1、Designation: C1111 10Standard 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 adoption or, in the c
2、ase 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 elements in waste str
3、eams 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. Results from this
4、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 radioactivity levels that
5、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 and industrial proc
6、essliquids. 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 on a semi-quantitat
7、ive 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 provided becauseof
8、 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 between instru-ments of
9、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 does not purport
10、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 Standards:2C859 Te
11、rminology 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 Digestionfor Trace Element D
12、eterminations3D1193 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:4ISO 1042 Laboratory GlasswareOne-mark VolumetricFlasksIS
13、O 3585 Borosilicate Glass 3.3PropertiesISO 8655 Piston-Operated Volumetric Instruments (6 parts)2.3 US EPA Standard: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 approve
14、d Oct. 1, 2010. Published October 2010. Originallyapproved in 1988. Last previous edition approved in 2004 as C1111 04. DOI:10.1520/C1111-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandardsvolum
15、e information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org
16、.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Method 6010, Inductively Coupled Plasma Method, SW-846, Test Methods for Evaluating Solid Waste53. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, refer to
17、Terminology C859, Terminology E135, andPractice C1109.4. Summary of Test Method4.1 The general principles of emission spectrometric analy-sis are given in reference (1).6In this test method, elements aredetermined, either sequentially or simultaneously, by ICP-AES(Method 6010, SW-846).4.2 If the sam
18、ple is a clear acidified solution, the elementsare determined with no further pretreatment. 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
19、determination ofconcentrations of metals in many waste streams from variousnuclear and non-nuclear manufacturing processes. The testmethod is useful for characterizing liquid wastes and liquidwastes containing undissolved solids prior to treatment, stor-age, or stabilization. It has the capability f
20、or the simultaneousdetermination of up to 26 elements.5.2 The applicable concentration 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 Interference
21、sInterelement interfer-ences are characterized by spectral overlap of one element 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 th
22、e recommended wavelengthsgiven in Table 1. The data in Table 2 are intended for use 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
23、each individual system.6.1.2 Molecular Band InterferenceMolecular band inter-ference 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 compensa
24、ted for by backgroundcorrection adjacent to the analyte line.6.2 Non-Spectral InterferencesThese include physical orchemical effects, such as high solids content or high acidconcentration, that affect nebulization or the transport of the5Available from U.S. Government Printing Office Superintendent
25、of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.6The boldface numbers in parentheses refer to a list of references at the end ofthis standard.TABLE 1 Analytical Wavelengths and Applicable ConcentrationRangesAElementLowerLimit,Bmg/LUpperLimit,mg/LWa
26、velength, 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, 259.94Lead 0.05 200 220
27、.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 0.2 250 283.73Titanium 0.003 150 334.94Ura
28、nium 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 concentrations may be expect
29、ed to vary also.BThese limits obtained using a Jarrell-Ash ICAP-9000 ICP Spectrometer.C1111 102sample 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 us
30、e of a peristaltic pump in conjunctionwith a high-solids nebulizer.7. Apparatus7.1 Ordinary 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 IS
31、O 3585. Glassware should becleaned before use by soaking in nitric acid and then rinsingthoroughly 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 sol
32、utions, acids, and so forth.7.5 Bottles, tetrafluoroethylene or polyethylene, for storageof calibration and check solutions.7.6 Disposable Gloves, impermeable, for protection fromcorrosive substances. Polyvinyl chloride (PVC) gloves aresuitable.7.7 Inductively Coupled Plasma Atomic Emission Spec-tro
33、meter, computer controlled, with a spectral bandpass of 0.05nm or less.NOTE 1A bandpass of 0.05 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, inert
34、gas path, or vacuum type, with spectral lines selected appropriately for usewith the specific 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 t
35、he preparation of the samples shall conform to thespecifications of the Committee on Analytical Reagents of theAmerican Chemical Society,7where such specifications areavailable.8.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Sp
36、ecification D1193, Type I, or water exceeding thesespecifications.8.3 Nitric 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.7Reagent Chemicals, American Chemical Society Specif
37、ications, 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.S. Pharmacopeial Convent
38、ion, 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 0.0199Aluminum 237.21 0.0022 0.0084
39、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 0.0015 0.0220Lead 220.35 0.
40、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 0.0014Silver 328.07 0.0003S
41、odium 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 1038.5 Stock SolutionsStandard stock solut
42、ions may be pur-chased or prepared from ultrahigh purity grade metals or metalsalts (Method 6010, SW-846). All salts must be dried for1hat105C unless otherwise specified. Stock solutions shouldcontain approximately 1 000 to 10 000 mg/Lof the element ofinterest to ensure long term stability in dilute
43、 nitric acid8.6 Multielement Working Calibration StandardsMultielement working calibration 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 de
44、terminepossible spectral interference or the presence of impurities.Care should be taken 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 broug
45、ht to100 mL with water to ensure that the final nitric acid concen-tration is 10 volume %. 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 concentr
46、ation canchange with time; the recommended maximum shelf-life forthese solutions is one 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 compatibil
47、ity andthe restrictions of the computer system used to control thespectrometer. Additional 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
48、given belowwhen using the specific analytical wavelengths listed in Table1.8.6.1 Mixed Standard Solution IAluminum, barium, chro-mium, copper, iron, potassium, magnesium, manganese,nickel, and sodium.8.6.2 Mixed Standard Solution IIBeryllium, calcium,lithium, silver, strontium, thorium, titanium, va
49、nadium, andzirconium.8.6.3 Mixed Standard Solution IIIBoron, cadmium, co-balt, lead, phosphorus, 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 preparedby adding one volume of nitric a
