CEN/TC 444/WG 2 - Organic analysis

This document specifies a method for quantitative determination of the concentration of selected alcohols with low boiling point in liquid waste and pasty waste by gas chromatography with flame ionization detection after static headspace extraction.
Under the conditions specified in this document, a limit of application of 20 mg/kg, expressed on dry matter for pasty waste and expressed on raw waste for liquid waste, can be achieved.

This document specifies different methods for quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) (see Table 2) in soil, sludge, treated biowaste, and waste, using GC-MS or HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels (see Table 2).
NOTE   The method can be applied to sediments provided that validity is demonstrated by the user.
When using fluorescence detection, acenaphthylene cannot be measured.
[Table 2 -Target analytes of this document]
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this document, the lower limit of application from 10 μg/kg (expressed as dry matter) for soils, sludge and biowaste to 100 μg/kg (expressed as dry matter) for solid waste can be achieved. For some specific samples (e.g. bitumen) the limit of 100 μg/kg cannot be reached.
Sludge, waste and treated biowaste can differ in properties as well as in the expected contamination levels of PAH and presence of interfering substances. These differences make it impossible to describe one general procedure. This document contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used.
The method can be applied to the analysis of other PAH not specified in the scope, provided suitability is proven by proper in-house validation experiments.
Sampling is not part of this standard. In dependence of the materials, the following standards need to be considered, e.g. EN 14899, ISO 5667-12 and EN ISO 5667-13.

This document specifies the measurement of explosives and related nitrocompounds (as given in Table 1) in soil and soil materials. This document is intended for the trace analysis of explosives and related compounds by liquid chromatography–tandem mass spectrometry (LC-MS/MS). Generally, LC-MS/MS measurement shows the lower LOQ (limit of quantification) for each compound in Table 1 than using high-performance liquid chromatography (HPLC) with UV-detection (see Annex B and Annex C).
Under the conditions specified in this document, concentrations as low as 0,005 mg/kg to 0,014 mg/kg-dry matter can be determined, depending on the substance. Similar compounds, in particular various nitroaromatics, by-products and degradation products of explosive compounds can be analysed using this method provided that the applicability is checked on a case-by-case basis.

This document specifies methods for quantitative determination of seven selected polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in soil, sludge, sediment, treated biowaste, and waste using GC-MS and GC-ECD (see Table 2).
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this document, lower limit of application from 1 μg/kg (expressed as dry matter) for soils, sludge and biowaste to 10 μg/kg (expressed as dry matter) for solid waste can be achieved. For some specific samples the limit of 10 μg/kg cannot be reached.
Sludge, waste and treated biowaste may differ in properties, as well as in the expected contamination levels of PCB and presence of interfering substances. These differences make it impossible to describe one general procedure. This document contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used.
NOTE   The analysis of PCB in insulating liquids, petroleum products, used oils and aqueous samples is referred to in EN 61619, EN 12766-1 and EN ISO 6468 respectively.
The method can be applied to the analysis of other PCB congeners not specified in the scope, provided suitability is proven by proper in-house validation experiments.

2020-02-13 - waiting TC decision to skip FV.

This draft European Standard specifies a method for quantitative determination of 17 2,3,7,8-chlorine substituted dibenzo-p-dioxins and dibenzofurans and dioxin-like polychlorinated biphenyls in sludge, treated biowaste and soil using liquid column chromatographic clean-up methods and GC/HRMS.
The analytes to be determined with this European Standard are listed in Table 1.
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The limit of detection depends on the kind of sample, the congener, the equipment used and the quality of chemicals used for extraction and clean-up. Under the conditions specified in this European Standard, limits of detection better than 1 ng/kg (expressed as dry matter) can be achieved.
This method is "performance based". It is allowed to modify the method if all performance criteria given in this method are met.
NOTE   In principle this method can also be applied for sediments, mineral wastes and for vegetation. It is the responsibility of the user of this European Standard to validate the application for these matrices. For measurement in complex matrices like fly ashes adsorbed on vegetation it can be necessary to further improve the clean-up. This can also apply to sediments and mineral wastes.

