5.1 This test method is intended to provide a tool for assessing whether fuel storage and distribution facilities or end user fuel tanks are subject to microbial growth and alert fuel suppliers or users to the potential for fuel quality or operational problems and/or the requirement for preventative or remedial measures.5.2 This test method detects numbers of microbial colony forming units (CFU), the same detection parameter used in the laboratory standard procedures Practice D6974 and IP 385. However, whereas Practice D6974 and IP 385 provide separate assessment of numbers of viable aerobic bacteria CFU and numbers of viable fungal CFU, this test method provides a combined total count of viable aerobic bacteria and fungal CFU.5.3 This test method is designed to detect a recognized group of microorganisms of significance in relation to contamination of distillate fuels, but it is recognized that microbiological culture techniques do not detect all microorganisms that can be present in a sample. Culturability is affected primarily by the ability of captured microbes to proliferate on the growth medium provided, under specific growth conditions. Consequently, a proportion of the active or inactive microbial population present in a sample can be viable but not detected by any one culture test.7 In this respect, the test is indicative of the extent of microbial contamination in a sample ,and it is assumed that when a fuel sample is significantly contaminated, some of the dominant microbial species present will be quantifiably detected, even if not all species present are culturable.5.4 Many samples from fuel systems can be expected to contain a low level of “background” microbial contamination, which is not necessarily of operational significance. The minimum detection level of this test method is determined by the volume of specimen tested and is set such that microbial contamination will generally only be detected when it is at levels indicative of active proliferation.5.5 The test will detect culturable bacteria and fungi that are metabolically active and dormant fungal spores. Presence of fungal spores in a fuel sample can be indicative of active microbial proliferation within a fuel tank or system, but at a point distant from the location sampled. Active microbial growth only occurs in free water, and this can be present only as isolated pockets at tank or system low points. Because fungal spores are more hydrophobic than active cells and fungal material (mycelium), they disperse more readily in fuel phase and are thus more readily detected when low points cannot be directly sampled and only fuel phase is present in samples.5.6 This test method can determine whether microbial contamination in samples drawn from fuel tanks and systems is absent or present at light, moderate, and heavy levels.5.7 The categorization of light, moderate, and heavy levels of contamination will depend on the fuel type, the sampling location, the facility sampled, and its specific operating circumstances.5.8 Further guidance or interpretation of test results can be found in Guide D6469, in the Energy Institute Guidelines for the investigation of the microbial content of petroleum fuels, and for the implementation of avoidance and remedial strategies and in the IATA Guidance Material on Microbiological Contamination in Aircraft Fuel Tanks.5.8.1 Further guidance on sampling can be found in Practice D7464.5.9 Testing can be conducted on a routine basis or to investigate incidents.5.10 Microbiological tests are not intended to be used to determine compliance with absolute fuel specifications or limits. The implementation of specification limits for microbiological contamination in fuels is generally not appropriate, and microbial contamination levels cannot be used alone or directly to make inferences about fuel quality or fitness for use.5.11 When interpreting results, it must be appreciated that the test result applies only to the specific sample and specimen tested and not necessarily to the bulk fuel. Microbiological contamination usually shows a highly heterogeneous distribution in fuel systems, and therefore, analysis of a single sample will rarely provide a complete assessment of the overall levels of contamination present.5.12 Water phase will usually contain substantially higher numbers of microbial CFU than fuel phase and, consequently, a different interpretation of results is required.1.1 This test method describes a procedure that can be used in the field or in a laboratory to quantify culturable, viable aerobic microorganisms present as contaminants in liquid fuels, including those blended with synthesized hydrocarbons or biofuels, with kinematic viscosities (at 40 °C) of ≤24 mm2 s-1 and heavy and residual fuels with kinematic viscosities (at 40 °C) of ≤700 mm2 s-1 and in fuel-associated water.1.1.1 This test method has been validated by an ILS for a range of middle distillate fuels meeting Specifications D975, D1655, ISO 8217 DMA, and NATO F-76.21.2 This test method quantitatively assesses culturable, viable aerobic microbial content present in the form of bacteria, fungi, and fungal spores. Results are expressed as the total number of microbial colony forming units (CFU)/L of fuel or total number of CFU/mL of associated water. The number of CFU should not be interpreted as absolute values but should be used as part of a diagnostic or condition monitoring effort; for example, these values can be used to assess contamination as absent, light, moderate, or heavy.NOTE 1: This test method is technically equivalent to IP 613, although the two methods are not currently jointed.