SIST EN ISO 17353:2005
(Main)Water quality - Determination of selected organotin compounds - Gas chromatographic method (ISO 17353:2004)
Water quality - Determination of selected organotin compounds - Gas chromatographic method (ISO 17353:2004)
This standard will provide a technique for determination of the strain-to-fracture of coatings deposited on a wide variety of substrates. Additionally, it will under certain circumstances provide data on coating adhesion.
Wasserbeschaffenheit - Bestimmung von ausgewählten Organozinnverbindungen - Verfahren mittels Gaschromatographie (ISO 17353:2004)
Diese Internationale Norm legt ein Verfahren zur Identifizierung und Quantifizierung von Organozinnverbindungen und/oder der in Tabelle 1 angegebenen Organozinnkationen in Trinkwasser, Oberflächenwasser und Abwasser, das nicht mehr als 2 g/l suspendierte Feststoffe enthält, fest. Der Arbeitsbereich beträgt 10 ng/l bis 1 000 ng/l. Die entsprechenden Anionen werden nicht bestimmt.
Nach diesem Verfahren können auch andere Verbindungen wie solche mit R = Methyl, n = 1 bis 2 und R = Phenyl, n = 1 bis 2 analysiert werden. Diese Internationale Norm ist auch auf marine Wässer anwendbar.
Qualité de l'eau - Dosage de composés organostanniques sélectionnés - Méthode par chromatographie en phase gazeuse (ISO 17353:2004)
L'ISO 17353:2004 spécifie une méthode pour l'identification et la quantification des composés et/ou des cations monobutylétain, dibutylétain, tributylétain, tétrabutylétain, monooctylétain, dioctylétain, triphénylétain, et trichlorohexylétain, dans l'eau potable, les eaux de surface et les eaux usées contenant au plus 2 g/l de matières en suspension. Le domaine de travail est compris entre 10 ng/l et 1 000 ng/l. Les anions respectifs ne sont pas dosés.
D'autres composés, tels que monométhylétain, diméthylétain, monophénylétain et diphénylétain, peuvent également être analysés avec ce mode opératoire. L'ISO 17353:2004 s'applique aussi à l'eau de mer.
Kakovost vode – Določevanje izbranih organokositrnih spojin - Metoda plinske kromatografije (ISO 17353:2004)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 17353:2005
01-december-2005
.DNRYRVWYRGH±'RORþHYDQMHL]EUDQLKRUJDQRNRVLWUQLKVSRMLQ0HWRGDSOLQVNH
NURPDWRJUDILMH ,62
Water quality - Determination of selected organotin compounds - Gas chromatographic
method (ISO 17353:2004)
Wasserbeschaffenheit - Bestimmung von ausgewählten Organozinnverbindungen -
Verfahren mittels Gaschromatographie (ISO 17353:2004)
Qualité de l'eau - Dosage de composés organostanniques sélectionnés - Méthode par
chromatographie en phase gazeuse (ISO 17353:2004)
Ta slovenski standard je istoveten z: EN ISO 17353:2005
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
SIST EN ISO 17353:2005 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 17353:2005
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SIST EN ISO 17353:2005
EUROPEAN STANDARD
EN ISO 17353
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2005
ICS 13.060.50
English Version
Water quality - Determination of selected organotin compounds -
Gas chromatographic method (ISO 17353:2004)
Qualité de l'eau - Dosage de composés organostanniques Wasserbeschaffenheit - Bestimmung von ausgewählten
sélectionnés - Méthode par chromatographie en phase Organozinnverbindungen - Verfahren mittels
gazeuse (ISO 17353:2004) Gaschromatographie (ISO 17353:2004)
This European Standard was approved by CEN on 18 July 2005.
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 Central Secretariat 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 Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 17353:2005: E
worldwide for CEN national Members.
