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5.1 This guide provides a protocol for detecting, characterizing, and quantifying nucleic acids (that is, DNA) of living and recently dead microorganisms in fuels and fuel-associated waters by means of a culture independent qPCR procedure. Microbial contamination is inferred when elevated DNA levels are detected in comparison to the expected background DNA level of a clean fuel and fuel system.5.2 A sequence of protocol steps is required for successful qPCR testing.5.2.1 Quantitative detection of microorganisms depends on the DNA-extraction protocol and selection of appropriate oligonucleotide primers.5.2.2 The preferred DNA extraction protocol depends on the type of microorganism present in the sample and potential impurities that could interfere with the subsequent qPCR reaction.5.2.3 Primers vary in their specificity. Some 16S and 18S RNA gene regions present in the DNA of prokaryotic and eukaryotic microorganisms appear to have been conserved throughout evolution and thus provide a reliable and repeatable target for gene amplification and detection. Amplicons targeting these conserved nucleotide sequences are useful for quantifying total population densities. Other target DNA regions are specific to a metabolic class (for example, sulfate reducing bacteria) or individual taxon (for example, the bacterial species Pseudomonas aeruginosa). Primers targeting these unique nucleotide sequences are useful for detecting and quantifying specific microbes or groups of microbes known to be associated with biodeterioration.5.3 Just as the quantification of microorganisms using microbial growth media employs standardized formulations of growth conditions enabling the meaningful comparison of data from different laboratories (Practice D6974), this guide seeks to provide standardization to detect, characterize, and quantify nucleic acids associated with living and recently dead microorganisms in fuel-associated samples using qPCR.NOTE 3: Many primers, and primer and probe combinations that are not covered in this guide may be used to perform qPCR. This guide does not attempt to cover all of the possible qPCR assays and does not suggest nor imply that the qPCR assays (that is, combinations of primers and probes, and reaction conditions) discussed here are better suited for qPCR than other qPCR assays not presented here. Additional, primers, primers and probes combination, and qPCR assay conditions may be added in the future to this guide as they become available to the ASTM scientific community. Guide D6469 reviews the types of damage that uncontrolled microbial growth in fuels and fuel systems can cause.5.4 Culture-based microbiological tests depend on the ability of microbes to proliferate in liquid, solid or semisolid nutrient media, in order for microbes in a sample to be detected.5.5 There is general consensus among microbiologists that only a fraction of the microbes believed to be present in the environment have been cultured successfully.5.6 Since the mid-1990s, genetic test methods that do not rely on cultivation have been increasingly favored for the detection and quantification of microorganisms in environmental samples.5.7 qPCR is a quantitative, culture-independent method that is currently used in the medical, food, and cosmetic industries for the detection and quantification of microorganisms.5.8 Since the early 2000s, qPCR methodology has evolved and is now frequently used to quantify microorganisms in fuel-associated samples, but there is currently no standardized methodology for employing qPCR for this application (1-6).3 The purpose of this guide is to provide guidance and standardization for genetic testing of samples using qPCR to quantify total microbial populations present in fuel-associated samples.5.9 Although this guide focuses on describing recommended protocols for the quantification of total microorganisms present in fuel-associated samples using qPCR, the procedures described here can also be applied to the standardization of qPCR assays for other genetic targets and environmental matrices.5.10 Genetic techniques have great flexibility so that it is possible to design a nearly infinite number of methods to detect and quantify each and every gene. Because of this flexibility of genetic techniques, it is important to provide a standard protocol for qPCR so that data generated by different laboratories can be compared.5.11 This guide provides recommendations for primers sequences and experimental methodology for qPCR assays for the quantification of total microorganisms present in fuel-associated samples.1.1 This guide covers procedures for using quantitative polymerase chain reaction (qPCR), a genomic tool, to detect, characterize and quantify nucleic acids associated with microbial DNA present in liquid fuels and fuel-associated water samples.1.1.1 Water samples that may be used in testing include, but are not limited to, water associated with crude oil or liquid fuels in storage tanks, fuel tanks, or pipelines.1.1.2 While the intent of this guide is to focus on the analysis of fuel-associated samples, the procedures described here are also relevant to the analysis of water used in hydrotesting of pipes and equipment, water injected into geological formations to maintain pressure and/or facilitate the recovery of hydrocarbons in oil and gas recovery, water co-produced during the production of oil and gas, water in fire protection sprinkler systems, potable water, industrial process water, and wastewater.1.1.3 To test a fuel sample, the live and recently dead microorganisms must be separated from the fuel phase which can include any DNA fragments by using one of various methods such as filtration or any other microbial capturing methods.1.1.4 Some of the protocol steps are universally required and are indicated by the use of the word must. Other protocol steps are testing-objective dependent. At those process steps, options are offered and the basis for choosing among them are explained.1.2 The guide describes the application of quantitative polymerase chain reaction (qPCR) technology to determine total bioburden or total microbial population present in fuel-associated samples using universal primers that allow for the quantification of 16S and 18S ribosomal RNA genes that are present in all prokaryotes (that is, bacteria and archaea) and eucaryotes (that is, mold and yeast collectively termed fungi), respectively.1.3 This guide describes laboratory protocols. As described in Practice D7464, the qualitative and quantitative relationship between the laboratory results and actual microbial communities in the systems from which samples are collected is affected by the time delay and handling conditions between the time of sampling and time that testing is initiated.