D02.03 - Elemental Analysis

SIGNIFICANCE AND USE
5.1 Mercaptan sulfur has an objectionable odor, an adverse effect on fuel system elastomers, and is corrosive to fuel system components.
SCOPE
1.1 This test method covers the determination of mercaptan sulfur in gasolines, kerosines, aviation turbine fuels, and distillate fuels containing from 0.0003 % to 0.01 % by mass of mercaptan sulfur. Organic sulfur compounds such as sulfides, disulfides, and thiophene, do not interfere. Elemental sulfur in amounts less than 0.0005 % by mass does not interfere. Hydrogen sulfide will interfere if not removed, as described in 10.2.  
1.2 The values in acceptable SI units are to be regarded as the standard.  
1.2.1 Exception—The values in parentheses are for information only.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see Sections 7, 9, 10, and Appendix X1.  
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.

SIGNIFICANCE AND USE
5.1 Some oils are formulated with organo-metallic additives, which act, for example, as detergents, antioxidants, and antiwear agents. Some of these additives contain one or more of these elements: calcium, phosphorus, sulfur, and zinc. This test method provides a means of determining the concentrations of these elements, which in turn provides an indication of the additive content of these oils.  
5.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (Table 2).  
5.3 This test method is primarily intended to be used at a manufacturing location for monitoring of additive elements in lubricating oils. It can also be used in central and research laboratories.
SCOPE
1.1 This test method covers the quantitative determination of additive elements in unused lubricating oils, as shown in Table 1.  
1.2 This test method is limited to the use of energy dispersive X-ray fluorescence (EDXRF) spectrometers employing an X-ray tube for excitation in conjunction with the ability to separate the signals of adjacent elements.  
1.3 This test method uses interelement correction factors calculated from empirical calibration data.  
1.4 This test method is not suitable for the determination of magnesium and copper at the concentrations present in lubricating oils.  
1.5 This test method excludes lubricating oils that contain chlorine or barium as an additive element.  
1.6 This test method can be used by persons who are not skilled in X-ray spectrometry. It is intended to be used as a routine test method for production control analysis.  
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 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.

SIGNIFICANCE AND USE
5.1 Phosphorus in gasoline will damage catalytic convertors used in automotive emission control systems, and its level therefore is kept low.
SCOPE
1.1 This test method covers the determination of phosphorus generally present as pentavalent phosphate esters or salts, or both, in gasoline. This test method is applicable for the determination of phosphorus in the range from 0.2 mg to 40 mg P/L or 0.0008 g to 0.15 g P/U.S. gal.  
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see Section 7 and 10.5.  
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.

SIGNIFICANCE AND USE
5.1 This test method provides a rapid and precise elemental measurement with simple sample preparation. Typical analysis times are approximately 4 min to 5 min per sample with a preparation time of approximately 1 min to 3 min per sample.  
5.2 The quality of crude oil is related to the amount of sulfur present. Knowledge of the vanadium and nickel concentration is necessary for processing purposes as well as contractual agreements.  
5.3 The presence of vanadium and nickel presents significant risks for contamination of the cracking catalysts in the refining process.  
5.4 This test method provides a means of determining whether the vanadium and nickel content of crude meets the operational limits of the refinery and whether the metal content will have a deleterious effect on the refining process or when used as a fuel.
SCOPE
1.1 This test method covers the quantitative determination of total vanadium and nickel in crude and residual oil in the concentration ranges shown in Table 1 using X-ray fluorescence (XRF) spectrometry.  
1.2 Sulfur is measured for analytical purposes only for the compensation of X-ray absorption matrix effects affecting the vanadium and nickel X-rays. For measurement of sulfur by standard test method use Test Methods D4294, D2622 or other suitable standard test method for sulfur in crude and residual oils.  
1.3 This test method is limited to the use of X-ray fluorescence (XRF) spectrometers employing an X-ray tube for excitation in conjunction with wavelength dispersive detection system or energy dispersive high resolution semiconductor detector with the ability to separate signals of adjacent and near-adjacent elements.  
1.4 This test method uses inter-element correction factors calculated from XRF theory, the fundamental parameters (FP) approach, or best fit regression.  
1.5 Samples containing higher concentrations than shown in Table 1 must be diluted to bring the elemental concentration of the diluted material within the scope of this test method.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 The preferred concentrations units are mg/kg for vanadium and nickel.  
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.

SIGNIFICANCE AND USE
5.1 The hydrogen content represents a fundamental quality of a petroleum product that has been correlated with many of the performance characteristics of that product.  
5.2 This test method provides a simple and more precise alternative to existing test methods, specifically combustion techniques (Test Methods D5291) for determining the hydrogen content on a range of petroleum products.
SCOPE
1.1 These test methods cover the determination of the hydrogen content of petroleum products ranging from atmospheric distillates to vacuum residua using a continuous wave, low-resolution nuclear magnetic resonance spectrometer. (Test Method D3701 is the preferred method for determining the hydrogen content of aviation turbine fuels using nuclear magnetic resonance spectroscopy.)  
1.2 Three test methods are included here that account for the special characteristics of different petroleum products and apply to the following distillation ranges:    
Test Method  
Petroleum Products  
Boiling Range, °C (°F)
(approximate)  
A  
Light Distillates  
15–260 (60–500)  
B  
Middle Distillates  
200–370 (400–700)  
Gas Oils  
370–510 (700–950)  
C  
Residua  
510+ (950+ )  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. The preferred units are mass %.  
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 Sections 7.2 and 7.4.  
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.

SIGNIFICANCE AND USE
5.1 The combustion quality of aviation turbine fuel has traditionally been controlled in specifications by such tests as smoke point (see Test Method D1322), smoke volatility index, aromatic content of luminometer number (see Test Method D1740). Evidence is accumulating that a better control of the quality may be obtained by limiting the minimum hydrogen content of the fuel.  
5.2 Existing methods allow the hydrogen content to be calculated from other parameters or determined by combustion techniques. The method specified provides a quick, simple, and more precise alternative to these methods.
SCOPE
1.1 This test method covers the determination of the hydrogen content of aviation turbine fuels.  
1.2 Use Test Methods D4808 or D7171 for the determination of hydrogen in other petroleum liquids.  
1.3 The values stated in SI units are to be regarded as standard. The preferred units are mass percent hydrogen.  
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 a specific warning statement, see 7.1.  
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.

SIGNIFICANCE AND USE
5.1 This practice is intended for use in sampling liquid hydrocarbons including crude oils, condensates, refinery process intermediates, and refined products. Generally these samples are expected to contain mercury from the parts per billion (10–9 mass) to parts per million (10–6 mass) range.  
5.2 This practice is not intended for use when sampling aqueous systems where the concentrations of mercury are often in the parts per trillion (10–12 mass) range. These samples are often better addressed by using the rigorously clean techniques from the EPA Method 1669 “clean hands, dirty hands” sampling procedures.  
5.3 This practice is not intended for use for liquefied samples, for which special containers may be required for pressurized samples.  
5.4 This practice is only suitable for stabilized samples which remain 100 % liquid at ambient conditions. For samples that on depressurization lose some of the light hydrocarbon ends it is important to note that elemental mercury may be lost during sampling. Sampling modules which inject unstabilized liquid hydrocarbons close to process conditions directly to the mercury analyzer can be used to overcome this issue.  
5.5 Based on this practice, two Test Methods (D7622 and D7623) are available for determination of mercury in crude oil, based on cold vapor atomic absorption technique.  
5.6 In some refined streams and in tank samples free water may be present. Process streams that are water saturated may condense water as the sample cools from process temperature to ambient temperature. Ionic mercury species are water soluble and these water droplets may contain mercury or adsorb mercury over time.  
5.7 The presence of mercury during crude oil production, transport, and refining can be an environmental and industrial hygiene concern.
SCOPE
1.1 This practice covers the types of and preparation of containers found most suitable for the handling of hydrocarbon samples for the determination of total mercury.  
1.2 This practice was developed for sampling streams where the mercury speciation is predominantly Hg(0) present as a mixture of dissolved Hg(0) atoms, adsorbed Hg(0) on particulates (for example, carbonaceous or mineral fines and Fe2O3) and suspended droplets of metallic mercury.  
1.3 The presence of suspended droplets of metallic mercury (often called “colloidal” mercury, since the droplet size can be very small) can make obtaining a representative sample very difficult for a variety of reasons (for example, non-isokinetic sampling of the liquid can result in over- or under-collection of suspended droplets and collection of mercury that has accumulated in dense larger drops and pools on the bottom of piping and in sample taps). Pay strict attention to the detailed procedure (Section 7) to ensure representative samples are collected.  
1.4 When representative test portions are collected and analyzed in accordance with acceptable procedures, the total mercury is representative of concentrations in the sample.  
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 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central nervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury-containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website (http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.  
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 envi...