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SIST EN ISO 17353:2005
EN ISO 17353:2005 (E)
Foreword
The text of ISO 17353:2004 has been prepared by Technical Committee ISO/TC 147 "Water quality" of the
International Organization for Standardization (ISO) and has been taken over as EN ISO 17353:2005 by
Technical Committee CEN/TC 230 “Water analysis”, the secretariat of which is held by DIN.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, at the latest by February 2006, and conflicting national standards shall be withdrawn
at the latest by February 2006.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic,
Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland
and United Kingdom.
Endorsement notice
The text of ISO 17353:2004 has been approved by CEN as EN ISO 17353:2005 without any modifications.
2
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SIST EN ISO 17353:2005
INTERNATIONAL ISO
STANDARD 17353
First edition
2004-09-15
Water quality — Determination of
selected organotin compounds — Gas
chromatographic method
Qualité de l'eau — Dosage de composés organostanniques
sélectionnés — Méthode par chromatographie en phase gazeuse
Reference number
ISO 17353:2004(E)
©
ISO 2004
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
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Published in Switzerland
ii © ISO 2004 – All rights reserved
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope. 1
2 Normative references . 1
3 Terms and definitions. 2
4 Principle . 2
5 Interferences. 2
6 Reagents . 2
7 Apparatus. 7
8 Procedure. 8
9 Identification. 11
10 Calibration. 13
11 Calculation. 16
12 Precision . 18
13 Test report. 18
Annex A (informative) Gas chromatographic conditions. 19
Annex B (informative) Precision data. 29
Bibliography . 31
© ISO 2004 – All rights reserved iii
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SIST EN ISO 17353:2005
ISO 17353:2004(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 17353 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
Introduction
It should be noted whether and to what extent particular problems will require the specification of additional
boundary conditions.
This International Standard describes a gas-chromatographic/organotin specific determination of organotin
compounds after derivatization with sodium tetraethyl borate and liquid/liquid extraction.
The user should be aware that particular problems could require the specification of additional marginal
conditions.
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SIST EN ISO 17353:2005
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SIST EN ISO 17353:2005
INTERNATIONAL STANDARD ISO 17353:2004(E)
Water 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.
IMPORTANT — It is absolutely essential that tests conducted according to this International Standard
be carried out by suitably trained staff.
1 Scope
This International Standard specifies a method for the identification and quantification of organotin compounds
and/ or cations as mentioned in Table 1 in drinking water, surface water and wastewater containing not more
than 2 g/l of suspended material. The working range is 10 ng/l to 1 000 ng/l. The respective anions are not
determined.
This method can also be applicable to other compounds such as R = methyl, n = 1 to 2 and R = phenyl, n = 1
to 2. This International Standard is also applicable to marine water.
Table 1 — Organotin compounds and cations determined
using this International Standard
(4-n)+
R Sn
R n Name Acronym
n
3+
BuSn Butyl 1 Monobutyltin cation MBT
2+
Bu Sn
Butyl 2 Dibutyltin cation DBT
2
+
Bu Sn
Butyl 3 Tributyltin cation TBT
3
Bu Sn
Butyl 4 Tetrabutyltin TTBT
4
3+
Octyl 1 Monooctyltin cation MOT
OcSn
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
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 3696:1987, Water for analytical laboratory use — Specification and test methods
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design on sampling programmes
ISO 5667-2, Water quality — Sampling — Part 2: Guidance on sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples
3 Terms and definitions
For the purposes of this International Standard, the following terms and definitions apply.
3.1
organotin compound
OTC
substance with at least one Sn-C bond
NOTE The number of Sn-C bonds is a measure of the degree of substitution.
3.2
organotin cation
OC
part of the organotin compound that contains all Sn-C bonds (and which is formally loaded)
NOTE In this International Standard, the abbreviation OC is also used for the non-dissociated tetrasubstituted
organotin. OC therefore comprises the cations MBT, DBT, TBT, TTBT, MOT, DOT, TCyT, and TPhT.
