EN ISO 22892:2011

Soil quality - Guidelines for the identification of target compounds by gas chromatography and mass spectrometry (ISO 22892:2006)

ISO 22892:2006 gives criteria for gas chromatography and mass spectrometry (GC-MS) identification of target compounds in soil samples. ISO 22892:2006 is intended for use with standards developed for the determination of specific compounds. The identification criteria are based on the comparison of retention times followed by interpretation of the electron ionization mass spectra, or if necessary, additional mass spectrometric techniques and other relevant factors.

Bodenbeschaffenheit - Anleitungen für die Identifizierung von Zielverbindungen durch Gaschromatographie und Massenspektrometrie (ISO 22892:2006)

Diese Internationale Norm enthält Kriterien für die GC-MS-Identifizierung von Zielverbindungen in Bodenproben. Diese Internationale Norm kann mit solchen Normen angewendet werden, die für die Bestimmung von spezifischen Verbindungen entwickelt wurden. Die Identifizierungskriterien beruhen auf dem Vergleich der Retentionszeiten und der anschließenden Auswertung der Elektronenstoßmassenspektren oder, sofern erforderlich, zusätzlichen massenspektrometrischen Verfahren sowie weiteren relevanten Faktoren.
ANMERKUNG   Diese Internationale Norm ist auch für andere Umweltproben anwendbar.

Qualité du sol - Lignes directrices pour l'identification de composés cibles par chromatographie en phase gazeuse et spectrométrie de masse (ISO 22892:2006)

L'ISO 22892:2006 donne des critères pour l'identification par chromatographie en phase gazeuse et spectrométrie de masse (CG-SM) de composés cibles dans des échantillons de sol. Elle est destinée à être utilisée avec des normes élaborées pour permettre le dosage de composés spécifiques. Les critères d'identification sont fondés sur la comparaison des temps de rétention, puis sur l'interprétation des spectres de masse d'ionisation électronique ou, au besoin, sur des techniques de spectrométrie de masse supplémentaires et d'autres facteurs pertinents.

Kakovost tal - Smernice za identifikacijo ciljnih spojin s plinsko kromatografijo in masno spektrometrijo (ISO 22892:2006)

ISO 22892:2006 podaja kriterije za identifikacijo ciljnih spojin v vzorcih tal s plinsko kromatografijo in masno spektrometrijo (GC-MS). ISO 22892:2006 je namenjen uporabi s standardi, razvitimi za določevanje specifičnih spojin. Identifikacijski kriteriji temeljijo na primerjavi retencijskih časov, sledi interpretacija elektronskih ionizacijskih masnih spektrov ali po potrebi dodatne masne spektrometrične tehnike in drugi ustrezni dejavniki.

General Information

• Status: Published
• Publication Date: 28-Jun-2011
• Withdrawal Date: 30-Dec-2011
• ICS: 13.080.05 - Examination of soils in general
• Technical Committee: CEN/TC 444 - Environmental characterization
• Drafting Committee: CEN/TC 444/WG 2 - Organic analysis
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 29-Jun-2011
• Due Date: 03-Jun-2012
• Completion Date: 29-Jun-2011
• Ref Project: SIST EN ISO 22892:2011 - Soil quality - Guidelines for the identification of target compounds by gas chromatography and mass spectrometry (ISO 22892:2006)

Overview

EN ISO 22892:2011 (ISO 22892:2006) provides guidelines for identifying target compounds in soil by gas chromatography–mass spectrometry (GC‑MS). It sets out objective identification criteria based on relative retention times and electron ionization mass spectra, and describes when to apply additional mass spectrometric techniques or supporting information. The standard is intended to be used together with specific analytical methods for particular target compounds and is applicable to other environmental matrices as well.

Key topics and technical requirements

• Identification principle: Compare relative retention time to a retention time standard, then interpret MS spectra (full scan and/or selected ion monitoring, SIM). The outcome classification is identified, indicated, or absent.
• Retention time: Use a retention time standard or internal standard to calculate relative retention time (ratio of target RT to retention time standard). Relative RT values should be < 2.
• Diagnostic ions: Where possible select three diagnostic ions per target compound and measure their relative intensities in calibration standards. If three are not available (e.g., PAHs), use the available ions.
• Ion selection guidance:
  • Prefer high m/z values and even mass fragments.
  • Include the molecular ion when possible.
  • Diagnostic ion intensity preferably > 15% of base peak.
  • Use isotopic clusters (e.g., chlorine-containing compounds) for increased specificity.
  • Avoid common column artefact masses (e.g., m/z 73, 207, 281).
• Instrument minima:
  • Ionization mode: Electron ionization (commonly 70 eV).
  • Mass range: from m/z 35 to (highest target mass + 10 u) in full scan.
  • Scan rate: ≈10× peak frequency, minimum 7 scans/peak.
  • Mass resolution: tuned to nominal (peak width at half-height ≤ 0.7 u).
• Sensitivity and detection: Lowest concentration for identification depends on instrument/method; the least-intense diagnostic ion must have signal‑to‑noise > 3:1.
• Qualification & reporting: Includes requirements for method qualification and standardized reporting of identification results.

