EN ISO 10695:2000
(Main)Water quality - Determination of selected organic nitrogen and phosphorus compounds - Gas chromatographic methods (ISO 10695:2000)
Water quality - Determination of selected organic nitrogen and phosphorus compounds - Gas chromatographic methods (ISO 10695:2000)
Migrated from Progress Sheet (TC Comment) (2000-07-10): CEN/TC 230N285: V.A ISO lead + see file CEN/TC 230 CORR (TA/970918) ++ SPPJ_09_Y_199804 ++ 980120: ISO/DIS 10695-1 was sent out in June 1997 in ISO for ENQ. ISO agrees to ++ wait until we carry out our PQ because their texts for FDIS will not become ++ available before May/June 1998 (TA/980120)
Wasserbeschaffenheit - Bestimmung ausgewählter organischer Stickstoff- und Phosphorverbindungen -Gaschromatographische Verfahren (ISO 10695:2000)
Qualité de l'eau - Dosage de certains composés organiques azotés et phosphorés sélectionnés - Méthodes par chromatographie en phase gazeuse (ISO 10695:2000)
La présente Norme internationale spécifie deux méthodes de dosage par chromatographie en phase gazeuse de certains composés organiques azotés et phosphorés présents dans les eaux (voir Tableau 1).Les méthodes peuvent être étendues à d'autres types de substances, sous réserve qu'elles soient validées pour chaque cas particulier.L'article 3 décrit la méthode d'extraction liquide/liquide qui est applicable aux échantillons d'eaux destinées à la consommation humaine, d'eaux souterraines, d'eaux de surface et d'eaux usées, contenant jusqu'à 0,05 g/l de matières en suspension. En présence de matières organiques, de matières en suspension et de colloïdes, les interférences sont plus nombreuses et les limites de détection peuvent donc être plus élevées.NOTE Étant donné les très faibles concentrations habituellement présentes dans les eaux, le problème de la contamination est particulièrement important. Plus le niveau mesuré est faible, plus il faut prendre de précautions.L'article 4 décrit la méthode d'extraction liquide/solide qui est applicable aux échantillons d'eaux souterraines, d'eaux de surface et d'eaux destinées à la consommation humaine, contenant des concentrations en masse supérieures ou égales à 0,05 µg/l environ. Les interférences survenant lors de l'analyse de certains types d'eaux de surface peuvent empêcher l'application de cette méthode.Des limites de détection sont données pour information dans l'annexe A.NOTE Pour l'application de la présente Norme internationale, il est recommandé de se conformer au guide de contrôle qualité analytique pour l'analyse de l'eau (voir ISO/TR 13530).
Kakovost vode - Določevanje izbranih organskih dušikovih in fosfornih spojin - Metoda plinske kromatografije (ISO 10695:2000)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-december-2000
.DNRYRVWYRGH'RORþHYDQMHL]EUDQLKRUJDQVNLKGXãLNRYLKLQIRVIRUQLKVSRMLQ
0HWRGDSOLQVNHNURPDWRJUDILMH ,62
Water quality - Determination of selected organic nitrogen and phosphorus compounds -
Gas chromatographic methods (ISO 10695:2000)
Wasserbeschaffenheit - Bestimmung ausgewählter organischer Stickstoff- und
Phosphorverbindungen -Gaschromatographische Verfahren (ISO 10695:2000)
Qualité de l'eau - Dosage de certains composés organiques azotés et phosphorés
sélectionnés - Méthodes par chromatographie en phase gazeuse (ISO 10695:2000)
Ta slovenski standard je istoveten z: EN ISO 10695:2000
ICS:
13.060.70 Preiskava bioloških lastnosti Examination of biological
vode properties of water
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
INTERNATIONAL ISO
STANDARD 10695
First edition
2000-04-01
Water quality — Determination of selected
organic nitrogen and phosphorus
compounds — Gas chromatographic
methods
Qualité de l'eau — Dosage de certains composés organiques azotés et
phosphorés sélectionnés — Méthodes par chromatographie en phase
gazeuse
Reference number
ISO 10695:2000(E)
©
ISO 2000
ISO 10695:2000(E)
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ii © ISO 2000 – All rights reserved
ISO 10695:2000(E)
Contents Page
Foreword.iv
1 Scope .1
2 Normative references .2
3 Liquid/liquid extraction .2
3.1 Principle.2
3.2 Reagents.2
3.3 Apparatus .4
3.4 Sampling and sample preparation.4
3.5 Procedure .5
4 Liquid/solid extraction .6
4.1 Principle.6
4.2 Reagents.7
4.3 Apparatus .8
4.4 Sampling.8
4.5 Procedure (for RP-C18 material).8
5 Calibration .9
5.1 General.9
5.2 Calibration using external standards .9
5.3 Calibration using an internal standard.13
6 Identification and calculation .14
6.1 Identification of individual compounds.14
6.2 Calculation.14
6.3 Summary of results .15
7 Expression of results .16
8 Test report .16
Annex A (informative) Detection limits of certain organic nitrogen and phosphorus compounds.17
Annex B (informative) Examples of gas chromatograms .18
Annex C (informative) Characteristic ions for mass spectrometry.22
Annex D (informative) Precision data for certain organic nitrogen and phosphorus compounds
(liquid/solid extraction method) .23
ISO 10695:2000(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 3.