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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4.1 Bisphenol A is used for production of polycarbonate or epoxy resin. The presence of impurities in bisphenol A is undesirable because they may slow down the polymerization and be impurities in the final product.4.2 Determination of the trace impurities, such as isomer of bisphenol A and the unreacted raw material, is often required. This test method is suitable for setting specifications and for using as an internal quality control where these products are produced or used.4.3 Purity is commonly reported by subtracting the determined expected impurities and water from 100 %. However, a HPLC analysis cannot determine absolute purity if unknown components are contained within the material being examined.1.1 This test method covers the determination of trace impurities in bisphenol A (4,4′-Isopropylidenediphenol) by reverse-phase gradient high performance liquid chromatography (HPLC). It is generally meant for the analysis of bisphenol A of 99.5 % or greater.1.2 This method is applicable to bisphenol A samples containing impurity concentration between 2 and 400 mg/kg. Users of this method believe it is linear over a wider range.1.3 In determining the conformance of the test results using this method to applicable specification, results shall be rounded off in accordance with the rounding-off method of Practice E29.1.4 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. For a specific hazard statement, see Section 8.1.6 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 This test method is widely used for specification purposes and is considered of value in estimating the oxidation stability of lubricants, especially those that are prone to water contamination. It should be recognized, however, that correlation between results of this method and the oxidation stability of a lubricant in field service may vary markedly with field service conditions and with various lubricants. The precision statement for this method was determined on steam turbine oils.NOTE 1: Furthermore, in the course of testing a lubricant by this method, other signs of deterioration, such as sludge formation or catalyst coil corrosion, may appear that are not reflected in the calculated oxidation lifetime. The subcommittee responsible for this method is investigating the application of alternative criteria for evaluation of lubricants using this test apparatus. Test Method D4310 is now available for sludge measurement.1.1 This test method covers the evaluation of the oxidation stability of inhibited steam-turbine oils in the presence of oxygen, water, and copper and iron metals at an elevated temperature. This test method is limited to a maximum testing time of 10 000 h. This test method is also used for testing other oils, such as hydraulic oils and circulating oils having a specific gravity less than that of water and containing rust and oxidation inhibitors.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.2.1 Exception—The values in parentheses in the figures are provided for information for those using old equipment based on non-SI units.1.3 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.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. For specific warning statements, see Section 7.1.5 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 As with conventional radiography, radioscopic examination is broadly applicable to any material or examination object through which a beam of penetrating radiation may be passed and detected including metals, plastics, ceramics, composites, and other nonmetallic materials. In addition to the benefits normally associated with radiography, radioscopic examination may be either a dynamic, filmless technique allowing the examination part to be manipulated and imaging parameters optimized while the object is undergoing examination, or a static, filmless technique wherein the examination part is stationary with respect to the X-ray beam. Systems with digital detector arrays (DDAs) or an analog component such as an electro-optic device or an analog camera may be used in dynamic mode. If achievable video rates are not adequate to examine features of interest in dynamic mode then averaging techniques with no movement of the test object shall be used – in this case, if using a DDA, Practice E2698 shall be used. If used with a high speed camera system, the user must be aware