5.1 Ash, as determined by this test method, is the residue remaining after burning the coal and coke. Ash obtained differs in composition from the inorganic constituents present in the original coal. Incineration causes an expulsion of all water, the loss of carbon dioxide from carbonates, the conversion of iron pyrites into ferric oxide, and other chemical reactions. Ash, as determined by this test method, will differ in amount from ash produced in furnace operations and other firing systems because incineration conditions influence the chemistry and amount of the ash. References for correcting ash results determined by this test method to a mineral-matter-free basis are listed in Classification D388, Section 9.1.1 This test method covers the determination of the inorganic residue as ash in the analysis sample of coal or coke as prepared in accordance with Practice D2013 or Practice D346. The results obtained can be applied as the ash in the proximate analysis, Practice D3172, and in the ultimate analysis, Practice D3176. For the determination of the constituents in ash, reference is made to Test Methods D3682, D4326, and D6349. Test Methods D6357 should be used to prepare ash to be used for trace element analysis. See Terminology D121 for definition of ash.1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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 Volatile matter, when determined as herein described, can be used to establish the rank of coals, to indicate coke yield on carbonization process, to provide the basis for purchasing and selling, or to establish burning characteristics.1.1 This test method covers the determination of the gaseous products, exclusive of moisture vapor, as volatile matter in the analysis sample of coal or coke from coal.1.2 The test method for the determination of volatile matter is empirical.1.3 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided 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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Determination of sulfur is, by definition, part of the ultimate analysis of coal.Sulfur analysis results obtained by these methods are used to serve a number of interests: evaluation of coal preparation, evaluation of potential sulfur emissions from coal combustion or conversion processes, evaluation of the coal quality in relation to contract specification, and other purposes of commercial or scientific interest.1.1 These test methods cover two alternative procedures for the determination of total sulfur in samples of coal and coke. Sulfur is included in the ultimate analysis of coal and coke.1.2 The procedures appear in the following order: SectionsMethod A—Eschka Method 6-9Method B—Bomb Washing Method 10 and 111.3 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. Specific precautionary statements are given in Sections 11.1.1-11.1.1.7.1.3 The values stated in SI units are to be regarded as the standard.

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1.1 These test methods cover the determination of total carbon and hydrogen in samples of coal or coke. Both the carbon and hydrogen are determined in one operation. These test methods yield the total percentages of carbon and hydrogen in the coal as analyzed and the results include not only the carbon and hydrogen in the organic matter, but also the carbon present in mineral carbonates and the hydrogen present in the free moisture accompanying the sample as well as hydrogen present as water of hydration of silicates.Note 1—It is recognized that certain technical applications of the data derived from this test procedure may justify additional corrections. These corrections could involve compensation for the carbon present as carbonates, the hydrogen of free moisture accompanying the sample, and the calculated hydrogen present as water of hydration of silicates.1.2 When data are converted and reported on the "dry" basis, the hydrogen value is corrected for the hydrogen present in the free moisture accompanying the sample.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.1.4 The values stated in SI units are to be regarded as the standard.

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5.1 The analyzer sample system lag time estimated by this guide can be used in conjunction with the analyzer output to aid in optimizing control of blender facilities or process units. A known and constant lag time is key for the use in optimizing control.5.2 The lag time can be used in the tuning of control programs to set the proper optimization frequency.5.3 The application of this guide is not for the design of a sample system but to help understand the design and to estimate the performance of existing sample systems. Additional detailed information can be found in the references provided in the section entitled Additional Reading Material.1.1 This guide covers the application of routine calculations to estimate sample system lag time, in seconds, for gas, liquid, and mixed phase systems.1.2 This guide considers the sources of lag time from the process sample tap, tap conditioning, sample transport, pre-analysis conditioning and analysis.1.3 Lag times are estimated based on a prediction of flow characteristics, turbulent, non turbulent, or laminar, and the corresponding purge requirements.1.4 Mixed phase systems prevent reliable representative sampling so system lag times should not be used to predict sample representation of a mixed phase stream.1.5 The values stated in inch-pound units are to be regarded as standard. Other units of measurement are included in this standard and Appendix X1 examples where normally seen in industry.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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Nitrogen results obtained by these test methods are required to fulfill the requirements of the ultimate analysis, Practice D 3176. Also, results obtained may be used to evaluate the potential formation of nitrogen oxides as a source of atmospheric pollution.Nitrogen data are used in comparing coals and in research. When the oxygen content of coal is estimated by difference, it is necessary to make a nitrogen determination.1.1 These test methods cover the determination of total nitrogen in samples of coal and coke. The analytical data from these test methods shall be reported as part of ultimate analysis where ultimate analysis is requested. If ultimate analysis is not requested, the value shall be reported according to the request. Two methods are included as follows: SectionsTest Method A—Kjeldahl-Gunning Macro Analysis, with an alternative technique included 9 to 16Test Method B—Kjeldahl-Gunning Semi-Micro Determination 17 to 231.2 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.1.3 The values stated in SI units are to be regarded as the standard.