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard with the exception of the concept unit of gene copies/mL (that is, 16S or 18S gene copies/mL) to indicate the starting concentration of microbial DNA for the intended microbial targets (that is, bacteria, archaea, fungi).1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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3.1 General: 3.1.1 All testing shall define fender performance under velocities that decrease linearly or that are proportional to the square root of percent of remaining rated energy.3.1.2 Rated performance data (RPD) and manufacturers' published performance curves or tables, or both, shall be based on: (1) initial deflection (berthing) velocity of 0.15 m/s and decreasing to no more than 0.005 m/s at test end, (2) testing of fully broken-in fenders (break-in testing is not required for pneumatic fenders), (3) testing of fenders stabilized at 23 ± 5°C (excluding pneumatic fenders; see 6.3), (4) testing of fenders at 0° angle of approach, and (5) deflection (berthing) frequency of not less than 1 h (use a minimum 5-min deflection frequency for pneumatic fenders.).3.1.3 Catalogues shall also include nominal performance tolerances as well as data and methodology to adjust performance curves or tables or both for application parameters different from RPD conditions. Adjustment factors shall be provided for the following variables: (1) other initial velocities: 0.05, 0.10, 0.20, 0.25, and 0.30 m/s; (2) other temperatures: +50, +40, +30, +10, 0, −10, −20, −30; and (3) other contact angles: 3, 5, 8, 10, 15°. In addition, RPD shall contain a cautionary statement that published data do not necessarily apply to constant-load and cyclic-loading conditions. In such cases, designers are to contact fender manufacturers for design assistance.3.1.4 Adjustment factors for velocity and temperature shall be provided for every catalogue compound or other energy absorbing material offered by each manufacturer.3.2 Fender Testing—Performance testing to establish RPD must use either one of two methods:3.2.1 Method A—Deflection of full-size fenders at velocities inversely proportional to the percent of rated deflection or directly proportional to the square root of percent of remaining rated energy. Test parameters shall be as defined for published RPD. RPD tests shall start at 0.15 m/s. Tests to establish adjustment factors for initial berthing velocities other than 0.15 m/s shall start at those other initial velocities.3.2.2 Method B—Deflection of full size fenders at constant velocity with performance adjusted by velocity factors developed from model tests. Velocity factors shall be the ratio of performance test results of models under the following conditions: (1) a constant strain rate similar to the strain rate of the full-size fender at its test speed, and (2) decreasing speed deflection with initial strain rate similar to that of the full-size fender under RPD deflection conditions.3.2.3 The RPD for pneumatic fenders shall be determined using either Method A or Method B with miniature-size fenders; in which case, the compression performance of air shall be directly extrapolated from the test data of reduced scale models.1.1 This test method covers the recommended procedures for quantitative testing, reporting, and verifying the energy absorption and reaction force of marine fenders. Marine fenders are available in a variety of basic types with several variations of each type and multiple sizes and stiffnesses for each variation. Depending on the particular design, marine fenders may also include integral components of steel, composites, plastics, or other materials. All variations shall be performance tested and reported according to this test method.1.2 There are three performance variables: berthing energy, reaction, and deflection. There are two methods used to develop rated performance data (RPD) and published performance curves for the three performance variables.1.3 The primary focus is on fenders used in berthside and ship-to-ship applications for marine vessels. This testing protocol does not address small fendering “bumpers” used in pleasure boat marinas, mounted to hulls of work boats, or used in similar applications; it does not include durability testing. Its primary purpose is to ensure that engineering data reported in manufacturers' catalogues are based upon common testing methods.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Refer to Practice E261 for a general discussion of the determination of fast-neutron fluence rate with fission detectors.5.2 238U is available as metal foil, wire, or oxide powder (see Guide E844). It is usually encapsulated in a suitable container to prevent loss of, and contamination by, the 238U and its fission products.5.3 One or more fission products can be assayed. Pertinent data for relevant fission products are given in Table 1 and Table 2.(A) The lightface numbers in parentheses are the magnitude of plus or minus uncertainties in the last digit(s) listed.(B) With 137mBa (2.552 min) in equilibrium.(C) The recommended half-life and gamma emission probabilities have been taken from the Reference (3) data that was recommended at the time that the recommended fission yields were set.(D) Probability of daughter 140La decay.(E) This is the activity ratio of 140La/140Ba after reached transient equilibrium (t ≥ 19 days).(A) The JEFF-3.1/3.1.1 radioactive decay data and fission yields sub-libraries, JEFF Report 20, OECD 2009, Nuclear Energy Agency (5).