1、Designation: D8149 17Standard Practice forOptimization, Calibration, and Validation of IonChromatographic Determination of Heteroatoms and Anionsin Petroleum Products and Lubricants1This standard is issued under the fixed designation D8149; the number immediately following the designation indicates
2、the year oforiginal adoption or, 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. Scope1.1 This practice covers the information on calibrat
3、ion,quality control, and operational guidance for anionic measure-ments using ion chromatography (IC).1.2 IC Related StandardsChemically or electrolyticallyregenerated suppressed ion chromatography standards foraqueous matrices include Test Methods D2988, D4327, D5085,D5542, D5827, D5987, D5996, D65
4、81, D7319, D7328,D7359, D7773, D7994, and D8150; IC instrumentation re-quirements are described in Practices E1151, and E1511.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all
5、of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in
6、accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1
7、 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products andLiquid Fuels at Atmospheric PressureD975 Specification for Diesel Fuel OilsD1193 Specification for Reagent WaterD2988 Test Methods for Water-Soluble Halide Ion in Halo-genated Organic Solvents and Their AdmixturesD4057 Practi
8、ce for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4327 Test Method for Anions in Water by Suppressed IonChromatographyD5085 Test Method for Determination of Chloride, Nitrate,and Sulfate inAtmospheric Wet Deposition by C
9、hemicallySuppressed Ion ChromatographyD5542 Test Methods for Trace Anions in High Purity Waterby Ion ChromatographyD5827 Test Method for Analysis of Engine Coolant forChloride and Other Anions by Ion ChromatographyD5987 Test Method for Total Fluorine in Coal and Coke byPyrohydrolytic Extraction and
10、Ion Selective Electrode orIon Chromatograph MethodsD5996 Test Method for Measuring Anionic Contaminants inHigh-Purity Water by On-Line Ion ChromatographyD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6581
11、Test Methods for Bromate, Bromide, Chlorate, andChlorite in Drinking Water by Suppressed Ion Chroma-tographyD6751 Specification for Biodiesel Fuel Blend Stock (B100)for Middle Distillate FuelsD6792 Practice for Quality Management Systems in Petro-leum Products, Liquid Fuels, and Lubricants TestingLa
12、boratoriesD7318 Test Method for Existent Inorganic Sulfate in Ethanolby Potentiometric TitrationD7319 Test Method for Determination of Existent and Po-tential Sulfate and Inorganic Chloride in Fuel Ethanol andButanol by Direct Injection Suppressed Ion Chromatog-raphyD7328 Test Method for Determinati
13、on of Existent and Po-tential Inorganic Sulfate and Total Inorganic Chloride inFuel Ethanol by Ion Chromatography Using AqueousSample Injection1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubco
14、mmittee D02.03 on Elemental Analysis.Current edition approved Dec. 1, 2017. Published February 2018. DOI: 10.1520/D8149-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, re
15、fer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization establi
16、shed in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1D7359 Test Method for Total Fluorine, Chlorine and Sulfurin Aromatic Hydrocarbons and Their Mixtures by Oxi
17、da-tive Pyrohydrolytic Combustion followed by Ion Chroma-tography Detection (Combustion Ion Chromatography-CIC)D7591 Test Method for Determination of Free and TotalGlycerin in Biodiesel Blends by Anion Exchange Chro-matographyD7773 Test Method for Determination of Volatile InorganicAcids (HCl, HBr,
18、and HNO3) Using Filter Sampling andSuppressed Ion ChromatographyD7994 Test Method for Total Fluorine, Chlorine, and Sulfurin Liquid Petroleum Gas (LPG) by Oxidative Pyrohydro-lytic Combustion Followed by Ion Chromatography De-tection (Combustion Ion Chromatography-CIC)D8150 Test Method for Determina
19、tion of Organic ChlorideContent in Crude Oil by Distillation Followed by Detec-tion Using Combustion Ion ChromatographyE1151 Practice for Ion Chromatography Terms and Rela-tionshipsE1511 Practice for Testing Conductivity Detectors Used inLiquid and Ion Chromatography2.2 Other Standards:ISO/CEN 15492
20、 Ethanol as a blending component forpetrolDetermination of inorganic chlorideIon chro-matographic method3EPA Method 300.0 Determination of Inorganic Anions byIon Chromatography4EPA Method 300.1 Determination of Inorganic Anions inDrinking Water by Ion Chromatography43. Terminology3.1 Definition of t
21、erms relating to ion chromatography canbe found in Practices E1151 and E1511.3.2 Definitions of Terms Specific to This Standard:3.2.1 combustion ion chromatography, nan analytical sys-tem consisting of oxidative pyrohydrolytic combustion fol-lowed by ion chromatographic detection. D7994, D81503.2.2
22、existent inorganic sulfate, ninorganic sulfate speciesactually present in the sample at the time of analysis with nooxidation treatment. D7318, D7319, D73283.2.3 inorganic chloride, nchloride present as hydrochlo-ric acid, ionic salts of this acid, or mixtures of these.D7319, D73283.2.4 inorganic su
23、lfate, nsulfate (SO4)-2species present assulfuric acid, ionic salts of this acid, or mixtures of these.D7318, D7319, D73283.2.5 oxidative pyrohydrolytic combustion, na process inwhich a sample is combusted in an oxygen-rich environment attemperatures greater than 900 C and in the presence of excessw
24、ater vapor not originating from the combustion of the sample.3.2.5.1 DiscussionIn oxidative pyrohydrolyticcombustion, the sample is pyrolyzed into carbon dioxide,water, hydrogen halides (HX), and elemental oxides such asNOXand SOX, and residual ash typically of elemental oxides.D73593.2.6 potential