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5.1 The practice for taking a sample of molten metal during production and producing a chill cast disk, used in conjunction with the following appropriate quantitative spark atomic emission spectrochemical methods, Test Methods E607 and E1251, is suitable for use in manufacturing control or certifying, or both, that the entire lot of alloy sampled meets established composition limits.5.2 The practice for melting a piece of a product to produce a chill cast disk analyzed in conjunction with the following appropriate quantitative spark atomic emission spectrochemical methods, Test Methods E607 and E1251, is suitable, if a representative sample is taken, for determining if the piece sampled meets Aluminum Association composition limits.5.3 The practice for direct analysis of product is suitable for determining an approximate composition of the piece analyzed.1.1 These practices describe procedures for producing a chill cast disk sample from molten aluminum during the production process, and from molten metal produced by melting pieces cut from products.1.2 These practices describe a procedure for obtaining qualitative results by direct analysis of product using spark atomic emission spectrometry.1.3 These practices describe procedures for preparation of samples and products prior to analysis.1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units that are provided for information only and are not considered 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 precautionary statements are given in 6.1 and 7.2.1.6 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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This practice is useful for the preparation of specimens of ore bodies for the analysis of uranium by X-ray emission. Two separate preparation techniques are described.1.1 This practice covers the preparation of uranium ore samples to be analyzed by X-ray emission. Two separate techniques, the glass fusion method or the pressed powder method, may be used.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 problems, 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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4.1 This test method provides a practical estimate of nonburnable residues in commercially available graphite materials. The ash values determined by this test method are of use in comparing the relative purity of various grades of graphite. To facilitate use, this test method institutes simplifications that preclude the ability to determine absolutely the ash values of the test graphite material due to uncontrolled sources of trace contamination.4.2 This test method is not intended for use in determining the ash content of purified graphites, for example, nuclear materials. The relationship between the mineral content of a graphite sample and the ash content of that sample is unknown and is not determined by the application of this test method.1.1 This test method provides a practical determination for the ash content in a graphite sample.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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4.1 This test method is applicable only for determination of the volatile moisture content resulting from adsorption of water vapor from the atmosphere, and is not intended to give representative moisture data for graphite that has been exposed to liquid water contamination.1.1 This test method provides a practical determination for the percentage of moisture in a graphite sample.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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This specification describes the physical requirements and corresponding test methods for disposable glass blood sample capillary tubes for use in microhematocrit procedures. Covered here are two different types of capillary tubes, namely, Type I (coated with heparin), and Type II (uncoated). The tubes shall be fabricated from Type I, Class B borosilicate glass, or Type II soda lime glass. Conversely, the heparin used for coating Type I tubes shall be of ammonium salt isolated from the lungs or intestinal mucosa of beef or pork origin. The tubes shall conform to specified requirements for design, dimension, workmanship, color coding, and lot or control number. They should also pass the following tests for capillarity, fluidity, sheep plasma, positive and negative controls, human whole blood, heparin potency assay, and resistance to centrifugal force.1.1 This specification covers disposable glass blood sample capillary tubes for use in microhematocrit procedures.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 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 provides a standard procedure for the preparation of thermoplastic pavement marking material test specimens prior to testing for various properties as called for in the governing specification. Specimens that are prepared using this standard methodology yield test results that are consistent with the material from which it was sampled. Test results from specimens can be used to determine compliance of the thermoplastic pavement marking material to the specification. This practice can also be used by manufacturers of these materials to prepare specimens for testing to determine the uniformity of thermoplastic pavement marking materials from batch to batch.5.2 This practice does not address any issues related to specific testing of the thermoplastic pavement marking materials for any physical or chemical property.1.1 This practice covers the proper preparation of test specimens of thermoplastic pavement marking materials obtained to ensure test results are representative of the material being tested.1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information 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, 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 Often it is necessary to dissolve the sample, particularly if it is a solid, before atomic spectroscopic measurements. It is advantageous to use a microwave oven for dissolution of such samples since it is a far more rapid way of dissolving the samples instead of using the traditional procedures of dissolving the samples in acid solutions using a pressure decomposition vessel, or other means.5.2 The advantage of microwave dissolution includes faster digestion that results from the high temperature and pressure attained inside the sealed containers. The use of closed vessels also makes it possible to eliminate uncontrolled trace element losses of volatile