(B) All yield data given as a %; RC represents a cumulative yield; RI represents an independent yield.5.3.1 137Cs-137mBa is chosen frequently for long irradiations. Radioactive products 134Cs and 136Cs may be present, which can interfere with the counting of the 0.662 MeV  137Cs-137mBa gamma rays (see Test Method E320).5.3.2 140Ba-140La is chosen frequently for short irradiations (see Test Method E393).5.3.3 95Zr can be counted directly, following chemical separation, or with its daughter 95Nb using a high-resolution gamma detector system.5.3.4 144Ce is a high-yield fission product applicable to 2- to 3-year irradiations.5.4 It is necessary to surround the 238U monitor with a thermal neutron absorber to minimize fission product production from a quantity of 235U in the 238U target and from  239Pu from (n,γ) reactions in the 238U material. Assay of the 239Pu concentration when a significant contribution is expected.5.4.1 Fission product production in a light-water reactor by neutron activation product 239Pu has been calculated to be insignificant (<2 %), compared to that from 238U(n,f), for an irradiation period of 12 years at a fast-neutron (E > 1 MeV) fluence rate of 1 × 1011 cm−2 · s−1 provided the 238U is shielded from thermal neutrons (see Fig. 2 of Guide E844).5.4.2 Fission product production from photonuclear reactions, that is, (γ,f) reactions, while negligible near-power and research-reactor cores, can be large for deep-water penetrations (6).45.5 Good agreement between neutron fluence measured by 238U fission and the 54Fe(n,p)54Mn reaction has been demonstrated (7). The reaction  238U(n,f) F.P. is useful since it is responsive to a broader range of neutron energies than most threshold detectors.5.6 The 238U fission neutron spectrum-averaged cross section in several benchmark neutron fields is given in Table 3 of Practice E261. Sources for the latest recommended cross sections are given in Guide E1018. In the case of the 238U(n,f)F.P. reaction, the recommended cross section source is the ENDF/B-VI release 8 cross section (MAT = 9237) (8). Fig. 1 shows a plot of the recommended cross section versus neutron energy for the fast-neutron reaction 238U(n,f)F.P.FIG. 1 ENDF/B-VI Cross Section Versus Energy for the 238U(n,f)F.P. ReactionNOTE 1: The data is taken from the Evaluated Nuclear Data File, ENDF/B-VI, rather than the later ENDF/B-VII. This is in accordance with Guide E1018, Section 6.1, since the later ENDF/B-VII data files do not include covariance information. Some covariance information exists for 238U in the standard sublibrary, but this is only for energies greater than 1 MeV. For more details, see Section H of Ref 9.1.1 This test method covers procedures for measuring reaction rates by assaying a fission product (F.P.) from the fission reaction 238U(n,f)F.P.1.2 The reaction is useful for measuring neutrons with energies from approximately 1.5 to 7 MeV and for irradiation times up to 30 to 40 years, provided that the analysis methods described in Practice E261 are followed.1.3 Equivalent fission neutron fluence rates as defined in Practice E261 can be determined.1.4 Detailed procedures for other fast-neutron detectors are referenced in Practice E261.1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Refer to Practice E261 for a general discussion of the determination of fast-neutron fluence rate with fission detectors.5.2 237Np is available as metal foil, wire, or oxide powder. For further information, see Guide E844. It is usually encapsulated in a suitable container to prevent loss of, and contamination by, the   237Np and its fission products.45.3 One or more fission products can be assayed. Pertinent data for relevant fission products are given in Table 15 and Table 2.(A) The lightface numbers in parentheses are the magnitude of plus or minus uncertainties in the last digit(s) listed.(B) With  137mBa (2.552 min) in equilibrium.(C) Probability of daughter  140La decay.(D) With  140La (1.67850 d) in transient equilibrium.(E) Primary reference for half-life, gamma energy, and gamma emission probability is Ref (1) when data is available. Note this reference is to the BIPM data that was recommended at the time of the recommended fission yields were set, that is, as of 2009, and not to the latest Vol 8 data that was published in 2016.(A) The JEFF-3.1/3.1.1 radioactive decay data and fission yields sub-libraries, JEFF Report 20, OECD 2009, Nuclear Energy Agency (2).(B) All yield data given as a %; RC represents a cumulative yield; RI represents an independent yield.(C) The neutron energy represents a generic “fast neutron” spectrum and has been characterized in the JEFF 3.1.1 fission yield library as having an average neutron energy of 0.4 MeV.5.3.1 137Cs-137mBa is chosen frequently for long irradiations. Radioactive products 134Cs and  136Cs may be present, which can interfere with the counting of the 0.661657 MeV  137Cs-137mBa gamma ray (see Test Methods E320).5.3.2 140Ba-140La is chosen frequently for short irradiations (see Test Method E393).5.3.3 95Zr can be counted directly, following chemical separation, or with its daughter 95Nb, using a high-resolution gamma detector system.5.3.4 144Ce is a high-yield fission product applicable to 2- to 3-year irradiations.5.4 It is necessary to surround the 237Np monitor with a thermal neutron absorber to minimize fission product production from trace quantities of fissionable nuclides in the 237Np target and from  238Np and  238Pu from (n,γ) reactions in the   237Np material. Assay of   238Pu and   239Pu concentration is recommended when a significant contribution is expected.5.4.1 Fission product production in a light-water reactor by neutron activation products   238Np and   238Pu has been calculated to be insignificant (1.2 %), compared to that from  237Np(n,f), for an irradiation period of 12 years at a fast neutron (E > 1 MeV) fluence rate of 1 × 1011 cm−2 ·s−1, provided the  237Np is shielded from thermal neutrons (see Fig. 2 of Guide E844).5.4.2 Fission product production from photonuclear reactions, that is, (γ,f) reactions, while negligible near-power and research reactor cores, can be large for deep-water penetrations (3).5.5 This dosimetry reaction is important in the area of reactor retrospective dosimetry (4, 5). Good agreement between neutron fluence measured by  237Np fission and the  54Fe(n,p) 54Mn reaction has been demonstrated (6, 7). The reaction  237Np(n,f) F.P. is useful since it is responsive to a broader range of neutron energies than most threshold detectors.5.5.1 Fig. 1 shows the energy-dependent cross section for this dosimetry reaction. The figure shows that, while it is not strictly