SIST EN ISO 16703:2011
(Main)Soil quality - Determination of content of hydrocarbon in the range C10 to C40 by gas chromatography (ISO 16703:2004)
Soil quality - Determination of content of hydrocarbon in the range C10 to C40 by gas chromatography (ISO 16703:2004)
This International Standard specifies a method for the quantitative determination of the mineral oil (hydrocarbon) content in field-moist soil samples by gas chromatography.
The method is applicable to mineral oil contents (mass fraction) between 100 mg/kg and 10 000 mg/kg soil, expressed as dry matter, and can be adapted to lower limits of detection.
This International Standard is applicable to the determination of all hydrocarbons with a boiling range of 175 °C to 525 °C, of n-alkanes from C10H22 to C40H82, of isoalkanes, cycloalkanes, alkylbenzenes, alkylnaphthalenes and polycyclic aromatic compounds, provided that they are not absorbed on the specified column during the clean-up procedure.
This International Standard is not applicable to the quantitative determination of hydrocarbons < C10 originating from gasolines.
On the basis of the peak pattern of the gas chromatogram obtained, and of the boiling points of the individual n-alkanes listed in Annex B, the approximate boiling range of the mineral oil and some qualitative information on the composition of the contamination can be obtained.
Bodenbeschaffenheit - Gaschromatographische Bestimmung des Gehalts an Kohlenwasserstoffen von C10 bis C40 (ISO 16703:2004)
Diese Internationale Norm legt ein Verfahren zur gaschromatographischen quantitativen Bestimmung des Mineralöl-(Kohlenwasserstoff-)gehalts in originalfeuchten Bodenproben fest.
Das Verfahren ist auf Mineralölgehalte zwischen 100 mg/kg und 10 000 mg/kg Boden, bezogen auf die Trockenmasse, anwendbar und kann für niedrigere Nachweisgrenzen angepasst werden.
Mit diesem Verfahren werden alle Kohlenwasserstoffe mit einem Siedebereich von 175 °C bis 525 °C, n Alkane zwischen C10H22 bis C40H82, Isoalkane, Cycloalkane, Alkylbenzole, Alkylnaphthaline und polycyc-lische aromatische Verbindungen als Kohlenwasserstoffe bestimmt, vorausgesetzt, sie werden während der Reinigung nicht an der Florisilsäule adsorbiert.
Diese Internationale Norm ist für die quantitative Bestimmung von Kohlenwasserstoffen C10 nicht anwendbar.
Auf der Grundlage der Peakfolge des Gaschromatogramms und der Siedepunkte der einzelnen im Anhang B angeführten n-Alkane können der näherungsweise Siedebereich der Kohlenwasserstoffe und einige qualitative Hinweise zur Zusammensetzung der Kontamination erhalten werden.
Qualité du sol - Dosage des hydrocarbures de C10 à C40 par chromatographie en phase gazeuse (ISO 16703:2004)
L'ISO 16703:2004 spécifie une méthode de dosage quantitatif par chromatographie en phase gazeuse des huiles minérales (hydrocarbures) contenues dans des échantillons de sol bruts.
La méthode est applicable à des teneurs en huiles minérales (fraction massique) comprises entre 100 mg/kg et 10 000 mg/kg de sol, exprimées sous forme de matière sèche, et peut être adaptée à des limites inférieures de détection.
L'ISO 16703:2004 est applicable au dosage de tous les hydrocarbures ayant un domaine d'ébullition compris entre 175 °C et 525 °C, des n-alcanes entre C10H22 et C40H82, des isoalcanes, des cycloalcanes, des alkylbenzènes, des alkylnaphtalènes et des composés aromatiques polycycliques, à condition qu'ils ne soient pas absorbés sur la colonne spécifiée pendant l'étape de purification.
L'ISO 16703:2004 n'est pas applicable au dosage quantitatif des hydrocarbures < C10 provenant des essences.
Compte tenu de la forme des pics du chromatogramme en phase gazeuse obtenu et du point d'ébullition des différents n-alcanes indiqués à l'Annexe B, il est possible de déterminer le domaine d'ébullition approximatif des huiles minérales et d'obtenir quelques informations qualitatives sur la composition des polluants.
