ISO/TC 190/SC 3 - Chemical and physical characterization

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.

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 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.

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.

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.

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.

This document specifies a basic method of determining the particle size distribution applicable to a wide range of mineral soil materials, including the mineral fraction of organic soils. It also offers procedures to deal with the less common soils mentioned in the introduction. This document has been developed largely for use in the field of environmental science, and its use in geotechnical investigations is something for which professional advice might be required. A major objective of this document is the determination of enough size fractions to enable the construction of a reliable particle-size-distribution curve. This document does not apply to the determination of the particle size distribution of the organic components of soil, i.e. the more or less fragile, partially decomposed, remains of plants and animals. It is also realized that the chemical pre-treatments and mechanical handling stages in this document could cause disintegration of weakly cohesive particles that, from field inspection, might be regarded as primary particles, even though such primary particles could be better described as aggregates. If such disintegration is undesirable, then this document is not used for the determination of the particle size distribution of such weakly cohesive materials.

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.

This document specifies laboratory methods for determination of the soil water-retention characteristic. This document applies only to measurements of the drying or desorption curve. Four methods are described to cover the complete range of soil water pressures as follows: a) method using sand, kaolin or ceramic suction tables for determination of matric pressures from 0 kPa to −50 kPa; b) method using a porous plate and burette apparatus for determination of matric pressures from 0 kPa to −20 kPa; c) method using a pressurized gas and a pressure plate extractor for determination of matric pressures from −5 kPa to −1 500 kPa; d) method using a pressurized gas and pressure membrane cells for determination of matric pressures from −33 kPa to −1 500 kPa. Guidelines are given to select the most suitable method in a particular case.

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.

This document specifies a method for the determination of perchlorate in soil and soil materials. Under the conditions specified in this document, a concentration as low as 0,1 mg/kg can be determined. The working range is restricted by the ion-exchange capacity of the separator column. Dilution of the water extracts to the working range can be necessary.

This document specifies a method for the determination of cation exchange capacity (CEC) and the content of exchangeable cations (Al, Ca, Fe, K, Mg Mn, Na) in soils using a hexamminecobalt(III)chloride solution as extractant. For soils containing calcium carbonate a calcite saturated hexamminecobalt(III)chloride solution is specified particularly for determination of exchangeable Ca. This document is applicable to all types of air-dry soil samples which have been prepared according to ISO 11464.

This document specifies a method for rapid determination of water content in soils. The method is based on refractive index measurement of a sucrose solution after it is mixed with a soil sample. It is applicable to the determination of water content in geological or geotechnical research as well as geotechnical engineering. In addition, it can be used for commercial work in a variety of fields, e.g. agriculture and civil engineering. The working range is up to approximately 50 % moisture content. The precision of the method typically ranges between 0,5 % and 1 % and depends on the type of refractometer that is used. The result of this method is strongly influenced by soil matrices. Higher contents of clay and/or organic matter will lead to significant lower values for water content compared to standard methods such as that described in ISO 11465.

This document specifies a method for the determination of the cation exchange capacity (CEC) at the pH of the soil and for the determination of the content of exchangeable sodium, potassium, calcium and magnesium in soil. This document is applicable to all types of air-dried soil samples. ISO 11464 can be used for pre-treatment.

ISO 14254:2018 specifies a method for the determination of exchangeable acidity in barium chloride extracts of soil samples obtained according to ISO 11260. The procedure described herein mainly concerns the determination of total exchangeable acidity by means of a fixed pH end point titration. Two additional and optional procedures are given, describing respectively, determinations of free H+ acidity and aluminium in the extracts. ISO 14254:2018 is applicable to all types of air dry soil samples.

ISO 11508:2017 specifies two methods for the determination of particle density of soils calculated from the mass and the volume of soil particles. The first method (4.1) is applicable to fine soil (2 mm diameter). The particle density can be used for the calculation of the proportion of solids and of the porosity of soil layers in combination with the procedure given in ISO 11272.

ISO/TR 19588:2017 provides background information on the various International (ISO), American (ASTM, EPA), and European (CEN) cyanide methods for soils, waters, effluents and wastes. It gives guidance on how to carry out fit for purpose analysis of various forms of cyanide in environmental samples, the significance of the results, how to minimize interference effects and the preservation of samples. Some information is also provided on other national and international cyanide methods.

ISO 11272:2017 specifies three methods for the determination of dry bulk density of soils calculated from the mass and the volume of a soil sample. The methods involve drying and weighing a soil sample, the volume of which is either known [core method (see 4.1)] or determined [excavation method (see 4.2) and clod method (see 4.4)].