This document specifies a gas-chromatographic method for the identification and quantification of organotin compounds (OTCs) in soils as specified in Table 1.
This document is also applicable to samples from sediments, sludges and wastes (soil-like materials).
The working range depends on the detection technique used and the amount of sample taken for analysis.
The limit of quantification for each compound is about 10 µg/kg.

ISO 16558-1:2015 specifies a method for the quantitative determination of the total extractable volatile, the volatile aliphatic, and aromatic fractions of petroleum hydrocarbon content in field moist soil samples by gas chromatography with mass spectrometric detection. The aromatic fractions are determined by the sum of individual aromatic compounds.
The sum of the volatile aliphatic (C5 to C10) and aromatic (C6 to C10) fractions can be referred to as "volatile oil".
The results of the test carried out can be used for risk assessment studies related to contaminations with petroleum hydrocarbons.
ISO 16558-1:2015 provides a method applicable to petroleum hydrocarbon contents from about 5 mg/kg soil expressed as dry matter for the whole aliphatic fraction C5 to C10 and about 5 mg/kg soil expressed as dry matter for the aromatic fraction in the boiling range of C6 to C10.
With this method, all hydrocarbons with a boiling range of 36 °C to 184 °C, n-alkanes between C5H12 to C10H22, isoalkanes, cycloalkanes, BTEX, and di- and tri-alkyl benzenes compounds are determined as total volatile petroleum hydrocarbons C5 to C10. In addition, volatile aliphatic and aromatic fractions are specified.
For the determination of semi-volatile aliphatic and aromatic fractions of petroleum hydrocarbons in soil samples, see ISO/TS 16558-2.
NOTE          The sub-fractions proposed in this part of ISO 16558 have shown to be suitable for risk assessment studies. However, other sub-fractions between C5H12 to C10H22 can be determined in conformity with this part of ISO 16558.
On the basis of the peak pattern of the gas chromatogram and of the boiling points of the individual n-alkanes listed in Annex A, the approximate boiling range of the mineral oil and some qualitative information on the composition of the contamination can be achieved.

ISO 15009:2016 specifies a method for quantitative gas-chromatographic determination of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons in soil.
This International Standard is applicable to all types of soil.
NOTE          In the case of unsaturated peaty soils, absorption of the extraction solution may occur.
The lower limit of quantification is dependent on the equipment used and the quality of the methanol grade used for the extraction of the soil sample.
Under the conditions specified in this International Standard the following limits of quantification apply (expressed on basis of dry matter):
Typical limit of quantification when using GC-FID:
-      Volatile aromatic hydrocarbons: 0,1 mg/kg
Typical limit of quantification when using GC-ECD:
-      Volatile halogenated hydrocarbons: 0,01 mg/kg
Lower limits of quantification for some compounds can be achieved by using mass spectrometry (MS) with selected ion detection.

ISO 22155:2016 specifies a static headspace method for quantitative gas chromatographic determination of volatile aromatic and halogenated hydrocarbons and selected aliphatic ethers in soil.
ISO 22155:2016 is applicable to all types of soil.
The limit of quantification is dependent on the detection system used and the quality of the methanol grade used for the extraction of the soil sample.
Under the conditions specified in this International Standard, the following limits of quantifications apply (expressed on basis of dry matter).
Typical limit of quantification when using GC-FID:
-   volatile aromatic hydrocarbons: 0,2 mg/kg;
-   aliphatic ethers as methyl tert.-butyl ether(MTBE) and tert.-amyl methyl ether (TAME): 0,5 mg/kg.
Typical limit of quantification when using GC-ECD:
-   volatile halogenated hydrocarbons: 0,01 mg/kg to 0,2 mg/kg.
Lower limits of quantification for some compounds can be achieved by using mass spectrometry (MS) with selected ion detection (see Annex D).

