5.1 The presence and content of various impurities in graphite are major considerations in determining the suitability of graphite for various applications. This test method provides an alternative means of determining the content of trace impurities in a graphite sample which has considerable advantages compared to classical wet-chemical analysis methods.5.2 The test method provides a standard procedure to measure impurities in graphite and to assure required graphite specifications.1.1 This test method covers the measurement of mass fractions of the elements silver (Ag), aluminum (Al), arsenic (As), boron (B), barium (Ba), berylium (Be), bismuth (Bi), calcium (Ca), cadmium (Cd), cobalt (Co), chromium (Cr), copper (Cu), iron (Fe), potassium (K), lithium (Li), magnesium (Mg), manganese (Mn), molybdenum (Mo), sodium (Na), nickel (Ni), phosphorus (P), lead (Pb), sulfur (S), antimony (Sb), silicon (Si), tin (Sn), strontium (Sr), titanium (Ti), vanadium (V), tungsten (W), yitrium (Y), zinc (Zn), and zirconium (Zr) in graphite.1.2 Provided that an appropriate validation procedure is carried out, this test method is also applicable to other carbon materials such as coal, coke, carbon black, graphite-felt, graphite-foil, graphite-foam, and fiber reinforced carbon-carbon composites.1.3 This test method is applicable to element contents from approximately 0.0001 mg/kg to 1000 mg/kg (0.1 ppmw to 1000 ppmw), depending on element, wavelength, measurement parameters, and sample mass.1.4 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.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This test method can be used on plutonium matrices in nitrate solutions.5.2 This test method has been validated for all elements listed in Test Methods C757 except sulfur (S) and tantalum (Ta).5.3 This test method has been validated for all of the cation elements measured in Table 1. Phosphorus (P) requires a vacuum or an inert gas purged optical path instrument.1.1 This test method covers the determination of 25 elements in plutonium (Pu) materials. The Pu is dissolved in acid, the Pu matrix is separated from the target impurities by an ion exchange separation, and the concentrations of the impurities are determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES).1.2 This test method is specific for the determination of impurities in 8 M HNO3 solutions. Impurities in other plutonium materials, including plutonium oxide samples, may be determined if they are appropriately dissolved (see Practice C1168) and converted to 8 M HNO3 solutions.1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions that are provided for information only and are not considered standard. Additionally, the non-SI units of molarity and centimeters of mercury 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. Some specific hazards statements are given in Section 9 on Hazards.1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This practice describes the essential components of an ICP-AES. The components include excitation/radio-frequency generators, sample introduction systems, spectrometers, detectors, and signal processing and displays. This description allows the user or potential user to gain a cursory understanding of an ICP-AES system. This practice also provides a means for comparing and evaluating various systems, as well as understanding the capabilities and limitations of each instrument.5.2 Training—The manufacturer should provide training in safety, basic theory of ICP-AES analysis, operations of hardware and software, and routine maintenance for at least one operator. Training ideally should consist of the basic operation of the instrument at the time of installation, followed by an in-depth course one or two months later. Advanced courses are also offered at several of the important spectroscopy meetings that occur throughout the year as well as by independent training institutes. Several independent consultants are available who can provide training, sometimes at the user's site.1.1 This practice describes the components of an inductively coupled plasma atomic emission spectrometer (ICP-AES) that are basic to its operation and to the quality of its performance. This practice identifies critical factors affecting accuracy, precision, and sensitivity. It is not the intent of this practice to specify component tolerances or performance criteria, since these are unique for each instrument. A prospective user should consult with the manufacturer before placing an order, to design a testing protocol that demonstrates the instrument meets all anticipated needs.1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 13.

