ISO/TC 147 - Water quality

This document specifies methods for the determination of five selected estrogens in whole water samples listed in Table 1 (see REF Section_sec_4 \r \h Clause 4 08D0C9EA79F9BACE118C8200AA004BA90B02000000080000000E000000530065006300740069006F006E005F007300650063005F0034000000 ). The methods are based on solid-phase extraction (SPE; disk or cartridge) followed by liquid or gas chromatography-mass spectrometry detection (tandem mass spectrometry or high resolution mass spectrometry). Depending on the sample preparation chosen, the sample preparation can be applicable to the analysis of selected estrogens in drinking water, groundwater and surface water containing suspended particulate matter (SPM) up to 500 mg/l, dissolved organic carbon (DOC) content up to 14 mg/l (whole water samples). The lower application range defined as verified limit of quantification can vary depending on the methods, the sensitivity of the equipment used and the matrix of the sample. The range is 0,006 ng/l to 1 ng/l for 17alpha-ethinylestradiol (EE2) and 0,038 ng/l to 1 ng/l for the other estrogens in drinking water, ground water and surface water. The upper limit of the working range is approximately tens of nanograms per litre. For application that targets the measurements of very low level concentrations (between the lowest LOQ and 0,1 ng/l), every single step of the procedure becomes critical. The methods can be used to determine further estrogens or hormones in other types of water, for example treated wastewater, if accuracy has been tested and verified for each case as well as storage conditions of both samples and reference solutions have been validated.

This document specifies a method for the photometric determination of dissolved chromium(VI) using manual, (e.g. hand photometry), automated static (e.g. discrete analyser system) or automated dynamic [e.g. flow injection analysis (FIA), continuous flow analysis (CFA)] or ion chromatography with post-column reaction (IC-PCR)] techniques. The method described in this document is applicable for other matrices, such as leachates from landfills and raw wastewater, after appropriate method validation.

This document establishes key principles for the investigation of microplastics in drinking water and water with low content of natural suspended solids using a microscopy technique coupled with vibrational spectroscopy. This method is applicable to: — determine the size of microplastics [which range from 1 µm to 5 000 µm], count them and classify them by size range; — identify the chemical composition of microplastics, the main ones (most used in industry and most abundant in the environment) being: polyethylene (PE), polypropylene (PP), polyethylene terephthalate (PET), polycarbonate (PC), polystyrene (PS), polytetrafluoroethylene (PTFE), polyvinyl chloride (PVC), polyamide (PA), polymethyl methacrylate (PMMA) and polyurethane (PU); This method is applicable to water with a low content of organic matter and other suspended matter as defined in ISO 6107 (1 mg/l to 100 mg/l or lower when interfering with the determination), i.e., — ultrapure water; — water intended for human consumption; — raw groundwaters. Given the very low concentrations of microplastics usually present in these waters, special attention needs to be paid to potential sources of contamination during sample preparation. This method is intended to determine and characterize large numbers of particles in the sample in automatic mode. This method can also identify the nature of the other particles that are outside the scope of this document, for example minerals, proteins, cellulose and pigments. This method does not apply to the characterization of substances intentionally added to or adsorbed on the surface of microplastics. This method does not apply to the determination of the geometric shape of microplastics.

This document specifies approaches for the estimation of measurement uncertainty of chemical and physicochemical methods in single laboratories based on validation data and quality control data obtained within the field of water analysis. However, this approach can also be used in many other areas of chemical analysis. NOTE 1 The principles of the estimation of uncertainty specified in this document are consistent with the principles described in ISO/IEC Guide 98-3. In this document, the quantification of measurement uncertainty relies on performance characteristics of a measurement procedure obtained from validation and the results of internal and external quality control. NOTE 2 The approaches specified in this document are mainly based on Nordtest TR 537[ REF Reference_ref_4 \r \h 3 08D0C9EA79F9BACE118C8200AA004BA90B0200000008000000100000005200650066006500720065006E00630065005F007200650066005F0034000000 ], but also QUAM[ REF Reference_ref_5 \r \h 4 08D0C9EA79F9BACE118C8200AA004BA90B0200000008000000100000005200650066006500720065006E00630065005F007200650066005F0035000000 ], and Eurolab TR 1/2007[ REF Reference_ref_3 \r \h 2 08D0C9EA79F9BACE118C8200AA004BA90B0200000008000000100000005200650066006500720065006E00630065005F007200650066005F0033000000 ]. NOTE 3 This document only addresses the evaluation of measurement uncertainty for results obtained from quantitative measurement procedures. The uncertainties associated with results obtained from qualitative procedures are not considered.

This document specifies methods to determine 226Ra by alpha spectrometry in supply water, drinking water, rainwater, surface and ground water, marine water, as well as cooling water, industrial water, domestic, and industrial wastewater after proper sampling, handling and test sample preparation. The detection limit depends on the sample volume, the instrument used, the background count rate, the detection efficiency, the counting time and the chemical yield. The detection limit of the methods described in this document, using currently available alpha spectrometry apparatus, is equal to or lesser than 3 mBq·l−1 (or mBq·kg−1), which is lower than the WHO criteria for safe consumption of drinking water (1 Bq·l−1)[ REF Reference_ref_12 \r \h 4 08D0C9EA79F9BACE118C8200AA004BA90B0200000008000000110000005200650066006500720065006E00630065005F007200650066005F00310032000000 ]. This value can typically be achieved with a counting time of 48 h for a test sample volume of 40 ml. The method described in this document is applicable in the event of an emergency situation. Filtration of the test sample is necessary for the methods described in this document if suspended solids are present. The analysis of 226Ra adsorbed to suspended matter is not covered by this method, because it requires a mineralization step. In this case, the measurement is made on the different phases obtained. The final activity is the sum of all the measured activity concentrations. It is the user’s responsibility to ensure the validity of this test method for the water samples tested.

