SIST EN ISO 15586:2003
(Main)Water quality - Determination of trace elements using atomic absorption spectrometry with graphite furnace (ISO 15586:2003)
Water quality - Determination of trace elements using atomic absorption spectrometry with graphite furnace (ISO 15586:2003)
The method will give a general guide for the determination of metals by flameless AAS.
Wasserbeschaffenheit - Bestimmung von Spurenelementen mittels Atomabsorptionsspektrometrie mit dem Graphitrohr-Verfahren (ISO 15586:2003)
Diese Internationale Norm enthält Grundlagen und Verfahrensweisen für die Bestimmung von: Ag, Al, As, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Se, Tl, V und Zn in Oberflächenwasser, Grundwasser, Trinkwasser, Abwasser und Sedimenten durch Atomabsorptionsspektrometrie mit elektrothermischer Atomisierung im Graphitrohrofen. Das Verfahren ist anwendbar für die Bestimmung niedriger Element-Konzentrationen.
Die Nachweisgrenze des Verfahrens hängt für jedes Element von der Probenmatrix, dem Gerät, dem Zerstäubertyp und den Matrixmodifikationslösungen ab. Für Wasserproben mit sehr geringer Matrixbelastung (z. B. geringe Konzentration an gelösten Feststoffen und Partikeln) wird die Nachweisgrenze in der Nähe der instrumentellen Nachweisgrenze liegen. Die Tabelle 1 enthält Werte, die bei Verwendung eines Probenvolumens von 20 µl mindestens erreicht werden.
Qualité de l'eau - Dosage des oligo-éléments par spectrométrie d'absorption atomique en four graphite (ISO 15586:2003)
L'ISO 15586:2003 décrit des principes et des modes opératoires permettant de déterminer les très faibles teneurs en éléments Ag, Al, As, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Se, TI, V et Zn présents à l'état de traces dans les eaux de surface, eaux souterraines, eaux potables, eaux usées et sédiments, par spectrométrie d'absorption atomique avec atomisation électrothermique en four graphite. Cette méthode est applicable au dosage des éléments en faible concentration.
Pour chaque élément, la limite de détection de la méthode dépend de la matrice de l'échantillon ainsi que de l'appareil, du type d'atomiseur et de l'emploi de modificateurs chimiques. Pour les échantillons d'eau à matrice simple (c'est-à-dire ayant une faible concentration en particules et substances solides dissoutes), les limites de détection de la méthode seront proches de celles de l'appareil. Les valeurs limites de détection acceptables sont spécifiées pour un volume d'échantillon de 20 microlitre.
Kakovost vode – Določevanje elementov v sledovih z atomsko absorpcijsko spektrometrijo z grafitno pečjo (ISO 15586:2003)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 15586:2003
01-december-2003
.DNRYRVWYRGH±'RORþHYDQMHHOHPHQWRYYVOHGRYLK]DWRPVNRDEVRUSFLMVNR
VSHNWURPHWULMR]JUDILWQRSHþMR ,62
Water quality - Determination of trace elements using atomic absorption spectrometry
with graphite furnace (ISO 15586:2003)
Wasserbeschaffenheit - Bestimmung von Spurenelementen mittels
Atomabsorptionsspektrometrie mit dem Graphitrohr-Verfahren (ISO 15586:2003)
Qualité de l'eau - Dosage des oligo-éléments par spectrométrie d'absorption atomique
en four graphite (ISO 15586:2003)
Ta slovenski standard je istoveten z: EN ISO 15586:2003
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
SIST EN ISO 15586:2003 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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EUROPEAN STANDARD
EN ISO 15586
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2003
ICS 13.060.50
English version
Water quality - Determination of trace elements using atomic
absorption spectrometry with graphite furnace (ISO 15586:2003)
Qualité de l'eau - Dosage des oligo-éléments par Wasserbeschaffenheit - Bestimmung von
spectrométrie d'absorption atomique en four graphite (ISO Spurenelementen mittels Atomabsorptionsspektrometrie
15586:2003) mit dem Graphitrohr-Verfahren (ISO 15586:2003)
This European Standard was approved by CEN on 1 September 2003.
