13.080.10 - Chemical characteristics of soils
ICS 13.080.10 Details
Chemical characteristics of soils
Bodenuntersuchung auf chemische Substanzen
Propriétés chimiques des sols
Kemijske značilnosti tal
General Information
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This European Standard specifies a method for the determination of the following elements in aqua regia, nitric acid digest solutions of sludge, treated biowaste and soil: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), chromium (Cr), cobalt (Co), copper (Cu), gallium (Ga), indium (In), iron (Fe), lead (Pb), lithium (Li), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), nickel (Ni), phosphorus (P), potassium (K), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), thallium (Tl), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), zinc (Zn) and zirconium (Zr).
The method has been validated for the elements given in Table A.1. The method is applicable for the other elements listed above, provided the user has verified the applicability.
- Standard37 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the determination of potential cation exchange capacity (CEC) and the content of exchangeable cations (Ca, K, Mg, Na) in soils using a molar ammonium acetate solution buffered at pH 7 as extractant.
This document is applicable to all types of air-dry soil samples which have been prepared, for example, according to ISO 11464.
- Technical specification13 pagesEnglish languagesale 10% offe-Library read for1 day
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- Technical specification8 pagesFrench languagesale 15% off
This European standard specifies a method for the differentiated determination of the organic carbon content (TOC400) which is released at temperatures up to 400 °C, the residual oxidizable carbon (ROC) (including e.g. lignite (brown coal), hard coal, charcoal, black carbon, soot) and the inorganic carbon (TIC900) which is released at temperatures up to 900 °C.
The basis is the dry combustion to CO2 in a in the presence of oxygen using using temperatures ranging from 150°C to 900 °C in dry solid samples of soil, soil with anthropogenic admixtures and solid waste (see Table 1) with carbon contents of more than 1 g per kg (0,1 % C) (per carbon type in the test portion).
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This document specifies a method for the determination of the following elements in aqua regia, nitric acid or mixture of hydrochloric (HCl), nitric (HNO3) and tetrafluoroboric (HBF4)/hydrofluoric (HF) acid digests of soil, treated biowaste, waste, sludge and sediment:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gallium (Ga), gadolinium (Gd), germanium (Ge), gold (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (Lu) magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rhodium (Rh), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tantalum (Ta), tellurium (Te), terbium (Tb), thallium (Tl), thulium (Tm), thorium (Th), tin (Sn), titanium (Ti), tungsten (W), vanadium (V), yttrium (Y), ytterbium (Yb), zinc (Zn) and zirconium (Zr).
The method is also applicable to other extracts or digests originating from, for example, DTPA extraction, fusion methods or total digestion methods, provided the user has verified the applicability.
The method has been validated for the elements given in Table A.1 (sludge), Table A.2 (compost) and Table A.3 (soil). The method is applicable for other solid matrices and other elements as listed above, provided the user has verified the applicability.
This method is also applicable for the determination of major, minor and trace elements in aqua regia and nitric acid digests and in eluates of construction products (EN 17200[22]).
NOTE Construction products include e.g. mineral-based products; bituminous products; metals; wood-based products; plastics and rubbers; sealants and adhesives; paints and coatings.
- Standard37 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for the determination of the following elements in aqua regia, nitric acid or mixture of hydrochloric (HCl), nitric (HNO3) and tetrafluoroboric (HBF4)/hydrofluoric (HF) acid digests of soil, treated biowaste, waste, sludge and sediment: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gallium (Ga), gadolinium (Gd), germanium (Ge), gold (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (Lu) magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rhodium (Rh), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tantalum (Ta), tellurium (Te), terbium (Tb), thallium (Tl), thulium (Tm), thorium (Th), tin (Sn), titanium (Ti), tungsten (W), vanadium (V), yttrium (Y), ytterbium (Yb), zinc (Zn) and zirconium (Zr). The method is also applicable to other extracts or digests originating from, for example, DTPA extraction, fusion methods or total digestion methods, provided the user has verified the applicability. The method has been validated for the elements given in Table A.1 (sludge), Table A.2 (compost) and Table A.3 (soil). The method is applicable for other solid matrices and other elements as listed above, provided the user has verified the applicability. This method is also applicable for the determination of major, minor and trace elements in aqua regia and nitric acid digests and in eluates of construction products (EN 17200[22]). NOTE Construction products include e.g. mineral-based products; bituminous products; metals; wood-based products; plastics and rubbers; sealants and adhesives; paints and coatings.