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3.1 This terminology was drafted to exclude any commercial relevance to any one vendor by using only general terms that are acknowledged by all vendors and should be revised as charge-coupled device (CCD) technology matures. This terminology uses standard explanations, symbols, and abbreviations.1.1 This terminology brings together and clarifies the basic terms and definitions used with scientific grade cooled charge-coupled device (CCD) detectors, thus allowing end users and vendors to use common documented terminology when evaluating or discussing these instruments. CCD detectors are sensitive to light in the region from 200 nm to 1100 nm and the terminology outlined in the document is based on the detection technology developed around CCDs for this range of the spectrum.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This test method is useful for the determination of elemental concentrations in the range of approximately 0.1 µgg-1 to 10 percent (%) (See Table X1.1) in soda-lime glass samples (7 and 8). A standard test method can aid in the interchange of data between laboratories and in the creation and use of glass databases.5.2 The determination of elemental concentrations in glass provides high discriminating value in the forensic comparison of glass fragments.5.3 This test method produces minimal destruction of the sample. Microscopic craters of 50 µm to 100 µm in diameter by 80 µm to 150 µm deep are left in the glass fragment after analysis. The mass removed per replicate is approximately 0.4 µg to 3 µg (6).5.4 Appropriate sampling techniques shall be used to account for natural heterogeneity of the materials at a microscopic scale.5.5 The precision, bias, and limits of detection of the method (for each element measured) shall be established during validation of the method. The measurement uncertainty of any concentration value used for a comparison shall be recorded with the concentration.5.6 Acid digestion of glass followed by either Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) can also be used for trace elemental analysis of glass, and offer similar detection levels and the ability for quantitative analysis. However, these methods are destructive, and require larger sample sizes and more sample preparation (Test Method E2330).5.7 Micro X-Ray Fluorescence (µ-XRF) uses comparable sample sizes to those used for LA-ICP-MS with the advantage of being non-destructive of the sample. Some of the drawbacks of µ-XRF include lower sensitivity and precision, and longer analysis time (Test Method E2926).5.8 Scanning Electron Microscopy with Energy Dispersive Spectrometry (SEM-EDS) is also available for elemental analysis, but it is of limited use for forensic glass source discrimination due to poor detection limits for higher atomic number elements present in glass at trace concentration levels. However, distinguishing between sources having similar RIs and densities is sometimes possible.1.1 This test method covers a procedure for the quantitative elemental analysis of the following seventeen elements: lithium (Li), magnesium (Mg), aluminum (Al), potassium (K), calcium (Ca), iron (Fe), titanium (Ti), manganese (Mn), rubidium (Rb), strontium (Sr), zirconium (Zr), barium (Ba), lanthanum (La), cerium (Ce), neodymium (Nd), hafnium (Hf) and lead (Pb) through the use of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for the forensic comparison of glass fragments. The potential of these elements to provide the best discrimination among different sources of soda-lime glasses has been published elsewhere (1-5).2 Silicon (Si) is also monitored for use as a normalization standard. Additional elements may be added as needed, for example, tin (Sn) can be used to monitor the orientation of float glass fragments.1.2 The method only consumes approximately 0.4 µg to 3 µg of glass per replicate and is suitable for the analysis of full thickness samples as well as irregularly shaped fragments as small as 0.1 mm by 0.1 mm by 0.2 mm (6) in dimension. The concentrations of the elements listed above range from the low parts per million (µgg-1) to percent (%) levels in soda-lime glass, the most common type encountered in forensic cases. This standard method can be applied for the quantitative analysis of other glass types; however, some modifications in the reference standard glasses and the element menu may be required.1.3 This standard is intended for use by competent forensic science practitioners with the requisite formal education, discipline-specific training (see Practice E2917), and demonstrated proficiency to perform forensic casework.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.

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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.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.