of the various image conversion materials decay time such that the converter signal can change as fast or faster than the frame rate. Linear Detector Arrays (LDAs) and flying spot systems may be considered radioscopic configurations as they are included in as shown in Guide E1000.5.2 This practice establishes the basic parameters for the application and control of the radioscopic examination method. This practice is written so it can be specified on the engineering drawing, specification, or contract.5.3 Weld Examination—Additional information on radioscopic weld examination may be found in Practice E1416.5.4 Casting Examination—Additional information on radioscopic casting examination may be found in Practice E1734.5.5 Electronic Components—Radioscopic examination of electronic components shall comply with Practice E1161.5.6 Explosives and Propellants—Radioscopic examination of explosives/propellant components shall comply with Practice E1742 Annex A3.5.7 Part-Specific Examination Technique—A detailed written procedure including a part-specific examination technique shall be prepared for each part, or group of parts, and shall be approved by the Cognizant Radiographic Level 3.5.8 Personnel Qualification—Personnel performing radioscopic examinations and interpretations to this practice shall be qualified in accordance with a nationally or internationally recognized NDT personnel qualification practice or standard and certified by the employer or certifying agency as applicable. Other equivalent qualification documents may be used when specified on the contract or purchase order. The applicable revision shall be the latest unless otherwise specified in the contractual agreement between parties.5.9 Agency Evaluation—If specified in the contractual agreement, the NDT supplier shall be qualified and evaluated in accordance with Practice E543. The applicable revision of Practice E543 shall be specified in the contractual agreement.1.1 This practice2 covers application details for radioscopic examination using penetrating radiation using an analog component such as an electro-optic device (for example, X-ray image intensifier (XRII) or analog camera, or both) or a Digital Detector Array (DDA) used in dynamic mode radioscopy. Radioscopy is a radiographic technique that can be used in (1) dynamic mode radioscopy to track motion or optimize radiographic parameters in real-time, or both (25 to 30 frames per second), near real-time (a few frames per second), or high speed (hundreds to thousands of frames per second) or (2) static mode radioscopy where there is no motion of the object during exposure as a filmless recording medium. This practice is not to be used for static mode radioscopy using DDAs. If static radioscopy using a DDA (that is, DDA radiography) is being performed, use Practice E2698.1.1.1 This practice also may be used for Linear Detector Array (LDA) applications where an LDA uses relative perpendicular motion of either the detector or component under examination to build an image line by line.1.1.2 This practice may also be used for “flying spot” applications where a pencil beam of X-rays rasters over an area to build an image point by point.1.2 This practice establishes the minimum requirements for radioscopic examination of metallic and non-metallic materials using X-ray or gamma radiation. Since the techniques involved and the applications for radioscopic examination are diverse, this practice is not intended to be limiting or restrictive, but rather to address the general applications of the technology and thereby facilitate its use. Refer to Guides E94 and E1000, and Terminology E1316, provide additional information and guidance.1.3 Basis of Application: 1.3.1 The requirements of this practice and Practice E1411 shall be used together. The requirements of Practice E1411 will provide the performance qualification and long-term stability test procedures for the radioscopic system. The user of the radioscopic system shall establish a written procedure that addresses the specific requirements and tests to be used in their application and shall be approved by the Cognizant Radiographic Level 3 before examination of production hardware. There are areas (listed below 1.3.1.1 – 1.3.1.14) in this practice that may require agreement between the cognizant engineering organization and the radioscopy supplier, or specific direction from the cognizant engineering organization. These items should be addressed in the purchase order or the contract.1.3.1.1 Systems, equipment, and materials that do not comply with this Practice (1.5);1.3.1.2 Modified tests and/or gauges when using a gamma source or radiation energy above 320 kV (1.6);1.3.1.3 Personnel qualification and certification (5.8);1.3.1.4 Qualification of the NDT supplier (5.9);1.3.1.5 Alternate image displays (6.1.3.1);1.3.1.6 Alternate image quality indicator (IQI) types (6.1.6.5);1.3.1.7 Non-requirement for IQI (8.9.7);1.3.1.8 Examination record archiving, hard copy, and recording (6.1.10);1.3.1.9 Radioscopic quality levels (8.8.1.16);1.3.1.10 Total image unsharpness (8.8.1.15);1.3.1.11 Performance verification (9.3);1.3.1.12 Interpreter duty and rest periods (10.2);1.3.1.13 Examination report (11.1);1.3.1.14 Retention and storage of radiographs (6.1.10, 8.16, and 11.1);1.3.2 Appendix X1 may be used to fulfill existing contracts that use Appendix X1 or the former Annex A1. The former mandatory Annex A1 “DEPARTMENT OF DEFENSE CONTRACTS, SUPPLEMENTAL REQUIREMENTS” was deleted and the detailed requirements are appended now in the non-mandatory Appendix X1.1.4 This practice also requires the user to perform a technique qualification suitable for its intended purpose and to issue a system qualification report (see 9.7). Additionally, the user shall develop part specific inspection procedures (see Section 8).1.5 Compliance—Systems, equipment, and materials that do not comply with this practice shall require approval from the Cognizant Engineering Organization (CEO).1.6 The general principles discussed in this practice apply broadly to penetrating radiation radioscopic systems. However, this document is written specifically for use with X-ray and gamma-ray systems. Other radioscopic systems, such as those employing neutrons, will involve equipment and application details unique to such systems.1.7 The user of this practice shall note that X-ray energies higher than 320 keV may require modified or different methods other than those described within this practice.1.8 Units—The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard. Where applicable, SI units are shown in brackets [xx].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. For specific safety statements, see Section 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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4.1 Advantages of Electrolytic Polishing: 4.1.1 For some metals, a high quality surface finish can be produced that is equivalent to, or better than, that which can be obtained by mechanical methods.4.1.2 Once procedures have been established, satisfactory results can be obtained rapidly with reproducibility.4.1.3 There can be a marked saving of time if many specimens of the same material are polished sequentially.4.1.4 Electropolishing a selected area on the surface of a relatively large metal part can be accomplished nondestructively, that is, without the need for sectioning to remove a piece.4.1.5 Soft, single-phase metals, which may be difficult to polish by mechanical methods, may be successfully electropolished.4.1.6 The true microstructure of a specimen can be obtained because artifacts (such as disturbed metal, scratches, and mechanical twins) produced on the surface, even by careful grinding and mechanical polishing operations, can be removed. These features are important in low-load hardness testing, X-ray diffraction studies, and in electron microscopy, where higher resolution puts a premium on undistorted metal surfaces.4.1.7 After electropolishing is completed, etching can often be accomplished by reducing the voltage (generally to about one-tenth that required for polishing) for a short time before it is turned off.NOTE 2: Not all electropolishing solutions produce good etching results.4.2 Disadvantages of Electrolytic Polishing: 4.2.1 Many of the chemical mixtures used in electropolishing are poisonous or dangerous if not properly handled (see Section 5). These hazards are similar to those involved in the mixing and handling of etchants, see Test Methods E407.4.2.2 In multi-phase alloys, the polishing rate of each phase may be different. The result may be a non-planar surface.4.2.3 Electropolished surfaces may be slightly undulated rather than perfectly planar and, therefore, may not be suitable for examination at all magnifications.4.2.4 The rate of polishing in areas adjacent to various inhomogeneities, such as nonmetallic inclusions and voids, is usually greater than that in the surrounding matrix and tends to exaggerate the size of the inclusions and voids.4.2.5 Dimples, pits, and waviness limit applications involving surface phenomena, coatings, interfaces, and cracks. Edges tend to be attacked preferentially, resulting in edge rounding.4.2.6 Artifacts may be produced by electropolishing.4.2.7 Specimen mounting materials may react with the electrolyte.4.2.8 The electropolished surfaces of certain materials may be passive and difficult to etch.4.2.9 Metal removal rates by electropolishing are usually quite low, typically about 1 μm/min, and all of the prior induced damage from cutting and grinding may not be removed if preparation is stopped after a 600-grit SiC grind and electropolishing times are short.4.2.10 A large number of electrolytes may be needed to polish the variety of metals encountered by a given laboratory. Considerable time may be required to develop a procedure for a new alloy.1.1 This guide deals with electrolytic polishing as a means of preparation of specimens for metallographic purposes. Procedures are described for polishing a variety of metals.NOTE 1: References (1-133)2 on electrolytic polishing will provide the reader with specific information beyond the scope of this guide.