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This document specifies a method for the determination of potential cation exchange capacity (CEC) and the content of exchangeable cations (Ca, K, Mg, Na) in soils using a molar ammonium acetate solution buffered at pH 7 as extractant. This document is applicable to all types of air-dry soil samples which have been prepared, for example, according to ISO 11464.
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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 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.
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This document specifies a method for determining of perchlorate in soil and soil-like materials using liquid chromatography connected to a tandem mass spectrometry (LC-MS/MS). It defines pretreatment (including drying and sieving) of sample, extraction, clean-up, analysis using LC-MS/MS, and calculation of perchlorate content in dry soil. Under the conditions specified in this document, the limit of quantitation (LOQ) is approximately 4,6 μg/kg-dry soil.
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This document 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 document are listed in Table 1. 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 document, limits of detection better than 1 ng/kg (expressed as dry matter) can be achieved. This method is “performance based”. The method can be modified 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 document 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.
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This European Standard specifies a method for quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) (see Table ) in soil, sludge, sediment, treated biowaste, and waste, using GC-MS and HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels (see Table 2).
When using fluorescence detection, acenaphthylene cannot be measured.
Table —Target analytes of this European Standard
Target analyte CAS-RNa
Naphthalene 91–20–3
Acenaphthene 83–32–9
Acenaphthylene 208–96–8
Fluorene 86–73–7
Anthracene 120–12–7
Phenanthrene 85–01–8
Fluoranthene 206–44–0
Pyrene 129–00–0
Benz[a]anthracene 56–55–3
Chrysene 218–01–9
Benzo[b]fluoranthene 205–99–2
Benzo[k]fluoranthene 207–08–9
Benzo[a]pyrene 50–32–8
Indeno[1,2,3-cd]pyrene 193–39–5
Dibenz[a,h]anthracene 53–70–3
Benzo[ghi]perylene 191–24–2
a CAS-RN Chemical Abstracts Service Registry Number.
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, 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 may 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 European Standard contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used.
The method may be applied to the analysis of other PAH not specified in the scope, provided suitability is proven by proper in-house validation experiments.
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This European standard specifies a method for the differentiated determination of the organic carbon content (TOC400) which is released at temperatures up to 400 °C, the residual oxidizable carbon (ROC) (including e.g. lignite (brown coal), hard coal, charcoal, black carbon, soot) and the inorganic carbon (TIC900) which is released at temperatures up to 900 °C.
The basis is the dry combustion to CO2 in a in the presence of oxygen using using temperatures ranging from 150°C to 900 °C in dry solid samples of soil, soil with anthropogenic admixtures and solid waste (see Table 1) with carbon contents of more than 1 g per kg (0,1 % C) (per carbon type in the test portion).
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This document specifies an instrumental method for the routine determination of pH within the range pH 2 to pH 12 using a glass electrode in a 1:5 (volume fraction) suspension of soil, sludge and treated biowaste in either water (pH in H2O), in 1 mol/l potassium chloride solution (pH in KCl) or in 0,01 mol/l calcium chloride solution (pH in CaCl2).
This document is applicable to all types of air-dried soil and treated biowaste samples.
NOTE For example, pretreated in accordance with ISO 11464 or EN 16179 or EN 15002.
