5.1 Petroleum products may contain elements either in trace concentrations (for example, ng/g (ppb mass)) or in minor to major levels (ppm to mass %). These elements might be characteristic of the crude petroleum or might originate from specific inclusions of additives for beneficial effect in the refined product. Often, such additives have product specifications which control the quality of a product in commerce. Hence, it is important to determine these elements as accurately as possible. Other elements present at trace levels may be harmful to combustion engines causing wear or reduced performance, may cause poisoning of catalysts, or may be of environmental concern as combustion emissions. ICP-MS instrumentation is well-suited for determining these elements and is particularly useful for the determination of the trace level elements that may not be readily achieved by other techniques.5.2 Various elemental analytical techniques such as atomic absorption spectrometry (AAS), for example, Test Method D3605 and D4628; inductively coupled plasma atomic emission spectrometry (ICP-AES), for example, Test Methods D7111, D4951, and D5185; X-ray fluorescence (XRF), for example, Practice D7343, Test Method D7220, Test Methods D4927, and Test Method D6443; or graphite furnace atomic absorption spectrometry (GFAAS), for example, Test Method D6732 are used for this purpose. This test method is the first example where ICP-MS is used for elemental analysis of petroleum products.5.3 This test method covers the rapid determination of seven elements in distillate petroleum products. Test times approximate a few minutes per test specimen, and quantification for most elements is in the low to sub ng/g (ppb mass) range. High analysis sensitivity can be achieved for some elements that are difficult to determine by other techniques.1.1 This test method describes the procedure for the determination of trace elements in light and middle distillate petroleum products using inductively coupled plasma mass spectrometry (ICP-MS).1.2 This test method should be used by analysts experienced in the use of inductively coupled plasma mass spectrometry (ICP-MS) with knowledge of interpretation of spectral, isobaric, polyatomic, and matrix interferences, as well as procedures for their correction or reduction.1.3 The table in 6.1 lists elements for which the test method applies along with recommended isotope. Actual working detection limits are sample dependent and, as the sample matrix varies, these detection limits may also vary.1.4 The concentration range of this test method is typically from low to sub ng/g (ppb mass) to 1000 ng/g (ppb mass), however the precision and bias statement is specified for a smaller concentration range based on test samples analyzed in the ILS, see the table in Section 18. The test method may be used for concentrations outside of this range; however, the precision statements may not be applicable.1.4.1 This test method shall be further developed to extend that table to include additional elements.1.5 This test method uses metallo-organic standards (organometallic or organosoluble metal complex) for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent, and low results are obtained for particles larger than a few micrometers as these particles may settle out in the sample container and are not effectively transported through the sample introduction system.1.6 Elements present at concentrations above the upper limit of the calibration curves can be determined with additional, appropriate dilutions and with no degradation of precision.1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.8 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 warning statements are given in 8.2, 8.7, and Section 9.1.9 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 Some oils are formulated with organo-metallic additives which act as detergents, antioxidants, antiwear agents, and so forth. Some of these additives contain one or more of these elements: barium, calcium, phosphorus, sulfur, and zinc. These test methods provide a means of determining the concentration of these elements which in turn provides an indication of the additive content of these oils.4.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (see Table 2).1.1 These test methods cover the determination of barium, calcium, phosphorus, sulfur, and zinc in unused lubricating oils at element concentration ranges shown in Table 1. The range can be extended to higher concentrations by dilution of sample specimens. Additives can also be determined after dilution. Two different methods are presented in these test methods.1.2 Test Method A (Internal Standard Procedure)—Internal standards are used to compensate for interelement effects of X-ray excitation and fluorescence (see Sections 8 through 13).1.3 Test Method B (Mathematical Correction Procedure)—The measured X-ray fluorescence intensity for a given element is mathematically corrected for potential interference from other elements present in the sample (see Sections 14 through 19).1.4 The preferred concentration units are mass % barium, calcium, phosphorus, sulfur, or zinc.