Kakovost tal - Določevanje ogljikovodikov v območju C10 do C40 s plinsko kromatografijo (ISO 16703:2004)
Ta mednarodni standard opredeljuje metodo za količinsko določevanje mineralnih olj (ogljikovodikov) v vzorcih vlažnih poljskih tal.
Metoda velja za vsebnost (masni delež) mineralnih olj med 100 mg/kg in 10.000 mg/kg tal, izraženo kot suha snov, in se lahko prilagodi za nižje meje detekcije.
Ta mednarodni standard velja za določevanje vseh ogljikovodikov z razponom vrelišča med 175 °C in 525 °C, n-alkanov od C10H22 do C40H82, izoalkanov, cikloalkanov, alkilbenzenov, alkilnaftalenov in policikličnih aromatskih spojin, če se med postopkom čiščenja ne absorbirajo na določeno kolono.
Ta mednarodni standard ne velja za količinsko določevanje ogljikovodikov < C10, ki izhajajo iz bencina.
Na osnovi vzorca vrhov na dobljenem plinskem kromatogramu in vrelišča posameznih n-alkanov, navedenih v dodatku B, se lahko pridobi približen razpon vrelišča mineralnega olja in nekatere kvalitativne informacije o sestavi onesnaženja.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 16703:2011
01-november-2011
.DNRYRVWWDO'RORþHYDQMHRJOMLNRYRGLNRYYREPRþMX&GR&VSOLQVNR
NURPDWRJUDILMR ,62
Soil quality - Determination of content of hydrocarbon in the range C10 to C40 by gas
chromatography (ISO 16703:2004)
Bodenbeschaffenheit - Gaschromatographische Bestimmung des Gehalts an
Kohlenwasserstoffen von C10 bis C40 (ISO 16703:2004)
Qualité du sol - Dosage des hydrocarbures de C10 à C40 par chromatographie en phase
gazeuse (ISO 16703:2004)
Ta slovenski standard je istoveten z: EN ISO 16703:2011
ICS:
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
SIST EN ISO 16703:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 16703:2011
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SIST EN ISO 16703:2011
EUROPEAN STANDARD
EN ISO 16703
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2011
ICS 13.080.10
English Version
Soil quality - Determination of content of hydrocarbon in the
range C to C by gas chromatography (ISO 16703:2004)
10 40
Qualité du sol - Dosage des hydrocarbures de C à C Bodenbeschaffenheit - Gaschromatographische
10 40
par chromatographie en phase gazeuse (ISO 16703:2004) Bestimmung des Gehalts an Kohlenwasserstoffen von C
10
bis C (ISO 16703:2004)
40
This European Standard was approved by CEN on 10 June 2011.
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 CEN-CENELEC 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 CEN-CENELEC Management Centre has the same
status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2011 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 16703:2011: E
worldwide for CEN national Members.
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SIST EN ISO 16703:2011
EN ISO 16703:2011 (E)
Contents Page
Foreword .3
2
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SIST EN ISO 16703:2011
EN ISO 16703:2011 (E)
Foreword
The text of ISO 16703:2004 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the
International Organization for Standardization (ISO) and has been taken over as EN ISO 16703:2011 by
Technical Committee CEN/TC 345 “Characterization of soils” the secretariat of which is held by NEN.
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 December 2011, and conflicting national standards shall be withdrawn
at the latest by December 2011.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 16703:2004 has been approved by CEN as a EN ISO 16703:2011 without any modification.