This document specifies the general requirements for the in vitro amplification of nucleic acid sequences (DNA or RNA). This includes polymerase chain reaction (PCR)-based methods like quantitative PCR, qualitative PCR, reverse transcription-PCR and digital PCR. The minimum requirements laid down in this document are intended to ensure that comparable and reproducible results are obtained in different organizations. It covers quality assurance aspects to be considered when working with PCR-based methods in a laboratory as well as validation and verification. In addition to laboratory PCR-based methods, this document is also applicable to on-site PCR-based methods. This document is applicable to PCR-based methods used for the analysis of microorganisms and viruses in different water matrices, including but not limited to: — drinking water; — groundwater; — pool water; — process water; — surface water; — wastewater. This document is applicable to the detection and quantification of nucleic acids (DNA or RNA) of microorganisms by PCR-based methods in water such as bacteria, yeasts, fungi but also parasites such as Cryptosporidium, Giardia, amoebas and multicellular organisms. In addition, this document is applicable to the detection and quantification of nucleic acids from viruses in water by PCR-based methods. NOTE In the context of this document, viruses are considered to be microorganisms. Clauses in this document can also specifically apply to viruses and not to other types of microorganisms. In these clauses, viruses are mentioned separately.

This document specifies a method for assessing the effects of chemical and aqueous samples on the embryo-larval development of marine bivalves. This method allows the determination of the concentration levels that result in an abnormality in embryo-larval development. This test is suitable for salinity ranges: — between 20 PSU (practical salinity unit) and 40 PSU for mussels, and — between 25 PSU and 35 PSU for oysters. This method in this document applies to: — chemical substances and preparations, — marine and brackish waters, — streams and aqueous effluents (urban, agricultural, industrial effluents, etc.) as long as the salinity is adjusted or dilution is limited so that the aforementioned salinity ranges are respected, — aqueous extracts (pore water, elutriates, eluates and leachates) from sediments and petroleum products, and — samples of contaminated sediment or dredged material (see Annex C).

This document specifies a method for the enumeration of intestinal enterococci in water, including Enterococcus faecalis, Enterococcus faecium, Enterococcus durans, Enterococcus avium, Enterococcus gallinarum, Enterococcus hirae, Enterococcus casselifavus. The method is based on the growth of target organisms in a liquid medium and calculation of the “most probable number” (MPN) of microorganisms by reference to MPN tables or using suitable MPN informatic programs. This method can be applied to drinking water and bathing water (fresh or marine), together with other similar water types including those containing an appreciable amount of suspended matter, and allows the detection of enterococci at 1 colony-forming unit (CFU) per 100 ml with definitive results within (26 ± 2) h in the presence of heterotrophic bacteria in numbers as high as 1 × 106 per 100 ml of sample. For bathing waters, fresh and marine, enterococci are best enumerated when samples are diluted 1:10. The test specified in this document relies upon the detection of intestinal enterococci based upon expression of the enzyme ß-D-glucosidase and provides a confirmed result in 24 h without further testing of positive wells. This document does not apply to bottled waters, for which the method has not been validated and therefore is outside the scope of this document, unless appropriate validation of performance of this method has been undertaken by the laboratory prior to use.

This document specifies the basic methods for sampling suspended microplastics in water (domestic water, freshwater, seawater, treated wastewater and untreated wastewater), for their subsequent characterization. Suspended particles can also include synthetic or semi-synthetic polymeric materials (such as rubber). This document does not cover chemical analysis, biological (ecotoxicological) methods or physical methods, nor the pre-treatment or digestion methods intrinsic to such analyses. This document covers general methodologies: — for grab sampling, sampling using a set of successive filters of different pore sizes (cascade filtration), for water samples with low, medium and high content of suspended solids, and — for net sampling using, for example, manta, plankton or neuston nets.

This document specifies a method to determine radium-226 (226Ra) activity concentration in all types of water by coprecipitation followed by gamma-ray spectrometry (see ISO 20042[7]). The method covers the measurement of soluble 226Ra activity concentrations greater than 0,002 Bq·l−1 using a sample volume of up to 100 l of any water type. For water samples with a volume of less than a volume of 1 l, direct gamma-ray spectrometry can be performed following ISO 10703 but with a higher detection limit. The typical detection limit for samples of 1 l to 5 l is in the range of 0,002 to 0,000 40 Bq·l−1[8]. NOTE This test method can be adapted to determine other naturally occurring isotopes of radium, such as 223Ra, 224Ra and 228Ra, if the respective ingrowth periods are taken into account.

