(4−n)+
R Sn R n Name Acronym
n
3+
MeSn Methyl 1 Monomethyltin cation MMT
2+
Me Sn Methyl 2 Dimethyltin cation DMT
2
+
Me Sn Methyl 3 Trimethyltin cation TMT
3
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
Organotin cations can only be determined in accordance with this International Standard after derivatization.
The anionic part bound to the organotin cation is mainly dependent on the chemical environment and is not
determined using this method. The peralkylated organotin compounds behave in a completely different way
from their parent compounds. Tetraalkylated organotin compounds which are already peralkylated, such as
tetrabutyltin, are determined directly without derivatization.
The properties, such as particle size distribution, water content and organic matter content of the solids to be
analysed using this International Standard vary widely. Sample pretreatment is designed adequately with
respect to both the properties of the organotin compounds and the matrix to be analysed.
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 11465, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric
method
ISO 16720, Soil quality — Pretreatment of samples by freeze-drying for subsequent analysis
ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography and
mass spectrometry
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
organotin compound
substance containing 1 to 4 Sn-C bonds
NOTE The number of Sn-C bonds is a measure for the degree of substitution.
3.2
organotin cation
part of the organotin compound (3.1) that contains all Sn-C bonds and is formally charged
3.3
organotin cation derivatives
non-dissociated tetrasubstituted organotin compounds which are produced by derivatization
3.4
solid
soil, sediment, sludge and waste (soil-like material)
4 Principle
For the ionic and the non-ionic organotin compounds (see Table 1), a different sample pretreatment and
sample preparation are necessary. For the determination of organotin cations, laboratory samples are
pretreated by freeze drying and grinding. This procedure enables homogeneity of the sample to be achieved.
The determination of non-ionic TTBT cannot be carried out with freeze-dried materials due to evaporation
losses, thus, it shall be determined in the field-moist sample. Organotin cations can only be determined after
derivatization, whereas TTBT is already peralkylated and can be determined without derivatization (see the
flowchart in Figure 1).
2 © ISO 2009 – All rights reserved
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
Figure 1 — Flowchart for the pretreatment and analysis of selected organotin compounds
For the determination of organotin compounds, two alternative extraction methods are given, both followed by
in situ derivatization with a tetraethylborate compound and simultaneous extraction with hexane:
a) treatment with acetic acid;
b) treatment with methanolic potassium hydroxide.
NOTE 1 If it is necessary to take a large amount of sample, extraction and derivatization can be done in two steps. An
aliquot of the extract can be taken for derivatization. This also applies for samples with high levels of OTC contamination.
NOTE 2 During in situ derivatization, the solid phase is still present. This supports the extraction by continuous
changing of the polar organotin cations to the non-polar organotin cation derivates. In situ methods can improve the
extraction efficiency, particularly for monoalkylated organotin compounds.
NOTE 3 Other extraction techniques can be applied if a comparable extraction efficiency is achieved.
© ISO 2009 – All rights reserved 3
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
NOTE 4 Treatment with potassium hydroxide provides some degree of digestion and is recommended especially when
the solid contains high amounts of organic and biological materials.
The internal standard mix comprises four compounds representing four alkylation states in order to mimic the
behaviour of the target compounds. After alkylation, they cover a wide range of volatility. A recovery of at least
80 % for derivatization/extraction and again 80 % for each clean-up step of the internal standard compounds
should be achieved. (For more information, see A.3.) Tetraalkylborate is very reactive and will also alkylate
other compounds in the matrix. Those compounds (and also boroxines) may interfere with the target
compounds during gas chromatographic determination and influence detection. In order to protect the column
and to reduce the interference in chromatography, it will be necessary to apply a precleaning step to most
samples. Clean-up with silica or aluminium oxide is the minimum; further clean-up steps (e.g. aluminium
oxide/silver nitrate, silica/silver nitrate, pyrogenic copper; see Annex B) may be applied if necessary.
The determination of the tetrasubstituted organotin compounds is carried out after clean-up and concentration
steps by separation with capillary gas chromatography and detected with a suitable system [mass
spectrometer (MS), (MS/MS), flame photometric detector (FPD), atomic absorption spectrometer (AAS),
atomic emission detector (AED), inductively coupled plasma/mass spectrometer ICP/MS]. The concentrations
are determined by calibration over the total procedure using aqueous multi-component calibration standard
solutions in accordance with 5.4.3.