a threshold detector, because of its sensitivity in the greater than 0.1 MeV neutron energy range it can function as a detector with good sensitivity in the fast neutron region. In the fast fission 252Cf spontaneous fission benchmark field, ~1 % of the 237Np fission dosimeter response comes from neutrons with an energy less than 0.1 MeV. In the cavity of a fast burst 235U reactor, ~5 % of the 237Np ifssion dosimeter response comes from neutrons with an energy less than 0.1 MeV. In the cavity of a well-moderated pool-type research reactor ~50 % of the fission response from the 237Np(n,f) reaction comes from energies less than 0.1 MeV. The importance of this low neutron energy sensitivity should be determined based on the aplication.5.6 The  237Np fission neutron spectrum-averaged cross section in several benchmark neutron fields are given in Table 3 of Practice E261. Sources for the latest recommended cross sections are given in Guide E1018. In the case of the  237Np(n,f)F.P. reaction, the recommended cross section source is the Russian Reactor Dosimetry File, RRDF (8). This recommended cross section is identical, for energies up to 20 MeV, to what is found in the latest International Atomic Energy (IAEA) International Reactor Dosimetry and Fusion File, IRDFF-1.05 (9) . Fig. 1 shows a plot of the recommended cross section versus neutron energy for the fast-neutron reaction   237Np(n,f)F.P.FIG. 1 RRDF/IRDFF-1.05 Cross Section Versus Energy for the 237Np(n,f)F.P. Reaction1.1 This test method covers procedures for measuring reaction rates by assaying a fission product (F.P.) from the fission reaction  237Np(n,f)F.P.1.2 The reaction is useful for measuring neutrons with energies from approximately 0.7 to 6 MeV and for irradiation times up to 90 years, provided that the analysis methods described in Practice E261 are followed. If dosimeters are analyzed after irradiation periods longer than 90 years, the information inferred about the fluence during irradiation periods more than 90 years before the end of the irradiation should not be relied upon without supporting data from dosimeters withdrawn earlier.1.3 Equivalent fission neutron fluence rates as defined in Practice E261 can be determined.1.4 Detailed procedures for other fast-neutron detectors are referenced in Practice E261.1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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4.1 Two types of alkali reactivity of aggregates have been described in the literature: the alkali-silica reaction involving certain siliceous rocks, minerals, and artificial glasses (1),3 and the alkali-carbonate reaction involving dolomite in certain calcitic dolomites and dolomitic limestones (2). This test method is not recommended as a means to detect combinations susceptible to expansion due to alkali-silica reaction since it was not evaluated for this use in the work reported by Buck (2). This test method is not applicable to aggregates that do not contain or consist of carbonate rock (see Descriptive Nomenclature C294).4.2 This test method is intended for evaluating the behavior of specific combinations of concrete-making materials to be used in the work. However, provisions are made for the use of substitute materials when required. This test method assesses the potential for expansion of concrete caused by alkali-carbonate rock reaction from tests performed under prescribed laboratory curing conditions that will probably differ from field conditions. Thus, actual field performance will not be duplicated due to differences in wetting and drying, temperature, other factors, or combinations of these (see Appendix X1).4.3 Use of this test method is of particular value when samples of aggregate from a source have been determined to contain constituents that are regarded as capable of participation in a potentially deleterious alkali-carbonate rock reaction either by petrographic examination, Guide C295/C295M, by the rock cylinder test, Test Method C586, by service record; or by a combination of these.4.4 Results of tests conducted as described herein should form a part of the basis for a decision as to whether precautions be taken against excessive expansion due to alkali-carbonate rock reaction. This decision should be made before a particular cement-aggregate combination is used in concrete construction (see Note 1).NOTE 1: Other elements that may be included in the decision-making process for categorizing an aggregate or a cement-aggregate combination with respect to whether precautions are needed, and examples of precautions that may be taken, are described in Appendix X1.4.5 While the basic intent of this test method is to develop information on a particular cement-aggregate combination, it will usually be very useful to conduct control tests in parallel using the aggregate of interest with other cements or the cement of interest with other aggregates.1.1 This test method covers the determination, by measurement of length change of concrete prisms, the susceptibility of cement-aggregate combinations to expansive alkali-carbonate reaction involving hydroxide ions associated with alkalies (sodium and potassium) and certain calcitic dolomites and dolomitic limestones.1.2 The text of this standard refers to notes and footnotes that provide explanatory material. These notes and footnotes (excluding those in tables and figures) shall not be considered as requirements of the standard.1.3 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard. When combined standards are cited, the selection of measurement system is at the user's discretion subject to the requirements of the referenced standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Thiodiglycol is a Schedule 2 compound under the Chemical Weapons Convention (CWC). Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents or have a number of other commercial uses. They are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. Schedule 2 chemicals can be found in applications unrelated to chemical weapons. Thiodiglycol is both a mustard gas precursor and degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes and some pesticides.45.2 This test method has been investigated for use with reagent and surface water.1.1 This procedure covers the determination of thiodiglycol (TDG) in surface water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). TDG is qualitatively and quantitatively determined by this test method. This test method adheres to single reaction monitoring (SRM) mass spectrometry.1.2 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 The detection verification level (DVL) and reporting range for TDG are listed in Table 1.TABLE 1 Detection Verification Level and Reporting RangeAnalyte DVL (μg/L) Reporting Range (μg/L)Thiodiglycol 20 100–10 0001.4.1 The DVL is required to be at a concentration at least 3 times below the reporting limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratio at the DVL.FIG. 1 Example SRM Chromatograms Signal/Noise at Detection Verification Level1.4.2 The RL is the concentration of the Level 1 calibration standard as shown in Table 2. The reporting limit for this test method is 100 μg/L.TABLE 2 Concentrations of Calibration Standards (PPB)Analyte/Surrogate LV 1 LV 2 LV 3 LV 4 LV 5 LV 6 LV 7Thiodiglycol 100 250 500 1 000 2 500 5 000 10 0003,3’-Thiodipropanol 100 250 500 1 000 2 500 5 000 10 0001.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 N-Ethyldiethanolamine, N-methyldiethanolamine and triethanolamine are Schedule 3 compounds under the Chemical Weapons Convention (CWC). Schedule 3 chemicals include those that have been produced, stockpiled or used as a chemical weapon, poses otherwise a risk to the object and purpose of the CWC because they possess such lethal or incapacitating toxicity as well as other properties that might enable it to be used as a chemical weapon, poses otherwise a risk to the object and purpose of the CWC by virtue of it’s importance in the production of one or more chemicals listed in Schedules 1 or 2, or it may be produced in large commercial quantities for purposes not prohibited under the CWC.4 Ethanolamines have a broad spectrum of applications. They are used to produce adhesives, agricultural products, cement grinding aids, concrete additives, detergents, specialty cleaners, personal care products, gas treatments, metalwork, oil well chemicals, packaging and printing inks, photographic chemicals, rubber, textile finishing, urethane coatings, textile lubricants, polishes, pesticides, and pharmaceuticals. Ethanolamines are readily dissolved in water, biodegradable and the bio-concentration potential is low.55.2 This test method has been investigated for use with reagent and surface water.1.1 This procedure covers the determination of diethanolamine, triethanolamine, N-methyldiethanolamine and N-ethyldiethanolamine (referred to collectively as ethanolamines in this test method) in surface water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to single reaction monitoring (SRM) mass spectrometry.1.2 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 The Detection Verification Level (DVL) and Reporting Range for the ethanolamines are listed in Table 1.TABLE 1 Detection Verification Level and Reporting RangeAnalyte DVL (μg/L) Reporting Range (μg/L)Diethanolamine 5 25–500Triethanolamine 5 25–500N-Ethyldiethanolamine 5 25–500N-Methyldiethanolamine 10 50–5001.4.1 The DVL is required to be at a concentration at least 3 times below the Reporting Limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratios at the DVLs and at higher concentrations for N-methyldiethanolamine.FIG. 1 Example SRM Chromatograms Signal/Noise Ratios1.4.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for diethanolamine, triethanolamine, and N-ethyldiethanolamine and Level 2 for N-methyldiethanolamine. The reporting limit for N-methyldiethanolamine is set at 50 μg/L due to poor sensitivity at a 5 μg/L concentration which did not meet the DVL criteria. The DVL for N-methyldiethanolamine is at 10 μg/L, which forces a raised reporting limit (chromatograms are shown in Fig. 1). However, the multi-laboratory validation required a spike of all target analytes at 25 μg/L. The mean recovery for N-methyldiethanolamine at this level was 88 % as shown in Table 3. If your instrument’s sensitivity can meet the requirements in this test method, N-methyldiethanolamine may have a 25 μg/L reporting limit.TABLE 2 Concentrations of Calibration Standards (PPB)Analyte/Surrogate LV 1 LV 2 LV 3 LV 4 LV 5 LV 6 LV 7Diethanolamine 25 50 75 150 250 350 500Triethanolamine 25 50 75 150 250 350 500N-Ethyldiethanolamine 25 50 75 150 250 350 500N-Methyldiethanolamine 25 50 75 150 250 350 500Diethanolamine-D8 (Surrogate) 25 50 75 150 250 350 500TABLE 3 Multi-Laboratory Recovery Data in Reagent WaterAnalyte Spike Conc.(ppb) # Results # Labs Bias PrecisionMeanRecovery(%) MinRecovery(%) MaxRecovery(%) Overall SD(%) Pooledwithin-labSD (%) OverallRSD (%) Pooledwithin-labRSD (%)Diethanolamine 25 24 6 96.34 51.00 156.96 31.31 10.96 32.50 9.49Diethanolamine 50 24 6 101.41 54.00 154.80 29.54 7.97 29.13 7.91Diethanolamine 200 24 6 101.57 61.00 138.00 20.98 10.50 20.66 10.85Diethanolamine 425 24 6 102.06 70.00 138.82 17.98 5.90 17.61 5.70Triethanolamine 25 24 6 87.70 35.96 157.20 27.00 25.18 30.79 27.48Triethanolamine 50 24 6 94.95 67.00 121.66 16.39 9.57 17.26 9.66Triethanolamine 200 22 6 105.00 79.50 132.00 14.06 11.81 13.39 11.52Triethanolamine 425 24 6 96.94 40.00 144.94 27.56 4.41 28.43 5.76N-Ethyldiethanolamine 25 24 6 90.61 31.00 132.00 39.42 7.47 43.51 10.42N-Ethyldiethanolamine 50 23 6 111.88 49.00 146.00 28.71 7.19 25.66 7.56N-Ethyldiethanolamine 200 24 6 106.20 60.00 134.00 23.09 11.96 21.74 12.23N-Ethyldiethanolamine 425 24 6 99.67 51.00 130.00 23.07 4.68 23.15 6.01N-Methyldiethanolamine 25 24 6 88.43 41.72 133.60 25.24 13.29 28.55 16.70N-Methyldiethanolamine 50 24 6 102.28 56.00 153.80 25.85 8.73 25.27 8.22N-Methyldiethanolamine 200 24 6 101.02 59.00 136.50 20.07 9.51 19.87 9.54N-Methyldiethanolamine 425 24 6 94.75 63.00 115.76 15.02 3.34 15.85 3.72Diethanolamine-D8 (Surrogate) 200 96 6 103.02 60.00 151.95 21.13 9.40 20.51 9.251.