This document specifies methods to determine strontium-90 (90Sr) by inductively coupled plasma mass spectrometry (ICP-MS). The mass concentrations obtained can be converted into activity concentrations. The method described in this document is applicable to test samples of supply water, drinking water, rainwater, surface and ground water, as well as cooling water, industrial water, domestic and industrial wastewater after proper sampling and handling and test sample preparation. The limit of detection depends on the sample volume, the instrument used, the background count rate, the detection efficiency and the chemical yield. In this document, the limit of detection of the method using currently available apparatus and chemical pre-concentration, is approximately 5 Bq·l−1, which is lower than the WHO criteria for safe consumption of drinking water (10 Bq·l−1)[4]. The method described in this document covers the measurement of 90Sr in water at activity concentrations up to 1 000 Bq·l−1. Samples with higher activity concentrations than 1 000 Bq·l−1 can be measured if a dilution is performed. The method described in this document is applicable in the event of an emergency situation. Filtration of the test sample is necessary for the method described in this document. The analysis of 90Sr adsorbed to suspended matter is not covered by this method. The analysis of the insoluble fraction requires a mineralization step that is not covered by this document. In this case, the measurement is made on the different phases obtained. It is the user’s responsibility to ensure the validity of this test method for the water samples tested.

This document specifies a method to determine 93Zr by inductively coupled plasma mass spectrometry (ICP-MS). The mass concentrations obtained can be converted into activity concentrations. The method is applicable to test samples of drinking water, rainwater, surface and ground water, marine water, as well as cooling water, industrial water, domestic, and industrial wastewater after proper sampling and handling, and test sample preparation. The limit of detection depends on the sample volume, the instrument used, the background count rate, the detection efficiency and the chemical yield. In this document, the limit of detection of the method using currently available apparatus is approximately 0,09 Bq·l−1 (or Bq·kg−1), which is lower than the WHO criteria for safe consumption of drinking water (100 Bq·l−1)[4]. The method described in this document covers the measurement of 93Zr in water at activity concentrations between 0,09 Bq·l−1 and 100 Bq·l−1. Samples with higher activity concentrations than 100 Bq·l−1 can be measured if a dilution is performed. The method described in this document is applicable in the event of an emergency. Filtration of the test sample is necessary for the method described in this document. The analysis of 93Zr adsorbed to suspended matter is not covered by this method. The analysis of the insoluble fraction requires a mineralization step that is not covered by this document. In this case, the measurement is made on the different phases obtained. It is the user’s responsibility to ensure the validity of this test method for the water samples tested.

This document specifies a method to determine thorium 232 (232Th) by inductively coupled plasma mass spectrometry (ICP-MS). The mass concentrations obtained can be converted into activity concentrations. The method described in this document is applicable to test samples of drinking water, rainwater, surface and ground water, marine water, as well as cooling water, industrial water, domestic and industrial wastewater after proper sampling and handling and test sample preparation. The limit of detection depends on the sample volume, the instrument used, the background count rate, the detection efficiency and the chemical yield. In this document, the limit of detection of the method using currently available apparatus is approximately 2 mBq·l−1 (or mBq·kg−1), which is lower than the WHO criteria for safe consumption of drinking water (1 Bq·l−1)[4]. The method described in this document covers the measurement of 232Th in water at activity concentrations between 2 mBq·l−1 and 5 Bq·l−1. Samples with higher activity concentrations than 5 Bq·l−1 can be measured if a dilution is performed. The method described in this document is applicable in the event of an emergency situation. Filtration of the test sample is necessary for the method described in this document. The analysis of 232Th adsorbed to suspended matter is not covered by this method. The analysis of the insoluble fraction requires a mineralization step that is not covered by this document. In this case, the measurement is made on the different phases obtained. It is the user’s responsibility to ensure the validity of this test method for the water samples tested.

This document specifies a method to determine 231Pa by inductively coupled plasma mass spectrometry (ICP-MS). The mass concentrations obtained can be converted into activity concentrations. The method described in this document is applicable to test samples of drinking water, rainwater, surface and ground water, marine water, as well as cooling water, industrial water, domestic and industrial wastewater after proper sampling and handling and test sample preparation. The limit of detection depends on the sample volume, the instrument used, the background count rate, the detection efficiency and the chemical yield. In this document, the limit of detection of the method using currently available apparatus is approximately 0,1 Bq·l−1 (or Bq·kg−1), which is the same as the WHO criteria for safe consumption of drinking water (0,1 Bq·l−1)[4]. The method described in this document covers the measurement of 231Pa in water at activity concentrations between 0,1 Bq·l−1 and 100 Bq·l−1. Samples with higher activity concentrations than 100 Bq·l−1 can be measured if a dilution is performed. The method described in this document is applicable in the event of an emergency. Filtration of the test sample is necessary for the method described in this document. The analysis of 231Pa adsorbed to suspended matter is not covered by this method. The analysis of the insoluble fraction requires a mineralization step that is not covered by this document. In this case, the measurement is made on the different phases obtained. It is the user’s responsibility to ensure the validity of this test method for the water samples tested.

This document specifies a method to determine the total organic carbon (TOC), dissolved organic carbon (DOC), total bound nitrogen (TNb) and dissolved bound nitrogen (DNb) in the form of free ammonia, ammonium, nitrite, nitrate and organic compounds capable of conversion to nitrogen oxides. Cyanide, cyanate and particles of elemental carbon (soot), when present in the sample, can be determined together with the organic carbon. Dissolved nitrogen gas (N2) is not determined. NOTE Generally, the method can be applied for the determination of total carbon (TC) and total inorganic carbon (TIC) – see Annex A. The method is applicable to water samples (e.g. drinking water, raw water, ground water, surface water, sea water, waste water, leachates). This document is applicable to determination of TOC and DOC ≥1 mg/l and TNb and DNb ≥1 mg/l. The upper working range is restricted by instrument-dependent conditions (e.g. injection volume). Higher concentrations can be determined after appropriate dilution of the sample. The determination of concentrations For samples containing volatile organic compounds (e.g. industrial waste water), the application of the difference method can be considered – see Annex A. The procedure is carried out by automated analysis.