SIGNIFICANCE AND USE
5.1 Lubricating greases are used in almost all bearings used in any machinery. Lubricating grease is composed of ~90 % additized oil and soap or other thickening agent. There are over a dozen metallic elements present in greases, either blended as additives for performance enhancements or as thickeners, or in used greases present as contaminants and wear metals. Determining their concentrations can be an important aspect of grease manufacture. The metal content can also indicate the amount of thickeners in the grease. Additionally, a reliable analysis technique can also assist in the process of trouble shooting problems with new and used grease in the field.  
5.2 Although widely used in other sectors of the oil industry for metal analysis, ICP-AES based Test Methods D4951 or D5185 cannot be used for analyzing greases because of their insolubility in organic solvents used in these test methods. Hence, grease samples need to be brought into aqueous solution by acid decomposition before ICP-AES measurements.  
5.3 Test Method D3340 has been used to determine lithium and sodium content of lubricating greases using flame photometry. This technique is no longer widely used. This new test method provides a test method for multi-element analysis of grease samples. This is the first D02 standard available for simultaneous multi-element analysis of lubricating greases.
SCOPE
1.1 This test method covers the determination of a number of metals such as aluminum, antimony, barium, calcium, iron, lithium, magnesium, molybdenum, phosphorus, silicon, sodium, sulfur, and zinc in unused lubricating greases by inductively coupled plasma atomic emission spectrometry (ICP-AES) technique.  
1.1.1 The range of applicability for this test method, based on the interlaboratory study conducted in 2005,2 is aluminum (10 to 600), antimony (10 to 2300), barium (50 to 800), calcium (20 to 50 000), iron (10 to 360), lithium (300 to 3200), magnesium (30 to 10 000), molybdenum (50 to 22 000), phosphorus (50 to 2000), silicon (10 to 15 000), sodium (30 to 1500), sulfur (1600 to 28 000), and zinc (300 to 2200), all in mg/kg. Lower levels of elements may be determined by using larger sample weights, and higher levels of elements may be determined by using smaller amounts of sample or by using a larger dilution factor after sample dissolution. However, the test precision in such cases has not been determined, and may be different than the ones given in Table 3.  
1.1.2 It may also be possible to determine additional metals such as bismuth, boron, cadmium, chromium, copper, lead, manganese, potassium, titanium, etc. by this technique. However, not enough data is available to specify the precision for these latter determinations. These metals may originate into greases through contamination or as additive elements.  
1.1.3 During sample preparation, the grease samples are decomposed with a variety of acid mixture(s). It is beyond the scope of this test method to specify appropriate acid mixtures for all possible combination of metals present in the sample. But if the ash dissolution results in any visible insoluble material, the test method may not be applicable for the type of grease being analyzed, assuming the insoluble material contains some of the analytes of interest.  
1.2 Elements present at concentrations above the upper limit of the calibration curves can be determined with additional appropriate dilutions of dissolved samples and with no degradation of precision.  
1.3 The development of the technique behind this test method is documented by Fox.3  
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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 dete...

SIGNIFICANCE AND USE
5.1 Sulfur present as mercaptans or as hydrogen sulfide in distillate fuels and solvents can attack many metallic and non-metallic materials in fuel and other distribution systems. A negative result in the doctor test ensures that the concentration of these compounds is insufficient to cause such problems in normal use.
SCOPE
1.1 This test method covers and is intended primarily for the detection of mercaptans in motor fuel, kerosine, and similar petroleum products. This method may also provide information on hydrogen sulfide and elemental sulfur that may be present in these sample types.  
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.  For specific warning statements, see 7.3.  
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.

SIGNIFICANCE AND USE
5.1 This practice is intended as a solution to the difficulty of obtaining reproducible test results from heterogeneous samples.  
5.2 This practice works best with multilayered liquids, but can also be applied to samples with solid particles that are sufficiently small in size to be suspended in an emulsion.  
5.3 The emulsified/suspended sample can be used for all bulk property testing such as microwave digestion/inductively coupled argon plasma (ICAP), ion chromatography, heat of combustion, ash content, water, nonvolatile residue, and pH. It may be prudent to retain a portion of the sample in its original, multiphase form for some types of analyses.
SCOPE
1.1 This practice covers the generation of a uniform mixture or emulsion from multiphase samples which are primarily liquid in order to facilitate sample preparation, transfer, and analysis.  
1.2 This practice is designed to keep a multiphase fluid sample in an emulsified/suspended state long enough to take a single, composite sample that is representative of the sample as a whole. The sample may reform multiple layers after standing.  
1.3 The emulsion/suspension generated by following this practice can be used only for analytical procedures designed for the total sample and procedures not significantly affected by the emulsifier or the presence of an emulsion/suspension.  
1.4 This practice assumes that a representative sample of not more than 1 L has been obtained.  
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.

SIGNIFICANCE AND USE
5.1 Most often determined trace elements in crude oils are nickel and vanadium, which are usually the most abundant; however, as many as 45 elements in crude oils have been reported. Knowledge of trace elements in crude oil is important because they can have an adverse effect on petroleum refining and product quality. These effects can include catalyst poisoning in the refinery and excessive atmospheric emission in combustion of fuels. Trace element concentrations are also useful in correlating production from different wells and horizons in a field. Elements such as iron, arsenic, and lead are catalyst poisons. Vanadium compounds can cause refractory damage in furnaces, and sodium compounds have been found to cause superficial fusion on fire brick. Some organometallic compounds are volatile which can lead to the contamination of distillate fractions, and a reduction in their stability or malfunctions of equipment when they are combusted.  
5.2 The value of crude oil can be determined, in part, by the concentrations of nickel, vanadium, and iron.  
5.3 Inductively coupled plasma-atomic emission spectrometry (ICP-AES) is a widely used technique in the oil industry. Its advantages over traditional atomic absorption spectrometry (AAS) include greater sensitivity, freedom from molecular interferences, wide dynamic range, and multi-element capability. See Practice D7260.
SCOPE
1.1 This test method covers the determination of several elements (including iron, nickel, sulfur, and vanadium) occurring in crude oils.  
1.2 For analysis of any element using wavelengths below 190 nm, a vacuum or inert gas optical path is required.  
1.3 Analysis for elements such as arsenic, selenium, or sulfur in whole crude oil may be difficult by this test method due to the presence of their volatile compounds of these elements in crude oil; but this test method should work for resid samples.  
1.4 Because of the particulates present in crude oil samples, if they do not dissolve in the organic solvents used or if they do not get aspirated in the nebulizer, low elemental values may result, particularly for iron and sodium. This can also occur if the elements are associated with water which can drop out of the solution when diluted with solvent.  
1.4.1 An alternative in such cases is using Test Method D5708, Procedure B, which involves wet decomposition of the oil sample and measurement by ICP-AES for nickel, vanadium, and iron, or Test Method D5863, Procedure A, which also uses wet acid decomposition and determines vanadium, nickel, iron, and sodium using atomic absorption spectrometry.  
1.4.2 From ASTM Interlaboratory Crosscheck Programs (ILCP) on crude oils data available so far, it is not clear that organic solvent dilution techniques would necessarily give lower results than those obtained using acid decomposition techniques.2  
1.4.3 It is also possible that, particularly in the case of silicon, low results may be obtained irrespective of whether organic dilution or acid decomposition is utilized. Silicones are present as oil field additives and can be lost in ashing. Silicates should be retained but unless hydrofluoric acid or alkali fusion is used for sample dissolution, they may not be accounted for.  
1.5 This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent and low results may be obtained for particles larger than a few micrometers.  
1.6 The precision in Section 18 defines the concentration ranges covered in the interlaboratory study. However, lower and particularly higher concentrations can be determined by this test method. The low concentration limits are dependent on the sensitivity of the ICP instrument and the dilution factor used. The high concentration limits are determined by the product of the maximum concentration defined by the calibration curve and the sample di...

SIGNIFICANCE AND USE
5.1 Excessive amounts of sodium can indicate the presence of materials that cause high wear of burner pumps and valves, and contribute to deposits of boiler heating surfaces.
SCOPE
1.1 This test method covers the determination of sodium in residual fuel oil by means of a flame photometer. Its precision in low ranges limits its application to samples containing more than 15 mg/kg sodium. Other elements commonly found in residual fuel oil do not interfere.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety problems 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 hazard statements see 7.3, 7.5, 7.7, 9.2, 7.8, 7.9, and Note 3.  
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.

SIGNIFICANCE AND USE
5.1 Some oils are formulated with metal-containing additives that act as detergents, antioxidants, antiwear agents, etc. Some of these additives contain one or more of these metals: barium, calcium, zinc, and magnesium. This test method provides a means of determining the concentration of these metals that gives an indication of the additive content in these oils.  
5.2 Several additive metals and their compounds are added to the lubricating oils to give beneficial performance. (See Table 1.)
SCOPE
1.1 This test method is applicable for the determination of mass percent barium from 0.005 % to 1.0 %, calcium and magnesium from 0.002 % to 0.3 %, and zinc from 0.002 % to 0.2 % in lubricating oils.  
1.2 Higher concentrations can be determined by appropriate dilution. Lower concentrations of metals such as barium, calcium, magnesium, and zinc at about 10 ppm level can also be determined by this test method. Use of this test method for the determination at these lower concentrations should be by agreement between the buyer and the seller.  
1.3 Lubricating oils that contain viscosity index improvers may give low results when calibrations are performed using standards that do not contain viscosity index improvers.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 4.1, 7.3, and 9.1.  
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.

