2019-01-2991 - Pravilnik o monitoringu kakovosti tal
Pravilnik o monitoringu kakovosti tal
Pravilnik o monitoringu kakovosti tal
General Information
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 the elements aluminium, antimony, arsenic,
barium, beryllium, bismuth, boron, cadmium, caesium, calcium, cerium, chromium, cobalt, copper,
dysprosium, erbium, gadolinium, gallium, germanium, gold, hafnium, holmium, indium, iridium, iron,
lanthanum, lead, lithium, lutetium, magnesium, manganese, mercury, molybdenum, neodymium, nickel,
palladium, phosphorus, platinum, potassium, praseodymium, rubidium, rhenium, rhodium, ruthenium,
samarium, scandium, selenium, silver, sodium, strontium, terbium, tellurium, thorium, thallium,
thulium, tin, titanium, tungsten, uranium and its isotopes, vanadium, yttrium, ytterbium, zinc and
zirconium in water (e.g. drinking water, surface water, ground water, waste water and eluates).
Taking into account the specific and additionally occurring interferences, these elements can be
determined in water and digests of water and sludge (e.g. digests of water as described in ISO 15587-1
or ISO 15587-2).
The working range depends on the matrix and the interferences encountered. In drinking water and
relatively unpolluted waters, the limit of quantification (LOQ) lies between 0,002 μg/l and 1,0 μg/l for
most elements (see Table 1). The working range typically covers concentrations between several ng/l
and mg/l depending on the element and specified requirements.
The quantification limits of most elements are affected by blank contamination and depend
predominantly on the laboratory air-handling facilities available on the purity of reagents and the
cleanliness of glassware.
The lower limit of quantification is higher in cases where the determination suffers from interferences
(see Clause 5) or memory effects (see ISO 17294-1).
Elements other than those mentioned in the scope can also be determined according to this document
provided that the user of the document is able to validate the method appropriately (e.g. interferences,
sensitivity, repeatability, recovery).
- Standard42 pagesEnglish languagesale 10% offe-Library read for1 day
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 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 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 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.
- Standard47 pagesEnglish languagesale 10% offe-Library read for1 day
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.
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This document provides guidance on the description of soil in the field and its environmental context. It is applicable to natural, near-natural, urban and industrial sites. The soil observations and measurements can be made on a project site level, on a plot level, on layer or horizon level and on specific soil constituents.
It also provides guidance on how to describe layers of anthropogenic (artificial) material or layers that were not modified by pedogenic processes in the strict sense and how to describe coarse material of natural or artificial origin.
This document can be used in combination with other publications that provide guidance or requirements regarding specific aspects of soil observations and measurements.
NOTE 1 It might not be possible or necessary to record data under all the headings listed in Clauses 4 to 11.
NOTE 2 Overall guidance for presentation of information from soil surveys is given in ISO 15903.
NOTE 3 The guidance provided assumes that sampling will be done in accordance with ISO 18400.
- Standard61 pagesEnglish languagesale 10% offe-Library read for1 day
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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ISO 18287:2006 specifies the quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) according to the priority list of the Environmental Protection Agency, USA (EPA, 1982). ISO 18287:2006 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 ISO 18287:2006, 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/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.
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ISO 10382:2002 specifies a method for quantitative determination of seven polychlorinated biphenyls and seventeen organochlorine pesticides in soil.
ISO 10382:2002 is applicable to all types of soil.
Under the conditions specified in ISO 10382:2002, limits of detection of 0,1 micrograms per kilogram to 4 micrograms per kilogram (expressed as dry matter) can be achieved.
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ISO 14507:2003 specifies three methods for the pretreatment of soil samples in the laboratory prior to the determination of organic contaminants:
if volatile organic compounds are to be measured;
if moderately volatile to non-volatile organic compounds are to be measured, if the result of the subsequent analysis must be accurate and reproducible, and if the sample contains particles larger than 2 mm and/or the contaminant is heterogeneously distributed;
if non-volatile organic compounds are to be measured and the extraction procedure prescribes a field-moist sample, or if the largest particles of the sample are smaller than 2 mm and the contaminant is homogeneously distributed. This procedure is also applicable if reduced accuracy and repeatability are acceptable.
The pretreatment described in ISO 14507:2003 is used in combination with an extraction procedure in which the contaminant is available for the extraction liquid.