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This document specifies two methods for the determination of total organic carbon (TOC) in sludge, treated biowaste, soil and waste samples containing more than 0,1 % carbon in relation to the dry mass (dm).
NOTE This method can also be applied to other environmental solid matrices, provided the user has verified the applicability.
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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.
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This document specifies an operationally defined method for the direct determination of organically bound halogens (chlorine, bromine and iodine) adsorbed and occluded to the sample matrix. AOX being a methodologically defined parameter, it is essential that the procedure is applied without any modification.
This document is intended for analysis of sludge, treated biowaste or soil in concentrations ranging from 5 mg/kg dry matter. The upper limit and exact concentration range covered depend on the instrumentation used for determination.
NOTE This method can also be applied to other environmental solid matrices, provided the user has verified the applicability.
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This European Standard specifies two methods for the determination of total organic carbon (TOC) in sludge, treated biowaste, soil, waste and sediment samples containing more than 1 g carbon per kg of dry matter (0,1 %).
When present, elementary carbon, carbides, cyanides, cyanates, isocyanates, isothiocyanates and thio-cyanates are determined as organic carbon using the methods described in this European Standard. An interpretation of the measured value may therefore be problematic in cases where the samples contain relevant levels of the above mentioned components. If necessary, these components should be determined separately by means of a suitable validated procedure and be recorded in the test report.
For sludge, treated biowaste and soil only Method A is validated.
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This document specifies an instrumental method for the routine determination of pH within the range pH 2 to pH 12 using a glass electrode in a 1:5 (volume fraction) suspension of soil, sludge and treated biowaste in water (pH in H2O), in 1 mol/l potassium chloride solution (pH in KCl) or in 0,01 mol/l calcium chloride solution (pH in CaCl2).
This International Standard is applicable to all types of soil, sludge and biowaste, for example
pretreated in accordance with ISO 11464 or EN 16179.
- Standard15 pagesEnglish languagesale 10% offe-Library read for1 day
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.
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- Standard31 pagesEnglish languagesale 10% offe-Library read for1 day
This European Standard describes an empirical method for the direct determination of organically bound chlorine, bromine and iodine (but not fluorine) adsorbed and occluded to the sample matrix. Non-volatile organically bound halogens adsorbable on activated carbon present in the aqueous phase of the sample prior to drying or adsorbed to sample surface are included in the determination.
This European Standard is intended for analysis of sludge, treated biowaste or soil in concentrations ranging from 5 mg/kg dry matter to approximately 6 g/kg dry matter. The exact concentration range covered depends on the instrument used for determination.
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This document specifies the determination of Cr(VI) in solid waste material and soil by alkaline digestion and ion chromatography with spectrophotometric detection. This method can be used to determine Cr(VI)-mass fractions in solids higher than 0,1 mg/kg.
NOTE In case of reducing or oxidising waste matrix no valid Cr(VI) content can be reported.
- Standard32 pagesEnglish languagesale 10% offe-Library read for1 day
This document specifies a method for quantitative determination of organochlorine pesticides (OCPs) and semi-volatile chlorobenzenes in soil and sediment, using GC-MS and GC-ECD. The limit of detection and the limit of application depends on the determinants, the sample intake, 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 limits of application from 1 μg/kg (expressed as dry matter) for soils to 10 μg/kg (expressed as dry matter) for sediments can be achieved. The necessity to achieve these lower limits of application depends on the analyses order and the current limit values. Soils and sediments can differ in properties as well as in the expected contamination levels of OCPs and the presence of interfering substances. These differences make it impossible to describe one general procedure. Based on the properties of the samples, this document contains decision tables regarding drying-, extraction- and clean-up procedures. This method is performance based. The method can be modified if all performance criteria given in this method are met. The method can be applied to the analysis of other chlorinated compounds not specified in the scope in cases where suitability has been proven by proper in-house validation experiments. NOTE The validation data are shown in Annex A. This document is validated only for α-HCH, β-HCH, γ-HCH, δ-HCH, o,p′-DDE, p,p′-DDE, o,p′-DDD, p,p′-DDD, o,p′-DDT and p,p′-DDT. For sediments, data are displayed measured using an ECD detection. The comparability of ECD and MS data in terms of the approach of this document was demonstrated on additional matrices.