Applications and users

EN ISO 22892 is practical for:

• Environmental and soil testing laboratories performing GC‑MS analysis of pesticides, PAHs, PCBs, organics, and other target analytes in soil.
• Regulatory agencies and consultants needing robust, reproducible identification criteria for compliance monitoring.
• Method developers and instrument vendors who design or validate GC‑MS protocols for environmental matrices.
• Research groups working on contaminant fate, remediation monitoring, and forensic soil analysis.

Keywords: soil quality, GC‑MS identification, gas chromatography mass spectrometry, diagnostic ions, retention time, electron ionization, environmental analysis, target compounds.

Related standards

• ISO/IEC 17025 (laboratory quality and competence) - referenced for quality assurance.
• Specific analytical standards for individual target compounds (used in conjunction with ISO 22892).

Standards Content (Sample)

SLOVENSKI STANDARD
01-november-2011
Kakovost tal - Smernice za identifikacijo ciljnih spojin s plinsko kromatografijo in
masno spektrometrijo (ISO 22892:2006)
Soil quality - Guidelines for the identification of target compounds by gas
chromatography and mass spectrometry (ISO 22892:2006)
Bodenbeschaffenheit - Anleitungen für die Identifizierung von Zielverbindungen durch
Gaschromatographie und Massenspektrometrie (ISO 22892:2006)
Qualité du sol - Lignes directrices pour l'identification de composés cibles par
chromatographie en phase gazeuse et spectrométrie de masse (ISO 22892:2006)
Ta slovenski standard je istoveten z: EN ISO 22892:2011
ICS:
13.080.05 Preiskava tal na splošno Examination of soils in
general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 22892
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2011
ICS 13.080.05
English Version
Soil quality - Guidelines for the identification of target
compounds by gas chromatography and mass spectrometry
(ISO 22892:2006)
Qualité du sol - Lignes directrices pour l'identification de Bodenbeschaffenheit - Anleitungen für die Identifizierung
composés cibles par chromatographie en phase gazeuse von Zielverbindungen durch Gaschromatographie und
et spectrométrie de masse (ISO 22892:2006) Massenspektrometrie (ISO 22892:2006)
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 22892:2011: E
worldwide for CEN national Members.

Contents Page
Foreword .3

Foreword
The text of ISO 22892:2006 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 22892:2011 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 22892:2006 has been approved by CEN as a EN ISO 22892:2011 without any modification.

INTERNATIONAL ISO
STANDARD 22892
First edition
2006-02-01
Soil quality — Guidelines for the
identification of target compounds by gas
chromatography and mass spectrometry
Qualité du sol — Lignes directrices pour l'identification des composés
cibles par chromatographie en phase gazeuse et spectrométrie de
masse
Reference number
ISO 22892:2006(E)
©
ISO 2006
ISO 22892:2006(E)
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ii © ISO 2006 – All rights reserved

ISO 22892:2006(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope . 1
2 Principle. 1
3 Terms and definitions. 1
4 Apparatus . 2
5 Procedure . 3
5.1 Retention times . 3
5.2 Mass spectra, selection of diagnostic ions . 3
6 Qualification . 4
6.1 GC-MS procedure . 4
6.2 Additional information. 5
6.3 Reporting the presence of target compounds. 7
6.3.1 Identification. 7
6.3.2 Indication . 8
6.3.3 Absence of the target compound (< detection limit). 8
7 Test report . 8
Annex A (informative) Diagnostic ions to be used for identification using GC-MS . 9
Annex B (informative) Examples . 12
Annex C (informative) Examples of Spectra. 18
Bibliography . 20

ISO 22892:2006(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 22892 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
methods and soil characteristics.
iv © ISO 2006 – All rights reserved

ISO 22892:2006(E)
Introduction
In many analytical standards, use is made of gas chromatography (GC) in combination with mass
spectrometric (MS) detection. This detector is a powerful tool provided it is properly used. In this International
Standard, guidelines are given for the identification of target compounds. This International Standard can be
used in combination with specific analytical standards or in combination with any GC-MS procedure. The
result of the procedure described is: identified, indicated or absent.