4 Principle
Organotin compounds in water are alkylated with sodium tetraethylborate and extracted with hexane. The
extract can be cleaned with silica. After concentration, the tetrasubstituted OTC are separated by capillary gas
chromatography and detected with a suitable system such as MS (mass spectrometry), FPD (flame
photometric detection), AED (atomic emission detection). The concentration is determined by calibration for
the total procedure using an internal standard mixture.
5 Interferences
The reagents sometimes contain impurities of organotin compounds. It is absolutely essential to verify the
blanks (see A.4.6).
6 Reagents
Use reagents of highest purity.
6.1 Water, free of substances causing interference with this method and complying with ISO 3696:1987,
Grade 1.
6.2 Nitric acid, ρ(HNO ) = 1,4 g/ml.
3
6.3 Acetic acid, CH COOH, glacial.
3
6.4 Sodium hydroxide solution, c(NaOH) = 1 mol/l.
6.5 Sodium acetate, CH COONa, anhydrous.
3
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
6.6 Sodium sulfate, Na SO , anhydrous.
2 4
6.7 Silica, grain size 0,2 mm to 0,063 mm (200 mesh to 63 mesh).
6.8 Tetrahydrofurane, C H O, free of peroxides and water.
4 8
6.9 Acetone, (propanone) (CH ) CO.
3 2
6.10 Methanol, CH OH.
3
6.11 Hexane, C H .
6 14
6.12 Sodium tetraethylborate, NaB(C H ) .
2 5 4
6.13 Monobutyltin trichloride, MBTCl, C H SnCl .
4 9 3
6.14 Dibutyltin dichloride, DBTCl, (C H ) SnCl .
4 9 2 2
6.15 Tributyltin chloride, TBTCl, (C H ) SnCl.
4 9 3
6.16 Tetrabutyltin, TTBT, (C H ) Sn.
4 9 4
6.17 Monooctyltin trichloride, MOTCl, C H SnCl .
8 17 3
6.18 Dioctyltin dichloride, DOTCl, (C H ) SnCl .
8 17 2 2
6.19 Triphenyltin chloride, TPhTCl, (C H ) SnCl.
6 5 3
6.20 Tricyclohexyltin chloride, TCyTCl, (C H ) SnCl.
6 11 3
6.21 Monoheptyltin trichloride, MHTCl, C H SnCl ; (internal standard).
7 15 3
6.22 Diheptyltin dichloride, DHTCl, (C H ) SnCl ; (internal standard).
7 15 2 2
6.23 Tripropyltin chloride, TPTCl, (C H ) SnCl; (internal standard).
3 7 3
6.24 Tetrapropyltin, TTPT, (C H ) Sn; (internal standard).
3 7 4
6.25 Multicomponent solutions and prepared reagents.
Since stability of multicomponent standard solutions is a matter of concern, it is recommended to prepare
several solutions containing solely organotin compounds with the same degree of alkylation/arylation (e.g. four
solutions respectively for mono-, di-, tri-, and tetrasubstituted compounds). Stability can be assessed by the
absence of degradation products.
6.25.1 Multicomponent-standard solution in methanol, Stock solution A.
For the preparation of 1 mg/ml of organotin cation stock solution, weigh, to the nearest 0,1 mg, the amounts of
organotin compounds specified in Table 2 into a 100 ml volumetric flask. Dissolve these compounds in a small
amount of methanol (6.10). Then make up to volume with methanol and mix well.
If stored at 4 °C in the dark, the solution is stable for up to one year.
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ISO 17353:2004(E)
6.25.2 Solution of the internal standards in methanol, Stock solution B.
Weigh, to the nearest 0,1 mg, into a 100 ml volumetric flask, about:
120 mg of diheptyltin dichloride,
150 mg of monoheptyltin trichloride,
115 mg of tripropyltin chloride, and
100 mg of tetrapropyltin
and dissolve in a small amount of methanol (6.10). Make up to volume with methanol and mix well.
For the preparation of exactly 1 mg/ml of OC as specified in Table 2, weigh exactly 122,4 mg of diheptyltin
dichloride, 148,8 mg of monoheptyltin trichloride, 114,3 mg of tripropyltin chloride and 100 mg of tetrapropyltin
into the 100 ml volumetric flask and prepare as described above.