SIGNIFICANCE AND USE
4.1 This test method provides a means of monitoring the sulfur level of various petroleum products and additives. This knowledge can be used to predict performance, handling, or processing properties. In some cases the presence of sulfur compounds is beneficial to the product and monitoring the depletion of sulfur can provide useful information. In other cases the presence of sulfur compounds is detrimental to the processing or use of the product.
SCOPE
1.1 This test method covers procedures for the determination of total sulfur in petroleum products including lubricating oils containing additives, and in additive concentrates. This test method is applicable to samples boiling above 177 °C (350 °F). Other sulfur concentrations outside of those listed in 1.1.1 and 1.1.2 may be analyzed, but the precision stated may or may not apply. These procedures use IR detection or TCD following combustion in a furnace.  
1.1.1 Procedure A, IR Detection:  
1.1.1.1 This procedure is applicable to samples containing a mass fraction of sulfur between 0.22 % and 24.2 %.
1.1.1.2 Petroleum coke containing a mass fraction of sulfur between 2.53 % to 3.79 % sulfur may be analyzed.  
1.1.2 Procedure B, TCD Detection:  
1.1.2.1 This procedure is applicable to samples containing a mass fraction of sulfur between 0.071 % and 25.8 %.
1.1.2.2 Petroleum coke containing a mass fraction of sulfur between 0.19 % to 6.38 % sulfur may be analyzed.  
1.2 Petroleum coke containing a mass fraction of sulfur between 2.53 % to 3.79 % sulfur may be analyzed. Other sulfur concentrations may be analyzed, but the precision stated may or may not apply.
Note 1: The D1552 – 08 (2014) version of this standard contained two other procedures using iodate titrations. Since these procedures are no longer being used in the industry laboratories based on a survey of D02.SC 3 laboratories conducted in September 2014, they are being deleted. For earlier information on the deleted procedures, D1552 – 08 (2014) may be perused.  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
5.1 The sulfated ash can be used to indicate the concentration of known metal-containing additives in new oils. When phosphorus is absent, barium, calcium, magnesium, sodium and potassium are converted to their sulfates and tin (stannic) and zinc to their oxides (Note 4). Sulfur and chlorine do not interfere, but when phosphorus is present with metals, it remains partially or wholly in the sulfated ash as metal phosphates.
Note 4: Since zinc sulfate slowly decomposes to its oxide at the ignition temperature specified in the test method, samples containing zinc can give variable results unless the zinc sulfate is completely converted to the oxide.  
5.2 Because of above inter-element interferences, experimentally obtained sulfated ash values may differ from sulfated ash values calculated from elemental analysis. The formation of such non-sulfated species is dependent on the temperature of ashing, time ashed, and the composition of metal compounds present in oils. Hence, sulfated ash requirement generally should not be used in product specifications without a clear understanding between a buyer and a seller of the unreliability of an ash value as an indicator of the total metallic compound content.4
SCOPE
1.1 This test method covers the determination of the sulfated ash from unused lubricating oils containing additives and from additive concentrates used in compounding. These additives usually contain one or more of the following metals: barium, calcium, magnesium, zinc, potassium, sodium, and tin. The elements sulfur, phosphorus, and chlorine can also be present in combined form.  
1.2 Application of this test method to sulfated ash levels below 0.02 % by mass is restricted to oils containing ashless additives. The lower limit of the test method is 0.005 % by mass sulfated ash.  
Note 1: This test method is not intended for the analysis of used engine oils or oils containing lead. Neither is it recommended for the analysis of nonadditive lubricating oils, for which Test Method D482 can be used.
Note 2: There is evidence that magnesium does not react the same as other alkali metals in this test. If magnesium additives are present, the data is interpreted with caution.
Note 3: There is evidence that samples containing molybdenum can give low results because molybdenum compounds are not fully recovered at the temperature of ashing.  
1.3 Fatty acid methyl ester (FAME) conforming to EN 14213 and EN 14214, when tested using this test method, were shown to meet its precision.  
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.  
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.

SIGNIFICANCE AND USE
5.1 Sulfates and chlorides may be found in filter plugging deposits and fuel injector deposits. The acceptability for use of the fuel components and the finished fuels depends on the sulfate and chloride content.  
5.2 Existent and potential inorganic sulfate and total chloride content, as measured by this test method, can be used as one measure of the acceptability of gasoline components for automotive spark-ignition engine fuel use.
SCOPE
1.1 This test method covers an ion chromatographic procedure for the determination of the existent inorganic and potential sulfate and total inorganic chloride content in hydrous and anhydrous denatured ethanol to be used in motor fuel applications. It is intended for the analysis of ethanol samples containing between 0.55 mg/kg and 20 mg/kg of existent inorganic sulfate, 4.0 mg/kg to 20 mg/kg of potential inorganic sulfate, and 0.75 mg/kg to 50 mg/kg of total inorganic chloride.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage  
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.

SIGNIFICANCE AND USE
5.1 When fuels are combusted, metals present in the fuels can form low melting compounds that are corrosive to metal parts. Metals present at trace levels in petroleum can deactivate catalysts during processing. These test methods provide a means of quantitatively determining the concentrations of vanadium, nickel, iron, and sodium. Thus, these test methods can be used to aid in determining the quality and value of the crude oil and residual oil.
SCOPE
1.1 These test methods cover the determination of nickel, vanadium, iron, and sodium in crude oils and residual fuels by flame atomic absorption spectrometry (AAS). Two different test methods are presented.  
1.2 Procedure A, Sections 8–14—Flame AAS is used to analyze a sample that is decomposed with acid for the determination of total Ni, V, and Fe.  
1.3 Procedure B, Sections 15–20—Flame AAS is used to analyze a sample diluted with an organic solvent for the determination of Ni, V, and Na. This test method uses oil-soluble metals for calibration to determine dissolved metals and does not purport to quantitatively determine nor detect insoluble particulates. Hence, this test method may underestimate the metal content, especially sodium, present as inorganic sodium salts.  
1.4 The concentration ranges covered by these test methods are determined by the sensitivity of the instruments, the amount of sample taken for analysis, and the dilution volume. A specific statement is given in Note 1.  
1.5 For each element, each test method has its own unique precision. The user can select the appropriate test method based on the precision required for the specific analysis.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard, unless specifically stated. Other units that appear in this standard are included for information purposes only or because they are in embedded pictures that cannot be edited.  
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. Specific warning statements are given in 8.1, 9.2, 9.5, 11.2, 11.4, and 16.1.  
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.

SIGNIFICANCE AND USE
5.1 This test method provides rapid and precise measurement of total silicon in naphthas, gasoline, gasoline-ethanol blends, RFG, ethanol and ethanol-fuel blends, and toluene with minimum sample preparation. Typical analysis time is 5 min to 10 min per sample.  
5.2 Excitation by monochromatic X-rays reduces background, simplifies matrix correction, and increases the signal/background ratio compared to polychromatic excitation used in conventional WDXRF techniques.3  
5.3 Silicone oil defoamer can be added to coker feedstocks to minimize foaming in the coker. Residual silicon in the coker naphtha can adversely affect downstream catalytic processing of the naphtha. This test method provides a means to determine the silicon content of the naphtha.  
5.4 Silicon contamination of gasoline, gasoline-ethanol blends, denatured ethanol, and their blends has led to fouled vehicle components (for example, spark plugs, exhaust oxygen sensors, catalytic converters) requiring parts replacement and repairs. Finished gasoline, gasoline-ethanol blends, and ethanol-fuel blends can come into contact with silicon a number of ways. Waste hydrocarbon solvents such as toluene can be added to gasoline. Such solvents can contain soluble silicon compounds. Silicon-based antifoam agents can be used in ethanol plants, which then pass silicon on to the finished ethanol-fuel blend. This test method can be used to determine if gasoline, gasoline-ethanol blends, and ethanol-fuel blends meet specifications with respect to silicon content of the fuel, and for resolution of customer problems.  
5.5 Some silicon compounds covered by this test method are significantly more volatile than the silicon compounds typically used for the preparation of the calibration standards. Volatile compounds may not meet the stated precision from this test method because of selective loss of light materials during the analysis.
SCOPE
1.1 This test method covers the determination of total silicon by monochromatic, wavelength-dispersive X-ray fluorescence (MWDXRF) spectrometry in naphthas, gasoline, gasoline-ethanol blends, reformulated gasoline (RFG), ethanol and ethanol-fuel blends, and toluene at concentrations of 3 mg/kg to 100 mg/kg. The precision of this test method was determined by an interlaboratory study using representative samples of the liquids described in 1.1 and 1.2. The pooled limit of quantitation (PLOQ) was estimated to be 3 mg/kg.
Note 1: Volatile samples such as high-vapor-pressure gasolines or light hydrocarbons might not meet the stated precision because of the evaporation of light components during the analysis.
Note 2: Aromatic compounds such as toluene are under the jurisdiction of Committee D16 on Aromatic Hydrocarbons and Related Chemicals. However, toluene can be a contributor to silicon contamination in gasoline (see 5.4), thus its inclusion in this test method.  
1.2 Gasoline samples containing ethanol and other oxygenates may be analyzed with this test method provided the matrix of the calibration standards is either matched to the sample matrices or the matrix correction described in Annex A1 is applied to the results. The conditions for matrix matching and matrix correction are provided Section 6, Interferences.  
1.3 Samples with silicon concentrations above 100 mg/kg can be analyzed after dilution with appropriate solvent. The precision and bias of silicon determinations on diluted samples have not been determined and may not be the same as shown for neat samples (Section 17).  
1.4 A fundamental assumption in this test method is that the standard and sample matrices are well matched, or that the matrix differences are accounted for (see 14.5). Matrix mismatch can be caused by C/H ratio differences between samples and standards or by the presence of other interfering heteroatoms; observe the cautions and recommendations in Section 6.  
1.5 The values stated in SI units are to be regarded as standard...