NOTE For the pretreatment of soil samples for the purposes of determining non-volatile inorganic compounds and physico-chemical soil characteristics, see ISO 11464.
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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.
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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 document gives guidance on the:
— investigation of sites, where either it is known that soil contamination is present, or the presence of soil contamination is suspected;
— investigation of sites where no soil contamination is expected, but the soil quality is to be determined (e.g. to make sure that there is no contamination present);
— investigation in anticipation of a need to manage re-use or disposal of excavated soil which might be contaminated;
— collection of information that is necessary for risk assessment and/or the development of remedial action plans (e.g. whether remediation is required and suggestions as to how this might be best achieved).
Although the information on soil quality for the risk assessment and/or the development of remedial action plans is gathered by applying this document, it does not give guidance on the decisions and actions that follow from a site investigation, for example, risk assessment and decisions about the requirements for remediation (if any).
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This document provides guidance on the sampling of soils of
— natural and near-natural sites,
— natural arboreal areas including forests and woods,
— areas used for agriculture (arable and pasture sites),
— areas used for horticulture (including domestic gardens, allotments), and
— areas used for special crop-cultivation, orchards, vineyards, commercial plantations and forests, etc.
It is applicable to
— soil investigations and evaluations in the field, and
— collection of samples for chemical, geochemical, physical, and biological characterization of soil and soil materials in the laboratory.
This document sets out appropriate strategies for the design of sampling programmes, field procedures and subsequent treatment of samples for transport and storage prior to sample pretreatment (e.g. drying, milling). It is intended to be used in conjunction with the other parts of the ISO 18400 series. Attention is, in particular, drawn to the requirements concerning collection, handling and storage of soil for assessment of biological functions in ISO 18400-206.
NOTE 1 Groundwater and surface water can be adversely impacted by agricultural and related activities, such as nitrates and pesticides, and by translocation of soil particles. In turn, knowledge about water quality can provide information about possible sources of groundwater contamination or contaminating run-off. Investigation of groundwater and surface water quality is outside of the scope of this document; relevant guidance is given in the ISO 5667 series of standards. ISO 15175 provides guidance on the relationship between soil properties and groundwater quality.
NOTE 2 It could also be appropriate to investigate ambient air, vegetation, potable water supplies and a variety of other media depending on the findings of the preliminary investigation.
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ISO 18512:2007 gives guidance on how to store and preserve soil samples for laboratory determinations and how to prepare them for analysis after storage. Special emphasis is given to maximum storage times as a function of different storage conditions.
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ISO 18400-105:2017 establishes general principles for packing, preservation, transport and delivery of samples of soil and related materials with an emphasis on requirements for when chemical analysis of the samples is required, but with the intention that the general procedures are to be adapted as appropriate when other forms of testing are required (e.g. biological testing, physical tests on disturbed or undisturbed samples). Special procedures for specific sampling purposes are given in other parts of ISO 18400 (see also 7.2).
ISO 18400-105:2017 is intended to be read in conjunction with ISO 18512.
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ISO 18400-102:2017 gives guidelines for techniques for taking samples so that these can subsequently be examined for the purpose of providing information on soil quality. It gives information on equipment that is typically applicable in particular sampling situations to enable correct sampling procedures to be carried out and representative samples to be collected. Guidance is given on the selection of the equipment and the techniques to use to enable both disturbed and undisturbed samples to be correctly taken at different depths.
ISO 18400-102:2017 does not cover:
- investigations for geotechnical purposes, though where redevelopment of a site is envisaged, the soil quality investigation and the geotechnical investigation may sometimes be beneficially combined;
- sampling of hard strata such as bedrock;
- methods for the collection of information on soil quality without taking samples such as geophysical methods;
- collection of water samples (these are to be collected in accordance with appropriate International Standards on ground or surface water sampling; for further information, see the ISO 5667 series);
- investigations of soil gas about which guidance is provided in ISO 18400‑204;
- investigation of radioactively contaminated sites.
NOTE 1 "Sampling technique" is defined in ISO 11074.
NOTE 2 Guidance on the investigation and assessment of radioactivity in soils is provided in the ISO 18589 series.
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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.
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ISO/IEC 17025:2017 specifies the general requirements for the competence, impartiality and consistent operation of laboratories.
ISO/IEC 17025:2017 is applicable to all organizations performing laboratory activities, regardless of the number of personnel.
