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5.1 This test method for the spectrometric analysis of metals and alloys is primarily intended to test such materials for compliance with compositional specifications. It is assumed that all who use this test method will be analysts capable of performing common laboratory procedures skillfully and safely. It is expected that work will be performed in a properly equipped laboratory.1.1 This test method covers the simultaneous determination of 21 alloying and residual elements in carbon and low-alloy steels by spark atomic emission vacuum spectrometry in the mass fraction ranges shown Note 1.Element Composition Range, %Applicable Range,Mass Fraction %A Quantitative Range,Mass Fraction %BAluminum 0 to 0.093 0.006 to 0.093Antimony 0 to 0.027 0.006 to 0.027Arsenic 0 to 0.1 0.003 to 0.1Boron 0 to 0.007 0.0004 to 0.007Calcium 0 to 0.003 0.002 to 0.003Carbon 0 to 1.1 0.02 to 1.1Chromium 0 to 8.2 0.007 to 8.14Cobalt 0 to 0.20 0.006 to 0.20Copper 0 to 0.5 0.006 to 0.5LeadC 0 to 0.2 0.002 to 0.2Manganese 0 to 2.0 0.03 to 2.0Molybdenum 0 to 1.3 0.007 to 1.3Nickel 0 to 5.0 0.006 to 5.0Niobium 0 to 0.12 0.003 to 0.12Nitrogen 0 to 0.015 0.01 to 0.055Phosphorous 0 to 0.085 0.006 to 0.085Silicon 0 to 1.54 0.02 to 1.54Sulfur 0 to 0.055 0.001 to 0.055Tin 0 to 0.061 0.005 to 0.061Titanium 0 to 0.2 0.001 to 0.2Vanadium 0 to 0.3 0.003 to 0.3Zirconium 0 to 0.05 0.01 to 0.05NOTE 1: The mass fraction ranges of the elements listed have been established through cooperative testing2 of reference materials.1.2 This test method covers analysis of specimens having a diameter adequate to overlap and seal the bore of the spark stand opening. The specimen thickness can vary significantly according to the design of the spectrometer stand, but a thickness between 10 mm and 38 mm has been found to be most practical.1.3 This test method covers the routine control analysis in iron and steelmaking operations and the analysis of processed material. It is designed for chill-cast, rolled, and forged specimens. Better performance is expected when reference materials and specimens are of similar metallurgical condition and composition. However, it is not required for all applications of this 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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ASTM D4962-18 Standard Practice for NaI(Tl) Gamma-Ray Spectrometry of Water Active 发布日期 :  1970-01-01 实施日期 : 

5.1 Gamma-ray spectrometry is used to identify radionuclides and to make quantitative measurements. Use of a computer and a library of standard spectra will be required for quantitative analysis of complex mixtures of nuclides.5.2 Variation of the physical geometry of the sample and its relationship with the detector will produce both qualitative and quantitative variations in the gamma-ray spectrum. To adequately account for these geometry effects, calibrations are designed to duplicate all conditions including source-to-detector distance, sample shape and size, and sample matrix encountered when samples are measured. This means that a complete set of library standards may be required for each geometry and sample to detector distance combination that will be used.5.3 Since some spectrometry systems are calibrated at many discrete distances from the detector, a wide range of activity levels can be measured on the same detector. For high-level samples, extremely low efficiency geometries may be used. Quantitative measurements can be made accurately and precisely when high activity level samples are placed at distances of 1 m or more from the detector.5.4 Electronic problems, such as erroneous deadtime correction, loss of resolution, and random summing, may be avoided by keeping the gross count rate below 2000 counts per second and also keeping the deadtime of the analyzer below 5 %. Total counting time is governed by the activity of the sample, the detector source distance, and the acceptable Poisson counting uncertainty.1.1 This practice covers the measurement of radionuclides in water by means of gamma-ray spectrometry. It is applicable to nuclides emitting gamma-rays with energies greater than 50 keV. For typical counting systems and sample types, activity levels of about 40 Bq (1080 pCi) are easily measured and sensitivities of about 0.4 Bq (11 pCi) are found for many nuclides (1-10).2 Count rates in excess of 2000 counts per second should be avoided because of electronic limitations. High count rate samples can be accommodated by dilution or by increasing the sample to detector distance.1.2 This practice can be used for either quantitative or relative determinations. In tracer work, the results may be expressed by comparison with an initial concentration of a given nuclide which is taken as 100 %. For radioassay, the results may be expressed in terms of known nuclidic standards for the radionuclides known to be present. In addition to the quantitative measurement of gamma-ray activity, gamma-ray spectrometry can be used for the identification of specific gamma-ray emitters in a mixture of radionuclides but that ability is limited when using low energy resolution Na(Tl) detectors as compared to High Purity Germanium (HPGe) detectors. General information on radioactivity and the measurement of radiation has been published (11 and 12). Information on specific application of gamma-ray spectrometry is also available in the literature (13-16).1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are included for information only and are not considered 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 A knowledge of the hydrocarbon