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This document provides guidance on the selection and application of screening methods for assessing soil quality and waste characterization, including distribution of target parameters in soil and soil‑like material. The aim of this document is to set up criteria as to when the different kind of screening methods can be applied for the analysis of a certain parameter in soil, including soil‑like material, and waste, and which steps are required to prove their suitability.
This document does not recommend any particular screening method but confirms the principles of their selection and application.
- Standard32 pagesEnglish languagesale 10% offe-Library read for1 day
This International Standard specifies the measurement of explosive and related nitrocompounds
compounds using liquid chromatography–tandem mass spectrometry (LC-MS/MS) in soil and soilmaterials. This method is applicable to 12 compounds (1,3-DNB, 1,3,5-TNB, 2,4-DNT, 2,6-DNT, 2,4,6-TNT, 4-A-2,6-DNT, 2-A-4,6-DNT, Tetryl, Hexyl, RDX, HMX, PETN) listed in ISO 11916-1(soil, HPLC/UV method) except nitrobenzene, 2-nitortoluene, 3-nitrotoluene and 4-nitrotoluene. In particular,this method is effective for the analysis of PETN, 1,3,5-TNB and tetryl which showed poor interlaboratory trial results with ISO 11916-1. 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.
Purpose and justification of the proposal*
Currently two ISO standards exist for the analysis of explosives and related compounds in soil: ISO 11916-1(HPLC/UV method), ISO 11916-2(GC-ECD or MS method). According to the results of interlaboratory trial with ISO 11916-1, it showed some problematic aspects to analyze PETN, 1,3,5-TNB and tetryl. In case of ISO 11916-2, it also gave poor inter-laboratory trial results for 1,3,5-TNB. Therefore, it is necessary to develop new method effectively applicable to the determination of PETN, 1,3,5-TNB and tetryl.
In addition to this, lower risk-based PRGs (Preliminary Remediation Goal), new regulatory concerns, and change of land use have created the atmosphere to apply more sensitive and selective instruments to determine explosive and related compounds. From the view of these aspects, liquid chromatography–tandem mass spectrometry (LC-MS/MS) is one of alternative methods for these purposes. LC-MS/MS method provides 10-20 times or much lower detection limit than that of HPLC/UV method and is recommendable to determine PETN, 1,3,5-TNB and tetryl.
Also LC-MS/MS method is getting more familiar in ISO standard development (e.g. ISO/CD22104 Water quality--Microcystins, ISO/NP21677 Water quality--HBCD, ISO/CD21675 Water quality--PFAS).
Consider the following: Is there a verified market need for the proposal? What problem does this
standard solve? What value will the document bring to end-users? See Annex C of the ISO/IEC
Directives part 1 for more information. See the following guidance on justification statements on ISO Connect:
https://connect.iso.org/pages/viewpage.action?pageId=27590861
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- Standard31 pagesEnglish languagesale 10% offe-Library read for1 day
This document provides guidance on the selection and application of screening methods for assessing
soil quality and waste characterization, including distribution of target parameters in soil and soil‑like
material. The aim of this document is to set up criteria as to when the different kind of screening
methods can be applied for the analysis of a certain parameter in soil, including soil‑like material, and
waste, and which steps are required to prove their suitability.
This document does not recommend any particular screening method but confirms the principles of
their selection and application.
- Standard32 pagesEnglish languagesale 10% offe-Library read for1 day
ISO 15192:2010 specifies a method for the determination of Cr(VI) in solid waste material and soil by alkaline digestion and ion chromatography with spectrophotometric detection. This method can be used to determine Cr(VI) mass fractions in solids greater than 0,1 mg/kg.