species that are present in a sample or that are formed during sample dissolution. Volatile elements arsenic, boron, chromium, mercury, antimony, selenium, and tin may be lost with some open vessel acid dissolution procedures. Another advantage of microwave aided dissolution is to have better control of potential contamination in blank as compared to open vessel procedures. This is due to less contamination from laboratory environment, unclean containers, and smaller quantity of reagents used (9).5.3 Because of the differences among various makes and models of satisfactory devices, no detailed operating instructions can be provided. Instead, the analyst should follow the instructions provided by the manufacturer of the particular device.5.4 Mechanism of Microwave Heating—Microwaves have the capability to heat one material much more rapidly than another since materials vary greatly in their ability to absorb microwaves depending upon their polarities. Microwave oven is acting as a source of intense energy to rapidly heat the sample. However, a chemical reaction is still necessary to complete the dissolution of the sample into acid mixtures. Microwave heating is internal as well as external as opposed to the conventional heating which is only external. Better contact between the sample particles and the acids is the key to rapid dissolution. Thus, heavy nonporous materials such as fuel oils or coke are not as efficiently dissolved by microwave heating. Local internal heating taking place on individual particles can result in the rupture of the particles, thus exposing a fresh surface to the reagent contact. Heated dielectric liquids (water/acid) in contact with the dielectric particles generate heat orders of magnitude above the surface of a particle. This can create large thermal convection currents which can agitate and sweep away the stagnant surface layers of dissolved solution and thus, expose fresh surface to fresh solution. Simple microwave heating alone, however, will not break the chemical bonds, since the proton energy is less than the strength of the chemical bond (5).5.4.1 In the electromagnetic irradiation zone, the combination of the acid solution and the electromagnetic radiation results in near complete dissolution of the inorganic constituents in the carbonaceous solids. Evidently, the electromagnetic energy promotes the reaction of the acid with the inorganic constituents thereby facilitating the dissolution of these constituents without destroying any of the carbonaceous material. It is believed that the electromagnetic radiation serves as a source of intense energy which rapidly heats the acid solution and the internal as well as the external portions of the individual particles in the slurry. This rapid and intense internal heating either facilitates the diffusion processes of the inorganic constituents in solution or ruptures the individual particles thereby exposing additional inorganic constituents to the reactive acid. The heat generated in the aqueous liquid itself will vary at different points around the liquid-solid interface and this may create large thermal convection currents which can agitate and sweep away the spent acid solution containing dissolved inorganic constituents from the surface layers of the carbonaceous particles thus exposing the particle surfaces to fresh acid (16).5.4.2 Unlike other heating mechanisms, true control of microwave heating is possible because stopping of the application of energy instantly halts the heating (except the exotherms which can be rapid when pure compounds are digested). The direction of heat flow is reversed from conventional heating, as microwave energy is absorbed by the contents of the container, energy is converted to heat, and the bulk temperature of the contents rises. Heat is transferred from the reagent and sample mixture to the container and dissipated through conduction to the surrounding atmosphere. Newer synthesized containers made up of light yet strong polymers can withstand over 240 °C temperatures and over 800 psi pressure. During the digestion process of samples containing organic compounds, largely insoluble gases such as CO2 are formed. These gases combine with the vapor pressure from the reagents, at any temperature, to produce the total pressure inside the vessel. Since the heat flow from a microwave digestion vessel is reversed from that of resistive devices, the total pressures generated for microwave dissolutions are significantly lower at the same temperature than other comparably heated devices or systems. This means larger samples can be digested at higher temperatures and lower pressures than would normally be expected from such pressurized vessels. Sample size should be controlled to prevent rapid exotherm rupture, exacerbated by excess CO2 generation. However, the pressure limitations of the vessel still restrict both the sample size that can be used and the maximum temperature that can be achieved due to the vapor pressure resulting from the reagents (17).5.4.3 Organic and polymer samples can be especially problematic because they are highly volatile and produce large amounts of gaseous by-products such as CO2 and NOx. As a result larger sample sizes will produce higher pressures inside the digestion vessel. Generally, no more than 1 g of these sample types can be digested in a closed vessel (18).5.4.3.1 While in open digestion vessel systems the operating temperatures are limited by the acid solutions’ boiling points, temperatures in the 200 °C to 260 °C range can be typically achieved in sealed digestion vessels. This results in a dramatic acceleration of the reaction kinetics, allowing the digestion reactions to be carried out in a shorter time period. The higher temperatures, however, result in a pressure increase in the vessel and thus in a potential safety hazard. Rapid heating of the sample solution can induce exothermic reactions during the digestion process. Therefore in modern microwave digestion systems, sensors and interlocks for temperature and pressure control are introduced. Since different types of sample behave differently in microwave field, heating control is necessary in this operation (19).5.4.4 Microwave heating occurs because microwave reactors generate an electromagnetic field that interacts with polarizable molecules or ions in the materials. As the polarized species compete to align their dipoles with the oscillating field, they rotate, migrate, and rub against each other, causing them to heat up. This microwave effect differs from indirect heating by conduction achieved by using a hot plate (20).1.1 This practice covers the procedure for use of microwave radiation for sample decomposition prior to elemental determination by atomic spectroscopy.1.1.1 Although this practice is based on the use of inductively coupled plasma atomic emission spectrometry (ICP-AES) and atomic absorption spectrometry (AAS) as the primary measurement techniques, other atomic spectrometric techniques may be used if lower detection limits are required and the analytical performance criteria are achieved.1.2 This practice is applicable to both petroleum products and lubricants such as greases, additives, lubricating oils, gasolines, and diesels.1.3 Although not a part of Committee D02’s jurisdiction, this practice is also applicable to other fossil fuel products such as coal, fly ash, coal ash, coke, and oil shale.1.3.1 Some examples of actual use of microwave heating for elemental analysis of fossil fuel products and other materials are given in Table 1.