This document provides the guidelines, minimum requirements and performance characteristics intended to guarantee that manufactured systems intended for on-site/field use (i.e. outside the laboratory) provide reliable and reproducible results. This document specifies the requirements for technologies that enable on-site detection and quantification of Legionella spp. and L. pneumophila using a quantitative polymerase chain reaction assay (qPCR). It specifies general methodological requirements, performance evaluation requirements and quality control requirements. This document is intended to be used by manufacturers of these technologies so that they produce detection systems that end users can operate safely and effectively. End users will be guided by this document to adhere to manufacturer’s instructions, to ensure user competency and to perform the necessary controls. Technical details specified in this document are given for information only. Any other technical solutions complying with the performance requirements are suitable. NOTE For validation and performance requirements, see Clause 9. This document is intended to be applied in the bacteriological investigation of all types of water (hot or cold water, cooling tower water, etc.), unless the nature and/or content of suspended matter and/or background microorganisms interfere with the determination. This interference can result in an adverse effect on both the detection limit and the quantification limit. The results are expressed as the number of genome units of Legionella spp. and/or L. pneumophila per millilitre (or litre) of sample. Although the method described in this document is applicable to all types of water, some additives, such as chemicals used for water treatment, can interfere with and/or affect the sensitivity of the method. The qPCR methods do not give any information about the physiological state of the Legionella. However, there are on-site qPCR methodologies which are able to distinguish intact bacteria from free DNA.

This document specifies the general requirements for sampling, preservation, handling, transport and storage of all water samples for physicochemical, chemical, hydrobiological and microbiological analyses and determination of radiochemical analytes and activities. Guidance on the validation of storage times of water samples is provided in ISO/TS 5667-25. This document is not applicable to water samples intended for ecotoxicological assays, biological assays (which is specified in ISO 5667-16), passive sampling (which is specified in ISO 5667-23) and microplastics (which is specified in ISO 5667-27). This document is particularly appropriate when samples cannot be analysed on site and have to be transported to a laboratory for analysis.

This document specifies the principles of inductively coupled plasma mass spectrometry (ICP-MS) and provides general requirements for the use of this technique to determine elements in water, digests of sludges and sediments (e.g. digests of water as described in ISO 15587-1 or ISO 15587-2). Generally, the measurement is carried out in water, but gases, vapours or fine particulate matter can be introduced too. This document applies to the use of ICP-MS for aqueous solution analysis. The ultimate determination of the elements is described in a separate International Standard for each series of elements and matrix. The individual clauses of this document refer the user to these guidelines for the basic principles of the method and the configuration of the instrument.

This document specifies a method for the determination of hexavalent chromium [Cr(VI)] and trivalent chromium [Cr(III)] in water by liquid chromatography with inductively coupled plasma mass spectrometry (LC-ICP-MS) after chelating pretreatment. This method is applicable to the determination of Cr(VI) and Cr(III) dissolved in wastewater, surface water, groundwater, or drinking water from 0,20 μg/l to 500 μg/l of each compound as chromium (Cr) mass. Samples containing Cr at concentrations higher than the working range can be analysed following appropriate dilution of the sample.

This document specifies methods to determine 226Ra concentration by inductively coupled plasma mass spectrometry (ICP-MS). The mass concentrations obtained can be converted into activity concentrations. The method is applicable to test samples of drinking water, rainwater, surface and ground water, after proper sampling and handling, and test sample preparation. The detection limit depends on the sample volume, the instrument used, the background count rate, the detection efficiency, the counting time and the chemical yield. The detection limit of the method described in this document, using currently available equipment, is approximately 10 mBq·l-1, which is better than the WHO criteria for safe consumption of drinking water (1 Bq·l-1). This method covers the measurement of 226Ra in water at activity concentrations between 0,001 Bq·l−1 and 100 Bq·l−1. Samples with concentrations higher than 1 Bq·l−1 can be measured if a dilution is performed. The method described in this document is applicable in the event of an emergency situation. In this method, filtration of the test sample is necessary. The analysis of 226Ra adsorbed to suspended matter is not covered by this method. The analysis of the insoluble fraction requires a mineralization step that is not covered by this document. In this case, the measurement is made on the different phases obtained. It is the user’s responsibility to ensure the validity of this test method for the water samples tested.

This document specifies a method for the simultaneous measurement of 3H and 14C in water samples by liquid scintillation counting of a source obtained by mixing the water sample with a hydrophilic scintillation cocktail. The method presented in this document is considered a screening method because of the potential presence of interfering radionuclides in the test sample. However, if the sample is known to be free of interfering radionuclides then 3H and 14C can be measured quantitatively. The method can be used for any type of environmental study or monitoring. This method is applicable to test samples of supply/drinking water, rainwater, surface and ground water, marine water, as well as cooling water, industrial water, domestic, and industrial wastewater having an activity concentration ranging from 5 Bq∙l-1 to 106 Bq∙l-1 (upper limit of the liquid scintillation counters for direct counting). For higher activity concentrations, the sample can be diluted to obtain a test sample within this range.