ISO 14869-3:2017 specifies a method for microwave-assisted dissolution of soil samples for determination of total element contents of Al, As, Ba, Ca, Cd, Co, Cr, Cs, Cu, Fe, Hg, K, Li, Mg, Mn, Na, Ni, P, Pb, S, Se, Sb, Sr, Tl, V, Zn using an acid mixture of nitric acid (HNO3), hydrofluoric acid (HF) and hydrochloric acid (HCl). This method is applicable to all types of soil and soil material. The main field of application is geological and pedological survey. The acid mixture is suitable for total dissolution of element contents in soil (major, minor and trace), but some refractory compounds such as SiO2, TiO2, spinel, Al2O3 or other compounds may remain as a residue. In such a case, the use of alkaline fusion, following ISO 14869‑2, is recommended to determine the true total element content. NOTE 1 In environmental studies, usually, aqua regia extraction is applied using ISO 12914 or ISO 11466. Solutions produced by the microwave method are suitable for analysis, for example, by using atomic absorption spectrometry (FAAS, HGAAS, CVAAS, GFAAS), inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). NOTE 2 Due to the presence of chloride in the digestion solution, limitations for the application of some analytical techniques can occur.

ISO 17183:2016 specifies the procedure to screen highly contaminated soils to detect organic compounds extractable with isopropanol, including a wide range of fuels, oils, and greases. The method is useful for finding hot spots. It is applicable both in laboratories and for site screening in the field. The working range is approximately 0,01 to 0,3 in absorbance units, corresponding to approximately 500 mg/kg to 10 000 mg/kg of isopropanol-extractable organic compounds in soil. The light attenuation due to light scattering/absorption approach in this method is designed to quickly screen soil samples using calibration with the most appropriate substance(s) likely to be present on a given site to indicate the concentration levels. This screening technique is applicable for a broad spectrum of organic compounds, mainly hydrocarbons. Organic compounds are a very broadly defined mixture of compounds, which show their own specific emulsification indices (see Annex A) and a gross emulsification index in a mixture sample, defined primarily by their insolubility in water. The more insoluble the compounds (e.g. non-polar compounds), the higher the response. Hydrocarbons are generally less-reactive and have little polarity. Determination of emulsification indexes uses their non-polar nature to detect organic compounds including a wide range of hydrocarbons from about C8 to about C36. NOTE This method can also be applied to biological substances such as vegetable oils. This method is not applicable for determination of specific organic compounds or groups of compounds that may be part of a larger organic compound mixture. As with other screening techniques, it is advisable to confirm a certain percentage of both positive and negative test results, especially when near or above a regulatory action limit or when the presence of background or when interfering organic compounds such as surface active substances are suspected to be present. This method does not address the evaporation of any volatile organic compound mixtures (i.e., gasoline) during sampling, preparation and detection. Although the screening method can be used for the quantitative detection of volatile hydrocarbons, it is not intended that the method be used for the quantitative determination of volatile petroleum hydrocarbons unless evaporation during sample handling is addressed; the response factor be appropriately corrected, or the method performance be demonstrated on real samples. If emulsifiers or surface active substances (e.g. detergents) are present, significantly negatively-biased or false negative results can be obtained. If there is any evidence for the presence of surfactances in the soil, this method cannot be applied.

ISO 17586:2016 specifies a method of extracting trace elements from soil at approximately pH 0,5 using a dilute nitric acid solution. Using this method the potential environmental available trace elements as defined in ISO 17402 is extracted. The method is applicable for all soils and soil like materials.

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 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/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.

ISO/TS 17182:2014 describes the gas chromatographic determination of phenols, methyl phenols, di-methylphenols and tri-methylphenols (see Table 1) and selected chlorophenols (see Table 2) by using mass spectrometric detection in soil samples. This method can also be used for other solid samples, such as sediments and solid wastes. This International Standard describes an acidic liquid extraction of soil, followed by acetylation and then liquid/liquid extraction. Determination takes place by gas chromatography and mass spectrometric detection. With this method, phenols and chlorophenols can be determined at the lowest of mass concentrations ranging from approximately 0,01 mg/kg to 0,1 mg/kg depending on the component sensitivity and the quantity of sample used. In some cases, complete separation of isomers cannot be achieved. Then the sum is reported. NOTE With this method, other higher methylated phenols can also be analysed provided that the suitability and the validity of the method is proven.

ISO 14388-2:2014 specifies a suite of methods used to determine the net acidity in acid sulfate soils. ISO 14388-2:2014 specifies a method for measuring chromium reducible sulfur (SCR) by iodimetric titration of distilled hydrogen sulfide trapped as zinc sulfide, following acidic chromous chloride digestion. This method determines inorganic sulfides (e.g. pyrite, marcasite, greigite, mackinawite) and elemental sulfur in acid sulfate soil without interferences from organic sulfur and oxidized forms of sulfur such as sulfate. On a separate test portion of soil, the pH in a 1 mol/l KCl soil suspension (pHKCl) is determined. When pHKCl is KCl), calcium (CaKCl), and magnesium (MgKCl) can also be determined. Where jarosite is identified in the soil (or where pHKCl is NAS) is determined by the difference between hydrochloric acid extractable sulfur (SHCl) and potassium chloride extractable sulfur. On samples where pHKCl is IN) by combustion furnace, or ANCBT (ANC measured by back-titration of acid remaining following an acid digest).