ISO/TS 16558-2:2015 specifies a method for the quantitative determination of the total extractable semi-volatile, aliphatic, and aromatic fractions of petroleum hydrocarbon content in field moist soil samples by gas chromatography.
The results of the test carried out can be used for risk assessment studies related to contaminations with petroleum hydrocarbons.
ISO/TS 16558-2:2015 provides a method applicable to petroleum hydrocarbon contents from about 100 mg/kg soil expressed as dry matter for the whole aliphatic fraction C10 to C40, as well as the aromatic fraction C10 to C40. For sub-fractions, lower limits of determination can be reached.
If lower detection limits are required, large volume injection can be used or concentration of the final extract can be carried out.
NOTE 1       Low concentrations of aliphatic and aromatic compounds can be found in natural uncontaminated organic rich soils like peat soils.

This European Standard specifies a method for the determination of selected polybrominated flame retardants (BFR), chemically known as polybrominated diphenylethers (BDE), in waste materials using gas chromatography/mass spectrometry (GC-MS) in the electron impact (EI) ionisation mode (GC-EI-MS).
When applying GC-EI-MS, the method is applicable to samples containing 100 µg/kg to 5 000 µg/kg of tetra- to octabromodiphenylether congeners and 100 µg/kg to 10 000 µg/kg of decabromo diphenylether (see Table 1). It is also possible to analyse other brominated flame retardants applying the method described in this European Standard, provided the method's applicability has been proven.
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This Technical Specification specifies a method for the determination of nonylphenols (NP), nonylphenol-monoethoxylates (NP1EO) and nonylphenol-diethoxylates (NP2EO) in sludge using GC-MS.
For sludge a limit of detection of 0,1 mg/kg and for soil and treated bio-waste 0,02 mg/kg (expressed as dry matter) may be achieved.
Lower limits of detection may be achieved by concentrating the extract by solvent evaporation.
NOTE   4-tert-octylphenol can also be analysed with this method.

This Technical Specification specifies a method for the determination of linear alkylbenzene sulfonate (LAS) in sludge, treated biowaste and soil using high-performance liquid chromatography (HPLC) with a fluorescence detector (FLD) or a mass selective detector (MS).
This Technical Specification specifies the determination of the sum of LAS. Under the conditions specified in this Technical Specification, typically a limit of detection of 20 mg/kg (expressed as dry matter) for sludge and of 0,2 mg/kg to 0,5 mg/kg for soil and treated biowaste may be achieved.
Lower limits of detection may be achieved by concentrating the extract by solvent evaporation.
NOTE   The single LAS homologues C10 to C14 can be determined by this Technical Specification.

This Technical Specification specifies a method for the determination of selected phthalates in sludge, treated biowaste and soil, after extraction and gas chromatographic analysis with mass spectrometric detection.
The method is applicable for the determination of phthalates (see Table 2) at the lowest mass content of 0,1 mg/kg to 0,5 mg/kg (expressed as dry matter), depending on the individual substance.
The applicability of the method to other phthalates not specified in Table 2 is not excluded except the isomeric mixtures e.g. DiNP (Di-isononylphthalate), but shall be verified in each case.

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.

ISO 16703:2004 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 detection limits.
ISO 16703:2004 is applicable to the determination of all hydrocarbons with a boiling range of 175 °C to 525 °C, n-alkanes from C10H22 to C40H82, isoalkanes, cycloalkanes, alkylbenzenes, alkylnaphthalenes and polycyclic aromatic compounds, provided that they are not absorbed on the specified column during the clean-up procedure.
ISO 16703:2004 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 achieved.

This document specifies a gravimetric method for the determination of the hydrocarbon content in solid waste. It is applicable to hydrocarbon content greater than 0,5 % (m/m) on dry matter basis. This method does not permit to provide qualitative information on the nature and the source of the hydrocarbons.
NOTE   Aqueous liquid waste samples can be analysed in accordance with prEN ISO 9377 1 or the procedure specified in Annex B.