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 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 Management Centre has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, 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
© 2003 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 15586:2003 E
worldwide for CEN national Members.
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EN ISO 15586:2003 (E)
CORRECTED 2003-12-03
Foreword
This document (EN ISO 15586:2003) has been prepared by Technical Committee ISO/TC 147
"Water quality" in collaboration with Technical Committee CEN/TC 230 "Water analysis", the
secretariat of which is held by DIN.
This European Standard shall be given the status of a national standard, either by publication of
an identical text or by endorsement, at the latest by April 2004, and conflicting national
standards shall be withdrawn at the latest by April 2004.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium, Czech
Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and
the United Kingdom.
Endorsement notice
The text of ISO 15586:2003 has been approved by CEN as EN ISO 15586:2003 without any
modifications.
NOTE: Normative references to International Standards are listed in annex ZA (normative).
2
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EN ISO 15586:2003 (E)
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions of
any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).
NOTE Where an International Publication has been modified by common modifications, indicated
by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 3696 1987 Water for analytical and laboratory EN ISO 3696 1995
use — Specification and test methods
ISO 5667-1 1980 Water quality — Sampling — Part 1: EN 25667-1 1993
Guidance on the design of sampling
programs
ISO 5667-2 1991 Water quality — Sampling — Part 2: EN 25667-2 1993
Guidance on sampling techniques
ISO 5667-3 1994 Water quality — Sampling — Part 3: EN ISO 5667-3 1995
Guidance on the preservation and
handling of samples
ISO 15587-1 2002 Water quality - Digestion for the EN ISO 15587-1 2002
determination of selected elements in
water - Part 1: Aqua regia digestion
ISO 15587-2 2002 Water quality - Digestion for the EN ISO 15587-2 2002
determination of selected elements in
water - Part 2: Nitric acid digestion
3
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INTERNATIONAL ISO
STANDARD 15586
First edition
2003-10-01
Water quality — Determination of trace
elements using atomic absorption
spectrometry with graphite furnace
Qualité de l'eau — Dosage des éléments traces par spectrométrie
d'absorption atomique en four graphite
Reference number
ISO 15586:2003(E)
©
ISO 2003
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ISO 15586:2003(E)
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ii © ISO 2003 — All rights reserved
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ISO 15586:2003(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 Principle . 2
4 Interferences. 3
5 Reagents . 3
6 Apparatus. 5
7 Sampling and pre-treatment . 6
8 Chemical modification. 8
9 Determination . 10
10 Calibration. 10
11 Calculation. 11
12 Precision . 12
13 Test report. 17
Annex A (informative) Preparation of stock solutions, 1 000 mg/l. 18
Annex B (normative) Digestion of sediment samples . 20
Annex C (informative) Examples of instrumental parameter settings . 22
Bibliography . 23
© ISO 2003 — All rights reserved iii
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ISO 15586:2003(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 15586 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
iv © ISO 2003 — All rights reserved
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INTERNATIONAL STANDARD ISO 15586:2003(E)
Water quality — Determination of trace elements using atomic
absorption spectrometry with graphite furnace
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 includes principles and procedures for the determination of trace levels of: Ag, Al,
As, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Se, Tl, V, and Zn in surface water, ground water, drinking water,
wastewater and sediments, using atomic absorption spectrometry with electrothermal atomization in a
graphite furnace. The method is applicable to the determination of low concentrations of elements.
The detection limit of the method for each element depends on the sample matrix as well as of the instrument,
the type of atomizer and the use of chemical modifiers. For water samples with a simple matrix (i.e. low
concentration of dissolved solids and particles), the method detection limits will be close to instrument
detection limits. The minimum acceptable detection limit values for a 20-µl sample volume are given in Table 1.