- Standard32 pagesEnglish languagesale 10% offe-Library read for1 day
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.
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This document specifies two methods for digestion of soil, treated biowaste, sludge and waste by the use of an aqua regia digestion.
Digestion with aqua regia will not necessarily accomplish total decomposition of the sample. The extracted analyte concentrations may not necessarily reflect the total content in the sample but represent the aqua regia soluble metals under the condition of this test procedure. It is generally agreed that for environmental analysis purposes, the results are fit for the intended purpose to protect the environment.
This document is applicable for the following elements:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), boron (B), cadmium (Cd), calcium (Ca), chromium (Cr), cobalt (Co), copper (Cu), iron (Fe), lead (Pb), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), nickel (Ni), phosphorus (P), potassium (K), selenium (Se), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tellurium (Te), thallium (Tl), tin (Sn), titanium (Ti), vanadium (V), and zinc (Zn).
This document can also be applied for the digestion of other elements, provided the user has verified the applicability.
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This document specifies the determination of Cr(VI) in solid waste material and soil by alkaline digestion and ion chromatography with spectrophotometric detection. This method can be used to determine Cr(VI)-mass fractions in solids higher than 0,1 mg/kg. NOTE In case of reducing or oxidising waste matrix no valid Cr(VI) content can be reported.
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This document provides guidance on the selection and application of screening methods for assessing soil quality and waste characterization, including distribution of target parameters in soil and soil‑like material. The aim of this document is to set up criteria as to when the different kind of screening methods can be applied for the analysis of a certain parameter in soil, including soil‑like material, and waste, and which steps are required to prove their suitability. This document does not recommend any particular screening method but confirms the principles of their selection and application.
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This document specifies an instrumental method for the routine determination of pH within the range pH 2 to pH 12 using a glass electrode in a 1:5 (volume fraction) suspension of soil, sludge and treated biowaste in either water (pH in H2O), in 1 mol/l potassium chloride solution (pH in KCl) or in 0,01 mol/l calcium chloride solution (pH in CaCl2). This document is applicable to all types of air-dried soil and treated biowaste samples. NOTE For example, pretreated in accordance with ISO 11464 or EN 16179 or EN 15002.
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This Technical Specification describes an approach for the validation of physico-chemical analytical methods for environmental matrices.
The guidance in this document addresses two different validation approaches, in increasing order of complexity. These are:
a) method development and validation at the level of single laboratories (intra-laboratory validation);
b) method validation at the level of several laboratories (between-laboratory or inter-laboratory validation), with a focus on methods that are sufficiently mature and robust to be applied not only by a few expert laboratories but by laboratories operating at the routine level.
The concept of these two approaches is strictly hierarchical, i.e. a method shall fulfil all criteria of the first level before it can enter the validation protocol of the second level.
This Technical Specification is applicable to the validation of a broad range of quantitative physico-chemical analytical methods for the analysis of water (including surface water, groundwater, waste water, and sediment). Analytical methods for other environmental matrices, like soil, sludge, waste, and biota can be validated in the same way. It is intended either for analytical methods aiming at substances that have recently become of interest or for test methods applying recently developed technologies.
The minimal requirements that are indispensable for the characterization of the fitness for purpose of an analytical method are: selectivity, precision, bias and measurement uncertainty. The aim of validation is to prove that these requirements are met.
- Technical specification53 pagesEnglish languagesale 10% offe-Library read for1 day
This European Standard specifies two methods for digestion of soil, treated biowaste, sludge and waste by the use of aqua regia as digestion solution.
This European Standard is applicable for the following elements:
aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), gold (Au), hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (Lu), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rubidium (Rb), rhenium (Re), rhodium (Rh), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), ytterbium (Yb), yttrium (Y), zinc (Zn), and zirconium (Zr).
This European Standard may also be applicable for the digestion of other elements.