SIGNIFICANCE AND USE
5.1 This test method provides measurement of total sulfur in automotive, No. 2 heating, and jet fuels with a minimum of sample preparation. A typical analysis time is 180 s to 360 s per sample.  
5.2 The quality of automotive, No. 2 heating, and jet fuel can be related to the amount of sulfur present. Knowledge of sulfur concentration is necessary for processing purposes. There are also regulations promulgated in federal, state, and local agencies that restrict the amount of sulfur present in some fuel.  
5.3 If this test method is applied to petroleum materials with matrices significantly different from the calibration materials specified in this test method, the cautions and recommendations in Section 6 should be observed when interpreting the results.
SCOPE
1.1 This test method specifies an energy-dispersive X-ray fluorescence (EDXRF) method for the determination of total sulfur in automotive, No. 2 heating, and jet fuels with a concentration range of 3 mg/kg to 942 mg/kg.  
1.1.1 The pooled limit of quantitation of this test method as obtained by statistical analysis of inter laboratory test results is 3 mg/kg sulfur.  
1.1.2 This test method is applicable to gasoline, oxygen enriched gasoline (RFG), diesel, diesel/biodiesel blends containing up to twenty volume percent biodiesel, kerosene, jet fuel, jet fuel/biodiesel blends containing up to five volume percent biodiesel and No. 2 home heating oil.  
1.2 A fundamental assumption in this test method is that the standard and sample matrix is well matched. Matrix mismatch can be caused by C/H ratio differences between samples and standards or by the presence of other heteroatoms.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3.1 The preferred concentration units are mg/kg sulfur.  
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.

SIGNIFICANCE AND USE
5.1 Sulfates and chlorides can be found in filter plugging deposits and fuel injector deposits. The acceptability for use of the fuel components and the finished fuels depends on the sulfate and chloride content.  
5.2 Existent and potential inorganic sulfate and total chloride content, as measured by this test method, can be used as one measure of the acceptability of gasoline components for automotive spark-ignition engine fuel use.
SCOPE
1.1 This test method covers a direct injection ion chromatographic procedure for determining existent and potential inorganic sulfate and total inorganic chloride content in hydrous and anhydrous denatured ethanol and butanol to be used in motor fuel applications. It is intended for the analysis of ethanol and butanol samples containing between 1.0 mg/kg to 20 mg/kg of existent or potential inorganic sulfate and 1.0 mg/kg to 50 mg/kg of inorganic chloride.
Note 1: Tertiary butanol is not included in this test method. 1-butanol, 2-butanol, and isobutanol are included in the testing and research report for this test method.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.  
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.

SIGNIFICANCE AND USE
5.1 Organic chlorides do not occur naturally in crude oil. When present, they result from contamination in some manner, such as disposal of chlorinated solvent used in many dewaxing pipeline or other equipment operations.  
5.1.1 Uncontaminated crude oil will contain no detectable organic chloride, and most refineries can handle very small amounts without deleterious effects.
5.1.1.1 Most trade contracts specify that no organic chloride is present in the crude oil.  
5.1.2 Several pipelines have set specification limits at  
5.1.2.1 To ensure Eq 3).  
5.1.3 Organic chloride present in the crude oil (for example, methylene chloride, perchloroethylene, etc.) is usually distilled into the naphtha fraction. Some compounds break down during fractionation and produce hydrochloric acid, which has a corrosive effect. Some compounds survive fractionation and are destroyed during hydro-treating (desulfurization of the naphtha).  
5.2 Other halides can also be used for dewaxing crude oil; in such cases, any organic halides will have similar impact on the refining operations as the organic chlorides.  
5.3 Organic chloride species are potentially damaging to refinery processes. Hydrochloric acid can be produced in hydrotreating or reforming reactors and the acid accumulates in condensing regions of the refinery. Unexpected concentrations of organic chlorides cannot be effectively neutralized and damage can result. Organic chlorides are not known to be naturally present in crude oils and usually result from cleaning operations at producing sites, pipelines, or tanks. It is important for the oil industry to have common methods available for the determination of organic chlorides in crude oil, particularly when transfer of custody is involved.
SCOPE
1.1 The procedures in this test method cover the determination of organic chloride (above 1 μg/g organically-bound chlorine) in crude oils, using either distillation and sodium biphenyl reduction, distillation and microcoulometry, or distillation and X-ray fluorescence (XRF) spectrometry.  
1.2 The procedures in this test method involve the distillation of crude oil test specimens to obtain a naphtha fraction prior to chloride determination. The chloride content of the naphtha fraction of the whole crude oil can thereby be obtained. See Section 6 regarding potential interferences.  
1.3 Procedure A covers the determination of organic chloride in the washed naphtha fraction of crude oil by sodium biphenyl reduction followed by potentiometric titration.  
1.4 Procedure B covers the determination of organic chloride in the washed naphtha fraction of crude oil by oxidative combustion followed by microcoulometric titration.  
1.5 Procedure C covers the determination of organic chloride in the washed naphtha fraction of crude oil by X-ray fluorescence spectrometry.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 The preferred concentration units are micrograms of chloride per gram of sample, though milligrams of chloride per kilogram of sample is commonly used for Procedure C.  
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.

SIGNIFICANCE AND USE
5.1 Catalyst fines in fuel oils can cause abnormal engine wear. These test methods provide a means of determining silicon and aluminum, the major constituents of the catalysts.
SCOPE
1.1 These test methods cover the determination of aluminum and silicon in fuel oils at concentrations between 5 mg/kg and 150 mg/kg for aluminum and 10 mg/kg and 250 mg/kg for silicon.  
1.2 Test Method A—Inductively coupled plasma atomic emission spectrometry is used in this test method to quantitatively determine aluminum and silicon.  
1.3 Test Method B—Flame atomic absorption spectrometry is used in this test method to quantitatively determine aluminum and silicon.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in Sections 7.6, 10.1, and 11.5.  
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.

SIGNIFICANCE AND USE
5.1 Organic chlorides do not occur naturally in crude oil. When present, they result from contamination in some manner, such as disposal of chlorinated solvent used in many dewaxing pipeline or other equipment operations.  
5.1.1 Uncontaminated crude oil will contain no detectable organic chloride, and most refineries can handle very small amounts without deleterious effects.
5.1.1.1 Most trade contracts specify that no organic chloride is present in the crude oil.  
5.1.2 Several pipelines have set specification limits less than 1 μg/g organic chlorides in the whole crude, and less than 5 μg/g in the light naphtha, based on the yield of naphtha being 20 % of the original sample.
5.1.2.1 To ensure less than 1 μg/g organic chloride in the crude oil, the amount measured in the naphtha fraction shall be less than 1/f (where f is the naphtha fraction calculated with Eq 1). For example, a crude oil sample with 1 μg/g of organic chloride but a 10 % yield of naphtha would create a naphtha containing 10 μg/g organic chloride. Further, a crude containing 1 μg/g of organic chloride but a 40 % yield of naphtha would create a naphtha containing 2.5 μg/g organic chloride. Due to the difference in naphtha yields, the impact on refining operations can be significantly different.
5.1.2.2 Since crude oil deposits worldwide exhibit different yields of naphtha, the working range of detection for this method shall cover a broad range, possibly as high as 50 μg/g in a naphtha fraction.  
5.1.3 Organic chloride present in the crude oil (for example, methylene chloride, perchloroethylene, etc.) is usually distilled into the naphtha fraction. Some compounds break down during fractionation and produce hydrochloric acid, which has a corrosive effect. Some compounds survive fractionation and are destroyed during hydro-treating (desulfurization of the naphtha).  
5.2 Other halides can also be used for dewaxing crude oil; in such cases, any organic halides will have similar impact on ...
SCOPE
1.1 This test method covers the determination of organic chloride (above 1 μg/g organically-bound chlorine) in crude oils, using distillation and combustion ion chromatography.  
1.2 This test method involves the distillation of crude oil test specimens to obtain a naphtha fraction prior to chloride determination. The chloride content of the naphtha fraction of the whole crude oil can thereby be obtained. See Section 6 regarding potential interferences.  
1.3 The test procedure covers the determination of organic chloride in the washed naphtha fraction of crude oil by combustion ion chromatography. Other halides can be determined but are not included in the precision statement of the test method.  
1.4 The values stated in SI units are to be regarded as standard. The preferred concentration units are micrograms of chloride per gram of sample.  
1.4.1 Exception—The values given in parentheses are for information only.  
1.5 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.  
1.6 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 ...

SIGNIFICANCE AND USE
5.1 This test method is used to ensure compliance of trace lead as required by federal regulation for lead-free gasoline (40 CFR part 80).
SCOPE
1.1 This test method covers the determination of the total lead content of gasoline within the concentration range of 0.010 g to 0.10 g of lead/U.S. gal (2.5 mg/L to 25 mg/L). This test method compensates for variations in gasoline composition and is independent of lead alkyl type.  
1.2 The values given in grams per U.S. gallon are to be regarded as the standard in the United States. Note that in other countries, other units can be preferred.  
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. For specific hazard statements, see 7.6 and 7.8.  
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.