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
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of 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
ISO 5667-4, Water quality — Sampling — Part 4: Guidance on sampling from lakes, natural and man-made
ISO 5667-5, Water quality — Sampling — Part 5: Guidance on sampling of drinking water and water used for
food and beverage processing
ISO 5667-6, Water quality — Sampling — Part 6: Guidance on sampling of rivers and streams
ISO 5667-10, Water quality — Sampling — Part 10: Guidance on sampling of waste waters
ISO 5667-11, Water quality — Sampling — Part 11: Guidance on sampling of groundwaters
ISO 5667-15, Water quality — Sampling — Part 15: Guidance on preservation and handling of sludge and
sediment samples
ISO 15587-1, Water quality — Digestion for the determination of elements in water — Part 1: Aqua regia
digestion
© ISO 2003 — All rights reserved 1
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ISO 15586:2003(E)
ISO 15587-2, Water quality — Digestion for the determination of elements in water — Part 2: Nitric acid
digestion
Table 1 — Approximate characteristic masses, instrument detection limits and optimum working
ranges for water samples using a 20 µl sample volume
b c
Characteristic mass
Detection limit Optimum working range
a
m
0
Element
pg µg/l µg/l
Ag 1,5 0,2 1 to 10
Al 10 1 6 to 60
As 15 1 10 to 100
Cd 0,7 0,1 0,4 to 4
Co 10 1 6 to 60
Cr 3 0,5 2 to 20
d
Cu 0,5 3 to 30
5
Fe 5 1 3 to 30
Mn 2,5 0,5 1,5 to 15
Mo 10 1 6 to 60
Ni 13 1 7 to 70
Pb 15 1 10 to 100
Sb 20 1 10 to 100
Se 25 2 15 to 150
d
Tl 10 1 6 to 60
V 35 2 20 to 200
Zn 0,8 0,5 0,5 to 5
a
The characteristic mass (m ) of an element is the mass in picograms, corresponding to a signal of 0,004 4 s, using the integrated
0
absorbance (peak area) for evaluation.
b
The detection limits are calculated as three times (3 ×) the standard deviation of repeated measurements of a blank solution.
c
The optimum working range is defined as the concentration range that corresponds to integrated absorbance readings between
0,05 s and 0,5 s.
d
If Zeeman effect background correction is used, the m -value will be higher.
0
3 Principle
Water samples are preserved by acid treatment, filtered and preserved by addition of acid, or digested.
Sediment samples are digested. A small sub-sample of sample solution is injected into a graphite furnace of
an atomic absorption spectrometer. The furnace is electrically heated. By increasing the temperature stepwise,
the sample is dried, pyrolized and atomized. Atomic absorption spectrometry is based on the ability of free
atoms to absorb light. A light source emits light specific for a certain element (or elements). When the light
beam passes through the atom cloud in the heated graphite furnace, the light is selectively absorbed by atoms
of the chosen element(s). The decrease in light intensity is measured with a detector at a specific wavelength.
The concentration of an element in a sample is determined by comparing the absorbance of the sample with
the absorbance of calibration solutions. If necessary, interferences may be overcome by adding a matrix
modifier to the samples before analysis, or by performing the calibration with the standard addition technique.
The results are given as the mass of analyte (micrograms, µg, or milligrams, mg) per litre of water, or per
kilogram of dried material in sediments.
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ISO 15586:2003(E)
4 Interferences
Some sample solutions, especially wastewaters and digestions of sediments, may contain large amounts of
substances that may affect the results. High concentrations of chloride may cause low results, because the
volatility of many elements is increased and analyte loss may occur during the pyrolysis step. Matrix effects
may be overcome, partially or completely, by optimization of the temperature programme, the use of
pyrolytically-coated tubes and platforms, the use of chemical modifiers, the standard addition technique and
the use of background correction.
5 Reagents
For pre-treatment of samples and preparation of solutions, use only chemicals and solutions of highest
possible purity unless stated otherwise.
5.1 Water, Grade 1 as specified in ISO 3696:1987 (u 0,01 mS/m), or better.
Use this water to prepare all solutions. Check the quality of the water before use.