Digestion with aqua regia will not necessarily accomplish total decomposition of the sample. The extracted analyte concentrations may not necessarily reflect the total content in the sample.
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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.
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ISO 17512-1:2008 specifies a rapid screening method for evaluating the habitat function of soils and the influence of contaminants and chemicals on earthworm behaviour.
The sublethal test is a rapid method that reflects the bioavailability of contaminant mixtures in natural soils and substances spiked into soils to Eisenia fetida and Eisenia andrei. The avoidance behaviour of the worms is the measurement endpoint of the test. This test is not intended to replace the earthworm reproduction test.
Two different designs (a two section unit and a six section unit) have been developed and successfully applied. Both designs are applicable to either single-concentration (e. g. for assessing the quality of a field soil) or multi-concentration (e. g. for assessing the toxicity of a spiked chemical) tests. In both cases, the earthworms are allowed to make the initial choice on which compartment, control and a treatment [in the two section test vessel between right and left side; in the six section test vessel between the (3 + 3) alternating compartments], to enter.
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This European Standard specifies a method for quantitative determination of seven selected polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in soil, sludge, sediment, treated biowaste and waste and using GC-MS and GC-ECD.
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, 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 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.
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, provided suitability is proven by proper in-house validation experiments
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This document specifies two methods for digestion of soil, treated biowaste, sludge and waste by the use of an aqua regia digestion. Digestion with aqua regia will not necessarily accomplish total decomposition of the sample. The extracted analyte concentrations may not necessarily reflect the total content in the sample but represent the aqua regia soluble metals under the condition of this test procedure. It is generally agreed that for environmental analysis purposes, the results are fit for the intended purpose to protect the environment. This document is applicable for the following elements: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), boron (B), cadmium (Cd), calcium (Ca), chromium (Cr), cobalt (Co), copper (Cu), iron (Fe), lead (Pb), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), nickel (Ni), phosphorus (P), potassium (K), selenium (Se), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tellurium (Te), thallium (Tl), tin (Sn), titanium (Ti), vanadium (V), and zinc (Zn). This document can also be applied for the digestion of other elements, provided the user has verified the applicability.
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This document specifies methods for the measurements of magnetic susceptibility of soils (κ) as an indicator of potential soil pollution/contamination with trace elements associated with technogenic magnetic particles (TMPs) and describes related procedures, protocols and guidelines to be applied as a screening geophysical method of determination of soil pollution with trace elements. The results of measurements are used for preparing the maps of magnetic susceptibility of soils in the area of interest. From these maps, the areas of elevated and high magnetic susceptibility indicating high trace element total pollution load are discriminated for further identification of pollutants by geochemical methods. This document is applicable to screening all TMPs-related anthropogenic emission sources including long-range transport of airborne elements, of which TMPs are carriers and indicators. Such emission sources comprise the majority of high-temperature industrial processes, where iron is present in any mineralogical form in raw materials, additives or fuels, is transformed into ferrimagnetic iron oxides (e.g. fossil solid and liquid fuels combustion, metallurgy, cement and ceramics industry, coke production, industrial waste landfills, land transport). This document is not applicable to screening anthropogenic emissions not associated with TMPs, e.g. organic pollutants or emissions from agricultural sources. NOTE 1 Copper, zinc and other non-ferrous metal ores also contain iron (in many sulfides) as this element is abundant in almost all environments. During smelting, the iron occurring in sulfides is transformed into ferrimagnetic oxides (TMPs). However, in such cases, the proportion of TMPs and related PTEs is usually less than at coal combustion or iron metallurgy, for example, and not all PTEs are physically associated and transported by TMPs. Non-airborne elements are deposited in the close proximity of the emission source, while TMPs can be used in these cases as indicators of airborne elements and of the spatial distribution of the total element deposition from a smelter in the area. In rare cases, some soils are developed on bedrock exhibiting geogenically high magnetism, which can cause false-positive results. This influence can, however, be easily indicated by measurements of magnetic susceptibility along soil profiles. This method is not applicable when the bedrock exhibits extremely high magnetic signals. NOTE 2 Such cases are rare.
