1、Designation: C1111 10 (Reapproved 2015)Standard Test Method forDetermining Elements in Waste Streams by InductivelyCoupled Plasma-Atomic Emission Spectroscopy1This standard is issued under the fixed designation C1111; the number immediately following the designation indicates the year oforiginal ado
2、ption 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 test method covers the determination of trace,minor, and major ele
3、ments in waste streams by inductivelycoupled plasma-atomic emission spectroscopy (ICP-AES) fol-lowing an acid digestion of the sample. Waste streams frommanufacturing processes of nuclear and non-nuclear materialscan be analyzed. This test method is applicable to the deter-mination of total metals.
4、Results from this test method can beused to characterize waste received by treatment facilities andto formulate appropriate treatment recipes. The results are alsousable in process control within waste treatment facilities.1.2 This test method is applicable only to waste streams thatcontain radioact
5、ivity levels that do not require special person-nel or environmental protection.1.3 A list of the elements determined in waste streams andthe corresponding lower reporting limit is found in Table 1.1.4 This test method has been used successfully for treat-ment of a large variety of waste solutions a
6、nd industrial processliquids. The composition of such samples is highly variable,both between waste stream types and within a single wastestream. As a result of this variability, a single acid digestionscheme may not be expected to succeed with all samplematrices. Certain elements may be recovered o
7、n a semi-quantitative basis, while most results will be highly quantita-tive.1.5 This test method should be used by analysts experiencedin the use of ICP-AES, the interpretation of spectral andnon-spectral interferences, and procedures for their correction.1.6 No detailed operating instructions are
8、provided becauseof differences among various makes and models of suitableICP-AES instruments. Instead, the analyst shall follow theinstructions provided by the manufacturer of the particularinstrument. This test method does not address comparativeaccuracy of different devices or the precision betwee
9、n instru-ments of the same make and model.1.7 This test method contains notes that are explanatory andare not part of the mandatory requirements of the method.1.8 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.9 This standard
10、 does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM
11、Standards:2C859 Terminology Relating to Nuclear MaterialsC1109 Practice for Analysis of Aqueous Leachates fromNuclear Waste Materials Using Inductively CoupledPlasma-Atomic Emission SpectroscopyC1234 Practice for Preparation of Oils and Oily WasteSamples by High-Pressure, High-Temperature Digestionf
12、or Trace Element DeterminationsD1193 Specification for Reagent WaterE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE177 Practice for Use of the Terms Precision and Bias inASTM Test Methods2.2 ISO and European Standards:3ISO 1042 Laboratory GlasswareOne-mark V
13、olumetricFlasksISO 3585 Borosilicate Glass 3.3PropertiesISO 8655 Piston-Operated Volumetric Instruments (6 parts)1This test method is under the jurisdiction of ASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved J
14、une 1, 2015. Published June 2015. Originallyapproved in 1988. Last previous edition approved in 2010 as C1111 10. DOI:10.1520/C1111-10R15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandardsvolume i
15、nformation, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-295
16、9. United States12.3 US EPA Standard:Method 6010, Inductively Coupled Plasma Method, SW-846, Test Methods for Evaluating Solid Waste43. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to Terminology C859, Terminology E135, andPractice C1109.4. Summary of Test Method
17、4.1 The general principles of emission spectrometric analy-sis are given in Footnote 5.5In this test method, elements aredetermined, either sequentially or simultaneously, by ICP-AES(Method 6010, SW-846).4.2 If the sample is a clear acidified solution, the elementsare determined with no further pret
18、reatment. If the samplecontains undissolved solids, the elements are determined usingan aliquot of the thoroughly mixed sample after a nitric aciddigestion.5. Significance and Use5.1 This test method is useful for the determination ofconcentrations of metals in many waste streams from variousnuclear
19、 and non-nuclear manufacturing processes. The testmethod is useful for characterizing liquid wastes and liquidwastes containing undissolved solids prior to treatment,storage, or stabilization. It has the capability for the simulta-neous determination of up to 26 elements.5.2 The applicable concentra
20、tion ranges of the elementsanalyzed by this procedure are listed in Table 1.6. Interferences6.1 Spectral interferences in ICP-AES, and ways to com-pensate for them, include the following:6.1.1 Interelement InterferencesInterelement interfer-ences are characterized by spectral overlap of one element
21、lineover another. This interference can be compensated for bycorrection of the raw data, which requires measurement of theinterfering element at the wavelength of interest. Table 2 listssome interference effects for the recommended wavelengthsgiven in Table 1. The data in Table 2 are intended for us
22、e onlyas a rudimentary guide for indicating potential spectral inter-ferences. Various analytical systems may exhibit somewhatdifferent levels of interferences. Therefore, the interferenceeffects must be evaluated for each individual system.6.1.2 Molecular Band InterferenceMolecular band inter-feren
23、ce arising from overlap of molecular band spectra at thewavelength of interest can be eliminated by careful selection ofwavelength.6.1.3 High BackgroundHigh background effects fromscattered light, etc., can be compensated for by backgroundcorrection adjacent to the analyte line.4Available from U.S.