SIGNIFICANCE AND USE
5.1 The concentration of nitrogen is a measure of the presence of nitrogen-containing additives. Knowledge of its concentration can be used to predict performance.
SCOPE
1.1 This test method covers the determination of nitrogen in lubricating oils when present in the concentration from 0.03 % to 0.10 % by mass, and for the determination of nitrogen in fuel oils when present in the concentration from 0.015 % to 2.0 % by mass. This test method is also applicable to the analysis of additive concentrates and additive packages.  
Note 1: This test method may not be applicable to certain materials containing N–O or N–N linkage. However, the samples used in the cooperative program to establish the precision of the test method were compounded with currently available ashless additives containing nitrogen. Complete recovery of the nitrogen present in these additives was obtained.  
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. For specific warning statements, see 7.6, 7.9, and 9.8.  
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.

SIGNIFICANCE AND USE
5.1 Used Lubricating Oil—The determination of debris in used oil is a key diagnostic method practiced in machine condition monitoring programs. The presence or increase in concentration of specific wear metals can be indicative of the early stages of wear if there are baseline concentration data for comparison. A marked increase in contaminant elements can be indicative of foreign materials in the lubricants, such as antifreeze or sand, which may lead to wear or lubricant degradation. The test method identifies the metals and their concentration so that trends relative to time or distance can be established and corrective action can be taken prior to more serious or catastrophic failure.
SCOPE
1.1 This test method covers the determination of wear metals and contaminants in used lubricating oils and used hydraulic fluids by rotating disc electrode atomic emission spectroscopy (RDE-AES).  
1.2 This test method provides a quick indication for abnormal wear and the presence of contamination in new or used lubricants and hydraulic fluids.  
1.3 This test method uses oil-soluble metals for calibration and does not purport to relate quantitatively the values determined as insoluble particles to the dissolved metals. Analytical results are particle size dependent and low results may be obtained for those elements present in used oil samples as large particles.  
1.4 The test method is capable of detecting and quantifying elements resulting from wear and contamination ranging from dissolved materials to particles approximately 10 μm in size.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5.1 The preferred units are mg/kg (ppm by mass).  
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.

SIGNIFICANCE AND USE
5.1 The presence and concentration of various metallic elements in a petroleum coke are major factors in the suitability of the coke for various uses. This test method provides a means of measuring the amounts of those metallic elements in the coke sample.  
5.2 The concentration of these elements is one factor in determining the economic value of the coke. Coke used for production of electrodes will have different specification requirements dependent on what service the electrodes will be used in. Generally the fuel cokes are highest in metallic element concentration and have the least economic value.  
5.3 The test method provides a standard procedure for use by the purchaser and seller in the commercial transfer of petroleum coke to determine whether the lot of coke meets the specifications of the purchasing party.
SCOPE
1.1 This test method covers the analysis for the commonly determined trace metals (aluminum, calcium, iron, nickel, silicon, sodium, and vanadium) in laboratory analysis samples of raw and calcined petroleum coke by atomic absorption spectroscopy.  
1.2 The elemental concentration ranges for which this test method is applicable and the limits of detection of this test method are listed in Table 1.  
1.3 The values stated in SI units are to be regarded as the 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. For warning statements, see Sections 9 – 11.  
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.

SIGNIFICANCE AND USE
5.1 Knowledge of the presence of trace metals in gas turbine fuels enables the user to predict performance and, when necessary, to take appropriate action to prevent corrosion.
SCOPE
1.1 This test method covers the determination of sodium, lead, calcium, and vanadium in Specification D2880 Grade Nos. 0-GT through 4-GT fuels at 0.5 mg/kg level for each of the elements. This test method is intended for the determination of oil-soluble metals and not waterborne contaminants in oil-water mixtures.  
1.1.1 Test Method D6728 is suggested as an alternative test method for the determination of these elements in Specification D2880.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

SIGNIFICANCE AND USE
5.1 Certain organo-manganese compounds act as antiknock agents when added to gasoline. This test method provides a means for determining the concentration of such a material in a gasoline sample.
SCOPE
1.1 This test method covers the determination of the total manganese content, present as methylcyclopentadienyl manganese tricarbonyl (MMT),2 of gasoline within the concentration range from 0.25 mg/L to 40 mg/L of manganese.  
1.2 This test method is applicable to reformulated gasoline containing up to 12 % volume methyl tertiary butylether or up to 10 % volume ethanol. This test method may not be applicable to highly cracked materials containing greater than 18 % by volume olefins as determined by Test Method D1319 (nondepentanized).  
1.3 This test method has been developed and tested specifically for the determination of MMT in gasoline over the recommended concentration range. Application of the method to other concentration ranges, to the determination of MMT in other materials, or to the determination of other manganese compounds in gasoline have not been tested  
1.4 The values stated in SI units are to be regarded as the standard. The preferred concentration units are mg/L manganese.  
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 specific warning statements, see Sections 6 and 7.  
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.

SIGNIFICANCE AND USE
5.1 The presence and concentration of various metallic elements in a petroleum coke are major factors in determining the suitability of the coke for various end uses. This test method provides a means of determining the concentrations of these metallic elements in a coke sample.  
5.2 The test method provides a standard procedure for use by buyer and seller in the commercial transfer of petroleum coke to determine whether the petroleum coke meets the specifications of the purchasing party.
SCOPE
1.1 This test method covers the analysis for commonly determined trace metals in test specimens of raw and calcined petroleum coke by inductively coupled plasma atomic emission spectroscopy.  
1.2 Elements for which this test method is applicable are listed in Table 1. Detection limits, sensitivity, and optimum ranges of the metals will vary with the matrices and model of spectrometer.  
1.3 This test method is applicable only to samples containing less than one mass % ash.  
1.4 Elements present at concentrations above the upper limit of the working ranges can be determined with additional, appropriate dilutions.  
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
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.

SIGNIFICANCE AND USE
5.1 This test method covers the determination of five elements (Ca, Mg, K, Na, and P) in biodiesel and biodiesel blends.  
5.2 The presence of metals and metalloids in engine fuels can influence the performance of engines and contribute to shortening the lifetime of the equipment. In addition, some elements act as catalyst poison contributing to increases in the amount of unwanted gases and particulate matter emitted by vehicles.
SCOPE
1.1 This test method covers the determination of elements in biodiesel and biodiesel blends by microwave plasma atomic emission spectrometry (MP-AES). The specific elements within the scope of this method are calcium (Ca), magnesium (Mg), phosphorus (P), potassium (K), and sodium (Na).  
1.2 This test method conforms to Practice D6300, subection 8.4.5, valid test result range, and subsection 8.4.6, working range specifications. The valid test result range and working range are recent additions to Practice D6300, and a graphical representation using example values is shown in Appendix X2, Test Method Operating Range.  
1.3 Method working range:    
high expected concentration limit = highest ILS sample mean  
low expected concentration limit = lowest ILS sample mean if:  
lowest ILS sample mean − Rlowest ILS sample mean > 0; otherwise it is
determined by solving for X using the following equation:  
X − RX = coarsest resolution, determined by 0.5*σr lowest ILS sample mean    
Biodiesel and Biodiesel Blends  
Element  
Method Working Range
(expected mg/kg)  
Calcium  
0.24 to 15.01  
Magnesium  
0.12 to 11.55  
Phosphorus  
1.69 to 14.24  
Potassium  
0.49 to 13.98  
Sodium  
0.90 to 14.30  
1.4 This test method uses organic elemental standards in organic solvents for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent, and particles larger than a few micrometers can cause results to appear low.  
1.5 Elements present at mass fractions above the upper limit of the calibration curves can be determined with additional appropriate dilutions. Elements shall be measured at the wavelengths presented in Table 1. Alternate wavelengths noted in Appendix X1 may be used in the rare case of spectral interference.  
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.

SIGNIFICANCE AND USE
5.1 This test method provides rapid and precise measurement of total sulfur in petroleum and petroleum products with a minimum of sample preparation. A typical analysis time is 1 min to 2 min per sample.  
5.2 The quality of many petroleum products is related to the amount of sulfur present. Knowledge of sulfur concentration is necessary for processing purposes. There are also regulations promulgated in federal, state, and local agencies that restrict the amount of sulfur present in some fuels.  
5.3 This test method provides a means of determining whether the sulfur content of petroleum or a petroleum product meets specification or regulatory limits.  
5.4 When this test method is applied to petroleum materials with matrices significantly different from the white oil calibration materials specified in this test method, the cautions and recommendations in Section 6 should be observed when interpreting results.
Note 2: The equipment specified for Test Method D2622 tends to be more expensive than that required for alternative test methods, such as Test Method D4294. Consult the Index to ASTM Standards for alternative test methods.
SCOPE
1.1 This test method covers the determination of total sulfur in petroleum and petroleum products that are single-phase and either liquid at ambient conditions, liquefiable with moderate heat, or soluble in hydrocarbon solvents. These materials can include diesel fuel, jet fuel, kerosene, other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, crude oil, unleaded gasoline, gasoline-ethanol blends, and biodiesel.  
1.2 The range of this test method is between the PLOQ value (calculated by procedures consistent with Practice D6259) of 3 mg/kg total sulfur and the highest level sample in the round robin, 4.6 % by weight total sulfur.
Note 1: Instrumentation covered by this test method can vary in sensitivity. The applicability of the test method at sulfur concentrations below 3 mg/kg may be determined on an individual basis for WDXRF instruments capable of measuring lower levels, but precision in this test method does not apply.  
1.2.1 The values of the limit of quantitation (LOQ) and method precision for a specific laboratory’s instrument depends on instrument source power (low or high power), sample type, and the practices established by the laboratory to perform the method.  
1.3 Samples containing more than 4.6 % by mass sulfur should be diluted to bring the sulfur concentration of the diluted material within the scope of this test method. Samples that are diluted can have higher errors than indicated in Section 15 than non-diluted samples.  
1.4 Volatile samples (such as high vapor pressure gasolines or light hydrocarbons) may not meet the stated precision because of selective loss of light materials during the analysis.  
1.5 A fundamental assumption in this test method is that the standard and sample matrices are well matched, or that the matrix differences are accounted for (see 13.2). Matrix mismatch can be caused by C/H ratio differences between samples and standards or by the presence of other interfering heteroatoms or species (see Table 1).  
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.