The solution is stable for three months when stored in the dark at 4 °C.
Table 2 — Amounts of organotin compounds and weighing factors for recalculation
to organotin cations (for 100 % purity of the substances)
a b c
Substance Weighing factor Mass Solution
mg
Monobutyltin trichloride 0,623 160,5 A
Dibutyltin dichloride 0,767 130,4 A
Tributyltin chloride 0,891 112,2 A
Tetrabutyltin 1,000 100,0 A
Monooctyltin trichloride 0,686 145,8 A
Dioctyltin dichloride 0,830 120,5 A
Triphenyltin chloride 0,908 110,1 A
Tricyclohexyltin chloride 0,912 109,6 A
Monoheptyltin trichloride 0,672 148,8 B
Diheptyltin dichloride 0,817 122,4 B
Tripropyltin chloride 0,875 114,3 B
Tetrapropyltin 1,000 100,0 B
a
Weighing factor = molar mass (OC)/molar mass (OTC).
b
If the mass weighed of the compound is different from that given in this table, use the weighing factor
to calculate the actual concentration of the OTC.
c
A for multicomponent standard solution in methanol.
B for the solution of the internal standards in methanol.
6.25.3 Multicomponent spiking solutions for reference solutions.
Prepare the spiking solutions as specified in Table 3 using pipettes. Pipette the respective starting volume
specified in Table 3 of the (stock) solution into a 100 ml volumetric flask. Make up to volume with methanol
and mix well. The final mass concentration of the resulting spiking solution shall be between 10 ng/ml and
1 000 ng/ml of organotin cations in methanol. Dilutions steps greater than 1:100 are not allowed.
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ISO 17353:2004(E)
Table 3 — Example for the dilution series for preparation of the spiked solutions
Starting Concentration of OC Volume of Final volume Final concentration Designation of final
solution in starting solution starting solution of OC solution
ng/ml ml ml ng/ml
A 1 000 000 10 100 100 000 A1
A1 100 000 10 100 10 000 A2
A1 100 000 15 100 15 000 A3
A2 10 000 20 50 4 000 A4
A2 10 000 5 100 500 A5
A2 + A3 10 000/15 000 1 + 6 100 1 000 AH6
10 000/15 000 100 850 AH5
A2 + A3 1 + 5
A2 + A3 10 000/15 000 1 + 4 100 700 AH4
A2 + A3 10 000/15 000 1 + 3 100 550 AH3
A2 + A3 10 000/15 000 1 + 2 100 400 AH2
10 000/15 000 100 250 AH1
A2 + A3 1 + 1
A4 4 000 6 100 240 AM6
A4 4 000 5 100 200 AM5
A4 4 000 4 100 160 AM4
A4 4 000 3 100 120 AM3
A4 4 000 2 100 80 AM2
A4 4 000 1 100 40 AM1
A5 500 7 100 35 AL6
A5 500 6 100 30 AL5
A5 500 5 100 25 AL4
A5 500 4 100 20 AL3
A5 500 3 100 15 AL2
A5 500 2 100 10 AL1
Solutions AH1 to AH6 are used for calibration AH (higher working range).
Solutions AM1 to AM6 are used for calibration AM (medium working range).
Solutions AL1 to AL6 are used for calibration AL (lower working range).
Solutions AH1 to AH6 are prepared from two Stock solutions A2 and A3.
6.25.4 Spiking solutions containing internal standards.
Dilution steps greater than 1:100 are not allowed.
Pipette 1 ml of Stock solution B (see Table 4) into a 100 ml volumetric flask. Make up to volume with methanol
(6.10) and mix well (Solution B1).
Pipette 1 ml of Solution B1 into a 100 ml volumetric flask. Make up to volume with methanol and mix well
(Solution B2).
Use Solution B2 for all samples. The mass concentration of Solution B2 is about 100 ng/ml of organotin cation
in methanol, depending on the original mass weighed according to 6.25.1 (Table 2).