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This International Standard specifies the quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) according to the priority list of the Environmental Protection Agency, USA (EPA, 1982). This International Standard is applicable to all types of soil (field-moist or chemically dried samples), covering a wide range of PAH contamination levels.
Under the conditions specified in this International Standard, a lower limit of application of 0,01 mg/kg
(expressed as dry matter) can be ensured for each individual PAH.
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ISO 16772:2004 specifies a method for the determination of mercury in an aqua regia extract of soil, obtained in accordance with ISO 11464 and ISO 11466, using cold-vapour atomic absorption spectrometry or cold-vapour atomic fluorescence spectrometry. The limit of determination of the method is at least 0,1 mg/kg.
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This International Standard specifies a method for quantitative determination of seven polychlorinated biphenyls
and seventeen organochlorine pesticides in soil.
This International Standard is applicable to all types of soil.
Under the conditions specified in this International Standard, limits of detection of 0,1 μg/kg to 4 μg/kg (expressed
as dry matter) can be achieved.
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This International Standard specifies a method for microwave-assisted extraction of elements from samples
using aqua regia as the extraction solution for the determination of elements. This method is applicable to all
types of soil and soil material.
Aqua regia extraction is suitable for the release of trace and major element fractions in soil. Aqua regia is not
suitable for the extraction of elements from refractory compounds, such as SiO2, TiO2 and Al2O3.
The extraction with aqua regia is operationally defined and will not necessarily release all elements completely.
The microwave method is generic and can be implemented using a wide variety of equipment, provided:
a) the extraction mixture ratio is unchanged;
b) the extraction temperature is known.
Solutions produced by the microwave method are suitable for analysis, for example, by using atomic
absorption spectrometry (flame: FAAS, hydride generation: HGAAS, cold vapour: CVAAS, graphite furnace;
GFAAS), inductively coupled plasma emission spectrometry (ICP/OES) and inductively coupled plasma mass
spectrometry (ICP/MS).
NOTE Due to the presence of chloride in the extraction solution, limitations for the application of analytical
techniques can occur.
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ISO 13876:2013 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.
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This Technical Specification specifies a method for the determination of the following elements in aqua
regia or nitric acid digests or other extraction solutions of sludge, treated biowaste and soil:
Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron
(B), cadmium (Cd), calcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu),
dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), gold (Au),
hafnium (Hf), holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li),
lutetium (Lu), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd),
nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rhenium
(Re), rhodium (Rh), rubidium (Rb), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se),
silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tellurium (Te), terbium (Tb), thallium
(Tl), thorium (Th), thulium (Tm), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V),
ytterbium(Yb), yttrium (Y), zinc (Zn) and zirconium (Zr).
The working range depends on the matrix and the interferences encountered.
The limit of detection is between 0,1 mg/kg dry matter and 2,0 mg/kg dry matter for most elements.
The limit of detection will be higher in cases where the determination is likely to have interferences (see
Clause 4) or in the case of memory effects (see e.g. 8.2 of ISO 17294-1:2004).
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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.
(...)
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.
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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.
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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.
(...)
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.
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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.
Organotin cations can only be determined in accordance with this document after derivatization. The anionic part bound to the organotin cation is mainly dependent on the chemical environment and is not determined using this method. The peralkylated organotin compounds behave in a completely different way from their parent compounds. Tetraalkylated organotin compounds which are already peralkylated, such as tetrabutyltin, are determined directly without derivatization.
The properties such as particle size distribution, water content and organic matter content of the solids to be analysed using this document vary widely. Sample pretreatment is designed adequately with respect to both the properties of the organotin compounds and the matrix to be analysed.
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