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 International Standard may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 10695 was prepared by Technical Committee ISO/TC 147, Water quality,
Subcommittee SC 2, Physical, chemical and biochemical methods.
Annexes A, B, C and D of this International Standard are for information only.
iv © ISO 2000 – All rights reserved
INTERNATIONAL STANDARD ISO 10695:2000(E)
Water quality — Determination of selected organic nitrogen and
phosphorus compounds — Gas chromatographic methods
WARNING — This International Standard makes use of flammable and toxic organic solvents and some
toxic organic and phosphorus compounds. Observe the safety regulations in effect.
1 Scope
This International Standard specifies two methods for the determination of certain organic nitrogen and phosphorus
compounds in waters by gas chromatography (see Table 1).
The methods may be extended to include additional substances, provided the methods are validated for each
individual case.
Clause 3 describes the liquid/liquid extraction method, which is applicable to samples of drinking waters, ground
waters, surface waters and waste waters containing up to 0,05 g/l of suspended solids. In the presence of organic
matter, suspended matter and colloids, interferences are more numerous and consequently the detection limits of
this method can be higher.
NOTE Because of the very low concentrations normally present in the waters, the problem of contamination is extremely
important. The lower the level measured, the more precautions have to be observed.
Clause 4 describes the liquid/solid extraction method which is applicable to samples of ground water, surface water
and drinking water containing mass concentrations of about W 0,05 μg/l. Interferences occurring with the
examination of some types of surface water can prevent the application of this method.
Detection limits are given for information in annex A.
NOTE When applying this International Standard, the guide on analytical quality control for water analysis (see
ISO/TR 13530) should be followed.
ISO 10695:2000(E)
Table 1 — Organic nitrogen and phosphorus compounds analysed by these methods
a
Name Molecular formula Molar mass
CAS No.
Atrazine C H ClN 215,7 001912-24-9
8 14 5
Cyanazine C H ClN 240,7 021725-46-2
9 13 6
Metazachlor C H ClN O 277,8 067129-08-2
14 16 3
Parathion (ethyl) C H NO PS 291,3 00056-38-2
10 14 5
Parathion (methyl) C H NO PS 263,2 298-00-0
8 10 5
C H N O
Pendimethalin 281,3 040487-42-1
13 19 3 4
C H ClN
Propazine 229,7 000139-40-2
9 16 5
C H ClN
Sebuthylazine 229,7 007286-69-3
9 16 5
Simazine C H ClN 201,7 000122-34-9
7 12 5
Terbuthylazine C H ClN 229,7 005915-41-3
9 16 5
Trifluralin C H F N O 335,3 001582-09-8
13 16 3 3 4
Vinclozolin C H Cl NO 286,1 050471-44-8
12 9 2 3
a
Chemical Abstracts Registry Number.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, any of these
publications do not apply. However, parties to agreements based on this International Standard are encouraged to
investigate the possibility of applying the most recent editions of the normative documents indicated below. For
undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC
maintain registers of currently valid International Standards.
ISO 5667-1:1980, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes.
ISO 5667-2:1991, Water quality — Sampling — Part 2: Guidance on sampling techniques.
ISO/TR 13530:1997, Water quality — Guide to analytical quality control for water analysis.
3 Liquid/liquid extraction
3.1 Principle
The organic nitrogen and phosphorus compounds in the water sample are extracted by liquid-liquid extraction with
dichloromethane. After concentration, the sample extracts are analysed by gas chromatography, using a nitrogen-
phosphorus detector.
3.2 Reagents
All reagents, including water, shall be of sufficient purity that they do not give rise to significant interfering peaks in
the gas chromatograms of the blanks. The purity of reagents used in the procedure shall be verified for each batch
of material by running blank determinations (3.5.6).
Reagents shall be stored in glass containers.
2 © ISO 2000 – All rights reserved
ISO 10695:2000(E)
NOTE Commercial "pesticide grade" solvents are available. The use of these products is recommended only after verifying
their quality. The quality of a solvent is checked by evaporation of about 200 ml down to 1 ml and analysis of the concentrate to
determine the compounds subsequently analysed. The solvent should be considered acceptable if it does not give any
detectable interfering peaks in the chromatogram for the substance of interest.
3.2.1 Water, purified using, for example, ion exchange and carbon column adsorption.
3.2.2 Dichloromethane (CH Cl ) extraction solvent.
2 2
3.2.3 Solvents for dissolution, e.g. acetone or ethyl acetate.
3.2.4 Sodium sulfate, anhydrous
Heat Na SO powder at 500 �C � 20 �Cfor 4h � 30 min, cool to about 200 �C in a muffle furnace and then to
2 4
ambient temperature in a desiccator containing magnesium perchlorate or equivalent alternative.
3.2.5 Solutions for neutralization
a) Sodium hydroxide, aqueous solution, c(NaOH) = 1 mo
...
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