ISO 14388-1:2014 provides a general introduction to acid sulfate soils and the approaches that can be used to measure the various components of this special group of soils and their potential to produce acidity. It provides a compilation of the test methods, identification and definitions of the symbols, terms, and acronyms used in this series of ISO 14388. While part of the decision-making process can involve the analysis of prepared wet or dry samples, ISO 14388-1:2014 specifically outlines the procedures that are involved for preparing and analysing dried samples. ISO 14388-1:2014 also provides a procedure for pre-treating acid sulfate soil following sampling, prior to their analysis as dried sample using appropriate methods of test. The procedure includes the handling of samples before delivery to the laboratory, and the drying, grinding, and storage of samples. The standard also provides a procedure for archiving a sample after analysis. ISO 14388-1:2014 provides an acid-base accounting method to calculate the net acid-producing potential of acid sulfate soil materials by individually assessing the acid-producing capacity due to oxidation of inorganic sulfides, the existing acidity, and the effective acid-consuming capacity using results obtained in ISO 14388-2 and ISO 14388-3.

ISO 14388-3:2014 specifies a suite of methods used to determine net acidity in acid sulfate soils. ISO 14388-3:2014 specifies a method for the determination of pH in a 1 mol/l potassium chloride soil suspension (pHKCl) and where required, titratable actual acidity (TAA). Following this, potassium chloride extractable sulfur (SKCl), calcium (CaKCl) and magnesium (MgKCl) are determined. On a separate test portion, following digestion with 30 % hydrogen peroxide, peroxide pH (pHOX), titratable peroxide acidity (TPA) and excess acid neutralizing capacity (ANCE) are determined. Following this, peroxide sulfur (SP), calcium (CaP) and magnesium (MgP) are determined. On samples where jarosite is present, or where pHKCl is RAS) is determined on the soil residue remaining after peroxide digestion. Titratable sulfidic acidity (TSA), reacted calcium (CaA), reacted magnesium (MgA) and peroxide oxidizable sulfur (SPOS) are then determined by difference. For peat samples containing substantial levels of organic sulfur, the SPOCAS suite is generally unsuitable for estimating sulfide content, and the chromium reducible suite of procedures should be used instead.

ISO/TR 18105:2014 describes the procedure to screen soil samples to detect Cr(VI) using test-kits based on water extraction of Cr(VI) in soil. The test-kit approach in this method is designed to quickly screen soil samples using calibration to indicate the concentration level.

ISO 17184:2014 specifies a method for the determination of carbon and nitrogen in soils by direct measurement of sample spectra in the near-infrared spectral region. The spectra are evaluated by a suitable calibration model derived from the results obtained by reference methods.

ISO 18227:2014 specifies the procedure for a quantitative determination of major and trace element concentrations in homogeneous solid waste, soil, and soil-like material by energy dispersive X-ray fluorescence (EDXRF) spectrometry or wavelength dispersive X-ray fluorescence (WDXRF) spectrometry using a calibration with matrix-matched standards. ISO 18227:2014 is applicable for the following elements: Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Y, Zr, Nb, Mo, Ag, Cd, Sn, Sb, Te, I, Cs, Ba, Ta, W, Hg, Tl, Pb, Bi, Th, and U. Concentration levels between approximately 0,000 1 % and 100 % can be determined depending on the element and the instrument used.

ISO 13913:2014 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 selected phthalates 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 is not excluded except the isomeric mixtures, e.g. DiNP (Di-isononylphthalate), but is to be verified in each case.

ISO 13859:2014 specifies the quantitative determination of 16 PAH in sludge, soil, and treated biowaste using GC-MS and HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels. 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. Sludge, soil, and treated biowaste can differ in properties and also in the expected contamination levels of PAH and presence of interfering substances. These differences make it impossible to describe one general procedure. ISO 13859:2014 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.

ISO 13914:2013 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.

ISO 16729:2013 specifies a method for microwave digestion of sludge, treated biowaste and soil using nitric acid. This method is applicable for microwave-assisted nitric acid digestion of sludge, treated biowaste and soils 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), 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). ISO 16729:2013 may also be applicable for the digestion of other elements. Digestion with nitric acid will not necessarily accomplish total decomposition of the sample. The extracted analyte concentrations may not necessarily reflect the total content in the sample.

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.

ISO/TS 16727:2013 specifies a method for the determination of mercury in aqua regia or nitric acid digests of sludge, treated biowaste and soil, obtained according to ISO 11466 or ISO 16729 using cold vapour atomic fluorescence spectrometry. The lower working range limit is 0,003 mg/kg (dry matter).