SIGNIFICANCE AND USE
5.1 This test method provides rapid and precise measurement of total sulfur in petroleum and petroleum products with a minimum of sample preparation. A typical analysis time is 1 min to 5 min per sample.  
5.2 The quality of many petroleum products is related to the amount of sulfur present. Knowledge of sulfur concentration is necessary for processing purposes. There are also regulations promulgated in federal, state, and local agencies that restrict the amount of sulfur present in some fuels.  
5.3 This test method provides a means of determining whether the sulfur content of petroleum or a petroleum product meets specification or regulatory limits.  
5.4 When this test method is applied to petroleum materials with matrices significantly different from the calibration materials specified in 10.1, the cautions and recommendations in Section 6 should be observed when interpreting results.
SCOPE
1.1 This test method covers the determination of total sulfur in petroleum and petroleum products that are single-phase and either liquid at ambient conditions, liquefiable with moderate heat, or soluble in hydrocarbon solvents. These materials can include diesel fuel, jet fuel, kerosine, other distillate oil, naphtha, residual oil, lubricating base oil, hydraulic oil, crude oil, unleaded gasoline, gasoline-ethanol blends, biodiesel (see Note 2), and similar petroleum products.
Note 1: Oxygenated fuels with ethanol or methanol contents exceeding the limits given in Table 1 can be dealt with using this test method, but the precision and bias statements do not apply (see Appendix X3).
Note 2: For samples with high oxygen contents (>3 % by weight) sample dilution as described in 1.3 or matrix matching must be performed to assure accurate results.  
1.2 Interlaboratory studies on precision revealed the scope to be 17 mg/kg to 4.6 % by mass. An estimate of this test method’s pooled limit of quantitation (PLOQ) is 16.0 mg/kg as calculated by the procedures in Practice D6259. However, because instrumentation covered by this test method can vary in sensitivity, the applicability of the test method at sulfur concentrations below approximately 20 mg/kg must be determined on an individual basis. An estimate of the limit of detection is three times the reproducibility standard deviation, and an estimate of the limit of quantitation2 is ten times the reproducibility standard deviation.  
1.3 Samples containing more than 4.6 % by mass sulfur can be diluted to bring the sulfur concentration of the diluted material within the scope of this test method. Samples that are diluted can have higher errors than indicated in Section 17 than non-diluted samples.  
1.4 Volatile samples (such as high vapor pressure gasolines or light hydrocarbons) may not meet the stated precision because of selective loss of light materials during the analysis.  
1.5 A fundamental assumption in this test method is that the standard and sample matrices are well matched, or that the matrix differences are accounted for (see 6.2). Matrix mismatch can be caused by C/H ratio differences between samples and standards (see Section 6) or by the presence of other heteroatoms.  
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.

SIGNIFICANCE AND USE
5.1 This is the first ASTM standard covering the simultaneous determination of carbon, hydrogen, and nitrogen in petroleum products and lubricants.  
5.2 Carbon, hydrogen, and particularly nitrogen analyses are useful in determining the complex nature of sample types covered by this test method. The CHN results can be used to estimate the processing and refining potentials and yields in the petrochemical industry.  
5.3 The concentration of nitrogen is a measure of the presence of nitrogen containing additives. Knowledge of its concentration can be used to predict performance. Some petroleum products also contain naturally occurring nitrogen. Knowledge of hydrogen content in samples is helpful in addressing their performance characteristics. Hydrogen to carbon ratio is useful to assess the performance of upgrading processes.
SCOPE
1.1 These test methods cover the instrumental determination of carbon, hydrogen, and nitrogen in laboratory samples of petroleum products and lubricants. Values obtained represent the total carbon, the total hydrogen, and the total nitrogen.  
1.2 These test methods are applicable to samples such as crude oils, fuel oils, additives, and residues for carbon and hydrogen and nitrogen analysis. These test methods were tested in the concentration range of at least 75 % to 87 % by mass for carbon, at least 9 % to 16 % by mass for hydrogen, and  
1.3 The nitrogen test method is not applicable to light materials or those containing  
1.3.1 However, using Test Method D levels of 0.1 % by mass nitrogen in lubricants could be determined.  
1.4 These test methods are not recommended for the analysis of volatile materials such as gasoline, gasoline-oxygenate blends, or gasoline type aviation turbine fuels.  
1.5 The results of these tests can be expressed as mass % carbon, hydrogen or nitrogen.  
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.

SIGNIFICANCE AND USE
5.1 Operating experience of gas turbines and diesel engines has shown that some of the ash-forming substances present in a fuel can lead to high temperature corrosion, ash deposition, and fuel system fouling. Ash-forming materials may be in a fuel as oil-soluble metallo-organic compounds as water-soluble salts or as solid foreign contamination. Their presence and concentration varies with the geographical source of a crude oil and they are concentrated in the residual fractions during the refining process. Although distillate fuel oils are typically contaminant free, ash-forming materials may be introduced later in the form of salt-bearing water or by contact with other petroleum products during transportation and storage. Specifications of gas turbine and diesel engine fuels and the significance of contamination and trace metals are detailed in Specifications D2880 and D975.  
5.1.1 Pre-conditioning of the fuel before it reaches the gas turbine or diesel engine has become a prerequisite for installations that use heavy petroleum fuel, and also for sites that use light distillate fuel oils. On-site fuel analysis to determine the extent of contamination is an integral part of a fuel quality management program. It is used first to determine the extent of the required treatment, and later, the effectiveness of the treatment. It starts with the delivery of the fuel, continues throughout fuel handling and ends only as the fuel is injected into the turbine or engine.  
5.1.2 Fuel contamination specifications vary among the different gas turbine manufacturers. However, without exception, each requires that contaminants must be as low as possible. In most power generation installations, it is the owner who has the responsibility of verifying fuel cleanliness in compliance with the turbine manufacturer's warranty specifications. This leads to an on-site analytical instrument performance requirement of below 1.0 mg/kg for several elements.
SCOPE
1.1 This test method covers the determination of contaminants and materials as a result of corrosion in gas turbine or diesel engine fuels by rotating disc electrode atomic emission spectroscopy (RDE-AES).  
1.1.1 The test method is applicable to ASTM Grades 0-GT, 1-GT, 2-GT, 3-GT, and 4-GT gas turbine fuels and Grades Low Sulfur No. 1-D, Low Sulfur No. 2-D, No. 1-D, No. 2-D, and No. 4-D diesel fuel oils.
1.1.1.1 Trace metal limits of fuel entering turbine combustor(s) are given as 0.5 mg/kg each for vanadium, sodium + potassium, calcium, and lead in Specification D2880 for all GT grades.  
1.1.2 This test method provides a rapid at-site determination of contamination and corrosive elements ranging from fractions of mg/kg to hundreds of mg/kg in gas turbine and diesel engine fuels so the fuel quality and level of required treatment can be determined.  
1.1.3 This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine or detect insoluble particles.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. The preferred units for concentration are mg/kg (ppm by mass).  
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.

SIGNIFICANCE AND USE
4.1 This test method can be used to determine total sulfur levels in process feeds and finished products that fall within the scope of this test method.  
4.2 Low levels of sulfur in process feed stocks can poison expensive catalysts used in petroleum refining processes. This test method can be used to monitor sulfur levels in these feedstocks.
SCOPE
1.1 This test method covers the determination of total sulfur in liquid hydrocarbons with a final boiling point less than 450 °C by gas chromatography using a flame photometric detector.  
1.2 This test method is applicable for total sulfur levels from 0.5 mg/kg S to 100 mg/kg S.
Note 1: The pooled limit of quantification (PLOQ) derived from the 2002 interlaboratory cooperative test program was determined to be 1 mg/kg S.
Note 2: Samples can also be tested at other total sulfur levels, but the precision statements may not apply.  
1.3 The values stated in SI units are to be regarded as 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. For specific hazard 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.