(A) The boldface numbers in parentheses refer to the list of references at the end of this standard.1.3.2 Some additional examples of ASTM methods for microwave assisted analysis in the non-fossil fuels area are included in Appendix X1.1.4 During the sample dissolution, the samples may be decomposed with a variety of acid mixture(s). It is beyond the scope of this practice to specify appropriate acid mixtures for all possible combinations of elements present in all types of samples. But if the dissolution results in any visible insoluble material, this practice may not be applicable for the type of sample being analyzed, assuming the insoluble material contains some of the analytes of interest.1.5 It is possible that this microwave-assisted decomposition procedure may lead to a loss of “volatile” elements such as arsenic, boron, chromium, mercury, antimony, selenium, and/or tin from the samples. Chemical species of the elements is also a concern in such dissolutions since some species may not be digested and have a different sample introduction efficiency.1.6 A reference material or suitable NIST Standard Reference Material should be used to confirm the recovery of analytes. If these are not available, the sample should be spiked with a known concentration of analyte prior to microwave digestion.1.7 Additional information on sample preparation procedures for elemental analysis of petroleum products and lubricants can be found in Practice D7455.1.8 The values stated in SI units are to be regarded as 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. Specific warning statements are given in Sections 6 and 7.1.10 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 Sulfates and chlorides may be found in filter plugging deposits and fuel injector deposits. The acceptability for use of the fuel components and the finished fuels depends on the sulfate and chloride content.5.2 Existent and potential inorganic sulfate and total chloride content, as measured by this test method, can be used as one measure of the acceptability of gasoline components for automotive spark-ignition engine fuel use.1.1 This test method covers an ion chromatographic procedure for the determination of the existent inorganic and potential sulfate and total inorganic chloride content in hydrous and anhydrous denatured ethanol to be used in motor fuel applications. It is intended for the analysis of ethanol samples containing between 0.55 mg/kg and 20 mg/kg of existent inorganic sulfate, 4.0 mg/kg to 20 mg/kg of potential inorganic sulfate, and 0.75 mg/kg to 50 mg/kg of total inorganic chloride.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. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage1.4 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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4.1 The purpose of this guide is to provide guidance for selecting appropriate device size(s) and determining appropriate sample size(s) for design verification of endovascular devices. The device size(s) and sample size(s) for each design input requirement should be determined before testing. The device size(s) selected for verification testing should establish that the entire device matrix is able to achieve the design input requirements. If testing is not performed on all device sizes, justification should be provided.4.2 The sample size justification and statistical procedures used to analyze the data should be based on sound scientific principles and should be suitable for reaching a justifiable conclusion. Insufficient sample size may lead to erroneous conclusions more often than desired.4.3 Guidance regarding methodologies for determining device size selection and appropriate sample size is provided in Sections 5 and 6.1.1 This guide provides guidance for selecting an appropriate device size(s) and determining an appropriate sample size(s) (that is, number of samples) for design verification testing of endovascular devices. A methodology is presented to determine which device size(s) should be selected for testing to verify the device design adequately for each design input requirement (that is, test characteristic). Additionally, different statistical approaches are presented and discussed to help guide the developer to determine and justify sample size(s) for the design input requirement being verified. Alternate methodologies for determining device size selection and sample size selection may be acceptable for design verification.1.2 This guide applies to physical design verification testing. This guide addresses in-vitro testing; in-vivo/animal studies are outside the scope of this guide. This guide does not directly address design validation; however, the methodologies presented may be applicable to in-vitro design validation testing. Guidance for sampling related to computational simulation (for example, sensitivity analysis and tolerance analysis) is not provided. Guidance for using models, such as design of experiments (DOE), for design verification testing is not provided. This guide does not address sampling across multiple manufacturing lots as this is typically done as process validation. Special considerations are to be given to certain tests such as fatigue (see Practice E739) and shelf-life testing (see Section 8).1.3 Regulatory guidance may exist for endovascular devices that should be considered for design verification device size and sample size selection.1.4 Units—The values stated in SI units are to be regarded as the 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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