5 Reagents
5.1 General
Use reagents of highest purity, typically of pesticide grade or better. The reagents may contain impurities of
organotin compounds. It is absolutely essential to verify the blanks.
The water shall be free of interferences. Use water in accordance with Grade 3 of ISO 3696.
5.2 Chemicals
5.2.1 Acetic acid, CH COOH, glacial.
3
5.2.2 Sodium hydroxide solution, NaOH, 40 % (m/V).
5.2.3 Sodium acetate, CH COONa.
3
5.2.4 Sodium sulfate, Na SO , anhydrous.
2 4
5.2.5 Potassium hydroxide, KOH.
5.2.6 Silica gel, grain size 0,085 mm to 0,28 mm (63 mesh to 200 mesh).
5.2.7 Aluminium oxide, Al O , alkaline.
2 3
5.2.8 Tetrahydrofurane, C H O, free of peroxides, free of water.
4 8
5.2.9 Acetone, (CH ) CO.
3 2
5.2.10 Hexane, C H .
6 14
NOTE Both n-hexane and 2-methylpentane (i-hexane) have been found to be suitable.
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
5.2.11 Tetraethylborate compound, e.g sodium tetraethylborate, NaB(C H ) .
2 5 4
NOTE The active species during derivatization is the tetraethylborate anion. The choice of the cation is arbitrary.
Sodium tetraethylborate was chosen since it is commercially available. In principle, any other tetraethylborate compound
can be used for analysis, including complexes formed with tetrahydrofuran (THF). A simple and rapid synthesis of a
suitable derivatization agent is described in A.1.
WARNING — Sodium tetraethylborate may contain traces of triethylboron, which may cause
instantaneous combustion.
5.2.12 Methanol, CH OH.
3
5.2.13 Dichloromethane, CH Cl .
2 2
5.3 Standards
WARNING — Organotin compounds vary largely regarding toxicological properties towards mammals
with respect to the alkylation stage and type of alkyl group. Cautious handling of reagents is
mandatory at any time.
Table 3 lists the standards used for calibration of the target compounds (solution A), internal standards
(solution B) and injection standard (solution C). Additional information is provided concerning weighing factors
for calculation to organotin cations (for 100 % purity of the substances).
Table 3 — Standards and internal standards for calibration of target compounds
a b c
No. Standard Abbreviation Formula CAS-RN WF Solution
5.3.1 Monobutyltin trichloride MBTCl C H SnCl 1118-46-3 0,623 A
4 9 3
5.3.2 Dibutyltin dichloride DBTCl (C H ) SnCl 683-18-1 0,767 A
4 9 2 2
5.3.3 Tributyltin chloride TBTCl (C H )SnCl 1461-22-9 0,891 A
4 9 3
5.3.4 Tetrabutyltin TTBT (C H )Sn 1461-25-2 1,000 A
4 9 4
5.3.5 Monooctyltin trichloride MOTCl C H SnCl 3091-25-6 0,686 A
8 17 3
5.3.6 Dioctyltin dichloride DOTCl (C H ) SnCl 3542-36-7 0,830 A
8 17 2 2
5.3.7 Triphenyltin chloride TPhTCl (C H )SnCl 639-58-7 0,908 A
6 5 3
5.3.8 Tricyclohexyltin chloride TCyTCl (C H )SnCl 3091-32-5 0,912 A
6 11 3
Internal standards
5.3.9 Monoheptyltin trichloride MHTCl C H SnCl 59344-47-7 0,672 B
7 15 3
5.3.10 Diheptyltin dichloride DHTCl (C H ) SnCl 74340-12-8 0,817 B
7 15 2 2
5.3.11 Tripropyltin chloride TPTCl (C H )SnCl 2279-76-7 0,875 B
3 7 3
5.3.12 Tetrapropyltin TTPT (C H )Sn 2176-98-9 1,000 B
3 7 4
5.3.13 Tetrapentyltin TTPeT (C H )Sn 3765-65-9 1,000 C
5 11 4
a
Chemical Abstracts Registration Number.
b
WF= Weighing factor = Molar mass of organotin cation/molar mass of organotin compound.
c
A for the multicomponent-standard solution in methanol.