SIGNIFICANCE AND USE
5.1 Trace elemental analysis is used to indicate the level of contamination of middle distillate fuels. Trace metals in turbine fuels can cause corrosion and deposition on turbine components at elevated temperatures. Some diesel fuels have specification limit requirements for trace metals to guard against engine deposits. Trace level copper in middle distillate aviation turbine fuel can significantly accelerate thermal instability of the fuel, leading to oxidation and production of detrimental insoluble deposits in the engine.  
5.2 Gas turbine fuel oil Specification D2880 provides recommended upper limits for five trace metals (calcium, lead, sodium, potassium, and vanadium). Military specification MIL-DTL-16884 for naval distillate fuel sets requirements for maximum concentrations of the same five metals. Both specifications designate Test Method D3605, an atomic absorption/flame emission method, for the quantitative analysis of four of the metals. Test Method D3605 does not cover potassium. This test method provides an alternative to Test Method D3605, covers potassium and a number of additional elements.  
5.3 There are several sources of multi-element contamination of naval distillate fuel. Sea water is pumped into the diesel fuel tanks (as ballast) to trim ships. Also, some of the oilers (fuel supply ships) have dirty tanks. Corrosion products come from unlined tanks, piping, pumps, and heat exchangers.
SCOPE
1.1 This test method covers the determination of selected elements in middle distillate fuels by inductively coupled plasma atomic emission spectrometry (ICP-AES). The specific elements are listed in Table 1. The concentration range of this test method is approximately 0.1 mg/kg to 2.0 mg/kg. The test method may be used for concentrations outside of this range; however, the precision statements may not be applicable. Middle distillate fuels covered in this test method have all distillation fractions contained within the boiling range of 150 °C to 390 °C. This includes, but is not limited to, diesel fuels and aviation turbine fuels.  
1.2 This test method is not intended to analyze insoluble particulates. However, very small particulate matter (smaller than a micrometre) will be carried into the plasma and be included in the quantitative analysis.  
1.3 This test method may give a result that is higher than the true value if an analyte is present in the sample in a form which is sufficiently volatile. For example, hexamethyldisiloxane will generate a biased high result for silicon.  
1.4 The values stated in SI units are to be regarded as 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.

SIGNIFICANCE AND USE
5.1 Lubricating oils are formulated with organo-metallic additives, which act, for example, as detergents, antioxidants, antifoaming, or antiwear agents, or a combination thereof. Some of these additives contain one or more of the following elements: magnesium, phosphorus, sulfur, chlorine, calcium, zinc, and molybdenum. This test method provides a means of determining the concentrations of these elements, which in turn provides an indication of the additive content of these oils.  
5.2 Several additive elements and their compounds are added to the lubricating oils to give beneficial performance (Table 2).  
5.3 Additive packages are the concentrates that are used to blend lubricating oils.  
5.4 This test method is primarily intended to be used for the monitoring of additive elements in lubricating oils.  
5.5 If this test method is applied to lubricating oils with matrices significantly different from the calibration materials specified in this test method, the cautions and recommendations in Section 6 should be observed when interpreting the results.
SCOPE
1.1 This test method covers the quantitative determination of additive elements in unused lubricating oils and additive packages, as shown in Table 1.    
1.2 Additive packages require dilution with a contamination free diluent (base oil) prior to analysis. The dilution factor has to be calculated from the expected concentrations to bring the concentrations for all elements into the ranges listed in Table 1.  
1.3 Some lubrication oils will contain higher concentrations than the maximum concentrations listed in Table 1. These samples require dilution with a contamination free diluent (base oil) prior to analysis. The dilution factor has to be calculated from the expected concentrations to bring the concentrations for all elements into the ranges listed in Table 1.  
1.4 This test method is limited to the use of energy dispersive X-ray fluorescence (EDXRF) spectrometers employing an X-ray tube for excitation in conjunction with the ability to separate the signals of adjacent elements by using a high resolution semiconductor detector.  
1.5 This test method uses inter-element correction factors calculated from a fundamental parameters (FP) approach or from another matrix correction method.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6.1 The preferred concentration units are mg/kg or mass %.  
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.

SIGNIFICANCE AND USE
4.1 The sulfur content of LPG, used for fuel purposes, contributes to SOx emissions and can lead to corrosion in engine and exhaust systems. Some process catalysts used in petroleum and chemical refining can be poisoned by sulfur bearing materials in the feed stocks. This test method can be used to determine sulfur in process feeds, to measure sulfur in finished products, and can also be used for compliance determinations when acceptable to a regulatory authority.
SCOPE
1.1 This test method covers the determination of total volatile sulfur in gaseous hydrocarbons and liquefied petroleum (LP) gases. It is applicable to analysis of natural, processed, and final product materials. Precision has been determined for sulfur in gaseous hydrocarbons in the range of 1 mg/kg to 100 mg/kg and for sulfur in LP gases in the range of 1 mg/kg to 196 mg/kg (Note 1).
Note 1: An estimate of pooled limit of quantification (PLOQ), information regarding sample stability and other general information derived from the interlaboratory studies on precision can be referenced in the ASTM research reports.2,3  
1.2 This test method may not detect sulfur compounds that do not vaporize under the conditions of the test.  
1.3 This test method is applicable for total volatile sulfur determination in LP gases containing less than 0.35 % (mass/mass) halogen(s).  
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. See 3.1 and Sections 6 and 7 for specific warning statements.  
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.

SIGNIFICANCE AND USE
4.1 These test methods determine the concentration of lead (from alkyl addition) in gasoline. These alkyl additives improve the antiknock properties.  
4.2 Test Method C is used to ensure compliance of trace lead as required by federal regulations for lead-free gasoline (40 CFR Part 80).  
4.3 Test Method D is used to determine the concentration of manganese in aviation gasoline.
SCOPE
1.1 These test methods cover the determination of lead and manganese gasoline additives content by X-Ray Fluorescence Spectroscopy (XRF). These test methods cover the determination of the total lead content of a gasoline within the following concentration ranges:    
0.010 g Pb/US gal to 5.0 g Pb/US gal  
0.012 g Pb/UK gal to 6.0 g Pb/UK gal  
0.0026 g Pb/L to 1.32 g Pb/L and total manganese content of aviation gasoline within the concentration range of 25 mg Mn/L to 250 mg Mn/L.  
1.1.1 Test Methods A and B cover the range of 0.10 g Pb/US gal to 5.0 g Pb/US gal. Test Method C covers the range of 0.010 g Pb/US gal to 0.50 g Pb/US gal.  
1.1.2 These Methods A, B, and C are applicable to gasoline containing lead additives. These test methods compensate for normal variation in gasoline composition and are independent of lead alkyl type.  
1.1.3 Test Method D is applicable to aviation gasoline containing manganese additives.  
1.2 Test Method A (formerly in withdrawn Test Method D2599)—Sections 5 – 10.
Test Method B (formerly in withdrawn Test Method D2599)—Sections 11 – 16.
Test Method C (formerly in withdrawn Test Method D3229)—Sections 17 – 23.
Test Method D—Sections 24 – 29.  
1.3 The values stated in SI are to be regarded as the standard. For reporting purposes the values stated in grams per U.S. gallon are the preferred units in the United States. Note that in other countries, other units can be preferred.  
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 hazard statements, see Sections 5, 6, 11, and 18.  
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.

SIGNIFICANCE AND USE
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).
SCOPE
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.

SIGNIFICANCE AND USE
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.
SCOPE
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.

SIGNIFICANCE AND USE
7.1 Accurate elemental analysis of petroleum products and lubricants is necessary for the determination of chemical properties, which are used to establish compliance with commercial and regulatory specifications.  
7.2 Ion chromatography is often used in cases where anion content of the material is desired. Some of the hetero-atoms can be converted by combustion in an oxygen atmosphere followed by aqueous dissolution to convert them into anions before ion chromatographic determination. A number of ion chromatographic ASTM standards issued are listed in Section 2. Of these, the D02, D05, and D16 Committee standards which use ion chromatography are listed in Table 1.
SCOPE
1.1 This practice covers the information on calibration, quality control, and operational guidance for anionic measurements using ion chromatography (IC).  
1.2 IC Related Standards—Chemically or electrolytically regenerated suppressed ion chromatography standards for aqueous matrices include Test Methods D2988, D4327, D5085, D5542, D5827, D5987, D5996, D6581, D7319, D7328, D7359, D7773, D7994, and D8150; IC instrumentation requirements are described in Practices E1151, and E1511.  
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.

