EN ISO 6468:1996
(Main)Water quality - Determination of certain organochlorine insecticides, polychlorinated biphenyls and chlorobenzenes - Gas chromatographic method after liquid-liquid extraction (ISO 6468:1996)
Water quality - Determination of certain organochlorine insecticides, polychlorinated biphenyls and chlorobenzenes - Gas chromatographic method after liquid-liquid extraction (ISO 6468:1996)
Describes a method for determining certain organochlorine insecticides, polychlorinated biphenyls (PCBs) and chlorobenzenes (except the mono- and dichlorobenzenes) in drinking water, ground water, surface waters and waste waters. The method is applicable to samples containing up to 0,05 g/l of suspended solids.
Wasserbeschaffenheit - Bestimmung bestimmter Organochlorinsektizide, Polychlorbiphenyle und Chlorbenzole - Gaschromatographisches Verfahren nach Flüssig-Flüssig-Extraktion (ISO 6468:1996)
Diese Internationale Norm beschreibt ein Verfahren zur Bestimmung einiger Organochlorinsektizide, Polychlorbiphenyle (PCB) und Chlorbenzole (ausgenommen Mono- und Dichlorbenzole) in Trinkwasser, Grundwasser, Oberflächenwasser und Abwasser. Dieses Verfahren eignet sich für Proben, die bis zu 0,05 g/l suspendierte Stoffe enthalten; in Gegenwart von organischem Material, suspendierten Stoffen und Kolloiden treten häufiger Störungen auf, und die Nachweisgrenzen sind demzufolge höher.
Qualité de l'eau - Dosage de certains insecticides organochlorés des polychlorobiphényles et des chlorobenzènes - Méthode par chromatographie en phase gazeuse après extraction liquide-liquide (ISO 6468:1996)
La présente Norme internationale décrit une méthode pour le dosage de certains insecticides organochlorés, des polychlorobiphényles (PCB) et des chlorobenzènes (sauf le mono- et le dichlorobenzène) présents dans les eaux destinées à la consommation humaine, les eaux souterraines, les eaux de surface et les eaux usées. La méthode est applicable aux échantillons 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 sont donc plus élevées. La méthode décrite dans la présente Norme internationale ne donne des informations que sur certains composés PCB spécifiques, et non sur le taux total de tous les composés PCB. Selon les types de composés à détecter et l'origine de l'eau, les limites de détection indiquées au tableau 1 sont applicables pour la méthode décrite dans la présente Norme internationale, pour des eaux à faible teneur organique. Compte tenu des 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 et tout particulièrement lorsque les concentrations sont inférieures à 10 ng/l.
Kakovost vode - Določevanje nekaterih organoklornih insekticidov, polikloriranih bifenilov in klorobenzenov - Plinska kromatografska metoda po tekočinski ekstrakciji (ISO 6468:1996)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-januar-1998
.DNRYRVWYRGH'RORþHYDQMHQHNDWHULKRUJDQRNORUQLKLQVHNWLFLGRYSROLNORULUDQLK
ELIHQLORYLQNORUREHQ]HQRY3OLQVNDNURPDWRJUDIVNDPHWRGDSRWHNRþLQVNL
HNVWUDNFLML ,62
Water quality - Determination of certain organochlorine insecticides, polychlorinated
biphenyls and chlorobenzenes - Gas chromatographic method after liquid-liquid
extraction (ISO 6468:1996)
Wasserbeschaffenheit - Bestimmung bestimmter Organochlorinsektizide,
Polychlorbiphenyle und Chlorbenzole - Gaschromatographisches Verfahren nach Flüssig
-Flüssig-Extraktion (ISO 6468:1996)
Qualité de l'eau - Dosage de certains insecticides organochlorés des
polychlorobiphényles et des chlorobenzenes - Méthode par chromatographie en phase
gazeuse apres extraction liquide-liquide (ISO 6468:1996)
Ta slovenski standard je istoveten z: EN ISO 6468:1996
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
INTERNATIONAL IS0
STANDARD 6468
First edition
Water quality - Determination of certain
organochlorine insecticides,
polychlorinated biphenyls and
chlorobenzenes - Gas chromatographic
method after liquid-liquid extraction
Qua/it& de I’eau - Dosage de cetiains insecticides organochlor&, des
polychlorobiph&yles et des chlorobenz&nes - M&hode par
chromatographie en phase gazeuse apr& extraction liquide-liquide
Reference number
IS0 6468: 1996(E)
ISO6468:1996(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide fed-
eration of national standards bodies IS0 member bodies). The work of
(
preparing International Standards is normally carried out through IS0
technical committees. Each member t: N )dy 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. IS0 collab-
orates closely with the International Electrotechnical Commission (IEC) on
all matters of electrotechnical standardization.