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. Specific safety precautions are described in Section 5 and 6.3.1.1.4 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 TSCs are susceptible to the formation of porosity due to a lack of fusion between sprayed particles or the expansion of gases generated during the spraying process. The determination of area percent porosity is important in order to monitor the effect of variable spray parameters and the suitability of a coating for its intended purpose. Depending on application, some or none of this porosity may be tolerable.4.2 These test methods cover the determination of the area percentage porosity of TSCs. Method A is a manual, direct comparison method utilizing the seven standard images in Figs. 1-7 which depict typical distributions of porosity in TSCs. Method B is an automated technique requiring the use of a computerized image analyzer.FIG. 1 —  0.5 % PorosityFIG. 2 —  1.0 % PorosityFIG. 3 —  2.0 % PorosityFIG. 4 —  5.0 % PorosityFIG. 5 —  8.0 % PorosityFIG. 6 —  10.0 % PorosityFIG. 7 —  15.0 % Porosity4.3 These methods quantify area percent porosity only on the basis of light reflectivity from a metallographically polished cross section. See Guide E1920 for recommended metallographic preparation procedures.4.4 The person using these test methods must be familiar with the visual features of TSCs and be able to determine differences between inherent porosity and oxides. The individual must be aware of the possible types of artifacts that may be created during sectioning and specimen preparation, for example, pullouts and smearing, so that results are reported only on properly prepared specimens. Examples of properly prepared specimens are shown in Figs. 8-10. If there are doubts as to the integrity of the specimen preparation it is suggested that other means be used to confirm microstructural features. This may include energy dispersive spectroscopy (EDS), wavelength dispersive spectroscopy (WDS) or cryogenic fracture of the coating followed by analysis of the fractured surfaces with a scanning electron microscope (SEM).FIG. 8 Ni/Al TSC—500XNOTE 1: V = void, O = oxide, L = linear detachmentFIG. 9 Monel TSC—200XNOTE 1: V = void, G = embedded grit, L = linear detachmentFIG. 10 Alloy 625 TSC—200XNOTE 1: V = void, O = oxide, G = embedded grit1.1 These test methods cover procedures to perform porosity ratings on metallographic specimens of thermal sprayed coatings (TSCs) prepared in accordance with Guide E1920 by direct comparison to standard images and via the use of automatic image analysis equipment.1.2 These test methods deal only with recommended measuring methods and nothing in them should be construed as defining or establishing limits of acceptability for any measured value of porosity.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 The angular distribution of scatter is a property of surfaces that may have direct consequences on an intermediate or final application of that surface. Scatter defines many visual appearance attributes of materials, and specification of the distribution and wavelength dependence is critical to the marketability of consumer products, such as automobiles, cosmetics, and electronics. Optically diffusive materials are used in information display applications to spread light from display elements to the viewer, and the performance of such displays relies on specification of the distribution of scatter. Stray-light reduction elements, such as baffles and walls, rely on absorbing coatings that have low diffuse reflectances. Scatter from mirrors, lenses, filters, windows, and other components can limit resolution and contrast in optical systems, such as telescopes, ring laser gyros, and microscopes.4.2 The microstructure associated with a material affects the angular distribution of scatter, and specific properties can often be inferred from measurements of that scatter. For example, roughness, material inhomogeneity, and particles on smooth surfaces contribute to optical scatter, and optical scatter can be used to detect the presence of such defects.4.3 The angular distribution of scattered light can be used to simulate or render the appearance of materials. Quality of rendering relies heavily upon accurate measurement of the light scattering properties of the materials being rendered.1.1 This practice describes procedures for determining the amount and angular distribution of optical scatter from a surface. In particular it focuses on measurement of the bidirectional scattering distribution function (BSDF). BSDF is a convenient and well accepted means of expressing optical scatter levels for many purposes. It is often referred to as the bidirectional reflectance distribution function (BRDF) when considering reflective scatter or the bidirectional transmittance distribution function (BTDF) when considering transmissive scatter.1.2 The BSDF is a fundamental description of the appearance of a