B for the solution of the internal standards in methanol.
C for the solution of the injection standards in hexane.
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
5.4 Preparation of reagents and solutions
5.4.1 General requirements
Prepare the following (see also Table 3):
⎯ multicomponent standard stock solution A in methanol (e.g. 1 mg/ml);
⎯ multicomponent standard spiking solutions for calibration, by diluting solution A with methanol;
⎯ stock solution B of internal standards in methanol (e.g. 1 mg/ml);
⎯ spiking solution of the internal standards, by diluting solution B with methanol (e.g. 100 ng/ml);
⎯ stock solution C of the injection standard in methanol (e.g. 2 mg/ml);
⎯ injection standard solution, by diluting solution C (e.g. 2 µg/ml).
5.4.2 Blank solution
Add 20 ml of water (5.1) to an Erlenmeyer flask with a ground joint or a screw-capped [polytetrafluoroethylene
(PTFE) lined] vial.
5.4.3 Aqueous calibration solutions (multicomponent solution of organotin compounds in water)
For each working range, prepare at least 6 calibration solutions with appropriate concentration levels.
Add 20 ml of water (5.1) to an Erlenmeyer flask with a ground joint or a screw-capped (PTFE-lined) vial. While
stirring vigorously, pipette an appropriate volume of the respective spiking solution underneath the surface
and ensure that the spiking solution is well distributed in the water. Stir for an additional 20 min.
5.4.4 Methanolic potassium hydroxide solution
Prepare a solution of 25 % (m/V) potassium hydroxide (5.2.5) in methanol (5.2.12). This is the methanolic
potassium hydroxide solution.
5.4.5 Acetate buffer solution
Dissolve about 1 mol of sodium acetate (equal to 82 g of anhydrous sodium acetate) (5.2.3) in 500 ml of water
(5.1) in a 1 L volumetric flask. Add sufficient glacial acetic acid (5.2.1) to adjust to a pH of 4,5. Dilute to volume
with water (5.1) and mix well.
5.4.6 Solvent mixture
Prepare a solvent mixture of acetic acid, methanol and water with a volume ratio of 1:1:1.
5.4.7 Derivatization agent
Prepare an approximately 10 % (m/V) solution of tetraethylborate compound (5.2.11) in tetrahydrofurane
(5.2.8).
NOTE This solution is stable for about three months if stored under an inert-gas blanket.
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SIST EN ISO 23161:2012
ISO 23161:2009(E)
5.5 Clean-up
5.5.1 General requirements
A silica or aluminium oxide clean-up is the minimum requirement. Further clean-up steps (aluminium
oxide/silver nitrate, silica/silver nitrate, pyrogenic copper) may be applied if necessary (see Annex B). A
recovery of > 80 % of the internal standards and target compounds shall be achieved for each clean-up step.
5.5.2 Silica gel for the clean-up column
Heat silica gel (5.2.6) for at least 12 h at (500 ± 20) °C on a quartz plate in a muffle furnace. Ensure that the
temperature does not exceed 520 °C.
Allow the plate to cool in an oven to about 200 °C, transfer the silica to a wide-necked glass bottle and allow
cooling to room temperature in a desiccator.
Add water to the cooled silica until a mass fraction of 3 % is reached. Close the bottle and homogenize the
contents for 2 h on a shaker.
5.5.3 Aluminium oxide for the clean-up column
Activate aluminium oxide (5.2.7) by heating to 600 °C for a minimum of 24 h.
Allow to cool in the oven to about 200 °C, transfer the aluminium oxide to a wide-necked glass bottle and
allow cooling to room temperature in a desiccator.
Add water to the cooled aluminium oxide until a mass fraction of 10 % is reached. Close the bottle and
homogenize the contents for 2 h on a shaker.
5.5.4 Clean-up column
Add about 5 g of adsorbent (5.5.2 or 5.5.3) to one column, and add about 3 g of drying agent. Ensure that the
clean-up column is filled homogeneously, for example, by using hexane as a moistening agent during the
filling process.
Commercially pre-packed columns may be used as an alternative if the requirement for recovery is met.
5.5.5 Eluent for extract cleaning with silica gel
A mixture of hexane (5.2.10) with a more polar solvent can be used as an eluent to
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