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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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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 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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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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