INTERNATIONAL STANDARD ISO 22892:2006(E)

Soil quality — Guidelines for the identification of target
compounds by gas chromatography and mass spectrometry
1 Scope
This International Standard gives criteria for gas chromatography and mass spectrometry (GC-MS)
identification of target compounds in soil samples. This International Standard is intended for use with
standards developed for the determination of specific compounds. The identification criteria are based on the
comparison of retention times followed by interpretation of the electron ionization mass spectra, or if
necessary, additional mass spectrometric techniques and other relevant factors.
NOTE This International Standard is also applicable for other environmental samples.
2 Principle
A target compound is identified if the measured values meet the criteria specified in this International Standard
or in the standard in which the procedures are described to analyse the target compound. Criteria are based
on the relative retention times and the intensity of diagnostics ions selected in the scan mode and measured
in the selected ion mode (SIM), and other relevant factors. Additional information regarding diagnostic ions
from specific international standards on the analysis of the target compound can be used. The principle of
identification points is used.
3 Terms and definitions
For the purpose of this document, the following terms and definitions apply.
3.1
target compound
selected component, the presence or absence of which is being established
NOTE This definition also applies to derivatives of the original compound which are formed during an intentional
derivatization procedure or on-line derivatization.
3.2
standard compound
target compound with the highest possible purity, which can be used as a reference during the analysis
NOTE Any impurities should not have any influence on the mass spectrum of the standard compound.
3.3
retention time standard
compound that is added to the sample (or to the sample extract) and to the calibration standard solution, and
used to calculate the relative retention times of the target compounds
NOTE The retention time standard may be identical to the internal standard(s).
ISO 22892:2006(E)
3.4
relative retention time
ratio between the retention time of the target compound and the retention time of the retention time standard
3.5
lowest concentration for identification
lowest concentration of the target compound, which, if present in the sample, can be identified using the
identification criteria in this International Standard
NOTE 1 It requires that the selected diagnostic ion with the lowest intensity is still present in the mass spectrum with a
signal to noise ratio (S/N) higher than 3:1.
NOTE 2 This concentration is very dependent on the sensitivity of the instrument and on the performance
characteristics of the analytical method.
3.6
diagnostic ion
selected fragment ion, molecular ion or other characteristic ion from the mass spectrum of the target
compound with the highest possible specificity
3.7
identification point
result of mass spectrometric investigation or other investigations/information to identify a component in
environmental matrices
3.8
selected ion mode
SIM
measuring the intensity of selected diagnostic ions only
4 Apparatus
As this International Standard is complementary to other standards using GC-MS, it is assumed that the
instrumentation used meets the requirements of those standards and a detailed description is not within the
scope of this International Standard. Suitable quality assurance requirements are set out in ISO/IEC 17025.
Minimum requirements are:
Ionization mode: Electron ionization.
Electron energy: Depending on the application (usually 70 eV).
Mass range: Peaks (masses) with a S/N < 3 are not taken into consideration and the scan range is
limited to 35 (to avoid the measurement of oxygen and nitrogen) to the highest mass of
the target compound + 10 unified atomic mass units (u) in full scan measurements.
Scan rate: The scan rate should be 10 times the peak frequency with a minimum of 7 scans per
peak.
Scan mode: Cyclic, linear.
Full scan or selected ion monitoring.
Mass resolution: To be tuned on nominal resolution, the peak width at half-height of every tune mass
should not exceed 0,7 u.
2 © ISO 2006 – All rights reserved