This document specifies a test method to determine the activity concentration of 227Ac in all types of waters by alpha spectrometry. The test method is applicable to test samples of supply/drinking water, rainwater, surface and ground water, marine water, as well as cooling water, industrial water, domestic, and industrial wastewater after proper sampling and handling and test sample preparation (see ISO 5667-1, ISO 5667-3, ISO 5667-10). Filtration of the test sample is necessary. The detection limit depends on the sample volume, the instrument used, the background count rate, the detection efficiency, the counting time, the chemical yield, and the progeny ingrowth. The method described in this document, using currently available alpha spectrometry apparatus, has a detection limit of approximately 0,03 Bq·l−1, when directly measuring the alpha peak of 227Ac. This detection limit is lower than the WHO criteria for safe consumption of drinking water for any actinide alpha emitter (0,1 Bq·l−1).[4] This value can be achieved with a counting time of 48 h for a sample volume of 1 l. Only a small fraction of 227Ac decays through alpha emissions (~1,42 %). An option to lower the detection limit of the method is to wait, let the progenies of 227Ac grow in, and measure an alpha progeny peak of 227Ac (e.g. 215Po). This is a longer technique, but a lower detection limit of approximately 0,000 2 Bq·l−1 can be obtained by re-counting the sample approximately 90 days after purification. The sample can be re-counted before 90 days, but with a higher detection limit. The test method(s) described in this document can be used during planned, existing and emergency exposure situations as well as for wastewaters and liquid effluents with specific modifications that can increase the overall uncertainty, detection limit and threshold. For an emergency situation, it is preferable to reduce the counting time rather than the sample volume. The analysis of 227Ac adsorbed to suspended matter is not covered by this document.

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).

This document specifies the method and the conditions for the determination of 232Th activity concentration in samples of environmental water (including sea waters) and waste waters before release to the environment using alpha spectrometry and 229Th as a recovery tracer. A chemical separation allows to separate and purify thorium from a test portion of the sample. The general principles outlined in this document can be applied for the analysis of other alpha-emitting thorium isotopes such as 228Th and 230Th in aqueous samples.

This document describes a test method for the determination of radon-222 (222Rn) activity concentration in non-saline waters by extraction and liquid scintillation counting. The 222Rn activity concentrations, which can be measured by this test method utilizing currently available instruments, are above 0,5 Bq·l−1 which is the typical detection limit for a 10 ml test sample and a measuring time of 1 h. It is the responsibility of the laboratory to ensure the validity of this test method for water samples of untested matrices. Annex A gives indication on the necessary counting conditions to meet the required detection limits for drinking water monitoring.

This document specifies requirements and recommendations for the design and execution of an interlaboratory comparison for validation of new standardized analytical methods in the field of water analysis, e.g. the number of participating laboratories and time schedules. This document is based on ISO 5725-1 and ISO 5725-2. NOTE The scope of other standards in the field of interlaboratory comparison, such as ISO/IEC 17043[3] and ISO 13528[1], is proficiency testing of analytical laboratories and not interlaboratory comparison for the validation of analytical methods.

This document specifies a test method for measuring actinides (238Pu, 239+240Pu, 241Am, 242Cm, 243+244Cm and 237Np) in water samples by alpha spectrometry following a chemical separation. This method can be used for any type of environmental study or monitoring after appropriate sampling and handling, and test sample preparation. The detection limit of the test method is 5 × 10−3 Bq·l-1 to 5 × 10−4 Bq·l-1 for a volume of test portion between 0,1 l to 5 l with a counting time of two to ten days. This is lower than the WHO criteria for safe consumption of drinking water (1 Bq·l-1 or 10 Bq·l-1 depending on radionuclide).[4] The method described in this document is applicable in the event of an emergency situation.

This document specifies a method for the determination of the inhibition of root re-growth in duckweeds (Lemna minor) by substances and mixtures contained in water or waste water. This method applies to environmental water samples including treated municipal wastewater and industrial effluents.

This document specifies methods and principles for detection of selected congeners of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated biphenyls (PCBs) in water and wastewater using a flow immunosensor. The flow immunosensor utilizes antibodies specific to 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) and 3,3’,4,4’,5-pentachlorobiphenyl (3,3’,4,4’,5-PeCB), which have the highest toxic equivalent factor (TEF) value among the congeners of each of PCDDs and PCBs. The method is applicable to timely monitoring of selected congeners of 2,3,7,8-TCDD and 3,3’,4,4’,5-PeCB in water and wastewater to prioritize those for subsequent confirmatory determination. This document specifies practical methods and procedures for sampling, extraction, clean-up, measurement in a flow immunosensor, data processing and validation of measurement results. The combined use of automated instruments for extraction, clean-up, and flow immunosensing can reduce time-consumption and labour-intensity, while providing reproducible precise data. This method can provide the lower limit of quantification (LOQ) for 2,3,7,8-TCDD and 3,3’,4,4’,5-PeCB of 28 pg/l and 152 pg/l, respectively at 20 % or less of coefficient variation (CV) depending on sampling, extraction, clean-up and measurement conditions.

This document sets out the general principles for, and provides guidance on, the design of sampling programmes and sampling techniques for all aspects of sampling of water (including waste waters, sludges, effluents, suspended solids and sediments). This document does not include detailed instructions for specific sampling situations, which are covered in various other parts of the ISO 5667 series and in ISO 19458.