composition of process streams and petroleum products boiling within the range 205 °C to 540 °C (400 °F to 1000 °F) is useful in following the effect of changes in process variables, diagnosing the source of plant upsets, and in evaluating the effect of changes in composition on product performance properties. This method, when used together with Test Method D2786, provides a detailed analysis of the hydrocarbon composition of such materials.1.1 This test method2 covers the determination by high ionizing voltage, low resolution mass spectrometry of 18 aromatic hydrocarbon types and 3 aromatic thiophenotypes in straight run aromatic petroleum fractions boiling within the range from 205 °C to 540 °C (400 °F to 1000 °F) (corrected to atmospheric pressure). Samples must be nonolefinic, must contain not more than 1 % by mass of total sulfur, and must contain not more than 5 % nonaromatic hydrocarbons. Composition data are in volume percent.NOTE 1: Although names are given to 15 of the compound types determined, the presence of other compound types of the same empirical formulae is not excluded. All other compound types in the sample, unidentified by name or empirical formula, are lumped into six groups in accordance with their respective homologous series.1.2 The values stated in acceptable SI units are to be regarded as the standard. The values given in parentheses are provided for information purposes only.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 and health practices and determine the applicability of regulatory limitations prior to use.

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5.1 Gamma-ray spectrometry of soil samples is used to identify and quantify certain gamma-ray emitting radionuclides. Use of a germanium semiconductor detector is necessary for high-resolution gamma-ray measurements.5.2 Much of the data acquisition and analysis can be automated with the use of commercially available systems that include both hardware and software. For a general description of the typical hardware in more detail than discussed in Section 7, see Ref (19). For best practices on set-up, calibration, and quality control of utilized spectrometry systems, see Practice D7282.5.3 Both qualitative and quantitative analyses may be performed using the same measurement data.5.4 The procedures described in this guide may be used for a wide variety of activity levels, from natural background levels and fallout-type problems, to determining the effectiveness of cleanup efforts after a spill or an industrial accident, to tracing contamination at older production sites, where wastes were purposely disposed of in soil. In some cases, the combination of radionuclide identities and concentration ratios can be used to determine the source of the radioactive materials.5.5 Collecting samples and bringing them to a data acquisition system for analysis may be used as the primary method to detect deposition of radionuclides in soil. For obtaining a representative set of samples that cover a particular area, see Practice C998. Soil can also be measured by taking the data acquisition system to the field and measuring the soil in place (in situ). In situ measurement techniques are not discussed in this guide.1.1 This guide covers the identification and quantitative determination of gamma-ray emitting radionuclides in soil samples by means of gamma-ray spectrometry. It is applicable to nuclides emitting gamma rays with an approximate energy range of 20 to 2000 keV. For typical gamma-ray spectrometry systems and sample types, activity levels of about 5 Bq (135 pCi) are measured easily for most nuclides, and activity levels as low as 0.1 Bq (2.7 pCi) can be measured for many nuclides. It is not applicable to radionuclides that emit no gamma rays such as the pure beta-emitting radionuclides hydrogen-3, carbon-14, strontium-90, and becquerel quantities of most transuranics. This guide does not address the in situ measurement techniques, where soil is analyzed in place without sampling. Guidance for in situ techniques can be found in Ref (1) and (2).2 This guide also does not discuss methods for determining lower limits of detection. Such discussions can be found in Refs (3), (4), (5) , and (6).1.2 This guide can be used for either quantitative or relative determinations. For quantitative assay, the results are expressed in terms of absolute activities or activity concentrations of the radionuclides found to be present. This guide may also be used for qualitative identification of the gamma-ray emitting radionuclides in soil without attempting to quantify their activities. It can also be used to only determine their level of activities relative to each other but not in an absolute sense. General information on radioactivity and its measurement may be found in Refs (7), (8), (9), (10) , and (11) and Standard Test Methods E181. Information on specific applications of gamma-ray spectrometry is also available in Refs (12) or (13). Practice D3649 may be a valuable source of information.