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
Table 4 — Example of a dilution series for the preparation
of the spiking solutions of the internal standards
Starting Concentration of OC Volume of Final volume Final concentration Designation of final
solution in starting solution starting solution of OC solution
ng/ml ml ml ng/ml
B 1 000 000 1 100 10 000 B1
B1 10 000 1 100 100 B2
6.25.5 Blank solution, consisting of 1 l of water (6.1) put into a 1 000 ml sampling bottle.
6.25.6 Reference solutions (aqueous multicomponent reference solution).
For each working range, prepare at least six reference solutions, distributed equidistantly over the chosen
working range. The working range should not exceed one order of magnitude.
Add 1 000 ml of water (6.1) to each of six 1 000 ml sampling bottles. Under vigorous stirring, dip the tip of the
pipette below the surface of the water and add 1 ml of the respective spiking solution (AH1 to AH6, AM1 to
AM6, or AL1 to AL6, see Table 3) ensuring that the spiking solution is distributed evenly in the water. Stir for
an additional 20 min.
Depending on the working range, the reference solutions shall contain the following mass concentration of OC
in water:
higher range: 1 000 ng/l, 850 ng/l, 700 ng/l, 550 ng/l, 400 ng/l and 250 ng/l;
medium range: 240 ng/l, 200 ng/l, 160 ng/l, 120 ng/l, 80 ng/l and 40 ng/l; or
lower range: 35 ng/l, 30 ng/l, 25 ng/l, 20 ng/l, 15 ng/l, and 10 ng/l.
6.25.7 Acetate buffer solution.
Dissolve about 1 mol of sodium acetate (equal to 82 g of anhydrous sodium acetate) (6.5) in 500 ml of water
(6.1) into a 1 000 ml volumetric flask. Add sufficient glacial acetic acid (6.3) to reach a pH of 4,5. Make up to
volume with water (6.1) and mix well.
6.25.8 Derivatization agent A (2 % mass concentration in water).
Weigh about 200 mg of sodium tetraethylborate (6.12) into a 10 ml volumetric flask and make up to volume
with water (6.1).
This solution is not stable, and should be used immediately.
6.25.9 Derivatization agent B (20 % mass concentration in tetrahydrofurane).
Weigh about 2 g of sodium tetraethylborate (6.12) into a 10 ml volumetric flask and make up to volume with
tetrahydrofurane (6.8).
This solution is stable for about three months if stored under an inert gas blanket. Its use is recommended for
large series of samples.
6.25.10 Drying agent.
Place about 250 g to 300 g of powdered sodium sulfate (6.6) onto a quartz plate and dry for at least 4 h at a
temperature of 180 °C. Add the dried sodium sulfate to a wide-necked bottle and allow to cool to room
temperature in a desiccator. Remove the bottle from the desiccator and close tightly.
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
6.25.11 Silica for the clean-up column.
It is recommended to prepare batches of no more than 120 g per batch.
Heat silica (6.7) for at least 12 h at (500 ± 20) °C on a quartz plate in a muffle furnace (the temperature should
not exceed 520 °C).
Allow the plate to cool in the oven to about 200 °C, transfer the silica to a wide-necked glass bottle and allow
to cool 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.
Check the homogeneity and the moisture content of the prepared silica by determining the moisture content of
different portions of the prepared silica. The moisture content shall not vary by more than 0,1 %.
6.25.12 Clean-up column.
Ensure that the clean-up column is filled homogeneously, e.g. by using a hexane slurry of silica.
Add about 5 g of silica (6.25.11) to the column (see 7.6), and add about 3 g of drying agent (6.25.10). Rinse
with 30 ml of hexane (6.11) and let the solvent pass through the column to the level of the upper surface of the
column bed.
The column is then ready for use.
Commercially available pre-packed columns may be used.