sample, and many other appearance attributes (such as gloss, haze, and color) can be represented in terms of integrals of the BSDF over specific geometric and spectral conditions.1.3 This practice also presents alternative ways of presenting angle-resolved optical scatter results, including directional reflectance factor, directional transmittance factor, and differential scattering function.1.4 This practice applies to BSDF measurements on opaque, translucent, or transparent samples.1.5 The wavelengths for which this practice applies include the ultraviolet, visible, and infrared regions. Difficulty in obtaining appropriate sources, detectors, and low scatter optics complicates its practical application at wavelengths less than about 0.2 µm (200 nm). Diffraction effects start to become important for wavelengths greater than 15 µm (15 000 nm), which complicate its practical application at longer wavelengths. Measurements pertaining to visual appearance are restricted to the visible wavelength region.1.6 This practice does not apply to materials exhibiting significant fluorescence.1.7 This practice applies to flat or curved samples of arbitrary shape. However, only a flat sample is addressed in the discussion and examples. It is the user’s responsibility to define an appropriate sample coordinate system to specify the measurement location on the sample surface and appropriate beam properties for samples that are not flat.1.8 This practice does not provide a method for ascribing the measured BSDF to any scattering mechanism or source.1.9 This practice does not provide a method to extrapolate data from one wavelength, scattering geometry, sample location, or polarization to any other wavelength, scattering geometry, sample location, or polarization. The user must make measurements at the wavelengths, scattering geometries, sample locations, and polarizations that are of interest to his or her application.1.10 Any parameter can be varied in a measurement sequence. Parameters that remain constant during a measurement sequence are reported as either header information in the tabulated data set or in an associated document.1.11 The apparatus and measurement procedure are generic, so that specific instruments are neither excluded nor implied in the use of this practice.1.12 For measurements performed for the semiconductor industry, the operator should consult Guide SEMI ME 1392.1.13 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.1.14 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 Building products made with caulks and sealants are often used for applications for which Test Method E84 is used for compliance with building code, life safety code or mechanical code requirements. This practice describes, in detail, specimen mounting procedures for those caulks and sealants which are not able to be supported by their own structural characteristics during the test.5.2 Codes are often silent with regard to testing caulks and sealants for the assessment of flame spread index and smoke developed index as surface burning characteristics. This practice describes specimen preparation and mounting procedures for such materials and products.5.3 The material shall be representative of the materials used in actual field installations.5.4 The limitations for this procedure are those associated with Test Method E84.1.1 This practice describes procedures for specimen preparation and mounting when testing caulks and sealants to assess flame spread and smoke development as surface burning characteristics using Test Method E84.1.1.1 Caulks and sealants up to 8 in. (203.2 mm) in width shall follow the requirements of 7.1.1.1.2 Caulks and sealants in excess of 8 in. (203.2 mm) in width shall follow the requirements of 7.2.1.1.2.1 Caulks and sealants in excess of 8 in. (203.2 mm) in width can be considered coatings.1.2 This practice applies to caulks and sealants intended for various uses within buildings. The caulks and sealants addressed in this practice are not able to be supported by their own structural characteristics during the test.1.2.1 This practice does not apply to adhesives that are used to adhere or bind together surfaces. Annex A12 of Test Method E84 provides a procedure for testing adhesives.1.3 Testing is conducted in accordance with Test Method E84.1.4 This practice does not provide pass/fail criteria that can be used as a regulatory tool.1.5 This practice does not apply to materials for which the test specimen does not remain in place before and during the test until maximum flame propagation has occurred.1.6 This practice is not for system evaluation. It is for the comparison of the materials only.1.7 The results obtained by using this mounting procedure are confined to the materials themselves as tested and are not comparable to those obtained with materials that are tested in a full tunnel width application.1.8 This fire standard cannot be used to provide quantitative measures.1.9 Fire testing is inherently hazardous. Adequate safeguards for personnel and property shall be employed