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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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