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 This standard may involve hazardous material, 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 and health 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 This practice is used for reporting the experimental conditions as specified in Section 6 in the “Methods” or “Experimental” sections of other publications (subject to editorial restrictions).5.2 The report would include specific conditions for each data set, particularly, if any parameters are changed for different sputter depth profile data sets in a publication. For example, footnotes of tables or figure captions would be used to specify differing conditions.1.1 This practice covers the information needed to describe and report instrumentation, specimen parameters, experimental conditions, and data reduction procedures. SIMS sputter depth profiles can be obtained using a wide variety of primary beam excitation conditions, mass analysis, data acquisition, and processing techniques (1-4).21.2 Limitations—This practice is limited to conventional sputter depth profiles in which information is averaged over the analyzed area in the plane of the specimen. Ion microprobe or microscope techniques permitting lateral spatial resolution of secondary ions within the analyzed area, for example, image depth profiling, are excluded.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 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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6.1 The health of workers in many industries, for example, mining, metal refining, battery manufacture, construction, etc., is at risk through exposure by inhalation of particulate lead and lead compounds. Industrial hygienists and other public health professionals need to determine the effectiveness of measures taken to control workers' exposure, and this is generally achieved by making workplace air measurements. This standard has been published in order to make available a method for making valid exposure measurements for lead. It will be of benefit to: agencies concerned with health and safety at work; industrial hygienists and other public health professionals; analytical laboratories; industrial users of metals and metalloids and their workers, etc. It has been assumed in the drafting of this standard that the execution of its provisions, and the interpretation of the results obtained, is entrusted to appropriately qualified and experienced people.6.2 The measuring procedure shall comply with any relevant International, European or National Standard that specifies performance requirements for procedures for measuring chemical agents in workplace air (for example, ISO 20581).1.1 This standard specifies flame and graphite furnace atomic absorption spectrometric methods for the determination of the time-weighted average mass concentration of particulate lead and lead compounds in workplace air.1.2 The method is applicable to personal sampling of the inhalable fraction of airborne particles, as defined in ISO 7708, and to static (area) sampling.1.3 The sample dissolution procedure specifies hot plate or microwave digestion, or ultrasonic extraction (10.2). The sample dissolution procedure is not effective for all lead compounds (see Section 5). The use of an alternative, more vigorous dissolution procedure is necessary when it is desired to extract lead from compounds present in the test atmosphere that are insoluble using the dissolution procedures described herein. For example if it is desired to determine silicate lead, a hydrofluoric acid dissolution procedure is required.1.4 The flame atomic absorption method is applicable to the determination of masses of approximately 1 to 200 μg of lead per sample, without dilution (1).2 The graphite furnace atomic absorption method is applicable to the determination of masses of approximately 0.01 to 0.5 μg of lead per sample, without dilution (1).1.5 The ultrasonic extraction procedure has been validated for the determination of masses of approximately 20 to 100 μg of lead per sample, for laboratory-generated lead fume air filter samples (2).1.6 The concentration range for lead in air for which this procedure is applicable is determined in part by the sampling procedure selected by the user (see Section 9).1.7 Anions that form precipitates with lead may interfere, but this potential interference is overcome by the addition of the disodium salt of ethylenediamine tetraacetic acid (EDTA) when necessary.1.8 The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.1.9 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.1.10 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 for the chemical analysis of nickel alloys is primarily intended to test material for compliance with specifications such as those under jurisdiction of ASTM Committee B02. It may also be used to test compliance with other specifications that are compatible with the test method.5.2 It is assumed that all who use this test method will be trained analysts capable of performing common laboratory procedures skillfully and safely, and that the work will be performed in a properly equipped laboratory.5.3 This is a performance-based test method that relies more on the demonstrated quality of the test result than on strict adherence to specific procedural steps. It is expected that laboratories using this test method will prepare their own work instructions. These work instructions will include detailed operating instructions for the specific laboratory, the specific reference materials employed, and performance acceptance criteria. It is also expected that, when applicable, each laboratory will participate in proficiency test programs, such as described in Practice E2027, and that the results from the participating laboratory will be satisfactory.1.1 This test method describes the inductively coupled plasma atomic emission spectrometric analysis of nickel alloys, such as specified by Committee B02, and having chemical compositions within the following limits:Element Application Range (%)Aluminum 0.01–1.00Boron 0.001–0.050Calcium 0.001–0.05Carbon 0.10–0.20Chromium 0.01–33.0Cobalt 0.10–20.0Copper 0.01–3.00Iron 0.01–50.0Lead 