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Vapor intrusion testing has been performed traditionally using multiple canister samples or thermal desorption tube samples. These discontinuous measurements have been shown to be snapshots and provide averages of exposure. In many cases a higher temporal resolution is desirable to identify peaks of emissions due to specific occupancy or environmental changes. For these cases, a continuous real-time monitoring solution is desirable. These continuous monitoring setups can be either short-term or be part of a long-term monitoring plan as described in ASTM guide “Standard Guide for the development of LongTerm Monitoring Plans for Vapor Mitigation Systems” (E2600).5.2 The PTR-MS provides real-time measurement of multiple VOCs at ultra-trace levels, that is, in the µL/L (ppm) to less than pL/L (ppt) range. Its strengths lie with the ability to measure VOCs in real-time and continuously (that is, ~1 Hz or faster, using time-of-flight analyzers), and with limited sample pre-treatment, compared to a gas chromatograph (GC) system, which is commonly the method of choice to measure VOCs using a variety of detectors. In case of PTR-MS with quadrupole analyzers, the terms would be nearreal-time and semi-continuous. The high temporal resolution of the PTR-MS measurement in the range of second(s) is often desired when studying the atmospheric chemistry or source emissions that result in unpredictable, sudden, and short-term fluctuations. For a detailed description on the design and theory and practical aspects of operation for the different types of PTR-MS, please refer to Yuan et al. (2017)(1).5.3 For ambient air measurements, such as vapor intrusion (VI) related emission testing, the PTR-MS can be used in three different modes of operation: (1) in scanning mode to identify sources and VI entry points within buildings; (2) in variation identification mode, as a continuous monitoring instrument with seconds to minutes of temporal resolution covering a large number of VOCs; (3) in source tracking mode, as a scanner of indoor and outdoor sources and as a rapid tracking device for external emissions; this requires the instrument to be mounted on a moveable platform, such as on an (autonomous) vehicle or trolley. The same operation can be used to identify various other constituents in air, depending on the application—be it fugitive emissions from toxic materials or illicit materials, or metabolic reactions to infections expressed in different breath emissions.5.4 Spatial and temporal variability are two common challenges with ambient air measurements and source assessments. Within a given building, the sources for vapors can be few or many and are generally irregularly spaced; they may be obscured from view by floor coverings, furniture or walls, which in itself can be a large source of VOC. The current methods of choice require the use of time-discreet monitoring or time-averaged monitoring of a specific sampling spot. Real-time monitoring provides a method to assess the spatial distribution of vapor concentrations, which may help to rapidly and efficiently identify the location of vapor entry points.5.5 Real time assessment is valuable as a component of a program of assessment with two or more supporting lines of evidence and can be used to:5.5.1 Provide support for real-time decisions such as where and when to collect long-term samples for fixed laboratory analysis using canisters or sorbent tubes;5.5.2 Verify data quality (for example, monitoring the efficacy of soil gas probe purging prior to sampling, providing leak checks; and5.5.3 Measure changes in VOC vapor concentrations in response to changes in building pressure, temperature, solar irradiation, or other weather conditions and factors affecting vapor fate and transport, including secondary chemistry occurring within the building.5.5.4 Identify alternative pathways based on prior identified intrusion compounds or based on emissions within such pathways, such as stormwater drains.5.6 Screening of a property prior to a real estate transaction based on site specific potential sources of concern. The option for voluntary investigative assessments of potential VI in the real estate business is described in ASTM method E2600-15.NOTE 1: The quality of the result produced by this standard is dependent on the competence of the personnel performing it, and the suitability of the equipment and facilities used. Agencies that meet the criteria of Practice D3740 are generally considered capable of competent and objective testing/sampling/inspection/etc. Users of this standard are cautioned that compliance with Practice D3740 does not in itself assure reliable results. Reliable results depend on many factors; Practice D3740 provides a means of evaluating some of those factors.1.1 This test method describes a technique of quantifying the results from measuring various volatile organic compound contents using a chemical ionization mass spectrometer resulting in the production of positively charged target compound ions. Depending on the nature of production of so-called primary ions, the associated instruments having the capability to perform such analyses are either named Proton Transfer Reaction Mass Spectrometers (PTR-MS), Selected Ion Flow Tube Mass Spectrometers (SIFT-MS) or, in the most generic term, Mid-pressure chemical ionization mass spectrometers (MPCI-MS). Within this standard, the term PTR-MS is used to represent any of these instrumentations.1.2 Either of the instrument types can be used with the two main mass analyzers on the market, that is, with either quadrupole (QMS) or time-of-flight (TOFMS) mass analyzer. This method relates only to the quantification portion of the analysis. Due to large differences in user interfaces and operating procedures for the instruments of the main instrument providers, the specifics on instrument operation are not described in this method.1.3 Details on the theoretical aspects concerning ion production and chemical reactions are included in this standard as far as required to understand the quantification aspects and practical operation of the instrument in the field of vapor intrusion analyses. Specifics on the operation and/or calibration of the instrument need to be identified by using the user’s manual of the individual instrument vendor. A comprehensive discussion on the technique including individual mass-line interferences and in-depth comparison with alternate methods are given in multiple publications, such as Yuan et al. (2017) (1) and Dunne et al. (2018) (2)2.1.4 Units—Values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. Reporting of test results in units other than SI shall not be regarded as nonconformance with this standard.1.5 All observed and calculated values shall conform to the guidelines for significant digits and rounding established in Practice D6026.1.5.1 The procedures used to specify how data are collected/recorded or calculated in the standard are regarded as the industry standard. In addition, they are representative of the significant digits that generally should be retained. The procedures used do not consider material variation, purpose for obtaining the data, special purpose studies, or any considerations for the user’s objectives; and it is common practice to increase or reduce significant digits of reported data to be commensurate with these considerations. It is beyond the scope of this standard to consider significant digits used in analysis methods for engineering data.1.6 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Refer to Guide E844 for the selection, irradiation, and quality control of neutron dosimeters. 