SIGNIFICANCE AND USE
4.1 Accurate elemental analysis of petroleum products and lubricants is necessary for the determination of chemical properties, which are used to establish compliance with commercial and regulatory specifications.  
4.2 Inductively coupled plasma-atomic emission spectrometry is one of the more widely used analytical techniques in the oil industry for multi-element analysis as evident from at least twelve standard test methods (for example, Test Methods C1111, D1976, D4951, D5184, D5185, D5600, D5708, D6130, D6349, D6357, D7040, D7111, D7303, and D7691) published for the analysis of fossil fuels and related materials. These have been briefly summarized by Nadkarni (1).5  
4.2.1 Determination of mercury and trace metals in crude oils using atomic spectroscopic methods is discussed in Guide D8056.  
4.3 The advantages of using an ICP-AES analysis include high sensitivity for many elements of interest in the oil industry, relative freedom from interferences, linear calibration over a wide dynamic concentration range, single or multi-element capability, and ability to calibrate the instrument based on elemental standards irrespective of their elemental chemical forms, within limits described below such as solubility and volatility assuming direct liquid aspiration. Thus, the technique has become a method of choice in most of the oil industry laboratories for metal analyses of petroleum products and lubricants.  
4.4 In addition to the ICP-AES standards listed in 2.2, a new ICP-MS standard, Test Method D8110, has been issued for analysis of distillate products for multi-element determination of Al, Ca, Cu, Fe, Pb, Mg, and K.
SCOPE
1.1 This practice covers information on the calibration and operational guidance for the multi-element measurements using inductively coupled plasma-atomic emission spectrometry (ICP-AES).  
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

SIGNIFICANCE AND USE
5.1 Accurate elemental analysis of petroleum products and lubricants is necessary for the determination of chemical properties, which are used to establish compliance with commercial and regulatory specifications.  
5.2 Atomic Absorption Spectrometry (AAS) is one of the most widely used analytical techniques in the oil industry for elemental analysis. There are at least twelve Standard Test Methods published by ASTM D02 Committee on Petroleum Products and Lubricants for such analysis. See Table 1.  
5.3 The advantage of using an AAS analysis include good sensitivity for most metals, relative freedom from interferences, and ability to calibrate the instrument based on elemental standards irrespective of their elemental chemical forms. Thus, the technique has been a method of choice in most of the oil industry laboratories. In many laboratories, AAS has been superseded by a superior ICP-AES technique (see Practice D7260).  
5.4 Some of the ASTM AAS Standard Test Methods have also been issued by other standard writing bodies as technically equivalent standards. See Table 2. (A) Excerpted from ASTM MNL44, Guide to ASTM Test Methods for the Analysis of Petroleum Products and Lubricants, 2nd edition, Ed., Nadkarni, R. A. Kishore, ASTM International, West Conshohocken, PA, 2007.
SCOPE
1.1 This practice covers information on the calibration and operational guidance for elemental measurements using atomic absorption spectrometry (AAS).  
1.1.1 AAS Related Standards—Test Methods D1318, D3237, D3340, D3605, D3831, D4628, D5056, D5184, D5863, D6732; Practices D7260 and D7455; and Test Methods D7622 and D7623.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

SIGNIFICANCE AND USE
4.1 These test methods cover, in single procedures, the determination of Ni, V, and Fe in crude oils and residual oils. These test methods complement Test Method D1548, which covers only the determination of vanadium.  
4.2 When fuels are combusted, vanadium present in the fuel can form corrosive compounds. The value of crude oils can be determined, in part, by the concentrations of nickel, vanadium, and iron. Nickel and vanadium, present at trace levels in petroleum fractions, can deactivate catalysts during processing. These test methods provide a means of determining the concentrations of nickel, vanadium, and iron.
SCOPE
1.1 These test methods cover the determination of nickel, vanadium, and iron in crude oils and residual fuels by inductively coupled plasma (ICP) atomic emission spectrometry. Two different test methods are presented.  
1.2 Test Method A (Sections 7 – 11 and 18 – 22)—ICP is used to analyze a sample dissolved in an organic solvent. This test method uses oil-soluble metals for calibration and does not purport to quantitatively determine or detect insoluble particulates.  
1.3 Test Method B (Sections 12 – 22)—ICP is used to analyze a sample that is decomposed with acid.  
1.4 The concentration ranges covered by these test methods are determined by the sensitivity of the instruments, the amount of sample taken for analysis, and the dilution volume. A specific statement is given in 15.2. Typically, the low concentration limits are a few tenths of a milligram per kilogram. Precision data are provided for the concentration ranges specified in Section 21.  
1.5 The values stated in SI units are to be regarded as standard.  
1.5.1 Exception—The values given in parentheses are for information only.  
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.

SIGNIFICANCE AND USE
5.1 This test method covers the determination of V, Ni, Ca, Na, Al, Si, Zn, P, and S for residual fuels and Fe, V, Ni,Ca, Na, K, and S for crude oils. This test method complements and extends the capabilities of Test Methods D1548 and D5708, which only apply to the determination of Ni, V, and Fe in crude oils and residual fuels.  
5.2 The metals and other elements tested for in this method may occur naturally or may be added as a result of production (that is, catalyst fines).
SCOPE
1.1 This test method covers the determination of metals and other elements in residual fuel and crude oil by microwave plasma atomic emission spectroscopy (MP-AES). The specific elements within the scope of this method are V, Ni, Ca, Na, Al, Si, Zn, P, and S for residual fuel oil and Fe, V, Ni, Ca, Na, K, and S for crude oils.  
1.2 Method working range:
high expected concentration limit = highest ILS sample mean
low expected concentration limit = lowest ILS sample mean if:
(1) lowest ILS sample mean − Rlowest ILS sample mean > 0; otherwise it is determined by solving for X using the following equation:
(2) X − RX= coarsest resolution, determined by
0.5*σr lowest ILS sample mean    
Crude Oil:  
Element  
Method Working Range  
(expected mg/kg)  
Iron  
0.70 to 161.02  
Vanadium  
2.88 to 417.50  
Nickel  
0.36 to 107.66  
Calcium  
5.41 to 96.78  
Sodium  
1.18 to 97.13  
Potassium  
7.01 to 63.83  
Sulfur  
1059 to 35194    
Residual Fuel Oil:  
Element  
Method Working Range  
(expected mg/kg)  
Vanadium  
3.88 to 370.09  
Nickel  
1.47 to 96.68  
Calcium  
4.41 to 102.01  
Sodium  
2.80 to 112.67  
Aluminum  
4.13 to 154.12  
Silicon  
5.99 to 237.56  
Zinc  
2.75 to 102.46  
Sulfur  
1314 to 30134  
1.3 This test method uses soluble metals in organic solvents for calibration and does not purport to quantitatively determine insoluble particulates. Analytical results are particle size dependent, and particles larger than a few micrometers may cause results to appear low  
1.4 Elements present at mass fractions above the upper limit of the calibration curves can be determined with additional appropriate dilutions. Elements shall be measured at the wavelengths presented in Table 1.  
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.

SIGNIFICANCE AND USE
5.1 Used Industrial Oil—The detection of large particles are important inputs for used industrial lubricant condition mornitoring. For wear metals, these particles, in size, are represented by those between 20 μm and 50 μm in engine oil, 80 μm or greater in gear-box oil. In desert or windy areas, large sand and dust particles can enter in-service lubricant. The concentrations contributed from large particles can be more sensitive to serious or catastrophic failure of industrial equipment than those from 10 μm or less. In spectroscopic analysis, excluding large particles significantly under-reports the concentrations of wear and contamination elements. The corresponding results may not represent the actual state of in-service lubricant. Because this test method posts less limitation on the size of wear metal particles while still reporting normal fine wear particles, it provides a means to assess wear and contamination elements in a comprehensive range of the size of particulates and raises the fidelity of spectroscopic analysis of in-service lubricant.  
5.2 Non-suspendable Particles in Used Industrial Oil—The increase of non-suspendable particles suggests excessive wear or poor sealing of machinery, or both. Large amounts of such particulate in industrial oil bulk itself are harmful to moving parts of machinery. This test method provides another means to identify the presence or absence of the non-suspendable particles for machinery condition monitoring.
SCOPE
1.1 This test method covers the determination of wear metals and contaminants in used industrial oils by sweeping flat electrode atomic emission spectroscopy (SFE-AES).2  
1.2 Industrial oil includes lubricant oil, gear box oil, hydraulic fluid, compressor oil, turbine oil, synthetic oils, and other petroleum oils.  
1.3 Method working range for every element is evaluated by equations in 15.2.1 and tabulated in Table 6.  
1.4 Though this technique is designed to analyze non-suspended particles in lubricant samples, the precision statements published here were established solely from homogeneous oil samples per Practice D6300 requirements. Non-suspended particles, which are inhomogeneous by nature, were not sampled and evaluated for deriving precision statements for this test method (see Annex A1).  
1.5 This test method provides a quick indication for abnormal wear and the presence of contamination in new or used industrial oils by immediately reporting:  
1.5.1 Normal fine particles of specific wear metals;  
1.5.2 Non-suspendable particles of specific wear metals and of contamination elements;  
1.5.3 Less populated large particles (10 μm to 50 μm) of specific wear metals;  
1.5.4 Contamination elements; and  
1.5.5 Additive elements.  
1.6 This test method uses oil-soluble elements for calibration and does not purport to relate quantitatively the values determined as insoluble particles to the dissolved metals. Analytical results are particle size dependent and low results may be obtained for those elements present in used oil samples as large particles (referenced by Test Methods D5185 and D6595).  
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.

SIGNIFICANCE AND USE
5.1 The emission of mercury during crude oil refining is an environmental concern. The emission of mercury may also contaminate refined products and form amalgams with metals, such as aluminum.  
5.2 When representative test portions are analyzed according to this procedure, the total mercury is representative of concentrations in the sample.
SCOPE
1.1 This test method covers the procedure to determine the total mercury content in a sample of crude oil. This test method can be used for total mercury determination in natural and processed liquid and oil products (gasoline, naphtha, etc.).  
1.2 This test method may be applied to samples containing between 5.0 ng/mL to 350 ng/mL of mercury. The results may be converted to mass basis.  
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 work has been published in “Determination of Mercury in Crude Oil by Atomic Spectroscopy.”2  
1.5 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.  
1.6 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.