Draft International Standards adopted by the technical committees are cir-
culated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard IS0 6468 was prepared by Technical Committee
lSO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical, bio-
chemical methods.
Annex A forms an integral part of this International Standard. Annexes B to
H are for information only.
0 IS0 1996
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronic or mechanical, including photocopying and
microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-1211 Gen&ve 20 l Switzerland
Printed in Switzerland
ii
IS0 6468: 1996(E)
INTERNATIONAL STANDARD @ IS0
Water quality - Determination of certain organochlorine
insecticides, polychlorinated biphenyls and chlorobenzenes -
Gas chromatographic method after liquid-liquid extraction
- This method makes use of flammable and toxic organic sol-
WARNING AND SAFETY PRECAUTIONS
vents. Observe the safety regulations in effect.
The electron-capture detector (ECD) contains radionuclides. Adequate safety precautions and legal re-
quirements must be observed.
The halogenated hydrocarbons and chloropesticides, used for the preparation of the calibration standards
are toxic. Therefore, the safety regulations pertaining must be strictly observed.
1 Scope 2 Normative references
The following standards contain provisions which,
This International Standard describes a method for
through reference in this text, constitute provisions of
determining certain organochlorine insecticides, poly-
this International Standard. At the time of publication,
chlorinated biphenyls (PCBs) and chlorobenzenes
the editions indicated were valid. All standards are
(except the mono- and dichlorobenzenes) in drinking
subject to revision, and parties to agreements based
waters, ground waters, surface waters and waste
on the International Standard are encouraged to in-
waters.
vestigate the possibility of applying the most recent
The method is applicable to samples containing up to
editions of the standards indicated below. Members of
0,05 g/l of suspended solids. In the presence of or-
IEC and IS0 maintain registers of currently valid Inter-
ganic matter, suspended matter and colloids, interfer-
national Standards.
ences are more numerous and consequently the
detection limits are higher. IS0 5667-l :1980, Water quality- Sampling - Part 7:
Guidance on the design on sampling programmes.
The method described in this International Standard
only gives information on specific PCB compounds but
IS0 5667-2:1991, Water quality - Sampling - Part 2:
no information on the level of total PCBs.
Guidance on sampling techniques.
According to the types of compounds to be detected
and the source of the water, the detection limits given
in table 1 are applicable for the method described in
3 Principle
this International Standard, with waters of low organic
contents.
Liquid-liquid extraction of organochlorine insecticides,
chlorobenzenes and PCBs by an extraction solvent.
Given the very low concentrations normally present in
After the concentration of the components with low
the waters, the problem of contamination is extremely
volatility and after any clean-up steps which may be
important. The lower the level measured, the more
necessary, the sample extracts are analysed by gas
precautions have to be observed; below concen-
chromatography, using an electron-capture detector.
trations of 10 rig/l,, special care is necessary.
