SIST EN ISO 9377-2:2001

Water quality - Determination of hydrocarbon oil index - Part 2: Method using solvent extraction and gas chromatography (ISO 9377-2:2000)

Migrated from Progress Sheet (TC Comment) (2000-07-10): To be renumbered part 2 at DIS stage (Res BT 79/1998) (CC/981106) ++ Mr. Lingner has just confirmed that Part 2 & Part 3 have been deleted from the I ++ SO work programme and that consequently Part 4 has to be renumbered Part 2. Ho- ++ wever since the // DIS/ENQ has just been initiated, the change will be done at ++ FV/FDIS stage (TA/990319)

Wasserbeschaffenheit - Bestimmung des Kohlenwasserstoff-Index - Teil 2: Verfahren nach Lösemittelextraktion und Gaschromatographie (ISO 9377-2:2000)

Diese Internationale Norm legt ein Verfahren zur Bestimmung des Kohlenwasserstoffindex in Wasser mittels Gaschromatrographie fest. Das Verfahren ist für Trink- und Oberflächenwasser, Kläranlagenabläufe sowie Abwässer geeignet und erlaubt die Bestimmung des Kohlenwasserstoffindex in Konzentrationen oberhalb 0,1 mg/l. Das Verfahren ist nicht geeignet für die quantitative Bestimmung von flüchtigen Mineralölbestandteilen. Auf der Basis einer Peakmustererkennung kann eine qualitative Information zur Zusammensetzung der Mineralölbelastung erhalten werden.

Qualité de l'eau - Détermination de l'indice hydrocarbure - Partie 2: Méthode par extraction au solvant et chromatographie en phase gazeuse (ISO 9377-2:2000)

La présente partie de l'ISO 9377 spécifie une méthode pour la détermination de l'indice hydrocarbure dans les eaux au moyen d'une chromatographie en phase gazeuse. La présente méthode est applicable aux eaux de surface, aux eaux résiduaires et aux eaux des stations d'épuration et permet la détermination de l'indice hydrocarbure pour des concentrations supérieures à 0,1 mg/l. La présente méthode n'est pas applicable à la détermination quantitative de la teneur en huile minérale volatile. Toutefois, sur la base du profil des pics du chromatogramme, il est possible d'obtenir des informations d'ordre qualitatif concernant la composition de la contamination de l'huile minérale.  
NOTE 1: Pour la détermination de la teneur en huiles minérales des sols et sédiments, voir l'ISO/TR 11046.  
NOTE 2: Il convient que la concentration en masse de la graisse d'origine animale et végétale dans l'échantillon pour essai ne  dépasse pas 150 mg/l, car il est possible que la capacité d'adsorption de la garniture des colonnes pour purification ne soit pas suffisante pour  des valeurs plus élevées.  
NOTE 3: Dans le cas d'eaux résiduaires très polluées, contenant en particulier une grande quantité d'agents de surface, une perte de rendement peut se produire.

Kakovost vode - Določevanje indeksa mineralnih olj - 2. del: Metoda z uporabo ekstrakcije s topilom in plinske kromatografije (ISO 9377-2:2000)

General Information

• Status: Published
• Publication Date: 30-Nov-2001
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: KAV - Water quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Dec-2001
• Due Date: 01-Dec-2001
• Completion Date: 01-Dec-2001
• Directive: TP128 - Pravilnik o prvih meritvah in obratovalnem monitoringu odpadnih voda
• Directive: TRRTP064 - Rules on initial measurements and operational monitoring of wastewater
• Ref Project: EN ISO 9377-2:2000 - Water quality - Determination of hydrocarbon oil index - Part 2: Method using solvent extraction and gas chromatography (ISO 9377-2:2000)