3
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SIST EN ISO 16703:2011
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SIST EN ISO 16703:2011
INTERNATIONAL ISO
STANDARD 16703
First edition
2004-11-01
Soil quality — Determination of content
of hydrocarbon in the range C to C by
10 40
gas chromatography
Qualité du sol — Dosage des hydrocarbures de C à C par
10 40
chromatographie en phase gazeuse
Reference number
ISO 16703:2004(E)
©
ISO 2004
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SIST EN ISO 16703:2011
ISO 16703:2004(E)
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ii © ISO 2004 – All rights reserved
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SIST EN ISO 16703:2011
ISO 16703:2004(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 Terms and definitions. 2
4 Interferences. 2
5 Principle . 2
6 Reagents . 2
6.7 Hydrocarbon standard solution for calibration . 3
6.8 Control solution . 3
6.9 System-performance standard solution. 3
7 Apparatus . 3
8 Sampling, sample conservation and pretreatment . 4
9 Procedure . 5
9.1 Preparation of the clean-up column. 5
9.2 Blank. 5
9.3 Extraction and clean-up . 5
9.4 Determination by gas chromatography. 5
9.5 Quality control. 7
10 Precision . 8
11 Test report . 8
Annex A (informative) Examples of gas chromatograms of mineral oil hydrocarbon standard and
soil samples. 10
Annex B (informative) Determination of the boiling range of mineral oil hydrocarbons from the
gas chromatogram. 16
Annex C (informative) Precision data. 17
Bibliography . 18
© ISO 2004 – All rights reserved iii
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SIST EN ISO 16703:2011
ISO 16703:2004(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 16703 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
methods and soil characteristics.
iv © ISO 2004 – All rights reserved
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SIST EN ISO 16703:2011
INTERNATIONAL STANDARD ISO 16703:2004(E)
Soil quality — Determination of content of hydrocarbon in the
range C to C by gas chromatography
10 40
1 Scope
This International Standard specifies a method for the quantitative determination of the mineral oil
(hydrocarbon) content in field-moist soil samples by gas chromatography.
The method is applicable to mineral oil contents (mass fraction) between 100 mg/kg and 10 000 mg/kg soil,
expressed as dry matter, and can be adapted to lower limits of detection.
This International Standard is applicable to the determination of all hydrocarbons with a boiling range of
175 °C to 525 °C, of n-alkanes from C H to C H , of isoalkanes, cycloalkanes, alkylbenzenes,
10 22 40 82
alkylnaphthalenes and polycyclic aromatic compounds, provided that they are not absorbed on the specified
column during the clean-up procedure.
This International Standard is not applicable to the quantitative determination of hydrocarbons < C
10
originating from gasolines.
On the basis of the peak pattern of the gas chromatogram obtained, and of the boiling points of the individual
n-alkanes listed in Annex B, the approximate boiling range of the mineral oil and some qualitative information
on the composition of the contamination can be obtained.
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 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
ISO 10381-1, Soil quality — Sampling — Part 1: Guidance on the design of sampling programmes
ISO 11465:1993, Soil quality — Determination of dry matter and water content on a mass basis — Gravimetric
method
ISO 14507, Soil quality — Pretreatment of samples for determination of organic contaminants
© ISO 2004 – All rights reserved 1
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SIST EN ISO 16703:2011
ISO 16703:2004(E)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
hydrocarbon content
〈by gas chromatography〉 sum of compounds extractable with acetone/n-heptane (2+1) that do not adsorb on
1)
a Florisil column and can be chromatographed on a non-polar capillary column with retention times between
those of n-decane (C H ) and n-tetracontane (C H ).
10 22 40 82
NOTE Substances that comply with this definition are mainly long-chain or branched aliphatic, alicyclic, lower
polycyclic- or alkyl-substituted aromatic hydrocarbons.
4 Interferences
Non-polar and weakly polar compounds (e.g. halogenated hydrocarbons) and high contents of polar
compounds may interfere with the determination.
5 Principle
A known amount of the homogenized soil sample is extracted by mechanical shaking or sonication with
acetone/n-heptane. The organic layer is separated and washed twice with water. Polar compounds are
removed by adsorption on Florisil. An aliquot of the purified extract is analysed by capillary gas
chromatography with flame ionization detection. The total peak area in the range delimited by the standards
n-decane and n-tetracontane is measured, and the amount of hydrocarbons in the sample is quantified
against an external standard consisting of equal amounts of two different types of mineral oil.
Instead of heptane, another non-polar solvent (e.g. petroleum ether, cyclohexane, n-hexane) may be used,
however its suitability for the extraction of hydrocarbons from soil shall be proven.