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5.1 The composition of liquefied gaseous fuels (LNG, LPG) is important for custody transfer and production. Compositional determination is used to calculate the heating value, and it is important to ensure regulatory compliance. Compositional determination is also used to optimize the efficiency of liquefied hydrocarbon gas production and ensure the quality of the processed fluids.5.2 Alternatives to compositional measurement using Raman spectroscopy are described in Test Method D1945, Practice D1946, and Test Method D7833.5.3 The advantage of this practice over other standards stated in 5.2, is that Raman spectroscopy can determine composition by directly measuring the liquefied natural gas. Unlike chromatography, no vaporization step is necessary. Since incorrect operation of on-line vaporizers can lead to poor precision and accuracy, elimination of the vaporization step offers a significant improvement in the analysis of LNG.1.1 This practice is for both on-line and laboratory instrument-based determination of composition for liquefied natural gas (LNG) using Raman spectroscopy. Although the procedures in this practice refer specifically to liquids, the basic methodology can also be applied to other light hydrocarbon mixtures in either liquid or gaseous states, provided the data quality objectives and measurement needs are met. From the composition, gas properties such as heating value and the Wobbe index may be calculated. The components commonly determined according to this test method are CH4, C2H6, C3H8, i-C4H10, n-C4H10, iC5H12, n-C5H12. Components heavier than C5 are not measured as part of this practice.NOTE 1: Raman spectroscopy does not directly quantify the component percentages of noble gases; however, inert substances can be calculated indirectly by subtracting the sum of the other species from 100 %.1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This test method provides for a separation of coal-associated sulfur into two commonly recognized forms: pyritic and sulfate. Organic sulfur is calculated by difference. Results obtained by the test method are used to serve a number of interests, including the evaluation of coal preparation and processing operations designed to reduce coal sulfur levels.1.1 This test method applies to the determination of sulfate sulfur and pyritic sulfur in coal and calculates organic sulfur by difference. This test method is not applicable to coke or other carbonaceous materials.1.2 The values stated in SI units are to be regarded as standard. Non-SI units, if provided, are considered informational and are contained within parentheses1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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5.1 This test method is intended for use with other standards that address the collection and preparation of samples (dusts by wipe, dried paint chips, and soils) that are obtained during the assessment or mitigation of lead hazards from buildings and related structures.5.2 Laboratories analyzing samples obtained during the assessment or mitigation of lead hazards from buildings and related structures shall conform to Practice E1583, or shall be recognized for lead analysis as promulgated by authorities having jurisdiction, or both.NOTE 1: In the United States of America, laboratories performing analysis of samples collected during lead-based paint activities are required to be accredited to ISO/IEC 17025 and to other requirements promulgated by the Environmental Protection Agency (EPA).5.3 This test method may also be used to analyze similar samples from other environments such as toxic characteristic extracts of waste sampled using Guide E1908 as prepared for analysis using EPA SW-846 Test Method 1311.1.1 This test method specifies a procedure for analysis of dried paint, soil, and dust wipe samples collected in and around buildings and related structures for lead content using inductively coupled plasma-optical emission spectroscopy (ICP-OES).1.2 This test method should be used by analysts experienced in the use of ICP-OES, the interpretation of spectral and matrix interferences, and procedures for their correction. For determination of lead (Pb) and other metals in air by ICP-OES, see Test Method D7035.1.3 This test method cites specific methods for preparing test solutions of dried paint, soil, and wipe samples for analysis.1.4 It is the user’s responsibility to ensure the validity of this test method for sampling materials of untested matrices.1.5 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-OES instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices or the precision between instruments of the same make and model.1.6 This test method contains notes that are explanatory and are not part of the mandatory requirements of this test method.1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.7.1 Exception—The inch-pound and SI units shown for wipe sampling data are to be individually regarded as standard for wipe sampling data.1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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4.1 This technique is destructive, in that the glass fragments may need to be crushed, and digested in acid.4.2 Although the concentration ranges of the calibration curves shown in Appendix X1 are applicable to soda lime and borosilicate glass, this method is useful for the accurate measurement of element concentrations from a wide variety of glass samples.4.3 The determination of the element concentrations in glass yields data that can be used to compare fragments.4.4 It should be recognized that the method measures the bulk concentration of the target elements. Any extraneous material present on the glass that is not removed before digestion can result in inaccurate concentrations