24、Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.5ASTM Methods for Emission Spectrochemical Analysis, ASTM International,1967.TABLE 1 Analytical Wavelengths and Applicable ConcentrationRangesAElementLowerLim
25、it,Bmg/LUpperLimit,mg/LWavelength, nmAluminum 0.02 5000 308.22, 237.01Barium 0.001 100 493.41Beryllium 0.0003 100 313.04Boron 0.004 200 249.68Cadmium 0.003 200 226.50Calcium 0.004 1000 317.93, 393.37Chromium 0.01 5000 267.72, 298.92Cobalt 0.005 150 228.62Copper 0.004 150 324.75Iron 0.004 5000 271.44
26、, 259.94Lead 0.05 200 220.35Lithium 0.004 150 670.78Magnesium 0.0005 5000 293.65, 279.55Manganese 0.001 150 257.61Nickel 0.01 5000 231.60, 341.48Phosphorus 0.2 250 178.29Potassium 0.6 1000 766.49Silver 0.006 150 328.07Sodium 0.02 200 330.29, 588.99Strontium 0.0004 100 421.55Thorium 0.2 250 283.73Tit
27、anium 0.003 150 334.94Uranium 0.03 1000 409.01Vanadium 0.005 250 292.40Zinc 0.001 250 213.86Zirconium 0.005 250 339.20AThe estimated upper and lower concentration limits are to be used only as ageneral guide. These values are instrument and sample dependent, and as thesample matrix varies, these con
28、centrations may be expected to vary also.BThese limits obtained using a Jarrell-Ash ICAP-9000 ICP Spectrometer.C1111 10 (2015)26.2 Non-Spectral InterferencesThese include physical orchemical effects, such as high solids content or high acidconcentration, that affect nebulization or the transport of
29、thesample to the plasma and its vaporization, atomization, orexcitation in the plasma. Effects due to high solids content orhigh acid concentration can be reduced by a tenfold dilution ofthe sample and the use of a peristaltic pump in conjunctionwith a high-solids nebulizer.7. Apparatus7.1 Ordinary
30、laboratory apparatus are not listed, but areassumed to be present.7.2 Glassware, volumetric flasks complying with the re-quirements of ISO 1042, made of borosilicate glass complyingwith the requirements of ISO 3585. Glassware should becleaned before use by soaking in nitric acid and then rinsingthor
31、oughly with water.7.3 Filters, inert membrane, having pore size of 2.5 m.7.4 Piston-operated Volumetric Pipettors and Dispensers,complying with the requirements of ISO 8655, for pipettingand dispensing of solutions, acids, and so forth.7.5 Bottles, tetrafluoroethylene or polyethylene, for storageof
32、calibration and check solutions.7.6 Disposable Gloves, impermeable, for protection fromcorrosive substances. Polyvinyl chloride (PVC) gloves aresuitable.7.7 Inductively Coupled Plasma Atomic EmissionSpectrometer, computer controlled, with a spectral bandpass of0.05 nm or less.NOTE 1A bandpass of 0.0
33、5 nm or less is required to provide thenecessary spectral resolution.NOTE 2The spectrometer may be of the simultaneous multielement orsequential scanning type. The spectrometer may be of the air path, inertgas path, or vacuum type, with spectral lines selected appropriately for usewith the specific
34、instrument.NOTE 3An autosampler having a flowing rinse is recommended.8. Reagents8.1 Purity of ReagentsChemicals used in the preparationof the standards must be of ultrahigh purity grade. Chemicalsused in the preparation of the samples shall conform to thespecifications of the Committee on Analytica
35、l Reagents of theAmerican Chemical Society,6where such specifications areavailable.8.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Specification D1193, Type I, or water exceeding thesespecifications.6Reagent Chemicals, American
36、 Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.