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 9377-2:2001
01-december-2001
.DNRYRVWYRGH'RORþHYDQMHLQGHNVDPLQHUDOQLKROMGHO0HWRGD]XSRUDER
HNVWUDNFLMHVWRSLORPLQSOLQVNHNURPDWRJUDILMH,62
Water quality - Determination of hydrocarbon oil index - Part 2: Method using solvent
extraction and gas chromatography (ISO 9377-2:2000)
Wasserbeschaffenheit - Bestimmung des Kohlenwasserstoff-Index - Teil 2: Verfahren
nach Lösemittelextraktion und Gaschromatographie (ISO 9377-2:2000)
Qualité de l'eau - Détermination de l'indice hydrocarbure - Partie 2: Méthode par
extraction au solvant et chromatographie en phase gazeuse (ISO 9377-2:2000)
Ta slovenski standard je istoveten z: EN ISO 9377-2:2000
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
SIST EN ISO 9377-2:2001 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 9377-2:2001

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SIST EN ISO 9377-2:2001
EUROPEAN STANDARD
EN ISO 9377-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2000
ICS 13.060.50
English version
Water quality - Determination of hydrocarbon oil index - Part 2:
Method using solvent extraction and gas chromatography (ISO
9377-2:2000)
Qualité de l'eau - Détermination de l'indice hydrocarbure - Wasserbeschaffenheit - Bestimmung des
Partie 2: Méthode par extraction au solvant et Kohlenwasserstoff-Index - Teil 2: Verfahren nach
chromatographie en phase gazeuse (ISO 9377-2:2000) Lösemittelextraktion und Gaschromatographie (ISO 9377-
2:2000)
This European Standard was approved by CEN on 4 October 2000.
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,
Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, 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
© 2000 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 9377-2:2000 E
worldwide for CEN national Members.

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SIST EN ISO 9377-2:2001
Page 2
EN ISO 9377-2:2000
CORRECTED 2001-03-28
Foreword
The text of the International Standard ISO 9377-2:2000 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 2001, and conflicting national
standards shall be withdrawn at the latest by April 2001.
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, Iceland, Ireland, Italy,
Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United
Kingdom.
Endorsement notice
The text of the International Standard ISO 9377-2:2000 was approved by CEN as a European
Standard without any modification.
NOTE: Normative references to International Standards are listed in annex ZA (normative).

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SIST EN ISO 9377-2:2001
Page 3
EN ISO 9377-2:2000
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/HD Year
ISO 5667-3 1994 Water quality - Sampling - Part 3: EN ISO 5667-3 1995
Guidance on the preservation and
handling of samples

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SIST EN ISO 9377-2:2001

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SIST EN ISO 9377-2:2001
INTERNATIONAL ISO
STANDARD 9377-2
First edition
2000-10-15
Water quality — Determination of
hydrocarbon oil index —
Part 2:
Method using solvent extraction and gas
chromatography
Qualité de l'eau — Détermination de l'indice hydrocarbure —
Partie 2: Méthode par extraction au solvant et chromatographie en phase
gazeuse
Reference number
ISO 9377-2:2000(E)
©
ISO 2000

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SIST EN ISO 9377-2:2001
ISO 9377-2:2000(E)
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ii © ISO 2000 – All rights reserved

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SIST EN ISO 9377-2:2001
ISO 9377-2:2000(E)
Contents Page
Foreword.iv
1 Scope .1
2 Normative references .1
3 Term and definition .1
4 Interferences .2
5 Principle.2
6 Reagents.2
7 Apparatus .4
8 Sampling and sample preservation .5
9 Procedure .5
10 Test report .9
11 Precision.10
Annex A (informative) Example of a column and a microseparator .11
Annex B (informative) Examples of gas chromatograms of mineral oil standard and water samples .13
Annex C (informative) Determination of boiling range of a mineral oil from the gas chromatogram .18
Bibliography.19
© ISO 2000 – All rights reserved iii

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SIST EN ISO 9377-2:2001
ISO 9377-2:2000(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 part of ISO 9377 may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 9377-2 was prepared by Technical Committee ISO/TC 147, Water quality,
Subcommittee SC 2, Physical, chemical and biochemical methods.
ISO 9377 consists of the following parts, under the general title Water quality — Determination of hydrocarbon oil
index:
� Part 1: Method using solvent extraction and gravimetry
� Part 2: Method using solvent extraction and gas chromatography
Annexes A, B and C of this part of ISO 9377 are for information only.
iv © ISO 2000 – All rights reserved