25、sulfate, ntotal inorganic sulfate speciespresent after the sample has been reacted with an oxidizingagent. D7319, D73284. Summary of Practice4.1 Ion chromatography technique can be used to determinethe anions in various liquid matrices. Often solid samples areconverted into water-soluble forms after
26、 combustion, and areanalyzed for anionic forms of elements of interest. Thispractice summarizes the protocols to be followed during suchsample preparation, calibration, and verification of the analyti-cal performance.5. Principle of Analysis Technique5.1 Ion chromatography (IC) is a combination of i
27、on ex-change chromatography, eluent suppression, and conductivitydetection. Other detection devices can also be used such asamperometric, UV-fluorescence, mass spectrometry, induc-tively coupled plasma-mass spectrometry, and so on. Cationsand polar organic compounds such as amines, sugars, andorgani
28、c acids can also be determined using IC analysis.However, this practice covers only the determination of spe-cific anions using conductivity detection.5.2 For anion analysis, suppression is applied for minimiz-ing the background conductivity and increasing the response ofthe anions of interest. Supp
29、ressor devices with ion exchangerresin in the H+ form and membrane-based devices are avail-able. Regeneration is performed chemically in both versions orelectrolytically in the membrane type.5.2.1 A dilute base such as NaHCO3,Na2CO3, and NaOH(or KOH) as mixtures or alone can be used as eluent which
30、isconveniently neutralized to low conductivity acid in thesuppressor and to increased sensitivity. Hydroxide eluents areneutralized to water with very low conductivity. Carbonate/hydrogen carbonate eluents are neutralized to carbonic acidwith a low conductivity. An optional CO2removal devicereduces
31、the background conductivity further.5.2.2 The anions are eluted through the separating columnand detected by conductivity measurement. In the separatorcolumn, the anion exchange resin selectively causes the vari-ous anions of different types to migrate through the column atdifferent respective rates
32、, thus effecting their separation, andidentification based on their retention times.5.3 The non-selective nature of the conductimetric detectionallows several ions to be sequentially determined in the samesample. The conductimetric detection is highly specific andrelatively free from interferences.
33、Different valence states ofthe same element can be determined. However, because of thenon-selective nature of the detector, the chromatographic peaksare identified only by their retention times. Thus, it is importantthat there is separation of two ions having the same or closeretention times to avoi
34、d detection as one broad peak givingerroneous results.3Available from International Organization for Standardization (ISO), ISOCentral Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,Geneva, Switzerland, http:/www.iso.org.4Available from United States Environmental ProtectionAgenc
35、y (EPA), WilliamJefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,http:/www.epa.gov.D8149 1725.4 The advantages of IC analysis are (1) sequential multi-anion capability eliminating the individual anionic determina-tions by diverse techniques, such as those using wet chemistry
36、,(2) small sample size used, usually 1 0.2918 X0.67460.7599 X0.6746Where X is the anion concentration in mg/kg.ASupporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1614. Contact ASTM CustomerService at serviceastm.org.BSupportin
37、g data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1759. Contact ASTM CustomerService at serviceastm.org.CSupporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1611.
38、Contact ASTM CustomerService at serviceastm.org.DSupporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1853. Contact ASTM CustomerService at serviceastm.org.ESupporting data have been filed at ASTM International Headquarters and m
39、ay be obtained by requesting Research Report RR:D02-1737. Contact ASTM CustomerService at serviceastm.org.FSupporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1868. Contact ASTM CustomerService at serviceastm.org.D8149 1710REFER
40、ENCES(1) Nadkarni, R. A., “A Review of Modern Instrumental Methods ofElemental Analysis of Petroleum Related Materials: Part II Analyti-cal Techniques,” in “Modern Instrumental Methods of ElementalAnalysis of Petroleum Products and Lubricants,” ed. R. A. Nadkarni,ASTM International Press, STP 1109 (
41、1991), pp. 551.(2) Chassaniol, K., “Ion Chromatography in the Analysis of IndustrialProcess Waters and Petroleum Products,” in “Spectroscopic Analysisof Petroleum Products and Lubricants,” ed. R. A. Nadkarni, ASTMInternational Press, West Conshohocken, PA, MONO 9 (2011), pp.494510.(3) Weiss, J., Ion
42、 Chromatography, 4th ed., Wiley-VCH, Weinheim,Germany, 2016.(4) Small, H., Ion Chromatography, Plenum Press, New York, 1989.(5) Haddad, P. R. and Jackson, P. E., Ion Chromatography: Principles andApplications, Elsevier Science, B. V., Amsterdam, the Netherlands,1990.(6) Fritz, J. S. and Gjerde, D. T
43、., Ion Chromatography, Wiley-VCH,Weinheim, Germany, 2000.(7) Nadkarni, R. A., “Determination of Volatile Elements in Coal andOther Organic Materials by Oxygen Bomb Combustion,” Amer. Lab.,Vol 13, No. 8, 1981, pp. 2229.(8) Nadkarni, R. A., and Pond, D. M., “Applications of Ion Chromatog-raphy for Det
44、ermination of Selected Elements in Coal and Oil Shale,”Anal. Chim. Acta, 1983, Vol 146, pp. 261.(9) Nadkarni, R. A., and Brewer, J. M., “Applications of Ion Chromatog-raphy in Environmental Analysis,” Amer. Lab., Vol 19, No. 2, 1987,pp. 50.ASTM International takes no position respecting the validity
45、 of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject
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47、. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is
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