37、S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 2 Analyte Concentration Equivalents Arising from Interferents at the 1000 mg/L LevelAnalyteWave-lengths,nmInterferent, mg/LAluminum Chromium Copper Iron Nickel Antimony Silicon Tin Uranium VanadiumAluminum 308.22 0.0020 0.0044 0.0199Alumin
38、um 237.21 0.0022 0.0084 0.0350Barium 493.41Beryllium 313.04 0.0013Boron 249.68 0.0015Cadmium 226.50 0.0002 0.0004Calcium 317.93 0.0018Calcium 393.37 0.0002Chromium 267.72 0.0025 0.0018Chromium 298.92 0.0560Cobalt 228.62 0.0001 0.0001Copper 324.75Iron 259.94 0.0001 0.0001 0.0002Iron 271.44 0.0039 0.0
39、015 0.0220Lead 220.35 0.0012 0.0028 0.0002 0.0006 0.0016Lithium 670.78 0.0003Magnesium 279.55Magnesium 293.65 0.0270 0.1390 0.0350Manganese 257.61 0.0002Nickel 231.60 0.0002 0.0003 0.0001 0.0003Nickel 341.48 0.0027Phosphorus 178.29 0.0002 0.0079 0.0120 0.0004 0.0044Potassium 766.49 0.0010 0.0005 0.0
40、014Silver 328.07 0.0003Sodium 330.29 0.0035 0.0220 0.0145 0.1580Sodium 588.99 0.0006 0.0017 0.0002Strontium 421.55Thorium 283.73 0.0007 0.0005 0.0049 0.0500Titanium 334.94 0.0003Vanadium 292.40 0.0029 0.0014Zinc 213.85 0.0034 0.0001 0.0038Zirconium 339.20 0.0003 0.0002 0.0005C1111 10 (2015)38.3 Nitr
41、ic Acid (sp gr 1.42)Concentrated nitric acid(HNO3).8.4 Nitric Acid, 10 volume %One volume of concentratednitric acid (specific gravity 1.42) brought to ten volumes withwater.8.5 Stock SolutionsStandard stock solutions may be pur-chased or prepared from ultrahigh purity grade metals or metalsalts (Me
42、thod 6010, SW-846). All salts must be dried for1hat105C unless otherwise specified. Stock solutions shouldcontain approximately 1000 to 10 000 mg/L of the element ofinterest to ensure long term stability in dilute nitric acid.8.6 Multielement Working Calibration StandardsMultielement working calibra
43、tion standards are prepared fromthe single element stock solutions at appropriate concentrationlevels for each element. Prior to preparing the mixed standards,each stock solution should be analyzed separately to determinepossible spectral interference or the presence of impurities.Care should be tak
44、en when preparing each multielementcalibration standard solution that the elements be compatibleand stable.An appropriate amount of concentrated nitric acid isadded to stock standard aliquots and final volume brought to100 mL with water to ensure that the final nitric acid concen-tration is 10 volum
45、e %. Transfer each multielement calibrationstandard solution to a FEP fluorocarbon or new polyethylenebottle for storage. Fresh calibration standards should be pre-pared as needed with the realization that concentration canchange with time; the recommended maximum shelf-life forthese solutions is on
46、e month. Calibration standards must beinitially verified using a quality control sample monitoredweekly for stability. The actual number of calibration standardsneeded will be a function of both chemical compatibility andthe restrictions of the computer system used to control thespectrometer. Additi
47、onal calibration standards may be neededif a second, less sensitive emission line is used to extend thelinear range of one or more elements.Although not specificallyrequired, some typical standard combinations are given belowwhen using the specific analytical wavelengths listed in Table1.8.6.1 Mixed
48、 Standard Solution IAluminum, barium,chromium, copper, iron, potassium, magnesium, manganese,nickel, and sodium.8.6.2 Mixed Standard Solution IIBeryllium, calcium,lithium, silver, strontium, thorium, titanium, vanadium, andzirconium.8.6.3 Mixed Standard Solution IIIBoron, cadmium,cobalt, lead, phosp
49、horus, and zinc.8.6.4 Single Element StandardA single element standardsolution is suggested for uranium due to the high probability ofspectral interference with other elements.8.7 Interference Check SampleThe interference checksample is prepared from single element stock standard solu-tions to contain elements and concentrations appropriate to thesample type.8.8 Calibration BlankThe calibration blank is prepared byadding one volume of nitric acid (specific gravity 1.42) to ninevolumes of water. Prepare a sufficient quantity to be u