ISO 22892:2006(E)
5 Procedure
5.1 Retention times
The relative retention time of the target compound shall be determined using a calibration standard solution
containing an appropriate number of internal standards. The use of internal standards is often prescribed in
the specific standard describing the determination of the target compound. The relative retention times
are calculated using the retention time standard(s). The calculated relative retention time shall have a value
below 2.
5.2 Mass spectra, selection of diagnostic ions
If available, three diagnostic ions shall be selected for each target compound. Their intensities I , I , I shall
1 2 3
be determined in the calibration standard solution (at least three injections) as the peak area or peak height of
the corresponding extracted ion current chromatograms. The relative intensities are calculated as the ratio of
the determined peak heights (or areas) and the peak height (or area) of the most intensive diagnostic ion.
Annex A gives a table of suitable diagnostic ions for a range of substances. Diagnostic ions may also be
specified in the standard method being used.
It is not always possible to obtain three diagnostic ions (for instance, polycyclic aromatic hydrocarbons). In
that case, select the available ions.
[3]
Diagnostic ions should have a high "uniqueness value" . It is suggested that:
⎯ high m/z values should be preferred due to their higher significance;
⎯ even mass fragments are preferred over odd ones;
⎯ if possible, the molecular ion should be selected as one of the diagnostic ions;
⎯ the intensity of diagnostic ions is preferably higher than 15 % in relation to the base peak in the spectrum;
⎯ if characteristic isotope clusters are present in the mass spectrum (e.g. chlorine), two diagnostic ions
should be selected from one isotope cluster. Isotopes can be very characteristic for complex compounds,
i.e. organotin;
⎯ if during the sample preparation, the target compounds have been derivatized with a reagent with low
+ + +
specificity, only one of the ions M and [M-der] should be selected as a diagnostic ion (M is the
molecular ion of the derivatized target compound);
⎯ in the selection of the diagnostic ions, possible column artefacts have to be taken into consideration,
avoiding corresponding masses (e.g. m/z 73, 207, 281);
The peak shape and retention time of all measured diagnostic ions shall be identical. Co-eluting substances
may influence the peak shape. As long as the peak of interest can be separately integrated, it may be used.
Criteria for the retention time are the peak maxima of the extracted ion current chromatograms.
Diagnostic ions are supposed to originate from the analyte under investigation only. This implies that
theoretically all diagnostic ions belonging to one and the same analyte have the same retention time. If the
retention time of one selected diagnostic ion differs from the retention times of the other diagnostic ions from
the same analyte, a co-eluting substance or a partly-separated substance giving the same mass may be
present. In this case, the particular diagnostic ion cannot be used.
The accuracy of the retention time depends on the number of scans within the chromatographic peak and
hence, on the scan rate. Because the scan rate is limited, small differences in the retention times of the
diagnostic ions should be allowed.
ISO 22892:2006(E)
A suitable criterion for the allowed difference in retention times of all diagnostic ions of an analyte shall not be
greater than 20 % of the peak width at half the peak height. Therefore, the differences in retention times of the
peak maxima of all the selected diagnostic ions in the extracted ion current chromatograms belonging to the
same analyte shall not be greater than 20 % of the peak width at half the peak height. For most analyses, this
means an acceptable difference of 1 s. These criteria apply for both the calibration standard solution and the
sample.
NOTE 1 MTBE and TAME have m/z 73 as diagnostic ion.
NOTE 2 Due to overloading, the ratios of the diagnostic ions can change.
6 Qualification
6.1 GC-MS procedure
The procedure to qualify a component consists of three steps (see the flow scheme in Figure 1).
⎯ Step 1: Gas-chromatographic result
The relative retention time shall fulfil the specified criteria (see 6.3, Step 1). Only if Step 1 is positive, can
Step 2 be made.
⎯ Step 2: Gathering identification points using analytical procedures
[1]
For qualification, the principle of identification points is used . Identification points can be obtained from
mass spectrometric data, but also using other analytical information.
⎯ Step 3: Gathering additional identification points using knowledge and interpretation of this knowledge
about the sample or sampling site.
Then the following classification can be obtained.
a) Identification (see 6.3.1)
The target compound is present in the analysed extract. At least three identification points are obtained.
b) Indication (see 6.3.2)
The target compound may be present. One or two identification points are obtained.
c) Absence (below the detection limit) (see 6.3.3)
No identification points are obtained using mass spectrometry.
First, the mass spectrometric results are evaluated. For every ion peak meeting the criteria given in 6.3,
Step 2, an identification point is obtained. Three identification points give a positive identification. If less then
three ion peaks are available [due to sensitivity (S/N < 3) or absence of fragments (PAH)], additional
identification points shall be gathered using additional evidence. Possibilities are given in Table 1 and also
explained in Annex B.
4 © ISO 2006 – All rights reserved

ISO 22892:2006(E)
Table 1 — Examples of number of identification points, provided criteria are met
Source Identification Remark
points
n
Diagnostic ion 1 Every ion S/N > 3
Absence of any other ions in full scan 1 Diagnostic ions in full scan S/N > 3
a
Column with other polarity 1 GC-criterion (extra retention time value)
Isotope dilution 1
Component spike/standard addition 1
Chromatographic pattern 1 i.e. PCB, PAH, dioxins
Other analytical techniques 1 Every other selective detector (i.e. ECD) or
technique (i.e. LC)
GC-MS
...