0.001–0.01Magnesium 0.0001–0.100Manganese 0.01–3.0Molybdenum 0.01–30.0Niobium 0.01–6.0Nickel 25.0–80.0Nitrogen 0.001–0.20Oxygen 0.0001–0.003Phosphorous 0.001–0.030Sulfur 0.0001–0.010Silicon 0.01–1.50Tantalum 0.005–0.10Tin 0.001–0.020Titanium 0.001–6.0Tungsten 0.01–5.0Vanadium 0.01–1.0Zirconium 0.01–0.101.2 The following elements may be determined using this test method. The test method user should carefully evaluate the precision and bias statements of this test method to determine applicability of the test method for the intended use.Element Quantification Range (%)Aluminum 0.060–1.40Boron 0.002–0.020Calcium 0.001–0.003Copper 0.010–0.52Magnesium 0.001–0.10Manganese 0.002–0.65Niobium 0.020–5.5Phosphorous 0.004–0.030Tantalum 0.010–0.050Tin 0.002–0.018Titanium 0.020–3.1Tungsten 0.007–0.11Vanadium 0.010–0.50Zirconium 0.002–0.101.3 This test method has only been interlaboratory tested for the elements and ranges specified. It may be possible to extend this test method to other elements or different quantification ranges provided that method validation is performed that includes evaluation of method sensitivity, precision, and bias as described in this document. Additionally, the validation study must evaluate the acceptability of sample preparation methodology using reference materials or spike recoveries, or both. The user is cautioned to carefully evaluate the validation data against the laboratory’s data quality objectives. Method validation of scope extensions is also a requirement of ISO/IEC 17025.1.4 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. Specific warning statements are given in 8.2.6.3 and safety hazard statements are given in Section 9.1.6 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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4.1 This test method is useful when oils and fats are suspected as an ignition source or a fuel source in a fire.4.1.1 The identification of oil and fat residues in samples from a fire scene can support the field investigator’s opinion regarding the origin and cause of the fire.4.1.2 The positive identification of fatty acid(s) does not necessarily mean that the fire was caused by self heating.4.2 This test method specifically identifies fatty acid derivatives. Oils and fats are comprised primarily of triglycerides (which are fatty acids attached to a glycerol backbone), and some free fatty acids. Free fatty acids and triglycerides are not easily analyzed by the traditional ignitable liquid extraction techniques. Solvent extraction and derivatization to FAME will enable identification by GC-MS.4.2.1 The identification of an individual fatty acid in fire debris samples does not confirm the presence of oils or fats; however, there are times when large quantities of the oil or fat may be extracted. In such cases a more positive identification can be made.4.2.2 Oils and fats containing fatty acids with no double bonds will generally have no tendency to self-heat. With increasing unsaturation (1, 2, and 3 double bonds), the tendency to self-heat also increases, such that polyunsaturated fatty acids (PUFAs), such as C18:3, have a high tendency to self-heat.4.3 This test method is a sensitive separation technique and can detect quantities as small as 3 µL of oil or fat residue in an extract from a debris sample.4.4 This test method shall be performed after all required traditional testing for ignitable liquid residues is completed.4.5 This test method extracts liquids and residues from porous and nonporous materials of various sizes.4.6 This test method can be hampered by coincident extraction of interfering compounds present in the fire debris samples.4.7 This is a destructive technique and whenever possible the entire sample should not be used for the procedure. It is recommended that visual inspection be used to locate portions or areas exhibiting potential oily residue for sub-sampling which would preserve remaining portions for further analyses and also minimize solvent waste. The solvent extracted portions of the sample are not suitable for resampling.4.8 Alternate methods of extraction, derivatization, or analysis exist and may be suitable for use in obtaining similar results and conclusions.4.9 Biodiesel, an ignitable liquid, is a trans-esterified product containing FAMEs. The FAME compounds in biodiesel can be detected in fire debris using many fire debris extraction techniques followed directly by GC-MS analysis. Derivatization is not necessary to identify the FAMEs in biodiesel.4.10 For more information on oils, FAME, and fire debris analysis, see the references listed.3, 4, 5, 61.1 This test method covers the extraction, derivatization, and identification of fatty acids indicative of vegetable oils and fats in fire debris and liquid samples. This procedure will also extract animal oils and fats, as these are similar in chemical composition to vegetable oils and fats. Herein, the phrase “oils and fats” will be used to refer to both animal and vegetable derived oils and fats.1.2 This test method is suitable for successfully extracting oil and fat residues having 8 to 24 carbon atoms.1.3 The identification of a specific type of oil (for example, olive, corn, linseed) requires a quantitative analysis of the fatty acid esters and is beyond the scope of this test method.1.4 This test method cannot replace the requisite knowledge, skills, or abilities acquired through appropriate education, training, and experience and should be used in conjunction with sound professional judgment.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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