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 It has been shown in many industries that separating information regarding small or dissolved elemental materials in the lubricant from suspended particulate is crucial. In many cases only an overall elemental analysis is provided, which may not capture significant wear or even machinery failure events. Such events are often accompanied by a sudden increase in the production of large particulate, which is suspended in and can be detected in the machinery’s lubricant. This test method specifically targets such particulate, which has historically been difficult to quantify. Users of the technique include numerous military organizations, and maintainers of wind turbines, nuclear power facilities, and offshore rigs.1.1 This automatic wear particle analysis2 test method for in-service lubricants describes using a combination of pore blockage particle counting and energy dispersive X-ray fluorescence (EDXRF) spectrometry for the quantitative determination of solid particle counts larger than four (4) micrometres, and elemental content of suspended particulate of iron (Fe) and copper (Cu) in such lubricants.1.2 This test method provides for the determination of the elemental content of suspended particulate of Fe greater than 4 μm in the range of 6 mg/kg to 223 mg/kg. Suspended particulate of copper greater than 4 μm is determined in the range of 3.5 mg/kg to 92.4 mg/kg in the lubricant. Total particle count greater than 4 μm is determined in the range of 11 495 particles/mL greater than 4 μm to 2 169 500 particles/mL greater than 4 μm in the lubricant.1.3 This test method is applicable to all known in-service lubricants (API Groups I-V) at any stage of degradation.1.4 This test method uses an empirical inter-element correction methodology.1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Crude oil, petroleum, petroleum products, additives, biofuels, and lubricants are routinely analyzed for their elemental content such as chlorine, nitrogen, hydrogen, phosphorus, sulfur, and various metals using a variety of analytical techniques. Some of these methods require little to no method calibration; some others require only simple one step calibration; while others require elaborate calibration routine before the product is analyzed for its elemental content.5.2 Fairly often it can be shown that the round robin results by a co-operator are all biased with respect to those from other laboratories. Presumably, the failure to follow good laboratory practices and instructions in the test methods can be a causal factor of such errors. A further consequence is an unnecessarily large reproducibility estimate or the data being dropped from the study as an outlier.5.2.1 Another cause of such discrepancies could be different or inadequate calibration practice used in the laboratory. Most test methods spell out the calibration requirements but often do not quote the frequency required letting the laboratories use good laboratory practices for this task. Thus, uniform practice for instrument calibration would be beneficial in standardizing the test procedures and obtaining consistent results across the laboratories.5.3 Committee D02 has already issued standard practices for uniform sample preparation (D7455), standard operating procedures for ICP-AES (D7260) and XRF (D7343) as well as standard quality assurance protocol (D6792). This guide should be considered as a continuing effort on behalf of this subcommittee to achieve standardized practices in all parts of an analytical sequence.1.1 This guide covers different ways by which the test methods used for elemental analysis of petroleum product and lubricant samples are calibrated before the sample analysis.1.2 Uniform practice for test method calibration is beneficial in standardizing the procedures, and obtaining consistent results across different laboratories.1.3 This guide includes only the basic steps for generally encountered instrument types. Anything out of the ordinary may require special procedures. See individual test methods for instructions to handle such situations.1.4 This guide is not a substitute for a thorough understanding of the actual test method to be used, caveats it contains, and additional instrument preparation that may be required.1.5 The user should not expand the scope of the test methods to materials or concentrations outside the scope of the test methods being used.1.6 This guide should also be applicable to sample preparation of non-petroleum based bio-fuels for elemental analysis. Work is underway on these aspects in Subcommittee D02.03. As more information becomes available, it will be added to this standard.1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.8 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.1.9 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 Elemental analysis serves as a quality control measure for post-reactor studies, for additive levels in formulated resins, and for finished products. X-ray fluorescence spectrometry is an accurate and relatively fast method to determine mass fractions of multiple