This document specifies a method for the quantitative determination of the hydrocarbon content (C10 to C40) in solid waste by gas chromatography.
It is applicable to hydrocarbon content between 100 mg/kg and 10 000 mg/kg expressed as dry matter basis.
Using this standard all hydrocarbons with a boiling range of approximately 175 °C to 525 °C, e.g. n-alkanes from C10H22 to C40H82, isoalkanes, cycloalkanes, alkyl benzenes, alkyl naphthalenes and polycyclic aromatic compounds are determined as hydrocarbons, provided they do not adsorb on the Florisil column during clean-up. Volatile hydrocarbons cannot be quantitatively determined using this standard. This will affect the determination of some common hydrocarbon fuels, e.g. petrol.
NOTE 1   On the basis of the peak pattern of the gas chromatogram (see Annex A) and of the boiling points of the individual n alkanes listed in Annex B the approximate boiling range of the hydrocarbons and some qualitative information on the nature of the hydrocarbons can be obtained.
NOTE 2   At the moment there is no sufficient information on how to handle organic liquid wastes for the analysis of hydrocarbons.
NOTE 3   Aqueous liquid waste samples can be analysed in accordance with EN ISO 9377-2 or the procedure specified in Annex E.
NOTE 3   Aqueous liquid waste samples can be analysed according to EN ISO 9377-2 or the procedure specified in annex E.

2017-06-06: WI abandoned to follow cancellation of WI at ISO level (ISO notification received in dataservice on 2017-06-06).
MINOR REVISION

This European Standard specifies the quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) (see Table 2) in sludge, soil and treated biowaste using GC-MS and HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels (see also Annex B).
When using fluorescence detection, acenaphthylene cannot be measured.
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Typically, a lower limit of application of 0,01 mg/kg (expressed as dry matter) can be ensured for each individual PAH. This depends on instrument and sample.
Sludge, soil and treated biowaste can differ in properties and also in the expected contamination levels of PAHs and presence of interfering substances. These differences make it impossible to describe one general procedure. This European Standard contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used. Two general lines are followed, an agitation procedure (shaking) or use of soxhlet/pressurized liquid extraction.
NOTE   Other PAH compounds can also be analysed with this method, provided suitability has been proven.

This European Standard specifies the quantitative determination of 16 polynuclear aromatic hydrocarbons (PAH) according to the priority list of the Environmental Protection Agency (EPA, 1982). This European Standard is applicable for wastes such as contaminated soil, sludge and rubble, bitumen or waste containing bitumen.
This European Standard describes a gas chromatographic method with mass spectrometric detection (GC-MS). Under the conditions specified in this document, a typical lower limit of application of 0,1 mg/kg for each individual PAH can be achieved.
NOTE 1   This method may be applied to the analysis of other PAH compounds not specified in the scope provided its applicability has been proven by proper in-house validation experiments.
NOTE 2   For some materials, e. g. bitumen, the lower limit of application of 0,1 mg/kg cannot be achieved due to interferences.
NOTE 3   Under certain circumstances the method may be applicable to PAH concentrations lower than 0,1 mg/kg but it is in the responsibility of the laboratory to provide proper validation data for such low concentrations.

This draft European Standard specifies a method for quantitative determination of seven selected polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in sludge, treated biowaste and soil using GC-MS and GC-ECD (see Table 2).
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this European Standard, limit of application of 1 μg/kg (expressed as dry matter) can be achieved.
Sludge and treated biowaste may differ in properties and also in the expected contamination levels of PCBs and presence of interfering substances. These differences make it impossible to describe one general procedure. This European Standard contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used.

This draft European Standard specifies a method for quantitative determination of seven polychlorinated biphenyl congeners (PCB-28, PCB-52, PCB-101, PCB-118, PCB-138, PCB-153 and PCB-180) in solid waste using high-resolution gas chromatography with electron capture or mass spectrometric detection. The basic content of this standard is identical to that of the Horizontal PCB-standard and is therefore also applicable to soil, sludge and treated bio-waste. The detection and the quantification limits in this method are dependent on sample intake, the level of interferences as well as instrumental limitations. Under the conditions specified in this standard, minimum amounts of individual PCB congeners equal or above 0,01 mg/kg dry matter can typically be determined with no interferences present.
NOTE   For the analysis of PCB in insulating liquids, petroleum products, used oils and aqueous samples is referred to EN 61619, EN 12766–1 and EN ISO 6468 respectively.
The method may be applied to the analysis of other PCB congeners not specified in the scope, but its suitability should be proven by proper in-house validation experiments.