5.2 Nitric acid, concentrated, c(HNO ) = 14,4 mol/l, ρ ≈ 1,4 kg/l (65 %).
3
If the concentrated nitric acid contains significant amounts of analyte elements, purify it by sub-boiling
distillation in a quartz apparatus. The distillation should be performed under a fume cupboard.
Nitric acid is available both as ρ = 1,40 kg/l (65 %) and as ρ = 1,42 kg/l (69 %). Both are suitable for use in this
method provided there is minimal content of analytes.
5.3 Nitric acid, c(HNO ) ≈ 7 mol/l.
3
Add one volume of concentrated nitric acid (5.2) to one volume of water (5.1) while stirring.
5.4 Nitric acid, c(HNO ) ≈ 1 mol/l.
3
To about 500 ml of water (5.1), add 70 ml of concentrated nitric acid (5.2) and dilute with water (5.1) to
1 000 ml.
5.5 Nitric acid, c(HNO ) ≈ 0,1 mol/l.
3
To about 500 ml of water (5.1), add 7 ml of concentrated nitric acid (5.2) and dilute with water (5.1) to 1 000 ml.
5.6 Hydrochloric acid, concentrated, c(HCl) = 12,1 mol/l, ρ ≈ 1,19 kg/l (37 %).
If the concentrated hydrochloric acid contains significant amounts of analyte elements, purify e.g. by
sub-boiling distillation in a quartz apparatus. The distillation should be performed under a fume cupboard.
5.7 Hydrochloric acid, c(HCl) ≈ 6 mol/l.
Add one volume of concentrated hydrochloric acid (5.6) to one volume of water (5.1) while stirring.
5.8 Hydrochloric acid, c(HCl) ≈ 1 mol/l.
To about 500 ml of water (5.1), add 83 ml of concentrated hydrochloric acid (5.6) and dilute with water (5.1) to
1 000 ml.
5.9 Standard stock solutions, ρ = 1 000 mg/l.
Stock solutions may be purchased from a commercial source.
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ISO 15586:2003(E)
Procedures for preparation of stock solutions from metals or metal salts are described in Annex A. Stock
solutions are stable for about one year or in accordance with the manufacturer's recommendations.
5.10 Standard solution, ρ = 10 mg/l.
Using a pipette, transfer 1 000 µl of the stock solution (5.9) to a 100 ml volumetric flask, add 0,5 ml of
concentrated nitric acid (5.2), and dilute to volume with water (5.1).
This solution may be stored for 6 months.
5.11 Standard solution, ρ = 1 mg/l.
Using a pipette, transfer 100 µl of the stock solution (5.9) to a 100 ml volumetric flask, add 0,5 ml of
concentrated nitric acid (5.2), and dilute to volume with water (5.1).
This solution may be stored for six months.
5.12 Standard solution, ρ = 100 µg/l.
Using a pipette, transfer 1 000 µl of the standard solution 10 mg/l (5.10) to a 100 ml volumetric flask, add
0,5 ml of concentrated nitric acid (5.2), and dilute to volume with water (5.1).
This solution may be stored for one month.
5.13 Calibration solutions
Prepare calibration solutions from the standard solutions (5.10 to 5.12).
The following procedure can be used as an example:
To prepare a series of calibration solutions containing 2 µg/l; 4 µg/l; 6 µg/l; 8 µg/l and 10 µg/l of analyte,
pipette, 200 µl, 400 µl, 600 µl, 800 µl and 1 000 µl respectively of the standard solution 1 mg/l (5.11) to 100 ml
volumetric flasks. Add the same amount of acid to the calibration solutions as that of the samples. Cool if
necessary and dilute to volume with water (5.1).
Calibration solutions below 1 mg/l should not be used for more than one month, and those below 100 µg/l
should not be used for more than one day.
5.14 Blank calibration solution
Prepare a blank calibration solution in the same way as the calibration solutions, but add no standard solution.