5.2 Refer to Practice E261 for a general discussion of the measurement of neutron fluence rate and fluence. The neutron spectrum must be known in order to measure neutron fluence rates with a single detector. Also it is noted that cross sections are continuously being reevaluated. The latest recommended cross sections and details on how they can be obtained are discussed in Guide E1018. 5.3 The reaction rate of a detector nuclide of known cross section, when combined with information about the neutron spectrum, permits the determination of the magnitude of the fluence rate impinging on the detector. Furthermore, if results from other detectors are available, the neutron spectrum can be defined more accurately. The techniques for fluence rate and fluence determinations are explained in Practice E261. 5.4 140Ba is a radioactive nuclide formed as a result of fission. Although it is formed in fission of any heavy atom, the relative yield will differ. Table 1 gives recommended cumulative fission yields for 140Ba production and direct (independent) fission yields for the daughter product 140La. The independent fission yields for 140La are relatively low compared to the 140Ba cumulative fission yield and will not significantly affect the accuracy of the nondestructive procedure and need not be considered. (A) Thermal = 0.0253 eV19.(B) Fast = 0.4 MeV.(C) From JEF-3.1.1 (Ref (1, 2)), except as noted. Uncertainties in percent of given value.(D) From ENDF/B-VIII.0 (Ref (3)). Not available in JEF-3.1.1. Uncertainties in percent of given value. 5.5 The half-life of 140Ba is 12.752 days. Its daughter 140La has a half-life of 1.6781 days (4).3 The comparatively long half-life of 140Ba allows the counting to be delayed several weeks after irradiation in a high-neutron field. However, to achieve maximum sensitivity the daughter product 140La should be counted five to six days after the irradiation during nondestructive analysis or five to six days after chemical separation if the latter technique is used. An alternative method after chemical separation is to count the 140Ba directly. 5.6 Because of its 12.752 day half-life and substantial fission yield, 140Ba is useful for irradiation times up to about six weeks in moderate intensity fields. The number of fissions produced should be approximately 109 or greater for good counting statistics. Also, if the irradiation time is substantially longer than six weeks, the neutron fluence rate determined will apply mainly to the neutron field existing during the latter part of the irradiation. The 140Ba decay constant and yield are known more accurately than those of many fission products, so it is sometimes used as a standard or base reaction with which other measurements can be normalized. 1.1 This test method describes two procedures for the measurement of reaction rates by determining the amount of the fission product 140Ba produced by the non-threshold reactions 235U(n,f), 241Am(n,f), and 239Pu(n,f), and by the threshold reactions 238U(n,f), 237Np(n,f), and 232Th(n,f). 1.2 These reactions produce many fission products, among which is 140Ba, having a half-life of 12.752 days. 140Ba emits gamma rays of several energies; however, these are not easily detected in the presence of other fission products. Competing activity from other fission products requires that a chemical separation be employed or that the 140Ba activity be determined indirectly by counting its daughter product 140La. This test method describes both procedure (a), the nondestructive determination of 140Ba by the direct counting of 140La several days after irradiation, and procedure (b), the chemical separation of 140Ba and the subsequent counting of 140Ba or its daughter 140 La. 1.3 With suitable techniques, fission neutron fluence rates can be measured in the range from 107 n (neutrons) · cm−2 · s−1 to approximately 1015 n · cm−2 · s−1. 1.4 The measurement of time-integrated reaction rates with fission dosimeters by 140Ba analysis is limited by the half-life of 140Ba to irradiation times up to about six weeks. 1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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The reaction thresholds of a material are a measure of the tendency of the material or its decomposition products to undergo gas phase reactions of various types. Hot-flame and cool-flame thresholds relate directly to reactions which are involved in autoignition phenomena. Pre-flame, catalytic and thermal polymerization thresholds also relate to autoignition in that they represent reactions which can be under some conditions the precursors of ignition reactions.1.1 This test method covers determination of the pre-flame, cool-flame, and hot-flame reaction threshold temperatures and the incipient reaction temperature of liquids and solids. Data may be obtained at pressures from low vacuum to 0.8 MPa (115 psia) for temperatures within the range from room temperature to 925 K (1200°F).1.2 This test method may be applied to any substance that is a liquid or a solid at room temperature and atmospheric pressure and that, at room temperature, is compatible with glass and stainless steel. Air is the intended oxidizing medium; however, other media may be substituted provided appropriate precautions are taken for their safe use.1.3 The values stated in SI units are to be regarded as the standard. In cases where materials, products, or equipment are available in inch-pound units only, SI units are omitted.1.4 This standard is used to measure and describe the response of materials, products, or assemblies to heat and flame under controlled conditions, but does not by itself incorporate all factors required for fire hazard or fire risk assessment of the materials, products, or assemblies under actual fire conditions.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see 6.8, Sections 7 and 9.