Laboratory customers, regulatory authorities, organizations and schemes using peer-assessment, accreditation bodies, and others use ISO/IEC 17025:2017 in confirming or recognizing the competence of laboratories.
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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)].
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This European Standard specifies a method for the determination of the following elements in aqua regia or nitric acid digests 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 method detection limit of the method 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 be interfered (see Clause 4) or in case of memory effects (see e.g. 8.3 of EN ISO 17294-1:2006).
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 the other elements listed above, provided the user has verified the applicability.
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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).
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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.
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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.
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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.
- Technical specification28 pagesEnglish languagesale 10% offe-Library read for1 day
The determination of the specific electrical conductivity is carried out to obtain an indication of the content of water-soluble electrolytes in soil, treated biowaste and sludge.
WARNING — Persons using this Technical Specification should be familiar with usual laboratory practice. This Technical Specification does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this Technical Specification be carried out by suitably trained staff.
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This European Standard specifies the pretreatment required for sludge, treated biowaste and soil (including soil-like materials), that are subject to the analysis of organic as well as inorganic chemical and physico-chemical parameters.
The pretreatment of samples aims at preparing a (small) test sample which is representative for the original sample.
This European Standard describes the pretreatment which could be performed under field conditions if necessary (see Clause 8) and the sample pretreatment under laboratory conditions (Clause 10).
For determining inorganic chemical and physico-chemical parameters this European Standard describes procedures (see 10.2) to prepare:
- test samples for tests under field moist conditions;
- test samples for testing after drying, crushing, grinding, sieving etc.;
- test samples of liquid sludge.
For determination of organic compounds three pretreatment methods are specified:
- a pretreatment method if volatile organic compounds are to be measured (see 10.3.2);
- a pretreatment method if moderately volatile to non-volatile organic compounds are to be measured and the result of the following analysis will be accurate and reproducible (see 10.3.3);
- a pretreatment method if moderately volatile to non-volatile organic compounds are to be measured and the extraction procedure prescribes a field moist sample or if only indicative results are required (see 10.3.4).
The choice of the method depends above all on the volatility of the analyte. It also depends on the particle size distribution of the material (see Clause 5 and 8.3), the heterogeneity of the sample and the following analytical procedure.
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This European Standard specifies the determination of total nitrogen (organic and inorganic) according to the procedure of Dumas in sludge, treated biowaste and soil. A typical limit of detection is 0,02 % nitrogen, and a typical limit of quantification is 0,08 % nitrogen.
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This European Standard specifies methods for the calculation of the dry matter of sludge, treated biowaste, soil and waste for which the results of performed analysis are to be calculated to the dry matter basis. Depending on the nature and origin of the sample, the calculation is based on a determination of the dry residue (Method A) or a determination of the water content (Method B). It applies to samples containing more than 1 % (mass fraction) of dry residue or more than 1 % (mass fraction) of water.
Method A applies to sludge, treated biowaste, soil and solid waste, Method B applies to liquid waste and to samples which are suspected or known to contain volatiles except for water.
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ISO 12846:2012 specifies two methods for the determination of mercury in drinking, surface, ground, rain and waste water after appropriate pre-digestion. For the first method, an enrichment step by amalgamation of the Hg on, for example, a gold/platinum adsorber is used. For the second method, the enrichment step is omitted.
The choice of method depends on the equipment available, the matrix and the concentration range of interest. Both methods are suitable for the determination of mercury in water. The method with enrichment commonly has a practical working range from 0,01 µg/l to 1 µg/l. The mean limit of quantification (LOQ) reported by the participants of the validation trial was 0,008 µg/l. This information on the LOQ gives the user of ISO 12846:2012 an orientation and does not replace the estimation of performance data from laboratory specific data. It has to be considered that it is possible to achieve lower LOQs with specific instrumentation (e.g. single mercury analysers).
The method without enrichment commonly has a practical working range starting at 0,05 µg/l. The LOQ reported by the participants of the validation trial was 0,024 µg/l. It is up to the user, based on the specific application, to decide whether higher concentrations are determined by omitting the enrichment step and/or by diluting the sample(s). The sensitivity of both methods is dependent on the selected operating conditions.