elements in polyethylene and polypropylene materials.1.1 This test method covers a general procedure for the determination of elemental content in polyolefins by wavelength-dispersive X-ray fluorescence (WDXRF) spectrometry, in mass fraction ranges typical of those contributed by additives, catalysts, and reactor processes. The elements covered by this test method include fluorine, sodium, magnesium, aluminum, silicon, phosphorus, sulfur, calcium, titanium, chromium, and zinc in the composition ranges given in Table 1.1.1.1 This test method does not apply to polymers specifically formulated to contain flame retardants including brominated compounds and antimony trioxide.1.1.2 This test method does not apply to polymers formulated to contain high levels of compounds of vanadium, molybdenum, cadmium, tin, barium, lead, and mercury because the performance can be strongly influenced by spectral interferences or interelement effects due to these elements.NOTE 1: Specific methods and capabilities of users may vary with differences in interelement effects and sensitivities, instrumentation and applications software, and practices between laboratories. Development and use of test procedures to measure particular elements, mass fraction ranges or matrices is the responsibility of individual users.NOTE 2: One general method is outlined herein; alternative analytical practices can be followed, and are attached in notes, where appropriate.1.2 The values stated in SI units are to be regarded as the 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 precautionary statements are given in Section 10.NOTE 3: There is no known ISO equivalent to this standard.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 The measurement of particle-bound, oxidized, elemental, and total mercury in stationary-source flue gases provides data that can be used for emissions assessments and reporting, the certification of continuous mercury monitoring systems, regulatory compliance determinations and research programs associated with dispersion modeling, deposition evaluation, human health and environmental impact assessments. Particle-bound, oxidized, and elemental mercury measurements before and after control devices may be necessary for optimizing and evaluating the mercury removal efficiency of emission control technologies.5.2 This test method was developed for the measurement of mercury in coal-fired power plants and has been extensively validated for that application. With additional procedures given in this standard, it is also applicable to sources having a flue gas composition with high levels of hydrochloric acid, and low levels of sulfur dioxide.1.1 This test method applies to the determination of elemental, oxidized, particle-bound, and total mercury emissions from coal-fired stationary sources.1.2 This test method is applicable to elemental, oxidized, particle-bound, and total mercury concentrations ranging from approximately 0.5 to 100 μg/Nm3.1.3 This test method describes equipment and procedures for obtaining samples from effluent ducts and stacks, equipment and procedures for laboratory analysis, and procedures for calculating results.1.4 This test method is applicable for sampling elemental, oxidized, and particle-bound mercury in flue gases of coal-fired stationary sources. It may not be suitable at all measurement locations, particularly those with high particulate loadings, as explained in Section 16.1.5 Method applicability is limited to flue gas stream temperatures within the thermal stability range of the sampling probe and filter components.1.6 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.1.7 This standard requires users to be familiar with EPA stack-gas sampling procedures as stated in EPA Methods 1–4, Method 5, and Method 17.1.8 The method requires a high level of experience and quality control both in the field testing and analytical procedures in order to obtain high quality data.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 and health practices and determine the applicability of regulatory limitations prior to use.

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3.1 Accurate elemental analyses of samples of petroleum and petroleum products are required for the determination of chemical properties, which are in turn used to establish compliance with commercial and regulatory specifications.1.1 This practice covers information relating to sampling, calibration and validation of X-ray fluorescence instruments for elemental analysis, including all kinds of wavelength dispersive (WDXRF) and energy dispersive (EDXRF) techniques. This practice includes sampling issues such as the selection of storage vessels, transportation, and sub-sampling. Treatment, assembly, and handling of technique-specific sample holders and cups are also included. Technique-specific requirements during analytical measurement and validation of measurement for the determination of trace elements in samples of petroleum and petroleum products are described. For sample mixing, refer to Practice D5854. Petroleum products covered in this practice are considered to be a single