IS0 6468: 1996(E)
Table 1 - Detection limits
Acronyms Chemical names (IUPAC) Detection limits
Organochlorine insecticides:
HCH 1, 2, 3, 4, 5, 6-hexachlorocyclohexane,
five stereoisomers:
alpha-HCH
beta-HCH
Lindane gamma-HCH
delta-HCH
epsilon-HCH
o,/-DDE I,1 -dichloro-2-(2-chlorophenyl I)-2-(4-chlorophenyl)ethylene
JI,~ ‘-DDE I,1 -dichloro-2,2-bis(4-chlorophenyl)ethylene 1 rig/l
& ‘-DE I,1 -dichloro-2-(2-chlorophenyl)-2-(4-chlorophenyl)ethane (= o,/-DDD) to
10 rig/l
/J,JI ’-TDE I,1 -dichloro-2, 2-bis(4-chlorophenyl)ethane (= p,p ’-DDD)
depending
~,JI ’-DDT 1 ,I ,I -trichloro-2-(2-chlorophenyl)-2-(4-chlorophenyl)ethane
~,JI ’-DDT 1 ,I ,I -trichloro-2,2-bis(4-chlorophenyl)ethane on the
Methoxychlor 1 ,I ,I -trichloro-2,2-bis(4-methoxyphenyl)ethane compound
Aldrin (1 R, 4S, 4aS, 5S, 8R, 8aR)-1, 2, 3, 4, 10, IO-hexachloro-1, 4, 4a, 5, 8,
8a-hexahydro-1,4: 5,8-dimethanonaphthalene
Dieldrin (IR, 4S, 4aS, 5R, 6R, 7S, 8S, 8aR)-1,2,3,4,10, IO-hexachloro-1,4,4a, 5,
6,7,8,8a-octahydro-6,7-epoxy-l,4 : 5,8-dimethanonaphthalene
Endrin (1 R, 4S, 4aS, 5S, 6S, 7R, 8R, 8aR)-1,2,3,4,10, IO-hexachloro-l , 4,4a, 5,
6,7,8,8a-octahydro-6,7-epoxy-l,4 : 5,8=dimethanonaphthalene
Heptachlorl) 1,4,5,6,7,8,8-heptachloro-3a, 4,7,7a-tetrahydro-4,7-methanoindenel)
Heptachlor-epoxide 1, 4, 5, 6, 7, 8, 8-heptachloro-2,3-epoxy-3a,4,7,7a-tetrahydro-4,7
-methanoindane
Endosulfanl) *) 1,4,5,6,7,7,7-hexachloro-8,9, IO-trinorborn-5-en-2,3-ylene-dimethyl-
enesulfite:
alpha-Endosulfan
beta-Endosulfan
Chlorobenzenes:
trichlorobenzene 1 rig/l
TrCB
tetrachlorobenzene to
TeCB
PeCB pentachlorobenzene 10 rig/l
HCB hexachlorobenzene depending on
the compound
PCNB (Quintozene) pentachloronitrobenzene
Polychlorinated biphenyls:
PCB 28 2,4,4 ’-trichlorobiphenyl
PCB 52 2,2 ’, 5,5 ’-tetrachlorobiphenyl 1 rig/l
to
PCB 101 2,2 ’, 4,5,5 ’-pentachlorobiphenyl
50 rig/l
PCB 138 2,2 ’, 3,4,4 ’, 5 ’-hexachlorobiphenyl
2,2 ’, 4,4 ’, 5,5 ’-hexachlorobiphenyl depending on
PCB 153
2,2 ’, 3,4,4 ’, 5,5 ’-heptachlorobiphenyl the compound
PCB 180
PCB 194 2,2 ’, 3,3 ’, 4,4 ’, 5,5 ’-octachlorobiphenyl
1) The analysis of a and p - endosulfan as well as heptachlor requires special care due to its low stability.
2) The name “endosulfan” is not acceptable for use in Italy, as it is in conflict with a trade mark registered there.
IS0 6468: 1996(E)
0 IS0
muffle furnace. Cool to about 200 “C in the furnace
Any substance capable of producing a response on
and then to ambient temperature in a desiccator. Store
the electron-capture detector, at a retention time indis-
will in a sealed glass container.
tinguishable from compound of interest,
any
interfere. In practice, many potentially interfering sub-
stances will be removed during the extraction and
4.6 Deactivated alumina.
clean-up procedures.
Weigh a portion of dry alumina (4.5) into a sealable all-
NOTE 1 In general, the use of two capillary columns of
glass container and add 7 % + 0,2 % (m/m) of water
different polarity is sufficient for the organochlorine com-
(4.1). Seal and agitate for at least 2 h to ensure uni-
pounds analysed according to this International Standard.
formity. Store in a sealed glass container.
The results so calculated should be considered as the
maximum concentrations, possibly still influenced by coelut-
ing substances. It is possible that there will be cases where Once the seal has been broken, storage time is nor-
a more definite identification is required. mally about one week. After the maximum storage
time, reprocess batches as described in 4.5 and this
subclause.