NOTE If lower detection limits are required, petroleum ether can be used as extraction solvent in combination with
large-volume injection or concentration of the final extract.
6 Reagents
In general, all reagents shall be reagent grade and suitable for their specific purposes.
6.1 Acetone, (CH ) CO.
3 2
6.2 n-Heptane, C H .
7 16
1)
6.3 Florisil for preparation of clean-up column, particle size 150 µm to 250 µm (60 mesh to 100 mesh),
heated for at least 16 h at 140 °C and stored in a desiccator over a molecular sieve.
NOTE Commercially available cartridges containing 2 g of Florisil and 2 g of sodium sulfate are also applicable.
6.4 Anhydrous sodium sulfate (Na SO ), heated for at least 2 h at 550 °C.
2 4
6.5 Test solution of stearyl stearate (C H O ).
36 72 2
1) Florisil is a trade name for a prepared diatomaceous substance, mainly consisting of anhydrous magnesium silicate.
Florisil an example of a suitable product available commercially. This information is given for the convenience of users of
this International Standard and does not constitute an endorsement by ISO of this product.
2 © ISO 2004 – All rights reserved
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SIST EN ISO 16703:2011
ISO 16703:2004(E)
Dissolve about 100 mg of n-octadecanoic acid octadecyl ester in 100 ml n-heptane (6.2).
6.6 Retention-time window (RTW) standard solution, containing n-tetracontane and n-decane.
Retention-time window (RTW) standard solution is the range-defining standard solution. Weigh (30 ± 1) mg of
n-tetracontane into a 1 l volumetric flask, dissolve completely in an appropriate volume of n-heptane (6.2), add
30 µl of n-decane (about 21 mg), mix well, fill up to volume with n-heptane and homogenize. This solution shall
be used for all dilution steps of the hydrocarbon standard (6.7).
Store at room temperature.
NOTE n-Tetracontane is only moderately soluble in n-heptane. Slight warming and/or sonication accelerates the
dissolution process.
2)
6.7 Hydrocarbon standard solution for calibration
Mix approximately equal masses of two different types of mineral oil. Weigh accurately this mixture and
dissolve in the RTW standard solution (6.6) to give a hydrocarbon mass concentration of about 8 g/l.
The first oil type should show discrete peaks (e.g. a diesel fuel) in the gas chromatogram, as can be seen in
Figure A.1 (left part of the chromatogram). The second type should have a boiling range higher than the first one,
and should show a hump in the gas chromatogram, as can be seen in Figure A.1 (right part of the
chromatogram). A suitable oil of this type is for example a lubricating oil without any additives.
The calibration solutions can be prepared by diluting an aliquot of this standard solution (6.8) with different
volumes of the RTW standard solution (6.6).
6.8 Control solution
Prepare an independent control solution in accordance with (6.7) using a hydrocarbon concentration about in
the middle of the working range of the system-performance standard solution (6.9).
6.9 System-performance standard solution
Prepare a mixture of equal amounts, on a mass basis, of the n-alkanes having even carbon numbers from C
10
to C , dissolved in n-heptane (6.2), to give mass concentrations of about 50 mg/l of each n-alkane. Store at
40
room temperature.
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 provide information on the retention times of the n-alkanes, in order to characterise the
hydrocarbons in the samples.
7 Apparatus
7.1 Standard laboratory glassware, which shall be treated at high temperatures or rinsed with acetone
(6.1) and dried before use.
2) General purpose hydrocarbon standards for calibration are available commercially. Calibration standards specific to
this International Standard can be purchased from Bundesanstalt für Materialforschung und -prüfung, Fachgruppe I.2,
Richard-Willstätter-Strasse 11 D-12489 Berlin, Germany. This information is given for the convenience of users of this
International Standard and does not constitute an endorsement by ISO of this product.
© ISO 2004 – All rights reserved 3
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SIST EN ISO 16703:2011
ISO 16703:2004(E)
7.2 Mixing device.
A mechanical shaker with at least 120 horizontal shaking movements per minute, or alternatively an ultrasonic
bath, can be us
...
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