This document specifies a method for the determination of nitrate as NO3-N in water of various origin such as natural water (including groundwater, surface water and bathing water), drinking water and wastewater, in a measuring range of concentration between 0,20 mg/l and 30 mg/l of NO3-N using the small-scale sealed tube method. Different measuring ranges of small-scale sealed tube methods can be required. The measuring ranges can vary depending on the type of the small-scale sealed tube method of different manufacturers. It is up to the user to choose the small-scale sealed tube test with the appropriate application range or to adapt samples with concentrations exceeding the measuring range of a test by preliminary dilution. NOTE 1 The results of a small-scale sealed tube test are most precise in the middle of the application range of the test. Manufacturers' small-scale sealed tube methods are based on chromotropic colour reaction, depending on the typical operating procedure of the small-scale sealed tube used, see Clause 9. NOTE 2 Laws, regulations or standards can require that the data is expressed as NO3 after conversion with the stoichiometric conversion factor 4,426 81 in Clause 11. NOTE 3 In the habitual language, use of sewage treatment and on the displays of automated sealed-tube test devices, NO3 without indication of the negative charge has become the common notation for the parameter nitrate and especially for the parameter nitrate-N. This notation is adopted in this document even though not being quite correct chemical nomenclature.

This document specifies a method for the determination of total bound nitrogen (ST-TNb) in water of various origins: groundwater, surface water and wastewater, in a measuring range of concentration generally between 0,5 mg/l and 150 mg/l of ST-TNb using the small-scale sealed tube method. Different measuring ranges of small-scale sealed tube methods can be required. The measuring ranges can vary depending on the type of small-scale sealed tube method of different manufacturers. It is up to the user to choose the small-scale sealed tube test with the appropriate application range or to adapt samples with concentrations exceeding the measuring range of a test by preliminary dilution. NOTE The results of a small-scale sealed tube test are most precise in the middle of the application range of the test. All small-scale sealed tube methods are based on a heated alkaline potassium persulfate oxidation in a heating block at 100 °C and different digestion times are applicable. Chromotropic colour reaction is applied, depending on the typical operating procedure of the small-scale sealed tube used, see Clause 9.

This document specifies a method for the determination of nitrate as NO3-N in water of various origin such as natural water (including groundwater, surface water and bathing water), drinking water and wastewater, in a measuring range of concentration between 0,10 mg/l and 225 mg/l of N03-N using the small-scale sealed tube method. Different measuring ranges of small-scale sealed tube methods can be required. The measuring ranges can vary depending on the type of the small-scale sealed tube method of different manufacturers. It is up to the user to choose the small-scale sealed tube test with the appropriate application range or to adapt samples with concentrations exceeding the measuring range of a test by preliminary dilution. NOTE 1 The results of a sealed-tube test are most precise in the middle of the application range of the test. Manufacturers' small-scale sealed tube methods are based on dimethylphenol colour reaction depending on the typical operating procedure of the small-scale sealed tube used, see Clause 9. NOTE 2 Laws, regulations or standards can require that the data is expressed as NO3- after conversion with the stoichiometric conversion factor 4,426 81 in Clause 11. NOTE 3 In the habitual language, use of sewage treatment and on the displays of automated sealed-tube test devices, NO3 without indication of the negative charge has become the common notation for the parameter nitrate and especially for the parameter nitrate-N. This notation is adopted in this document even though not being quite correct chemical nomenclature.

This document specifies a method for the determination of total bound nitrogen (ST-TNb) in water of various origins: groundwater, surface water, and wastewater, in a measuring range of concentration generally between 0,5 mg/l and 220 mg/l of ST-TNb using the small-scale sealed tube method. Different measuring ranges of small-scale sealed tube methods can be required. The measuring ranges can vary depending on the type of small-scale sealed tube method of different manufacturers. It is up to the user to choose the small-scale sealed tube with the appropriate application range or to adapt samples with concentrations exceeding the measuring range of a test by preliminary dilution. NOTE The results of a small-scale sealed tube are most precise in the middle of the application range of the test. All small-scale sealed tube methods are based on a heated alkaline potassium persulfate oxidation in a heating block. Different digestion temperatures, 100 °C or 120 °C or 170 °C, and different digestion times are applicable. Dimethylphenol colour reactions are applied, depending on the typical operating procedure of the small-scale sealed tube used, see Clause 9.

This document specifies a method for the determination of ammonium nitrogen (NH4-N) in drinking water, groundwater, surface water, wastewater, bathing water and mineral water using the small-scale sealed tube method. The result can be expressed as NH4 or NH4-N or NH3 or NH3-N. NOTE 1 In the habitual language use of sewage treatment and on the displays of automated sealed-tube test photometers or spectrophotometers, NH4 without indication of the positive charge has become the common notation for the parameter ammonium. This notation is adopted in this document even though not being quite correct chemical nomenclature. This method is applicable to (NH4-N) concentration ranges from 0,01 mg/l to 1 800 mg/l of NH4-N. The measuring ranges of concentration can vary depending on the type of small-scale sealed tube method of different manufacturers. Concentrations even slightly higher than the upper limit indicated in the manufacturers manual relating to the small-scale sealed tube method used, cannot be reported as accurate results. It is up to the user to choose the small-scale sealed tube test with the appropriate application range or to adapt samples with concentrations exceeding the measuring range of a test by preliminary dilution. NOTE 2 The results of a small-scale sealed tube are most precise in the middle of the application range of the test. All manufacturers' methods are based on the Berthelot reaction and its modifications to develop indophenol blue colour. Reagents mixtures can differ slightly based on manufacturers small-scale sealed tube method, see Clause 9. This method is applicable to non-preserved samples by using small-scale sealed tubes for the determination of drinking water, groundwater, surface water, wastewater and to preserved samples. The method is applicable to samples with suspended materials if these materials are removable by filtration.