Use a 100 ml volumetric flask. Add the same amount of acid to the calibration solutions as that of the samples.
Cool if necessary and dilute to volume with water (5.1).
5.15 Palladium nitrate/magnesium nitrate modifier
Pd(NO ) solution is commercially available (10 g/l). Dissolve 0,259 g of Mg(NO ) ·6H O in 100 ml of water
3 2 3 2 2
(5.1). Mix the palladium nitrate solution with twice as much magnesium nitrate solution. 10 µl of the mixed
solution is equal to 15 µg Pd and 10 µg Mg(NO ) . The mixture is also commercially available.
3 2
Prepare a fresh solution monthly.
5.16 Magnesium nitrate modifier
Dissolve 0,865 g of Mg(NO ) ·6H O in 100 ml of water (5.1). 10 µl of this solution is equal to 50 µg Mg(NO ) .
3 2 2 3 2
5.17 Ammonium dihydrogen phosphate modifier
Dissolve 2,0 g of NH H PO in 100 ml of water (5.1). 10 µl of this solution is equal to 200 µg NH H PO .
4 2 4 4 2 4
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ISO 15586:2003(E)
5.18 Ammonium dihydrogen phosphate/magnesium nitrate modifier
Dissolve 2,0 g of NH H PO and 0,173 g of Mg(NO ) ·6H O in 100 ml of water (5.1). 10 µl of this solution is
4 2 4 3 2 2
equal to 200 µg NH H PO and 10 µg Mg(NO ) .
4 2 4 3 2
5.19 Nickel modifier
Dissolve 0,200 g of nickel powder in 1 ml concentrated nitric acid (5.2) and dilute to 100 ml with water (5.1).
10 µl of this solution is equal to 20 µg Ni. Solutions of Ni(NO ) are also commercially available.
3 2
5.20 Purge and protective gas, argon (Ar) (W 99,99 %).
6 Apparatus
The following general cleaning procedure is the absolute minimum required for glass and plastics if nothing
else is stated.
a) Prior to use, soak the equipment for at least one day in nitric acid, c ≈ 1 mol/l (5.4), or hydrochloric acid,
c ≈ 1 mol/l (5.8).
b) Rinse with water (5.1) at least three times.
Remove parts of equipment made from polyamide (e.g. screws and nuts in sampling equipment) prior to
soaking the equipment in acid.
Take the necessary precautions in such a way that equipment, once being used for samples with high
concentration of metals, will not be used for trace element samples in the future.
6.1 Sample containers for water, consisting of bottles made of polypropylene, polyethylene or fluorinated
ethylene propylene (FEP).
The material in bottles and caps should not contain or leach any analyte, and preferably be made of
colourless material.
For determinations at ultra trace levels (< 0,1 µg/l) it is necessary to follow a very strict cleaning procedure, as
described below.
a) Rinse new bottles with acetone to remove possible fatty remainders. Alternatively, a suitable detergent
may be used.
b) Rinse with water (5.1).
c) Soak in hydrochloric acid, c ≈ 6 mol/l (5.7), for one week, or at 45 °C to 50 °C for 24 h.
d) Rinse with water (5.1).
e) Soak in nitric acid, c ≈ 7 mol/l (5.3), for one week, or at 45 °C to 50 °C for 24 h.
f) Rinse with water (5.1), and transfer to clean laboratory.
g) Soak in nitric acid c ≈ 0,1 mol/l (5.5) for one week, to condition the bottles to the matrix in use.
h) Rinse with water (5.1) several times.
i) Dry under filtered air (clean bench), if drying is necessary.
j) Store the cleaned bottles in closed plastics bags.
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ISO 15586:2003(E)
If it is shown not necessary to use both steps c) and e), one of the acids may be excluded. In this case,
hydrochloric acid is shown to be more effective for polyethylene and polypropylene, while nitric acid preferably
should be used for FEP and glassware.