phase and exhibit Newtonian characteristics at the point of sampling.1.2 Applicable Test Methods—This practice is applicable to the XRF methods under the jurisdiction of ASTM Subcommittee D02.03 on Elemental Analysis, and those under the jurisdiction of the Energy Institute’s Test Method Standardization Committee (Table 1). Some of these methods are technically equivalent though they may differ in details (Table 2).1.3 Applicable Fluids—This practice is applicable to petroleum and petroleum products with vapor pressures at sampling and storage temperatures less than or equal to 101 kPa (14.7 psi). Use Practice D4057 or IP 475 to sample these materials. Refer to Practice D5842 when sampling materials that also require Reid vapor pressure (RVP) determination.1.4 Non-applicable Fluids—Petroleum products whose vapor pressure at sampling and sample storage conditions are above 101 kPa (14.7 psi) and liquefied gases (that is, LNG, LPG, etc.) are not covered by this practice.1.5 Sampling Methods—The physical sampling and methods of sampling from a primary source are not covered by this guide. It is assumed that samples covered by this practice are a representative sample of the primary source liquid. Refer to Practice D4057 or IP 475 for detailed sampling procedures.1.6 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.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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4.1 The elemental analysis of liquid hazardous waste is often important for regulatory and process-specific requirements. This test method provides the user an accurate, rapid method for trace and major element determinations.1.1 This test method covers the determination of trace and major element concentrations by energy-dispersive X-ray fluorescence spectrometry (EDXRF) in liquid hazardous waste (LHW).1.2 This test method has been used successfully on numerous samples of aqueous and organic-based LHW for the determination of the following elements: Ag, As, Ba, Br, Cd, Cl, Cr, Cu, Fe, Hg, I, K, Ni, P, Pb, S, Sb, Se, Sn, Tl, V, and Zn.1.3 This test method is applicable for other elements (Si-U) not listed in 1.2.1.4 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 The chemical composition of catalyst and catalyst materials is an important indicator of catalyst performance and is a valuable tool for assessing parameters in a FCCU process. This practice will be useful to catalyst manufacturers and petroleum refiners for quality verification and performance evaluation, and to environmental authorities at the state and federal levels for evaluation and verification of various compliance programs.3, 4, 55.2 Catalysts and catalyst type materials are difficult to prepare for analysis by ICP, and although the techniques presented in this practice are common, there is wide variation among laboratories in sample pretreatment and digestion recipes. This practice is intended to standardize these variables in order to facilitate the utility of comparative data among manufacturers, refiners, and regulatory agencies.1.1 This practice covers uniform dissolution techniques for preparing samples of fluid catalytic cracking catalysts (FCC) and exchanged zeolitic materials for analysis by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). These techniques describe standardized approaches to well-known, widely used laboratory practices of sample preparation utilizing acid digestions and borate salt fusions. This practice is applicable to fresh and equilibrium FCC catalysts, catalytic materials used to manufacture catalyst, and exchanged zeolite materials.1.2 Units—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 Crude oil, petroleum, petroleum products, additives, and lubricants are routinely analyzed for their elemental content such as chlorine, nitrogen, phosphorus, sulfur, and various metals using a variety of analytical techniques. Some of these test methods require little to no sample preparation; some others require only simple dilutions; while others require elaborate sample decomposition before the product is analyzed for its elemental content.4.2 Fairly often it can be shown that the round robin results by a co-operator are all biased with respect to those from other laboratories. Presumably, the failure to follow good laboratory practices and instructions in the test methods can be a causal factor of such errors. A further consequence is an unnecessarily large reproducibility estimate or the data being dropped from the study as an outlier.4.3 Uniform practice for sample preparation is beneficial in standardizing the procedures and obtaining consistent results across the laboratories.1.1 This practice covers different means by which petroleum product and lubricant samples may be prepared before the measurement of their elemental content using different analytical techniques.1.2 This practice includes only the basic steps for generally encountered sample types. Anything out of the ordinary may require special procedures. See individual test methods for instructions to handle such situations.1.3 This practice is not a substitute for a thorough