This document specifies the requirements for the performance testing of membrane filters used for the retention followed by direct enumeration of microorganisms by culture methods. This document is applicable to membrane filters which are used for retention followed by direct enumeration of specific microorganisms on solid media or on other devices containing media, like absorbent pads[19]. This document is not applicable for membrane filters used for concentration and elution or for qualitative methods. These tests are applicable to the membrane filters intended for the microbiological analysis of different types of water, such as: — drinking water, bottled water and other types of water with expected low numbers of microorganisms; — water with expected higher numbers of microorganisms, for example, surface water and process water. These tests are intended to demonstrate the suitability of the whole system (membrane filter together with the culture medium including the filtration step) required for the specific tests described in References [3], [6], [8], [10], [12] and [13]. This document applies to: — manufacturers producing membrane filters; — microbiological laboratories using membrane filters for their own testing or providing these to other end users.

This document specifies the determination of radium-226 (226Ra) activity concentration in non-saline water samples by extraction of its daughter radon-222 (222Rn) and its measurement using liquid scintillation analysis. The test method described in this document, using currently available scintillation counters, has a detection limit of approximately 50 mBq·l−1. This method is not applicable to the measurement of other radium isotopes.

This document specifies how to collect discrete seawater samples, from a Niskin or other water sampler, that are suitable for the analysis of the four measurable inorganic carbon parameters: total dissolved inorganic carbon, total alkalinity, pH and CO2 fugacity.

This document specifies a test method to determine radium-226 (226Ra) activity concentration in all types of water by emanometry. The test method specified is suitable for the determination of the soluble, suspended and total 226Ra activity concentration in all types of water with soluble 226Ra activity concentrations greater than 0,02 Bq l−1. The decay chains of 238U and 232Th are given in Annex A. Figure A.1 shows the 238U and its decay chain.

This document specifies the determination of nickel-59 and nickel-63 (59Ni and 63Ni) activity concentration in samples of all types of water using liquid scintillation counting (LSC). Using currently available liquid scintillation counters, this test method can measure 59Ni activity concentrations of 50 mBq·l−1 and 63Ni activity concentrations of 20 mBq·l−1 with a counting time of 200 min and a sample volume of 1,5 l. NOTE These performance indicators are wholly dependent on the measurement regimes in individual laboratories; in particular, the detection limits for 59Ni are entirely dependent on the levels of 63Ni that can be present. The range of application depends on the amount of dissolved material in the water and on the performance characteristics of the measurement equipment (background count rate and detection efficiency). It is the laboratory’s responsibility to ensure the suitability of this test method for the water samples tested.

This document specifies the determination of nickel-59 and nickel-63 (59Ni and 63Ni) activity concentration in samples of all types of water using inductively coupled plasma mass spectrometry (ICP-MS). Using currently available ICP-MS, this test method can measure 59Ni activity concentrations of 300 mBq⋅l−1 and 63Ni activity concentrations of 200 Bq⋅l−1. These values can be achieved with a sample volume of 1,0 l. Higher activity concentrations can be measured by either diluting the sample or using smaller sample aliquots or both. NOTE These performance indicators are wholly dependent on the measurement regimes in individual laboratories; in particular, the detection limit is influenced by amount of stable nickel present. The range of application depends on the amount of dissolved material in the water and on the performance characteristics of the measurement equipment (background count rate and counting efficiency). It is the laboratory’s responsibility to ensure the suitability of this test method for the water samples tested.

This document specifies a method for the determination of the dissolved anions chlorate, chloride and chlorite in water with low contamination (e.g. drinking water, raw water or swimming pool water). The diversity of the appropriate and suitable assemblies and the procedural steps depending on them permit a general description only. For further information on the analytical technique, see Bibliography.

The purpose of this document is to describe test plans and different operating methodologies of these test plans to define and verify the acceptable length of stability of a substance in a sample under specified conditions of preservation (temperature, matrix, light, addition of a stabilizer, where appropriate, type of preservation etc.) before starting analytical protocols (chemicals and physico-chemicals analysis). Biological and microbiological methods are excluded. It is necessary to have an analytical method with performances that have already been characterized (repeatability, intermediate precision, trueness, accuracy and uncertainty) in order to perform the stability study and implement its test plans.

This document specifies the derivation of biological equivalence (BEQ) concentrations for results of in vitro bioassays which are based on measuring effects on a biological process such as enzyme induction or cellular growth. The concept described here can be used for any biological assay after the proof of its applicability. To derive BEQ concentrations, the effect on a biological process caused by a sample – i.e. the activity of the sample – is expressed in terms of a concentration of a reference compound which results in an equivalent effect on the process. The term "sample" used in this document addresses environmental samples as well as defined mixtures and pure compounds used as test item in a bioassay. BEQ concentrations can be derived for environmental water samples, extracts of environmental water samples including tap water or solutions of pure chemicals or mixtures of chemicals.