in conducting these tests.1.10 This standard gives instructions on specimen preparation and mounting, but the fire-test-response method is given in Test Method E84. See also Section 9.1.11 The text of this standard references notes and footnotes which provide explanatory material. These notes and footnotes shall not be considered requirements of the standard.1.12 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.1.13 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.1.14 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 document provides guidance for the implementation of procedures for the preparation, testing, and documentation of an in-house reference material (hereafter called an iRM) to be used for a number of purposes, enumerated in the following document, associated with development, validation, and control of chemical and physical measurement processes.4.2 This guide is primarily concerned with characterization of the chemical compositions of metals, ores, and related materials. For all these materials, there is a continuing, strong demand for reference materials (RMs) that is difficult for metrology institutes and private certified reference material (CRM) developers to meet because CRM development requires substantial investments of time and money. The metals and mining industries consume RMs and create new product and by-product compositions at high rates. They use analytical methods that provide rapid and accurate determinations, and both quality assurance and quality control can be maintained using efficient procedures provided appropriate iRMs are available.4.3 The user of this guide must recognize that development of an iRM for any purpose carries with it the responsibility to design and execute the development process correctly, and to document the process thoroughly. In addition, the user of an iRM bears the responsibility for correct use of the iRM material within its design limitations.4.4 This guide contains discussions on material selection and sampling for RMs with some attention given to conversion to the final forms.4.5 The use of iRMs is appropriate for control chart procedures to demonstrate that chemical measurement processes are under statistical control. This function requires demonstration of sufficient homogeneity of a material, but it does not require assignment of chemical and physical property values with associated, exhaustively evaluated uncertainties.4.6 The use of iRMs is appropriate for calibration of test methods and evaluation of calibrations in several ways, including checking for bias, systematic testing of corrections for matrix effects, and testing of sample preparation procedures. See Section 6. This guide provides explanations of general cases in which an iRM can be used as part of a validation process (see Guide E2857).4.7 Because this document is a standard guide, it is intended to educate those who are involved in laboratory operation, quality system development and maintenance, and accreditation of laboratory operations within the scope of a quality system. However, this guide does not constitute requirements for assessment and accreditation.1.1 This document provides guidance for the implementation of procedures for preparation of in-house reference materials for analytical testing of metals, ores, slags, and other materials encountered within the metals and mining industries.1.2 This guide is applicable to the production of reference materials only (usually for internal use) and does not apply to the production of certified reference materials (CRMs). Materials may include metals, alloys, minerals, geological materials, manufacturing intermediates, and byproducts. Samples may be in a number of physical forms including blocks, disks, rods, wires, chips, granules, powders, and liquids.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 guide presents techniques and guidance for evaluating and assuring homogeneity of individual samples or bulk materials and can be used for either interlaboratory or intra-laboratory studies. The types of studies include, but are not limited to, studies to determine precision estimates for test methods, proficiency testing programs, and studies related to quality control of testing within a single laboratory.5.2 Because the test results of any laboratory study are affected by the quality of the samples tested, producing homogeneous samples and determining the degree of homogeneity is important for interpreting the results of the study.5.3 Five techniques are presented in this guide to evaluate sample homogeneity for a range of circumstances and degrees of rigor. The circumstances under which the studies are conducted and the degree of rigor required may differ. The user should consider the circumstances listed in each technique to determine which is appropriate for the study at hand.5.4 Each of the Techniques 1, 2, and 3 provides a procedure for testing and evaluating sample homogeneity when replicate testing of the samples is possible. Technique 4 provides a plan to evaluate sample