6.2 Sample containers for sediments, consisting of wide-necked containers of plastics or glass.
For cleaning of the containers, it may not be necessary to use acids. Washing with detergents and rinsing in
deionized water (5.1) may be sufficient.
6.3 Filtering equipment, made of glass or plastics material without metal parts, cleaned as stated in the
general cleaning procedure under Clause 6 heading.
6.4 Filters, either membrane filters or capillary filters, with a nominal pore width of 0,45 µm and 0,4 µm
respectively.
The material should not release or absorb analytes. Clean filters in nitric acid, c ≈ 0,1 mol/l (5.5), and rinse
several times with water (5.1).
6.5 Agate mortar, for crushing sediments into a fine powder.
6.6 Pipettes, of capacity varying from 100 µl to 1 000 µl.
Pipette tips preferably should be made of colourless plastics, which do not contain or leach any analyte to the
solutions. It is important to check that the pipette tips do not contaminate samples. Always rinse the pipette
tips with the solution to be used immediately before use.
Depending on the concentration levels to be determined, new and reused pipette tips may be cleaned with
dilute acid. For example, clean with nitric acid, c ≈ 1 mol/l (5.4), and rinse with water (5.1).
6.7 Atomic absorption spectrometer equipped with graphite furnace, equipped with a background
correction system and the necessary hollow cathode lamps.
Alternatively, electrode-less discharge lamps may be used.
It is necessary to place an exhaust venting system over the furnace to remove any smoke and vapours that
might be harmful.
6.8 Autosampler, may be used to improve the precision of the determination.
Depending on the concentration levels to be determined, new autosampler cups may be cleaned with dilute
acid. Reused caps should always be washed with acid. For example, clean the vessels with nitric acid,
c ≈ 1 mol/l (5.4), and rinse with water (5.1). If they will be used for ultra trace determination (< 0,1 µg/l), an
extra cleaning step before use may be necessary by filling them with acid of the same kind and concentration
as in the samples that are to be analysed. Allow to stand for at least 2 h. Rinse several times with water (5.1).
6.9 Graphite tubes, pyrolytically-coated with platforms, preferably for highly and medium volatile elements,
whereas elements of low volatility should be atomized from the wall.
Provided satisfactory results are achieved, manufacturer's recommendations regarding the use of graphite
tubes and platforms should be followed.
7 Sampling and pre-treatment
7.1 Sampling
Sampling shall be carried out in accordance with ISO 5667-1, ISO 5667-2, ISO 5667-3, ISO 5667-4,
ISO 5667-5, ISO 5667-6, ISO 5667-10, ISO 5667-11 and ISO 5667-15.
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ISO 15586:2003(E)
The sampling equipment for water samples should be constructed in such a way that the sample does not
come in contact with parts made of metal. It should be made of plastics not releasing analytes into the sample,
and be suitable for cleaning in dilute hydrochloric acid.
7.2 Pre-treatment of water samples
7.2.1 General
Pre-treatment and analysis of samples with especially low element concentrations should be carried out under
“clean laboratory” conditions. The “clean laboratory” technique requires that the laboratory be supplied with
filtered air, and that the samples be continuously protected from contamination originating from various
sources. In some cases, “clean benches” with filtered laminar airflow under a weak over-pressure, may be
used as a suitable alternative.
Trace elements in water samples are analysed in one or more of the following fractions.
a) Preserved by addition of acid (non-filtered). Preserve the sample by addition of nitric acid. Particles
should be allowed to sediment before analysis.
b) Filtered (dissolved). Filter the sample through a membrane or capillary filter and preserve the filtrate by
addition of nitric acid.
c) Digested in acid. Digest the preserved sample with nitric acid or aqua regia.
Store preserved water samples in cool conditions in accordance with ISO 5667-3 until analysis (1 °C to 5 °C).
7.2.2 Filtration
Filtration of samples is necessary if the dissolved forms of trace elements are analysed. Filter the sample
immediately after sampling and before preservation. Avoid equipment where the sample may come in contact
with metal parts. To reduce th
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Questions, Comments and Discussion
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