1、Designation: D5600 14D5600 17Standard Test Method forTrace Metals in Petroleum Coke by Inductively CoupledPlasma Atomic Emission Spectrometry (ICP-AES)1This standard is issued under the fixed designation D5600; the number immediately following the designation indicates the year oforiginal adoption o
2、r, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the analysis for commonly determined trace metals in
3、test specimens of raw and calcined petroleumcoke 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 ofthe metals will vary with the matrices and model of spectromete
4、r.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. Th
5、e 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 responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability
6、of regulatorylimitations prior to use.1.7 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade
7、 Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of Coke Samples for Laboratory AnalysisD1193 Specification for Reagent WaterD6299 Practice for Applying Statistical Quality Assurance and Control Charting
8、 Techniques to Evaluate Analytical Measure-ment System PerformanceD7260 Practice for Optimization, Calibration, and Validation of Inductively Coupled Plasma-Atomic Emission Spectrometry(ICP-AES) for Elemental Analysis of Petroleum Products and LubricantsE11 Specification for Woven Wire Test Sieve Cl
9、oth and Test Sieves3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 gross samplethe original, uncrushed, representative portion taken from a shipment or lot of coke.3.1.2 ICP-AESInductively Coupled PlasmaAtomic Emission Spectrometry.3.1.3 petroleum cokea solid, carbonaceous res
10、idue produced by thermal decomposition of heavy petroleum fractions andcracked stocks.4. Summary of Test Method4.1 A test sample of the petroleum coke is ashed at 700C.700 C. The ash is fused with lithium borate. The melt is dissolvedin dilute hydrochloric acid (HCl), and the resultant solution is a
11、nalyzed by inductively coupled plasma atomic emission1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved June 1, 2014May 1, 2017. Pub
12、lished July 2014May 2017. Originally approved in 1994. Last previous edition approved in 20092014 asD5600 09.D5600 14. DOI: 10.1520/D5600-14.10.1520/D5600-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of AS
13、TM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically p
14、ossible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standard
15、Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1spectrometry (ICP-AES) using simultaneous, or sequential multielemental determination of elements. The solution is introducedto the ICP instrument by free aspiration or by an optional pe
16、ristaltic pump. The concentrations of the trace metals are thencalculated by comparing the emission intensities from the sample with the emission intensities of the standards used in calibration.5. Significance and Use5.1 The presence and concentration of various metallic elements in a petroleum cok
17、e are major factors in determining thesuitability of the coke for various end uses. This test method provides a means of determining the concentrations of these metallicelements in a coke sample.5.2 The test method provides a standard procedure for use by buyer and seller in the commercial transfer
18、of petroleum coke todetermine whether the petroleum coke meets the specifications of the purchasing party.6. Interferences6.1 SpectralFollow the instrument manufacturers operating guide to develop and apply correction factors to compensate forthe interferences. To apply interference corrections, all
19、 concentrations shall be within the previously established linear responserange of each element.6.2 Spectral interferences are caused by: (1) overlap of a spectral line from another element; (2) unresolved overlap of molecularband spectra; (3) background contribution from continuous or recombination
20、 phenomena; and (4) stray light from the line emissionof high-concentration elements. Spectral overlap can be compensated for by computer-correcting the raw data after monitoring andmeasuring the interfering element. Unresolved overlap requires selection of an alternate wavelength. Background contri