Another possibility for the determination of extremely low Hg concentrations down to 0,002 µg/l without pre-concentration is the application of atomic fluorescence spectrometry (see ISO 17852). Specific atomic-absorption mercury analysers allow determinations down to 0,010 µg/l without pre-concentration.
In general, the determination of trace concentrations of Hg by AAS (or AFS) is dependent on clean operating conditions in the laboratory and on the use of high-purity chemicals with negligible low-Hg blanks.
Note that ISO 12846:2012 may be applied to industrial and municipal waste water after an additional digestion step performed under appropriate conditions and after suitable method validation. A potential sample stability issue (mercury loss) for anaerobic reducing industrial effluents has to be considered thoroughly.
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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.
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ISO 11885:2007 specifies a method for the determination of dissolved elements, elements bound to particles ("particulate") and total content of elements in different types of water (e.g. ground, surface, raw, potable and waste water) for the following elements: aluminium, antimony, arsenic, barium, beryllium, bismuth, boron, cadmium, calcium, chromium, cobalt, copper, gallium, indium, iron, lead, lithium, magnesium, manganese, molybdenum, nickel, phosphorus, potassium, selenium, silicon, silver, sodium, strontium, sulfur, tin, titanium, tungsten, vanadium, zinc and zirconium.
Taking into account the specific and additionally occurring interferences, these elements can also be determined in digests of water, sludges and sediments (for example, digests of water as specified in ISO 15587‑1 or ISO 15587‑2). The method is suitable for mass concentrations of particulate matter in waste water below 2 g/l. The scope of this method may be extended to other matrices or to higher amounts of particulate matter if it can be shown that additionally occurring interferences are considered and corrected for carefully. It is up to the user to demonstrate the fitness for purpose.
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ISO 11464:2006 specifies the pretreatments required for soil samples that are to be subjected to physico-chemical analyses of stable and non-volatile parameters and describes the following five types of pretreatment of samples: drying, crushing, sieving, dividing and milling.
The pretreatment procedures described in ISO 11464:2006 are not applicable if they affect the results of the determinations to be made. ISO 11464:2006 is also not applicable to samples when volatile compounds are measured. In general, International Standards for analytical methods will state when it is necessary to adopt other procedures.
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Specifies an instrumental method for the routine determination of the specific electrical conductivity in an aqueous extract of soil. The determination is carried out to obtain an indication of the content of water-soluble electrolytes in a soil.
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Specifies a method for the extraction, with aqua regia, of trace elements from soils and similar materials containing less than about 20 % (m/m) organic carbon. Materials containing more than about 20 % (m/m) organic carbon will require treatment with additional nitric acid. The resulting solution is suitable for the determination of trace elements using appropriate atomic spectrometric techniques.
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Specifies a method for the determination of the potential cation exchange capacity (CEC) of soil buffered at pH = 8,1 and of the determination of the content of exchangeable sodium, potassium, calcium and magnesium in soil. Applicable to all types of air-dried soil samples.
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Specifies a method for the determination of the total nitrogen (ammonium-N, nitrate-N, nitrite-N and organic N) content of a soil. Nitrogen in N-N-linkages, N-O-linkages and some heterocyclics (especially pyridine) is only partially determined. Applicable to all types of soils.
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Specifies a method for the determination of the total carbon content in soil after dry combustion. The organic carbon content is calculated from this content after correcting for carbonates present in the sample. If carbonates are removed beforehand, the organic carbon content is measured directly. Applicable to all types of air-dried soil samples.
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The method specified can be applied to all types of soil samples. Different procedures are specified for air-dried soil samples, e.g. samples pretreated according to ISO 11464, and for field-moist soil samples. Its principle is drying soil samples to constant mass at 105 °C and using the difference in mass of an amount of soil before and after the drying procedure to calculate the dry matter and water contents on a mass basis. For the determination of soil water content on a volume basis, refer to ISO 11461.
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The method is based on developing a potential difference between the measuring electrode and the reference electrode, when a fluoride ion-selective electrode comes into contact with an aqueous solution containing fluoride ions. On certain assumptions specified, the method will no longer refer to activities, but to fluoride ion concentration. The method is directly suitable for measuring fluoride concentrations from 0,2 mg/l to 2,0 g/l.
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Gives procedures for drinking waters, surface waters, brines (saline waters), domestic waters and industrial waters. After a preliminary distillation the test sample are analysed according to specific application by direct colorimetric method and by chloroform extraction method.
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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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