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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 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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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).54.2.1 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.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.

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5.1 This test method covers the rapid determination of 22 elements in used and unused lubricating oils and base oils, and it provides rapid screening of used oils for indications of wear. Test times approximate a few minutes per test specimen, and detectability for most elements is in the low mg/kg range. In addition, this test method covers a wide variety of metals in virgin and re-refined base oils. Twenty-two elements can be determined rapidly, with test times approximating several minutes per test specimen.5.2 When the predominant source of additive elements in used lubricating oils is the additive package, significant differences between the concentrations of the additive elements and their respective specifications can indicate that the incorrect oil is being used. The concentrations of wear metals can be indicative of abnormal wear if there are baseline concentration data for comparison. A marked increase in boron, sodium, or potassium levels can be indicative of contamination as a result of coolant leakage in the equipment. This test method can be used to monitor equipment condition and define when corrective actions are needed.5.2.1 The significance of metal analysis in used lubricating oils is tabulated in Table 4.5.3 The concentrations of metals in re-refined base oils can be indicative of the efficiency of the re-refining process. This test method can be used to determine if the base oil meets specifications with respect to metal content.1.1 This test method covers the determination of additive elements, wear metals, and contaminants in used and unused lubricating oils and base oils by inductively coupled plasma atomic emission spectrometry (ICP-AES). The specific elements are listed in Table 1.(A) These wavelengths are only suggested and do not represent all possible choices.1.2 This test method covers the determination of selected elements, listed in Table 1, in re-refined and virgin base oils.1.3 For analysis of any element using wavelengths below 190 nm, a vacuum or inert-gas optical path is required. The determination of sodium and potassium is not possible on some instruments having a limited spectral range.1.4 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 are obtained for particles larger than a few micrometers.21.5 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.1.6 For elements other than calcium, sulfur, and zinc, the low limits listed in Table 2 and Table 3 were estimated to be ten times the repeatability standard deviation. For calcium, sulfur, and zinc, the low limits represent the lowest concentrations tested in the interlaboratory study.(A) where: X = mean concentration, μg/g.(A) where: X = mean concentration, μg/g.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. Specific warning statements are given in 6.1, 8.2, and 8.4.1.9 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 The health of workers in many industries is at risk through exposure by inhalation to toxic metals and metalloids. Industrial hygienists and other public health professionals need to determine the effectiveness of measures taken to control workers’ exposures, and this is generally achieved by making workplace air measurements. This test method has been promulgated in order to make available a standard methodology for making valid exposure measurements for a wide range of metals and metalloids that are used in industry. It will be of benefit to agencies concerned with health and safety at work; industrial hygienists and other public health professionals; analytical laboratories; industrial users of metals and metalloids and their workers, and other groups.5.2 This test method specifies a generic method for determination of the mass concentration of metals and metalloids in workplace air using ICP-AES.5.3 The analysis results can be used for the assessment of workplace exposures to metals and metalloids in workplace air.5.4 When sampling and analysis is carried out in accordance with this test method, the overall procedure normally satisfies the performance requirements of ISO 20581.NOTE 2: Refer to Guide E1370 for guidance on the development of appropriate exposure assessment and measurement strategies.1.1 This test method specifies a procedure for collection, sample preparation, and analysis of airborne particulate matter for the content of metals and metalloids using inductively coupled plasma-atomic emission spectrometry (ICP-AES). The method is generally applicable to occupational exposure monitoring.1.2 This test method is applicable to personal sampling of the inhalable or respirable fraction of airborne particles and to area sampling.1.3 This test method should be used by analysts experienced in the use of ICP-AES, the interpretation of spectral and matrix interferences, and procedures for their correction.1.4 This test method specifies a number of alternative methods for preparing test solutions from samples of airborne particulate matter. One of the specified sample preparation methods is applicable to the measurement of soluble metal or metalloid compounds. Other specified methods are applicable to the measurement of total metals and metalloids.1.5 It is the user's responsibility to ensure the validity of this test method for sampling materials of untested matrices.1.6 The following is a non-exclusive list of metals and metalloids for which one or more of the sample dissolution methods specified in this document is applicable. However, there is insufficient information available on the effectiveness of dissolution methods for those elements in italics.Aluminum Indium SodiumAntimony Iron StrontiumArsenic Lead TantalumBarium Lithium TelluriumBeryllium Magnesium ThalliumBismuth Manganese TinBoron Molybdenum TitaniumCadmium Nickel TungstenCalcium Phosphorus UraniumCesium Platinum VanadiumChromium Potassium YttriumCobalt Rhodium ZincCopper Selenium ZirconiumHafnium Silver  1.7 This test method is not applicable to the sampling of elemental mercury, or to inorganic compounds of metals and metalloids that are present in the gaseous or vapor state.1.8 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-AES 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.1.9 This test method contains notes that are explanatory and are not part of the mandatory requirements of this test method.1.10 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.11 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.1.12 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 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 D7260.1.1 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.21.4.3 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 dilution factor.1.7 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.1.8 As a generality based on this interlaboratory study (see 18.1), the trace elements identifiable in crude oils can be divided into three categories:1.8.1 Element levels that are too low for valid detection by ICP-AES and hence, cannot be determined: aluminum, barium, lead, magnesium, manganese, and silicon.1.8.2 Elements that are just at the detection levels of the ICP-AES method and hence, cannot be determined with a great deal of confidence: boron, calcium, chromium, copper, molybdenum, phosphorus, potassium, sodium, and zinc. Perhaps the determination of these elements can be considered as semi-quantitative.1.8.3 Elements that are at higher levels of concentration and can be determined with good precision: iron, nickel, sulfur, and vanadium.1.9 The detection limits for elements not determined by this test method follow. This information should serve as an indication as to what elements are not present above the detection limits typically obtainable by ICP-AES instruments.Element mg/kgAluminum 1Barium 0.2Boron 1Calcium 0.1Chromium 0.1Copper 0.1Lead 1.4Magnesium 1Manganese 0.1Molybdenum 0.2Phosphorous 1Potassium 0.5Silicon 4Zinc 0.51.10 This test method determines all possible elements simultaneously and is a simpler alternative to Test Methods D5184, D5708, or D5863.1.11 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.12 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.1.13 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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