This draft European Standard specifies a method for quantitative determination of seven selected polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in sludge, treated biowaste and soil using GC-MS and GC-ECD (see Table 2).
(...)
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this European Standard, limit of application of 1 µg/kg (expressed as dry matter) can be achieved.
Sludge and treated biowaste may differ in properties and also in the expected contamination levels of PCBs and presence of interfering substances. These differences make it impossible to describe one general procedure. This European Standard contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used.

This Technical Specification specifies a method for quantitative determination of 17 2,3,7,8-chlorine substituted dibenzo-p-dioxins and dibenzofurans and dioxin-like polychlorinated biphenyls in sludge, treated biowaste and soil using liquid column chromatographic clean-up methods and GC/HRMS.
The analytes to be determined with this Technical Specification are listed in Table 2.
(...)
The limit of detection depends on the kind of sample, the congener, the equipment used and the quality of chemicals used for extraction and clean-up. Under the conditions specified in this Technical Specification, limits of detection better than 1 ng/kg (expressed as dry matter) can be achieved.
This method is "performance based". It is permitted to modify the method if all performance criteria given in this method are met.
NOTE   In principle this method can also be applied for sediments, mineral wastes and for vegetation. It is the responsibility of the user of this Technical Specification to validate the application for these matrices.

This European Standard specifies a method for quantitative determination of seven selected polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in sludge, treated biowaste and soil using GC-MS and GC-ECD (see Table 2).
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this European Standard, limit of application of 1 µg/kg (expressed as dry matter) may be achieved.
Sludge and treated biowaste may differ in properties and also in the expected contamination levels of PCBs and presence of interfering substances. These differences make it impossible to describe one general procedure. This European Standard contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used.

This Technical Specification specifies the quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) (see Table 2) in sludge, soil and treated biowaste using GC-MS and HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels (see also Annex B).
When using fluorescence detection, acenaphthylene cannot be measured.
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Typically, a lower limit of application of 0,01 mg/kg (expressed as dry matter) may be ensured for each individual PAH. This depends on instrument and sample.
Sludge, soil and treated biowaste may differ in properties and also in the expected contamination levels of PAHs and presence of interfering substances. These differences make it impossible to describe one general procedure. This Technical Specification contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used. Two general lines are followed, an agitation procedure (shaking) or use of soxhlet/pressurised liquid extraction.
NOTE   Other PAH compounds can also be analysed with this method, provided suitability has been proven.

This Technical Specification specifies a method to analyse pharmaceutical compounds in solid matrices. Pharmaceuticals analysis has been carried out on a LC/MS-MS quantum. The main difficulty in this project is the lack of sample certified in researched analytes. Even with spiked solid matrices it is still delicate to correctly verify the impact of extraction step, because it does not reproduce a real sample.
What is proposed here is an analytical method on pharmaceuticals products on sludge, soils and sediments.
This document provides a final protocol on the extraction and purification tested on sludge, soils and sediments spiked with pharmaceutical compounds.

This document specifies a method for quantitative determination of seven polychlorinated biphenyl congeners (PCB-28, PCB-52, PCB-101, PCB-118, PCB-138, PCB-153 and PCB-180) in solid waste using high-resolution gas chromatography with electron capture or mass spectrometric detection. The basic content of this standard is identical to that of the Horizontal PCB-standard and is therefore also applicable to soil, sludge and treated bio-waste. The detection and the quantification limits in this method are dependent on sample intake, the level of interferences as well as instrumental limitations. Under the conditions specified in this standard, minimum concentrations of individual PCB congeners equal or above 0,01 mg/kg dry matter can typically be determined with no interferences present.
NOTE 1   For the analysis of PCB in insulating liquids, petroleum products, used oils and aqueous samples is referred to EN 61619, EN 12766-1 and EN ISO 6468, respectively.
NOTE 2   The method may be applied to the analysis of other PCB congeners not specified in the scope, but its suitability should be proven by proper in-house validation experiments.