6.25.13 Eluent for cleaning extract, acetone in hexane.
To ensure quantitative elution of all organotin from the clean-up column, use a mixture of n-hexane and
acetone. Using an appropriate standard solution prior to applying the clean-up procedure, determine the
percentage of acetone to be added to the n-hexane and the volume of the resulting mixture necessary for
complete elution. Add the appropriate volume of acetone (6.9) to a 100 ml volumetric flask. Make up to
volume with hexane (6.11) and mix well.
7 Apparatus
The glassware should be free of contamination (see A.4.5).
7.1 Volumetric flasks, of 10 ml, 50 ml, 100 ml and 1 000 ml capacities.
7.2 Pipettes, of 1 ml, 2 ml, 3 ml, 4 ml, 5 ml, 6 ml, 7 ml, 10 ml, 15 ml, 20 ml and 50 ml capacities.
7.3 Microlitre syringes, of 10 µl and 250 µl capacities.
7.4 Sampling bottle, of 1 000 ml capacity, made of amber glass, with straight shoulders and fitted with a
glass stopper.
7.5 Separating funnel, 1 000 ml.
7.6 Glass column for clean up, for example of 15 cm length, 1 cm inner diameter, with a frit, but without a
cock stop.
7.7 Beaker, of 150 ml and 5 l capacities.
7.8 Shaker.
−1
7.9 Magnetic stirrer, for example with a stirring rate of 1 200 min , and a magnetic bar, 60 mm × 4,5 mm,
coated with polytetrafluoroethene.
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
7.10 Round bottomed flasks, fitted with a ground glass joint, of 100 ml and 250 ml capacities.
7.11 Concentration apparatus, for example a rotary evaporator.
7.12 Muffle furnace, capable of maintaining a temperature of 500 °C ± 20 °C.
7.13 Drying oven, capable of heating up to 180 °C.
7.14 Quartz plate, having a 12 cm diameter.
7.15 Desiccator.
7.16 Separator, for example a Schultze separator, see Figure 1.
7.17 Gas chromatograph, with suitable detector device (see 7.19).
7.18 Injector, split or splitless, preferably with automated sampling device.
7.19 Detectors, equipped with a suitable data processing system for acquisition and data evaluation.
7.19.1 Flame photometric detector (FPD), equipped with a cut-off filter of 590 nm or an interference filter of
610 nm or pulsed flame photometric detector equipped with a large bandpass filter working at 610 nm or
390 nm with time-selective acquisition.
7.19.2 Mass spectrometer for electron impact (EI) mode, with sufficient sensitivity.
7.19.3 Atomic emission detector.
8 Procedure
8.1 Sampling and sample storage
Carry out sampling in accordance with ISO 5667-1, ISO 5667-2, and ISO 5667-3.
For sampling of drinking water, surface water and wastewater, use 1 000 ml sampling bottles (7.4). Carry out
all the following steps including the extraction (see 8.2.1) in the sampling bottle.
Mark a 1 000 ml sampling bottle with a 1 l mark. Fill the bottle to the mark. Keep cool and in the dark and
pretreat within 24 h (see 8.2).
It is also appropriate to weigh prior to and after filling.
8.2 Derivatization and extraction
8.2.1 General
In cases where the concentration of organotin compounds in surface and wastewater exceeds the working
range, the samples need the following further treatment.
Dilute surface water and wastewater samples with water (6.1) to meet the working range (10 ng/l to
1 000 ng/l). If necessary, carry out a screening procedure in order to determine the approximate concentration
of organotin in the sample. Mark a 1 l sampling bottle with a 1 l mark. Add the appropriate amount of surface
water or wastewater, respectively. Make up with water to the mark. Note the surface water and wastewater
volume, respectively, used for analysis in order to calculate the final result.
8 © ISO 2004 – All rights reserved
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
Dimensions in millimetres (approximate)
Key
1 stopcock
2 ground glass joint
Figure 1 — Schultze separator
© ISO 2004 – All rights reserved 9
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SIST EN ISO 17353:2005
ISO 17353:2004(E)
Pretreat samples of drinking water, surface water and wastewater and aqueous reference sam
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