of the measured elements.4.5 The precision and accuracy of the method should be established in each laboratory that employs the method.1.1 One objective of a forensic glass examination is to compare glass samples to determine if they can be discriminated using their physical, optical or chemical properties (for example, color, refractive index (RI), density, elemental composition). If the samples are distinguishable in any of these observed and measured properties, it may be concluded that they did not originate from the same source of broken glass. If the samples are indistinguishable in all of these observed and measured properties, the possibility that they originated from the same source of glass cannot be eliminated. The use of an elemental analysis method such as inductively coupled plasma mass spectrometry yields high discrimination among sources of glass. (1-16)21.2 This test method covers a procedure for quantitative determination of the concentrations of magnesium (Mg), aluminum (Al), iron (Fe), titanium (Ti), manganese (Mn), rubidium (Rb), strontium (Sr), zirconium (Zr), barium (Ba), lanthanum (La), cerium (Ce), neodymium (Nd), samarium (Sm), and lead (Pb) in glass samples.1.3 This procedure is applicable to irregularly shaped samples as small as 200 micrograms, for the comparison of fragments of a known source to the recovered fragments from a questioned source. These elements are present in soda lime and borosilicate glass in μg/L to % levels.1.4 This procedure is applicable to other elements, other types of glass, and other concentration ranges with appropriate modifications of the digestion procedure (if needed for full recovery of the additional elements), calibration standards and the mass spectrometer conditions. Calcium and potassium, for example, could be added to the list of analytes in a modified analysis scheme. Alternative methods for the determination of concentrations of elements in glass are listed in the references.1.5 For any given glass, approximately 40 elements are likely to be present at detectable concentrations using this procedure with minor modifications. The element set stated here is an example of some of these elements that can be detected in glass and used for forensic comparisons.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 cannot replace knowledge, skills, or abilities acquired through education, training, and experience and is to be used in conjunction with professional judgment by individuals with such discipline-specific knowledge, skills, and abilities.1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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This test method measures the presence of uranium and thorium in soil that occurs naturally and as a result of contamination from nuclear operations and uranium ore processing. The reporting detection levels (RDLs) of total uranium and thorium are well below the normal background in soil. The normal background level for uranium is between 3 and 5 μg/g in most geographic areas and slightly higher for thorium. The 235U enrichment is also measured from an initial sample pass through the instrument. The other less abundant uranium isotopes (234U and 236U) are measured down to a typical soil background level after sample concentration and a second sample analysis. This allows for calculation of individual isotopic uranium and total uranium activity. The majority of the uranium activity results from 234U and 238U.1.1 This test method covers the measurement of total uranium (U) and thorium (Th) concentrations in soils, as well as the determination of the isotopic weight percentages of 234U, 235U, 236U, and 238U, thereby allowing for the calculation of individual isotopic uranium activity or total uranium activity. This inductively coupled plasma-mass spectroscopy (ICP-MS) method is intended as an alternative analysis to methods such as alpha spectroscopy or thermal ionization mass spectroscopy (TIMS). Also, while this test method covers only those isotopes listed above, the instrumental technique may be expanded to cover other long-lived radioisotopes since the preparation technique includes the preconcentration of the actinide series of elements. The resultant sample volume can be further reduced for introduction into the ICP-MS via an electrothermal vaporization (ETV) unit or other sample introduction device, even though the standard peristaltic pump introduction is applied for this test method. The sample preparation removes organics and silica from the soil by use of a high temperature furnace and hydrofluoric acid digestion. Thus, this test method can allow for sample variability of both organic and silica content. This test method is also described in ASTM STP 1291. Since this test method using quadrupole ICP-MS was approved, advances have been made in ICP-MS technology in terms of improved sensitivity and lower instrument background as well as the use of collision or reaction cells (or both) and sector field mass spectrometers with single and multiple detectors. These advances should allow this test method to be performed more effectively but it is the user’s responsibility to verify performance.1.2 The analysis is performed after an initial drying and grinding sample preparation process, and the results are reported on a dry weight basis. The sample preparation technique used incorporates into the sample any rocks and organic material present in the soil. The method of sample preparation applied differs from other techniques, such as those found in Practice C 999, which involve simply tumbling and sieving the sample; however, the user may select whichever technique is most appropriate to their needs.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 and health practices and determine the applicability of regulatory limitations prior to use.