21、bution andstray light can usually be compensated for by a background correction adjacent to the analyte line.6.3 Physical interferences are effects associated with the sample nebulization and transport processes. Changes in viscosity andsurface tension can cause significant inaccuracies, especially
22、in samples containing high dissolved solids or high acidconcentrations. If physical interferences are present, they shall be reduced by diluting the sample, by using a peristaltic pump, orby using the standard additions method. Another problem that can occur with high dissolved solids is salts build
23、up at the tip ofthe nebulizer, which can affect aerosol flow rate and cause instrumental drift. This problem can be controlled by wetting the argonprior to nebulization, using a tip washer, or diluting the sample.6.4 See Practice D7260 for explanation of ICP-AES interferences and other operational d
24、etails.7. Apparatus7.1 Balance, top loading, with automatic tare, capable of weighing to 0.0001 g, 150 g capacity.7.2 Ceramic Cooling Plate, desiccator plates have been found effective.7.3 Crucible Support, nichrome wire triangles.7.4 Furnaces, electric, capable of regulation of temperature at 70070
25、0 C 6 10C10 C and 10001000 C 6 10C,10 C, withallowances for exchange of combustion gases and air.TABLE 1 Elements Determined and Suggested WavelengthsElement Wavelengths, nmA ,B ConcentrationRange, mg/kgCAluminum 237.313, 256.799, 308.216, 396.152 15110Barium 455.403, 493.410 165Calcium 317.933, 393
26、367, 396.847 10140Iron 259.940 40700Magnesium 279.079, 279.553 550Manganese 257.610, 294.920 17Nickel 231.604, 241.476, 352.454 3220Silicon 212.412, 251.611, 288.159 60290Sodium 588.995, 589.3, 589.592 30160Titanium 334.941, 337.280 17Vanadium 292.402 2480Zinc 202.548, 206.200, 213.856 120A The wav
27、elengths listed were utilized in the round robin because of theirsensitivity. Other wavelengths can be substituted if they can provide the neededsensitivity and are treated with the same corrective techniques for spectralinterference (see 6.1). In time, other elements may be added as more informatio
28、nbecomes available and as required.B Alternative wavelengths can be found in references such as “Inductively CoupledPlasma Atomic Emission Spectroscopy,” Winge, R. K., Fassel, V. A., Peterson, V.J., and Floyd, M. A., Elsevier, 1985.C Based on this round robin round-robin study. This test method can
29、be applicableto other elements or concentration ranges but precision data is not available.D5600 1727.5 Inductively Coupled Plasma Atomic Emission SpectrometerEither sequential or simultaneous spectrometer is suitable.7.6 Magnetic Stirring Bars, polytetrafluoroethylene (PTFE) coated, approximately 1
30、2 mm (12 in.) in length.7.7 Magnetic Stirring Hot Plate.7.8 Meker Type Meker-Type Forced Air Burner.7.9 NebulizerAhigh-solids nebulizer is strongly recommended. This type of nebulizer reduces the possibility of clogging andminimizes aerosol particle effects.7.10 Peristaltic PumpA peristaltic pump is
31、 strongly recommended to provide a constant flow of solution.7.11 Platinum Dish, 5050 mL to 58 mL capacity.7.12 Platinum Dish, 100100 mL to 200 mL capacity.7.13 Platinum-tipped Tongs.7.14 Ring Stand, with crucible support.7.15 Sieves, 0.250 mm (No. 60) and 0.075 mm (No. 200), conforming to Specifica
32、tion E11.7.16 Tungsten Carbide Mill, laboratory size.7.17 Vacuum Filtration Apparatus.7.18 Filter Paper, sized to fit vacuum filtration apparatus, fine porosity, slow flow rate, 2.5 micron particle retention.8. Reagents8.1 Purity of ReagentsReagent-grade chemicals shall be used in all tests. It is i
33、ntended that all reagents shall conform to thespecifications of the Committee onAnalytical Reagents of theAmerican Chemical Society where such specifications are available.3Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use wi
34、thoutlessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean Type II reagent water asdefined in Specification D1193.8.3 Argon Gas Supply, welding grade.8.4 Lithium Borate, either, or a blend containing both.8.4.1 Lith
35、ium Metaborate (LiBO2), powder (high purity).8.4.2 Lithium Tetraborate (Li2B4O7), powder (high purity).8.5 Solution No. 1, Hydrochloric Acid, 20 % by volume (400 mL of concentrated HCl diluted to 2000 mL with water).8.6 Solution No. 2, Standard and Sample Solution Additive. AdditiveWeigh 20.020.0 g