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SIST EN ISO 9377-2:2001
INTERNATIONAL STANDARD ISO 9377-2:2000(E)
Water quality — Determination of hydrocarbon oil index —
Part 2:
Method using solvent extraction and gas chromatography
1 Scope
This part of ISO 9377 specifies a method for the determination of the hydrocarbon oil index in waters by means of
gas chromatography. The method is suitable for surface water, waste water and water from sewage treatment
plants and allows the determination of a hydrocarbon oil index in concentrations above 0,1 mg/l.
The method is not applicable to the quantitative determination of the content of volatile mineral oil. However, on the
basis of the peak pattern of the gas chromatogram, certain qualitative information on the composition of the mineral
oil contamination can be derived.
NOTE 1 For the determination of the mineral-oil content of soils and sediment, see ISO/TR 11046.
NOTE 2 The mass concentration of animal and vegetable fat in the test sample should not exceed 150 mg/l, because at
higher values the adsorption capacity of the clean-up column packing may not be sufficient.
NOTE 3 In the case of highly polluted waste water, especially if containing a high amount of surfactants, a loss in recovery
may occur.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this part of ISO 9377. For dated references, subsequent amendments to, or revisions of, any of these publications
do not apply. However, parties to agreements based on this part of ISO 9377 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 5667-3:1994, Water quality — Sampling — Part 3: Guidance on the preservation and handling of samples.
ISO 8466-1:1990, Water quality — Calibration and evaluation of analytical methods and estimation of performance
characteristics — Part 1: Statistical evaluation of the linear calibration function.
3 Term and definition
For the purposes of this part of ISO 9377, the following term and definition applies.
© ISO 2000 – All rights reserved 1

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SIST EN ISO 9377-2:2001
ISO 9377-2:2000(E)
3.1
hydrocarbon oil index by GC-FID
the sum of concentrations of compounds extractable with a hydrocarbon solvent, boiling point between 36 �Cand
1)
69 �C, not adsorbed on Florisil and which may be chromatographed with retention times between those of
n-decane (C H ) and n-tetracontane (C H )
10 22 40 82
NOTE Substances complying with this definition are long-chain or branched aliphatic, alicyclic, aromatic or alkyl-
substituted aromatic hydrocarbons.
4 Interferences
Compounds of low polarity (e.g. halogenated hydrocarbons) and high concentrations of polar substances can
interfere with the determination.
Surface-active substances interfere with the extraction step.
5Principle
The water sample is extracted with an extracting agent. Polar substances are removed by clean-up on Florisil. The
purified aliquot is analysed by capillary chromatography using a non-polar column and a flame ionization detector
(FID). The total peak area between n-decane and n-tetracontane is measured. The concentration of mineral oil is
quantified against an external standard consisting of two specified mineral oils, and the hydrocarbon oil index is
calculated.
It is absolutely essential that the test described in this part of ISO 9377 be carried out by suitably qualified staff.
It should be investigated whether and to what extent particular problems will require the specification of additional
marginal conditions.
6 Reagents
All reagents shall be reagent grade and suitable for their specific purpose. The suitability of the reagents and
solutions shall be checked by carrying out a blank test.
6.1 Water for the preparation of solutions.
Distilled water, or water from a generator of purified water capable of removing organic traces, for example using
activated carbon, shall be used.
6.2 Extracting agent.
Single hydrocarbon solvent or technical mixture of hydrocarbons, boiling range 36 �Cto 69 �C.
In case of a change of extracting agent, repeatability tests are necessary.
6.3 Sodium sulfate, anhydrous,Na SO .
2 4
6.4 Magnesium sulfate heptahydrate,MgSO � 7H O.
4 2
1) Florisil is a trade name for a prepared diatomaceous substance, mainly consisting of anhydrous magnesium silicate. This
information is given for the convenience of users of this part of ISO 9377 and does not constitute an endorsement by ISO of this
product.
2 © ISO 2000 – All rights reserved