understanding of the actual test method to be used, caveats the test method contains, and additional sample preparation that may be required.1.4 The user should not expand the scope of the test methods to materials or concentrations outside the scope of the test methods being used without thoroughly understanding the implications of such deviations.1.5 This practice may also be applicable to sample preparation of non-petroleum based bio-fuels for elemental analysis. Currently, work is ongoing in ASTM Subcommittee D02.03; as information becomes available, it will be added to this standard.1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 X-ray fluorescence spectrometry can provide an accurate determination of metallic and many non-metallic elements in a wide variety of solid and liquid materials. This guide covers the information that should be included in an X-ray spectrometric analytical method and provides direction to the user for determining the optimum conditions needed to achieve acceptable accuracy.5.2 The accuracy of a determination is a function of the calibration algorithm, the sample preparation, and the sample homogeneity. Close attention to all aspects of these areas is necessary to achieve acceptable results.5.3 All concepts discussed in this guide are explored in detail in a number of published texts and in the scientific literature.1.1 This standard provides guidelines for developing and describing analytical procedures using a wavelength dispersive X-ray spectrometer for elemental analysis of solid metals, ores, and related materials. Material forms discussed herein include solids, powders, and solid forms prepared by chemical and physical processes such as borate fusion and pressing of briquettes.1.2 Liquids are not discussed in this guide because they are much less frequently encountered in metals and mining laboratories. However, aqueous liquids can be processed by borate fusion to create solid specimens, and X-ray spectrometers can be equipped to handle liquids directly.1.3 Some provisions of this guide may be applicable to the use of an energy dispersive X-ray spectrometer.1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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3.1 This guide summarizes the test methods used in the elemental analysis of crude oils. Additional information on the significance and use of the test methods quoted in this guide can be found under discussion of individual test methods in Sections 8 through 15.3.2 Crude oils are highly complex hydrocarbons also containing some organometallic compounds, inorganic sediment, and water. Nearly 600 individual hydrocarbons, over 200 separate sulfur compounds, and about 40 trace elements have been found in crude oils (1).6 Generally, sulfur and nitrogen are the two most abundant elements found in crude oils except for carbon and hydrogen. Most other inorganic elements are present at trace levels (mg/kg). Sulfur, nitrogen, vanadium, nickel, and iron are the most frequently determined elements in the crude oils. Ratios such as vanadium to vanadium + nickel, and iron to vanadium are suggested as being useful for oil type characterizations. Since organometallic compounds are concentrated in the heavy ends of petroleum, transition element concentrations and ratios can serve as excellent oil-oil correlation parameters. Generally, vanadium and nickel content increases with asphaltic content of crude oil (API gravity is an indicator). Lighter crude oils contain lesser amounts of metals (2, 3).3.3 Metal complexes called porphyrins are a major component of metallic compounds in crude oils. The principal porphyrin complexes are Ni+2 and VO+2 compounds. There are also other non-porphyrin complexes and other metallic compounds present in crude oils (4, 5).3.4 Some typical literature citations in this area are included in the reference section at the end of this guide.1.1 This guide summarizes the current information about the test methods for elemental and associated analyses used in the analysis of crude oils. This information can be helpful in trade between the buyers and sellers of crude oil. Elemental analyses tests form an important part of quantifying the crude oil quality.1.2 The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 Elemental species such as Cr, Ni, As, Cd, Hg, and Pb are widely used in many industrial processes. These elements have been identified in many former industrial sites driving the need for a quick, easy method for testing on-site at trace levels in soil and solid waste matrices.5.2 This method may be used for quantitative determinations of Cr, Ni, As, Cd, Hg, and Pb in soil matrices and solid waste. Typical test time is 90 seconds to 15 minutes.1.1 This test method is based upon energy-dispersive X-ray Fluorescence (EDXRF) spectrometry using multiple monochromatic excitation beams for detection and quantification of selected heavy metal elements in soil and related solid waste.1.2 This test method is also known as High Definition X-ray Fluorescence (HDXRF) or Multiple Monochromatic Beam EDXRF (MMB-EDXRF).1.3 This test method is applicable to