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1. Scope This Guide has been written by Canadian experts on the diagnosis and treatment of concrete structures affected by alkali- aggregate reaction (AAR). The purpose of the Guide is to provide information on the signs and symptoms of concrete affected

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6.1 This test method is useful for research and development, quality assurance, regulatory compliance and specification-based acceptance.6.2 The kinetic parameters determined by this method may be used to calculate thermal hazard figures-of-merit according to Practice E1231.1.1 This test method describes the determination of the kinetic parameters of Arrhenius activation energy and pre-exponential factor using the Kissinger variable heating rate iso-conversion method (1, 2)2 and activation energy and reaction order by the Farjas method (3) for thermally unstable materials. The test method is applicable to the temperature range from 300 K to 900 K (27 °C to 627 °C).1.2 Both nth order and accelerating reactions are addressed by this method over the range of 0.5 < n < 4 and 1 < p < 4 where n is the nth order reaction order and p is the Avrami reaction order (4). Reaction orders n and p are determined by the Farjas method (3).1.3 This test method uses the same experimental conditions as Test Method E698. The Flynn/Wall/Ozawa data treatment of Test Method E698 may be simultaneously applied to these experimental results.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Information concerning the reaction model aids in the selection of the appropriate method (and test method) for evaluation of kinetic parameters. nth order reaction may be treated by isoconversion methods such as Test Methods E698 and E2890. Autocatalytic reactions are treated by Test Methods E2070.5.2 This practice may be used in research, forensic analysis, trouble shooting, product evaluation, and hazard potential evaluation.1.1 This practice describes a procedure for determining the “model” of an exothermic reaction using differential scanning calorimetry. The procedure is typically performed on 1 mg to 3 mg specimen sizes over the temperature range from ambient to 600 °C.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This test method measures the time to extrapolated onset of an exothermic reaction under constant temperature (isothermal) conditions for reactions which have an induction period, for example, those which are catalytic, autocatalytic, or accelerating in nature or which contain reaction inhibitors.5.2 The RIT determined by this test method is an index measurement that is useful for comparing one material to another at the test temperature of interest and in the same apparatus type only.5.3 This test method is a useful adjunct to dynamic thermal tests, such as Test Method E537, which are performed under conditions in which the sample temperature is increased continuously at constant rate. Results obtained under dynamic test conditions may result in higher estimates of temperature at which an exothermic reaction initiates because the detected onset temperature is dependent upon the heating rate and because dynamic methods allow insufficient time for autocatalytic reactions to measurably affect the onset temperature.5.4 RIT values determined under a series of isothermal test conditions may be plotted as their logarithm versus the reciprocal of the absolute temperature to produce a plot, the slope of which is proportional to the activation energy of the reaction as described in Test Methods E2070.5.5 This test method may be used in research and development, manufacturing, process and quality control, and regulatory compliance.5.6 This test method is similar to that for oxidation induction time (OIT) (for example, Specification D3350 and Test Methods D3895, D4565, D5483, D6186, and E1858) where the time to the oxidation reaction under isothermal test conditions is measured. The OIT test method measures the presence of antioxidant packages and is a relative measurement of a material’s resistance to oxidation.1.1 This test method describes the measurement of reaction induction time (RIT) of chemical materials that undergo exothermic reactions with an induction period. The techniques and apparatus described may be used for solids, liquids, or slurries of chemical substances. The temperature range covered by this test method is typically from ambient to 400 °C. This range may be extended depending upon the apparatus used.1.2 The RIT is a relative index value, not an absolute thermodynamic property. As an index value, the RIT value may change depending upon experimental conditions. A comparison of RIT values may be made only for materials tested under similar conditions of apparatus, specimen size, and so forth. Furthermore, the RIT value may not predict behavior of large quantities of material.1.3 The RIT shall not be used by itself to establish a safe operating temperature. It may be used in conjunction with other test methods (for example, Test Methods E487 and E537, and Guide E1981) as part of a hazard analysis of a particular operation.1.4 This test method may be used for RIT values greater than 15 min (as relative imprecision increases at shorter periods).1.5 This test method is used to study catalytic, autocatalytic, and accelerating reactions. These reactions depend upon time as well as temperature. Such reactions are often studied by fixing one experimental parameter (that is, time or temperature) and then measuring the other parameter (that is, temperature or time). This test method measures time to reaction onset detection under isothermal conditions. It is related to Test Method E487 that measures detected reaction onset temperature under constant time conditions1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this test method.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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