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SIST EN ISO 9377-2:2001
ISO 9377-2:2000(E)
6.5 Mineral acid, e.g. hydrochloric acid , c(HCl) = 12 mol/l (� = 1,19 g/ml).
6.6 Acetone,C H O.
3 6
1)
6.7 Florisil ,grain size 150�mto 250�m (60 mesh to 100 mesh), heated to 140 �C for 16 h and stored in a
desiccator.
6.8 Mixture of mineral oils.
2)
6.8.1 Standard mixture.
Weigh accurately equal amounts of two different types (type A and type B, both containing no additives) of mineral
oil and add enough extraction solvent (6.11.2) to give a total hydrocarbon concentration of about 10 mg/ml.
Type A should show discrete peaks in the gas chromatogram. An example is diesel fuel without any additives. See
EN 590 for further information. Type B should have a boiling range higher than that of type A and should have
unresolved signals in the gas chromatogram. An example of this type is a lubricant without any additives, boiling
range 325 �Cto460 �C.
6.8.2 Calibration mixture.
Prepare at least five different calibration solutions by diluting aliquots of standard mixture (6.8.1) with the extraction
solvent (6.11.2). The following concentrations may be suitable:
0 (blank), 0,2 mg/ml, 0,4 mg/ml, 0,6 mg/ml, 0,8 mg/ml and 1,0 mg/ml.
Higher concentrations may be advisable for other applications.
Store the calibration mixture tightly sealed in a refrigerator (4 �Cto 8 �C). The calibration mixtures are stable for up
to six months.
6.8.3 Quality Control (QC) standard.
Prepare a standard solution according to 6.8.1 in acetone (see 6.6) with a mass concentration of e.g. 1 mg/ml. The
exact concentration should be about a thousand times the desired application range.
NOTE When using a lubricant for QC, the stock solution is easily prepared in extracting agent (6.2), which is further diluted
in acetone about tenfold before spiking the QC water.
Store the solution tightly sealed in a refrigerator (4 �Cto8 �C). It is stable for up to six months.
6.9 Standard mixture of n-alkanes for system performance test.
Dissolve n-alkanes with even carbon numbers (C ,C and at least three further n-alkanes) in extracting agent
20 40
(6.2) to give concentrations of approximately 50�g/ml of the individual components. It may be necessary to use a
different solvent, e.g. heptane, for the first solution; in this case dilute this first solution with extracting agent (6.2).
Store the standard mixture tightly sealed in a refrigerator. It is stable for up to six months.
2) Standards are available from
Fachgruppe I.2
Bundesanstalt für Materialforschung und –prüfung
Richard-Willstätter-Strasse 11
D-12489 Berlin, Germany
This information is given for the convenience of users of this part of ISO 9377 and does not constitute an endorsement by ISO
of these products.
© ISO 2000 – All rights reserved 3

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SIST EN ISO 9377-2:2001
ISO 9377-2:2000(E)
NOTE 1 This solution is used to verify the suitability of the gas chromatographic system for the resolution of n-alkanes as
well as for the detector response.
NOTE 2 This solution is used to give information on the retention times of the n-alkanes to characterize the hydrocarbons in
the sample.
6.10 Reference compounds.
6.10.1 n-Decane, C H .
10 22
6.10.2 n-Tetracontane,C H .
40 82
6.10.3 n-Eicosane,C H .
20 42
6.11 Extraction solvent containing reference compounds.
6.11.1 Extraction solvent stock solution.
Dissolve20mgof n-tetracontane (6.10.2) in extracting agent (6.2). Then add 20�lof n-decane (6.10.1) and dilute
with extracting agent to 1 000 ml.
Store the solution tightly sealed in a refrigerator. It is stable for up to six months.
NOTE n-Tetracontane is only moderately soluble in the extracting agent. Slight warming or treatment with ultrasonics
accelerates the dissolution process.
6.11.2 Extraction solvent standard solution.
Immediately prior to use, dilute the stock solution (see 6
...