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This practice may be used as part of a bioassay program for workers potentially exposed to nuclear material by measuring 237Np, 232Th and 235U and 238U in their urine samples. ICP-MS has been used to analyze for many actinides in high-level radioactive wastes (1) , in soils (2) as well as uranium in urine (Test Method C1379). 237Np and 239Pu analysis by ICP-MS in bioassay samples has also been reported (3). Several days counting times are required for alpha-particle analysis of 237Np, 232Th and 235U and 238U whereas ICP-MS requires only four minutes per sample. Alpha-particle counting methods for neptunium may also require the use of 239Pu as a radiotracer for determination of chemical yield. ICP-MS sensitivity limits and isobaric interferences preclude accurate determination of 239Pu, 241Am and 234U at levels present in the urine samples. 234U may be estimated from the 235U: 238U ratio by inference.1.1 This practice covers the separation and preconcentration of neptunium-237 (237Np), thorium-232 (232Th), uranium-235 (235U) and uranium-238 (238U) from urine followed by quantitation using ICP-MS. 1.2 This practice can be used to support routine bioassay programs. The minimum detectable concentrations (MDC) for this method, taking the preconcentration factor into account, are approximately 1E-2Bq for 237Np (0.38ng), 2E-6Bq for 232Th (0.50ng), 4E-5Bq for 235U (0.50ng) and 6E-6Bq for 238U (0.48ng). 1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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5.1 This test method for the chemical analysis of nickel and nickel alloys is primarily intended to test material for compliance with specifications such as those under jurisdiction of ASTM committee B02. It may also be used to test compliance with other specifications that are compatible with the test method.5.2 It is assumed that all who use this method will be trained analysts capable of performing common laboratory procedures skillfully and safely, and that the work will be performed in a properly equipped laboratory.5.3 This is a performance-based method that relies more on the demonstrated quality of the test result than on strict adherence to specific procedural steps. It is expected that laboratories using this method will prepare their own work instructions. These work instructions will include detailed operating instructions for the specific laboratory, the specific reference materials employed, and performance acceptance criteria. It is also expected that, when applicable, each laboratory will participate in proficiency test programs, such as described in Practice E2027, and that the results from the participating laboratory will be satisfactory.1.1 This test method describes the inductively coupled plasma mass spectrometric analysis of nickel and nickel allys, as specified by Committee B02, and having chemical compositions within the following limits:Element Application Range (Mass Fraction %)Aluminum 0. 01–6.00Boron 0. 01–0.10Carbon 0. 01–0.15Chromium 0. 01–33.00Copper 0.01–35.00Cobalt 0. 01–20.00Iron 0.05–50.00Magnesium 0. 01–0.020Molybdenum 0. 01–30.0Niobium 0. 01–6.0Nickel 25.00–100.0Phosphorous 0.001–0.025Silicon 0.01–1.50Sulfur 0.0001–0.01Titanium 0.0001–6.0Tungsten 0.01–5.0Vanadium 0.0005–1.01.2 The following elements may be determined using this method.Element Quantification Range (μg/g)Antimony 0.5–50Bismuth 0.1–11Gallium 2.9–54Lead 0.4–21Silver 1–35Tin 2.2–97Thallium 0.5–3.01.3 This method has only been interlaboratory tested for the elements and ranges specified. It may be possible to extend this method to other elements or different composition ranges provided that method validation that includes evaluation of method sensitivity, precision, and bias as described in this document is performed. Additionally, the validation study must evaluate the acceptability of sample preparation methodology using reference materials and/or spike recoveries. The user is cautioned to carefully evaluate the validation data as to the intended purpose of the analytical results. Guide E2857 provides additional guidance on method validation.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 and health practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 9.

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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.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.

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

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