homogeneity when replicate testing is not possible. Technique 5 recommends practices for producing homogeneous samples for circumstances when homogeneity testing is not possible.5.5 When the conditions of adequate within-sample homogeneity and between-sample homogeneity are satisfied, any differences in test results on multiple samples can reasonably be attributed to testing variation and not due to sample variation.5.6 When differences within or between samples are discovered and the samples are deemed insufficiently homogeneous, the sample preparation process can be improved or corrected and a new set of samples can be prepared. Or, in cases where the sample homogeneity cannot be improved or for other reasons when the samples must be used, the method of evaluation for the laboratory study should account for the effect of differences between samples.5.7 When used in conjunction with studies to develop precision estimates, the guidance in this standard can be used to help quantify sources of test variation (such as effects due to sampling, test method repeatability, and the degree of inhomogeneity) and, therefore, can be useful for determining and stating the conditions under which the precision estimates are valid.5.8 For proficiency testing programs, the guidance in this standard can provide information to prevent laboratories from being unfairly penalized for testing variation due to inherent differences between samples.5.9 In a single laboratory, the guidance in this standard could be used to evaluate the homogeneity of samples for studies to measure test variation over time or for studies to compare the results of tests performed by different technicians.5.10 To minimize the resources required for homogeneity testing, a testing design using a minimum of ten samples with two replicate tests performed on each sample is recommended in Techniques 1, 2, and 3 of this guide. This test design is used in other international standards. See Ref (1)4 and ISO 13528. Technique 4, used when replicate testing is not possible, similarly recommends testing a minimum of ten samples. That does not preclude the use of more than ten samples or more than two replicates.NOTE 1: The spreadsheets provided in this guide for the examples in Techniques 1, 2, and 3 show the calculations when two replicate tests are performed on each sample. The spreadsheets shown for Techniques 1 and 2 may be adjusted using the equations provided in the text when more than two replicate tests are used. Use of Technique 3, as presented in Section 9, is limited to duplicate testing (that is, k = 2). To use Technique 3 when k > 2, preliminary testing for consistency of replicate results can be performed using the general form of the Cochran’s Test as presented in Technique 1, and the homogeneity analysis can be performed as described in the Appendix, X4.3. Also, if desired, the homogeneity criterion in Technique 3 can be used with the calculations using the spreadsheets shown in Technique 2.5.11 This guide is not sufficient for evaluation of certified reference materials (CRMs) or materials used for calibration. Even though homogeneity is required for CRMs, CRMs and calibration materials are typically subject to additional requirements (such as traceability and estimates of uncertainty) that are not addressed in this guide.1.1 This guide presents techniques and guidance for evaluating and assuring homogeneity of individual samples and bulk materials used for interlaboratory and intra-laboratory studies.1.2 This guide is applicable to samples and reference materials used for proficiency testing programs and for interlaboratory studies to determine precision estimates for test methods. It may also be useful for activities related to quality control of testing within a single laboratory.1.3 Five techniques are presented for assessing sample homogeneity. The five techniques are not an exhaustive list of available techniques for assessing homogeneity of samples, but the techniques were chosen to cover a range of circumstances (and various degrees of rigor required) for laboratory studies of various types and purposes.1.4 Each of the first four techniques provides a scheme for testing for homogeneity and a statistical procedure for evaluating the results of the homogeneity testing. The circumstances are described for which each of the techniques is suited.1.5 For circumstances when homogeneity testing is not possible, the fifth technique provides guidance for producing homogeneous samples.1.6 The appendixes of this guide provide example spreadsheets for Techniques 1, 2, 3, and 4.1.7 This guide is not intended for evaluation of certified reference materials (CRMs) or materials used for calibration.1.8 Units—The system of units for this standard is not specified. Dimensional quantities in the standard are presented only as illustrations of calculation methods. The examples are not binding on products or test methods treated.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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