ISO/TS 16965:2013 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.

ISO 11916-2:2013 specifies the measurement of explosive and related compounds (nitroaromatics and nitroamines) in soils and soil materials. ISO 11916-2:2013 is intended for the trace analysis of explosives and related compounds by gas chromatography (GC) using electron capture detector(s) (ECD) or a mass spectrometer (MS) as detector. ISO 11916-2:2013 can be used when reliable and specific identification of the compounds at low detection levels is required, e.g. for the evaluation of the toxic potential of soils contaminated with 2,6-DNT. Under the conditions specified in ISO 11916-2:2013, concentrations as low as 0,05 mg/kg dry matter can be determined, depending on the substance. Similar compounds may be analysed using this method. This is, however, to be verified experimentally. This method is not suitable for the analysis of hexogen (RDX), octogen (HMX), hexyl, tetryl and nitropenta (PETN).

ISO 11916-1:2013 specifies the measurement of explosive and related nitrocompounds in soils and soil materials. ISO 11916-1:2013 is intended for the trace analysis of explosives and related compounds by high-performance liquid chromatography (HPLC) using an ultraviolet (UV) detector. Under the conditions specified in ISO 11916-1:2013, concentrations as low as 0,1 mg/kg to 1 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 may be analysed using this method. However, the applicability should be checked on a case-by-case basis.

ISO 17380:2013 specifies a method for the photometric determination of the total cyanide and easily-liberatable cyanide content in soil using automated distillation/continuous-flow analysis. ISO 17380:2013 applies to all types of soil with cyanide contents above 1 mg/kg on the basis of dry matter, expressed as cyanide ion.

ISO 13196:2013 specifies the procedure for screening soils and soil-like materials for selected elements when handheld or portable energy-dispersive XRF spectrometers are used. This quick method is assumed to be applied on-site to obtain qualitative or semiquantitative data that assists decisions on further sampling strategy for assessing soil quality. The higher the efforts for pretreatment used on soil samples, the better the analytical results can be expected. ISO 13196:2013 does not explicitly specify elements for which it is applicable, since the applicability depends on the performance of the apparatus and the objective of the screening. The elements which can be determined are limited by the performance of the instruments used, the concentration of the element present in the soil, and the requirements of the investigation (e.g. guideline value). For Hg, Cd, Co, Mo, V and Sb, a majority of instruments are not sensitive enough to reach sufficiently low limits of quantification (LOQ) to meet the requirements (limit or threshold values) set in the ordinances of different countries. In this case, other methods need to be employed to measure these low concentrations. Usually, wet chemical methods are used, based on aqua regia extracts, in combination with optical or mass spectrometric (MS) methods like atomic absorption spectrometry (AAS), inductively coupled plasma/optical emission spectrometry (ICP/OES) or ICP/MS.

ISO/TS 13907:2012 specifies a method for the determination of nonylphenols (NP), nonylphenol-monoethoxylates (NP1EO) and nonylphenol-diethoxylates (NP2EO) in sludge, treated biowaste and soil using GC-MS. For sludge, a limit of detection of 0,1 mg/kg and for soil and treated biowaste of 0,02 mg/kg (expressed as dry matter) may be achieved.

ISO/TS 13896:2012 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 (MSD). ISO/TS 13896:2012 specifies the determination of the sum of LAS. Under the conditions specified in ISO/TS 13896:2012, 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.

This International Standard specifies the treatments for the measurement of the stability of soil aggregates. It can be applied to a wide range of materials originating mainly from the tilled horizons of cultivated soils. It can, however, also apply to any soil profile horizon, whether it is cultivated or not. Aggregates ranging from 3 mm to 5 mm are measured. However, the presence of gravel in the 2 mm to 5 mm fraction can distort the results. If the percentage of gravel is between 10 % and 40 %, the > 2 mm fraction of the gravel obtained from the tests should be washed and a mean weighted diameter (MWD, see 6.1) calculated with and without gravel. If the percentage of gravel is > 40 %, the structural stability tests are not significant. The method does not apply to unstructured materials, as they are not sufficiently cohesive to form millimetric aggregates.

ISO 12914:2012 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.

ISO 22036:2008 describes the determination of trace elements in digests or extraction solutions from soil by inductively coupled plasma - atomic emission spectrometry (ICP-AES) for 34 elements. This multi-element determination method is applicable to soil extracts obtained with aqua regia in accordance with ISO 11466, with DTPA in accordance with ISO 14870 or other weak extractants, or soil extracts for the determination of total element contents using the acid digestion method of ISO 14869-1 or the fusion method of ISO 14869-2. The choice of calibration method depends on the extractant and can be adapted to the extractant concentration.