36、6 0.1 g of lithium borate into a100100 mL to 200 mL platinum dish. Place in a furnace at 1000C1000 C for 5 min 5 min to fuse to a liquid. Remove and cool.Place the cooled platinum dish containing the fused recrystallized lithium borate and a magnetic stirring bar into a 2-L2 L glassbeaker. Add 1000
37、mL 1000 mL of Solution No. 1 (20 % HCl). Heat gently and stir the solution on a magnetic stirring hot plateuntil the lithium borate completely dissolves.After dissolution, remove the platinum dish with a glass rod. Rinse the platinum dishand glass rod with water into the lithium borate solution. Imm
38、ediately transfer the warm solution quantitatively to a 2-L2 Lvolumetric flask. Dilute to about 1800 mL with water to avoid crystallization. Mix the solution and cool to room temperature.Dilute to volume with water, mix thoroughly, and vacuum-filter the entire solution through filter paper.NOTE 1Fif
39、ty millilitres of Solution No. 2 contains exactly 0.5 g lithium borate and 25 mL Solution No. 1.8.7 Standard Stock SolutionsPrepare standard stock solutions from high purity (99.9 % or better) metals, oxides, or salts.Stock solutions of 1000 g/mL (ppm) for each metal are needed for preparation of di
40、lute standards in the range from1.01.0 gmL to 50 g/mL (ppm).NOTE 2To minimize the potential of contamination, prepare the platinum ware by boiling in dilute HCl (5 volume % HCl + 95 volume % water) andrinsing thoroughly with water. After this initial cleaning, handle the platinum ware with clean pla
41、tinum tipped platinum-tipped tongs and protect fromall sources of contamination. Similarly acid clean all glassware used in the analyses.NOTE 3Commercially available standards and other reagents solutions may be used in place of laboratory preparations.8.8 Quality Control MaterialsNIST SRM 2718A gre
42、en petroleum coke or 2719 calcined petroleum coke can be used as QCmaterials for this analysis.43 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual
43、Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.4 Available from National Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop 2300, Gaithersburg, MD 2
44、0899-2300, http:/www.nist.gov.D5600 1739. Sample Preparation9.1 Crush and divide the gross sample to obtain a laboratory analysis sample. Crush to pass a 0.250 mm (No. 60) sieve usingPractice D346.9.2 Use a tungsten carbide mill to crush approximately a 30 g representative portion of the minus 0.250
45、 mm (No. 60) sieveanalysis sample, as prepared in 9.1, to pass through a 0.075 mm (No. 200) sieve. Dry this sample to constant mass at 110110 Cto 115C115 C and store in a desiccator until cool and needed for the analysis.9.2.1 Preparation of the minus 0.075 mm analysis samples, from the minus 0.250
46、mm analysis samples, shall neither removemetals through loss nor increase metals through contamination. Full dissolution of the ash is required.10. Preparation of Apparatus10.1 ICP-AES InstrumentConsult the manufacturers instructions for operation of the inductively coupled plasma atomicemission spe
47、ctrometer.10.2 Peristaltic PumpWhen a peristaltic pump is used, inspect the pump tubing and replace it, as necessary, before startingeach day. Verify the solution uptake rate and adjust it to the desired rate.10.3 ICP Excitation SourceInitiate the plasma source at least 30 min before performing the
48、analysis. Some manufacturersrecommend even longer warm-up periods.10.4 Wavelength ProfilingPerform any wavelength profiling that is required in the normal operation of the instrument.10.5 Operating ParametersAssign the appropriate operating parameter to the instrument task file so that the desired e
49、lementscan be determined. Parameters to be included are element, wavelength, background correction points (optional), inter-elementcorrection factors (optional), integration time, and internal standard correction (optional).10.6 Each analyst shall determine the sensitivity and linear range of calibration of their own equipment and chooseconcentration ranges for standards compatible with the samples and instrument specific to their own work. Sample dilutions canbe required for the determination of some elements (see 11.6).10
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