This document specifies various calibration strategies for physicochemical and chemical analytical methods and specifies the calculation of analytical results. It defines the general context for linear calibration so that individual standards dealing with analytical methods for the examination of water quality can make reference to it.

This document specifies conditions for the determination of 90Sr and 89Sr activity concentration in samples of environmental water using liquid scintillation counting (LSC) or proportional counting (PC). The method is applicable to test samples of drinking water, rainwater, surface and ground water, marine water, as well as cooling water, industrial water, domestic, and industrial wastewater after proper sampling and handling, and test sample preparation. Filtration of the test sample and a chemical separation are required to separate and purify strontium from a test portion of the sample. The detection limit depends on the sample volume, the instrument used, the sample count time, the background count rate, the detection efficiency and the chemical yield. The method described in this document, using currently available LSC counters, has a detection limit of approximately 10 mBq l−1 and 2 mBq l−1 for 89Sr and 90Sr, respectively, which is lower than the WHO criteria for safe consumption of drinking water (100 Bq·l−1 for 89Sr and 10 Bq·l−1 for 90Sr)[3]. These values can be achieved with a counting time of 1 000 min for a sample volume of 2 l. The methods described in this document are applicable in the event of an emergency situation. When fallout occurs following a nuclear accident, the contribution of 89Sr to the total amount of radioactive strontium is not negligible. This document provides test methods to determine the activity concentration of 90Sr in presence of 89Sr. The analysis of 90Sr and 89Sr adsorbed to suspended matter is not covered by this method. It is the user’s responsibility to ensure the validity of this test method selected for the water samples tested.

This document specifies a method for the measurement of 210Pb in all types of waters by liquid scintillation counting (LSC). The method is applicable to test samples of supply/drinking water, rainwater, surface and ground water, as well as cooling water, industrial water, domestic, and industrial wastewater after proper sampling and handling, and test sample preparation. Filtration of the test sample is necessary. Lead‑210 activity concentration in the environment can vary and usually ranges from 2 mBq l-1 to 300 mBq l-1 [27][28]. Using currently available liquid scintillation counters, the limit of detection of this method for 210Pb is generally of the order of 20 mBq l-1 to 50 mBq l-1, which is lower than the WHO criteria for safe consumption of drinking water (100 mBq l−1).[4][6] These values can be achieved with a counting time between 180 min and 720 min for a sample volume from 0,5 l to 1,5 l. Higher activity concentrations can be measured by either diluting the sample or using smaller sample aliquots or both. The method presented in this document is not intended for the determination of an ultra-trace amount of 210Pb. The range of application depends on the amount of dissolved material in the water and on the performance characteristics of the measurement equipment (background count rate and counting efficiency). The method described in this document is applicable to an emergency situation. The analysis of Pb adsorbed to suspended matter is not covered by this method. It is the user’s responsibility to ensure the validity of this test method for the water samples tested.

This document specifies a method for the quantification of twelve microcystin variants (microcystin-LR, -LA, -YR, -RR, -LY, -WR, -HtyR, -HilR, -LW, -LF, [Dha7]-microcystin-LR, and [Dha7]-microcystin-RR) in drinking water and freshwater samples between 0,05 µg/l to 1,6 µg/l. The method can be used to determine further microcystins, provided that analytical conditions for chromatography and mass spectrometric detection has been tested and validated for each microcystin. Samples are analysed by LC-MS/MS using internal standard calibration. This method is performance based. The laboratory is permitted to modify the method, e.g. increasing direct flow injection volume for low interference samples or diluting the samples to increase the upper working range limit, provided that all performance criteria in this method are met. Detection of microcystins by high resolution mass spectrometry (HRMS) as an alternative for tandem mass spectrometry (MS/MS) is described in Annex A. An alternative automated sample preparation method based on on-line solid phase extraction coupled to liquid chromatography is described in Annex B. When instrumental sensitivity is not sufficient to reach the method detection limits by direct flow injection, a solid phase extraction clean-up and concentration step is described in Annex C.

This document specifies a method for the physical pre-treatment and conditioning of water samples and the determination of the activity concentration of various radionuclides emitting gamma-rays with energies between 40 keV and 2 MeV, by gamma‑ray spectrometry according to the generic test method described in ISO 20042. The method is applicable to test samples of drinking water, rainwater, surface and ground water as well as cooling water, industrial water, domestic and industrial wastewater after proper sampling, sample handling, and test sample preparation (filtration when necessary and taking into account the amount of dissolved material in the water). This method is only applicable to homogeneous samples or samples which are homogeneous via timely filtration. The lowest limit that can be measured without concentration of the sample or by using only passive shield of the detection system is about 5·10-2 Bq/l for e.g. 137Cs.1 The upper limit of the activity corresponds to a dead time of 10 %. Higher dead times may be used but evidence of the accuracy of the dead-time correction is required. Depending on different factors, such as the energy of the gamma-rays, the emission probability per nuclear disintegration, the size and geometry of the sample and the detector, the shielding, the counting time and other experimental parameters, the sample may require to be concentrated by evaporation if activities below 5·10-2 Bq/l need to be measured. However, volatile radionuclides (e.g. radon and radioiodine) can be lost during the source preparation. This method is suitable for application in emergency situations. 1The sample geometry: 3l Marinelli beaker; detector: GE HP N relative efficiency 55 % ; counting time: 18h.

This document defines terms used in certain fields of water quality characterization.