4 Reagents and materials
4.7 Alumina/silver nitrate.
All reagents shall be sufficiently pure to not give rise to
significant interfering peaks in the gas chromatograms
Dissolve 0,75 g + 0,Ol g of silver nitrate in 0,75 ml rfI
of the blanks. The purity of reagents used in the pro-
0,Ol ml of water (4.1) using a microburette. Add
cedure shall be checked by blank determinations
4,0 ml +_ 0,2 ml of acetone followed by 10 g + 0,2 g of
. .
(7 6)
deactivated alumina (4.6). Mix thoroughly by shaking
in an open-topped conical flask, protected from light.
NOTE 2 Commercial “pesticide grade” solvents are avail-
Allow the acetone to evaporate at room temperature
able. The use of these products is recommended only after
and prevent condensation, for example by warming
verifying their quality. The quality of a solvent is checked by
with the hand.
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
Store in the dark and use within 4 h after preparation.
does not give any detectable interfering peaks in the chro-
matogram for the substance of interest.
4.8 Silica gel, of particle size 63 pm to 200 pm,
heated at 500 “C + 30 “C in batches not larger than
4.1 Water purified, for example, using ion-exchange
500 g, for about 14 h. Cool to about 200 “C in the fur-
or carbon-column adsorption.
nace and then to ambient temperature in a sealed
flask which is placed in a desiccator without desiccant.
Use this material within one week. Deactivate the sil-
4.2 Extraction solvent.
ica gel by weighing a suitable quantity of silica and
adding 3 % (m/m) of water (4.1). Agitate for at least 2 h
Hexane, petroleum ether or heptane are suitable.
to ensure uniformity and store in a sealed glass con-
tainer.
NOTE 3 Any other solvents meeting the requirements of
8.3 (recovery rate a 60 Oh) may be used.
The deactivated silica gel shall be used within 24 h.
4.3 Sodium sulfate (NazSO,), anhydrous.
4.9 Toluene.
Heat a portion of about 250 ml to 300 ml of sodium
sulfate powder at 500 “C IfI 20 “C for 4 h + 30 min, cool
4.10 Diethylether, free from peroxides.
to about 200 “C in a muffle furnace and then to ambi-
ent temperature in a desiccator containing magnesium
4.11 Anti-bumping granules, washed with
perchlorate or an equivalent alternative.
acetone.
4.4 Decane (CloH22) or dodecane (C12H2s), or any
4.12 Standard stock solutions.
keeper which is not detected by the electron-capture
detector.
Pure or certified standards of organochlorine insecti-
tides, chlorobenzenes, and PCBs shall be used for
4.5 Dry alumina.
the preparation of standard stock solutions.
Heat a batch of inert alumina, containing particles of
NOTE 4 Suitable solvents for the preparation of standard
size 50 pm to 200 pm and of maximum mass 500 g, at
stock solutions are acetone, pentane, hexane, dimethyl-
500 “C + 20 “C for 4 h + 30 min on a silica dish in a
benzene or isooctane.
@ IS0
IS0 6468: 1996(E)
a length of 25 m to 60 m, coated with stationary
The containers containing the solutions shall be
marked or weighed so that any evaporation losses of phases capable of separating the compounds of inter-
est.
the solvent may be recognized. The solutions shall be
stored in volumetric flasks with ground-glass stoppers
Annex B provides examples of gas chromatographic
at a temperature of 4 ’“C in the dark. Prior to use, they
conditions (tables B.l, B.2 and B.3) and the corre-
shall be brought to ambient temperature and the level
of solvent shall be adjusted, if necessary. sponding gas chromatograms (figures B.1 and B.2).
NOTE 5 A convenient concentration of standard stock sol-
5.3 Separating funnels, of nominal capacities 1 litre
ution is obtained by weighing 50 mg of each determinand
to 5 litres, with a glass tap washed by hexane or a
and dissolving it in 100 ml of the solvent.
polytetrafluoroethylene (PTFE) tap.
The solution is stable for about 1 year.
5.4 High-speed stirrer and magnetic stirring bar,
washed with hexane and coated with polytetrafluoro-
ethylene (PTFE).
4.13 Intermediate standard solutions.
5.5 Microseparator, see example in figure C.I.
Prepare intermediate standard solutions by a suitable
dilution of the stock solution (4.12) with the extraction
solvent (4.2).
5.6 Kuderna-Danish evaporator, s
...
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