various soil matrices for the determination of Cr, Ni, As, Cd, Hg, and Pb in the range of 1 to 5000 mg/kg, as specified in Table 1 and determined by a ruggedness study using representative samples. The limit of detection (LOD) for each element is listed in Table 1. The LOD is estimated by measuring a SiO2 blank sample (see Table X1.1 in Appendix X1).1.4 This test method is applicable to other elements: Sb, Cu, Se, Ag, Tl, Zn, Ba, Au, Co, V, Fe, Mn, Mo, K, Rb, Sn, Sr, and Ti.1.5 X-ray Nomenclature—This standard names X-ray lines using the Siegbahn convention.21.6 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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5.1 Significance: 5.1.1 The application of elements (see 3.1.1 and Terminology E833) to the description and the summary and analysis of building construction cost provides a consistency, commonality, and utility through all stages of design that other forms of estimate presentation do not.5.1.2 This practice describes a simple format for elemental cost analysis presentation that is both valuable and informative when used during the various design stages of construction development.5.2 Use—Users include owners, developers, contractors, cost professionals, estimators, architects, engineers, quantity surveyors, facility managers, and others involved in property development, construction, maintenance, and management.5.2.1 Reporting—Cost reports structured by elements provide estimates, summaries, and analyses by applying “Cost to Function.” This application works whether the approach is “Design to Cost” or “Cost to Design.” Value analysis is greatly assisted through the allocation of estimated cost to elements.5.2.2 Controlling—Comparison of progressively more detailed estimates is simplified where cost is allocated to appropriate elements regardless of design or specification, permitting efficient review and checking of new estimates. Design estimating using elements allows for benchmarking and the setting of cost limits (baseline) for a building design from the outset, and also permits the establishment of an elemental cost plan (see 3.2.1). Baseline records and cost plans are accessed and compared with current reports.5.2.3 Recording—Historic and baseline cost records are easily kept for all forms of building construction, and in a format that can be used for the planning and design of future projects.5.2.4 Other Uses—Elemental summaries and analyses are equally useful in forensic estimating and in quantitative risk analysis.5.2.5 Relationship to “Trade” Estimating—Traditional trade (or construction) estimating summarizes cost to a product, or trade classification. This is valuable when construction work has been fully specified or contracted, but is less so through the planning and design stages. The two systems (trade and elemental) are compatible in that they both relate to the same end product, for example, a building; they differ solely in the way cost is aggregated. Each estimate form can be converted to the other by coding or allocating each construction component to an appropriate trade/product division or element. During design evolution, changes in design and specification can make trade estimates difficult to compare with previous or other, or both, estimates and so can hinder the process of cost control during the design phase.5.2.6 Additional Narrative Information—While costs presented in these formats are descriptive in themselves they do not tell the full story of a project’s design. Narrative description of the construction work should also be an integral part of any complete presentation. Reference and description of this narrative form can be found in Practice E1804, and in Classification E1557 Appendix X3—Preliminary Project Description (PPD).5.3 A detailed description of the presentation formats now follows. These descriptions are provided in eight sections, each intended to aid understanding of a particular facet of the formats:Appearance Section 6Element Inclusions and Exclusions Section 7Basic Rules Section 8Layout Section 9Numeric Precision Section 10Estimate Calculation Section 11Analysis Calculation Section 12Variations and Additions Section 131.1 This practice covers the concurrent use of relevant ASTM standards for the preparation of elemental cost estimates, summaries, and analyses and specifically their presentation in a concise, consistent, and logical manner.1.2 While the style and directions use construction terms applied to buildings, the principles apply equally well to other forms of construction where appropriate elemental classifications exist.1.3 This practice is not an estimating manual, nor is it a guide to the skills and knowledge required of an estimator or other cost professional.NOTE 1: The skills and knowledge acquired by a trained and experienced estimator are essential to the successful application of any elemental presentation format. They are the foundation of any estimate and the underpinning knowledge required when applying the elemental technique.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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