1、Designation: C1109 10 (Reapproved 2015)Standard Practice forAnalysis of Aqueous Leachates from Nuclear WasteMaterials Using Inductively Coupled Plasma-AtomicEmission Spectroscopy1This standard is issued under the fixed designation C1109; the number immediately following the designation indicates the
2、 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 is applicable to the determination of
3、 lowconcentration and trace elements in aqueous leachate solutionsproduced by the leaching of nuclear waste materials, usinginductively coupled plasma-atomic emission spectroscopy(ICP-AES).1.2 The nuclear waste material may be a simulated (non-radioactive) solid waste form or an actual solid radioac
4、tivewaste material.1.3 The leachate may be deionized water or any natural orsimulated leachate solution containing less than 1 % totaldissolved solids.1.4 This practice should be used by analysts experienced inthe use of ICP-AES, the interpretation of spectral and non-spectral interferences, and pro
5、cedures for their correction.1.5 No detailed operating instructions are 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
6、address comparativeaccuracy of different devices or the precision between instru-ments of the same make and model.1.6 This practice contains notes that are explanatory and arenot part of the mandatory requirements of the method.1.7 The values stated in SI units are to be regarded as thestandard.1.8
7、This standard 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 Docum
8、ents2.1 ASTM Standards:2C859 Terminology Relating to Nuclear MaterialsC1009 Guide for Establishing and Maintaining a QualityAssurance Program forAnalytical Laboratories Within theNuclear IndustryC1220 Test Method for Static Leaching of Monolithic WasteForms for Disposal of Radioactive WasteD1193 Spe
9、cification for Reagent WaterD7035 Test Method for Determination of Metals and Met-alloids in Airborne Particulate Matter by InductivelyCoupled Plasma Atomic Emission Spectrometry (ICP-AES)E135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE177 Practice for Use of
10、 the Terms Precision and Bias inASTM Test Methods2.2 ISO and European Standards:3ISO 1042 Laboratory GlasswareOne-mark VolumetricFlasksISO 3585 Borosilicate Glass 3.3PropertiesISO 8655 Piston-Operated Volumetric Instruments (6 parts)3. Terminology3.1 For definitions of pertinent terms not listed her
11、e, seeTerminology C859.3.2 Definitions:3.2.1 atomic emissioncharacteristic radiation emitted byan electronically excited atomic species. D70353.2.1.1 DiscussionIn atomic (or optical) emissionspectrometry, a very high-temperature environment, such as aplasma, is used to create excited state atoms. Fo
12、r analyticalpurposes, characteristic emission signals from elements in theirexcited states are then measured at specific wavelengths.1This practice is under the jurisdiction of ASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current e
13、dition approved June 1, 2015. Published June 2015. Originallyapproved in 1988. Last previous edition approved in 2010 as C1109 10. DOI:10.1520/C1109-10R15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM
14、Standards volume information, 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 Conshoho
15、cken, PA 19428-2959. United States13.2.2 background correctionprocess of correcting the in-tensity at an analytical wavelength for the intensity due to theunderlying spectral background of a blank. D70353.2.2.1 DiscussionDuring sample analysis, measurementsare made of the background intensity near t
16、he peak wavelengthof the analytical lines. Correction of the analytical line peakintensity to yield the net line intensity can be made bysubtraction of either (a) a single intensity measurement per-formed on the high or low wavelength side of the analyticalline (single-point background correction),
17、or (b) an interpo-lated background intensity from background measurementsacquired on both the high and low wavelength sides of theanalytical line (double-point background correction).3.2.3 biasbetween the expectation of the test results andan accepted reference value. E1773.2.4 calibrationthe proces
18、s by which the relationshipbetween net signal intensity and elemental concentration isdetermined for a specific element analysis.3.2.5 calibration blank solutioncalibration solution pre-pared without the addition of any reference solutions. D70353.2.6 calibration curveplot of net signal intensity ve
19、rsuselemental concentration using data obtained during calibration.3.2.7 calibration reference solution(s)solutions contain-ing known concentrations of one or more elements in 1 % (v/v)nitric acid for instrument calibration.3.2.8 critical limit (LC)minimum significant value of anestimated net signal
20、 or concentration, applied as a discrimina-tor against background noise. (1)3.2.9 inductively coupled plasma (ICP)a high-temperature discharge generated by a flowing conductive gas,normally argon, through a magnetic field induced by a load coilthat surrounds the tubes carrying the gas. D70353.2.10 i
21、nstrument check solution(s)solution(s) containingall the elements to be determined at concentration levelsapproximating the concentrations in the samples. These solu-tions must also contain 1 % (v/v) nitric acid.3.2.11 interelement correctiona spectral interference cor-rection technique in which emi
22、ssion contributions from inter-fering elements that emit radiation at the analyte wavelengthare subtracted from the apparent analyte emission after mea-suring the interfering element concentrations at otherwavelengths. D70353.2.12 limit of detection (LD)value for which the falsenegative error is B u
23、sing a given critical limit. (1)3.2.12.1 DiscussionIf the analytical standard deviation isconstant with respect to concentration, this can be computed as3.7 times the standard deviation of the analytical results fromten matrix blank samples spiked at approximately the antici-pated detection limit; o
24、therwise, see references (1, 2)4foradditional guidance.3.2.13 linear dynamic rangethe elemental concentrationrange over which the calibration curve remains linear to withinthe precision of the analytical method.3.2.14 linearity check solution(s)solution(s) containingthe elements to be determined at
25、concentrations that cover arange that is two to ten times higher and lower than theconcentration of these elements in the calibration referencesolutions. These solutions also contain 1 % (v/v) nitric acid.3.2.15 non-spectral interferencechanges in the apparentnet signal intensity from the analyte du
26、e to physical orchemical processes that affect the transport of the analyte to theplasma and its vaporization, atomization, or excitation in theplasma.3.2.16 sensitivitythe slope of the linear dynamic range.3.2.17 spectral interferencean interference caused by theemission from a species other than t
27、he analyte of interest.D70353.2.17.1 DiscussionSources of spectral interference in-clude spectral line overlaps, broadened wings of intensespectral lines, ion-atom recombination continuum emission,molecular band emission, and stray (scattered) light effects.4. Summary of Practice4.1 Aqueous leachate
28、s are prepared, using Test MethodC1220, for analysis using this practice.4.2 The general principles of emission spectrometric analy-sis are given in Ref (3). In this practice, elemental constituentsof aqueous leachate solutions are determined simultaneously orsequentially by inductively coupled plas
29、ma-atomic emissionspectroscopy (ICP-AES).4.3 Samples are prepared by filtration if needed to removeparticulates and acidification to match calibration referencesolutions. Filtration should be the last resort to clarify asolution since leach studies are designed to determine theabsolute amount of mat
30、erial removed from a waste form byaqueous leaching.4.4 Additional general guidelines are provided in GuideC1009, Specification D1193, Terminology C859, and Termi-nology E135.5. Significance and Use5.1 This practice may be used to determine concentrationsof elements leached from nuclear waste materia
31、ls (glasses,ceramics, cements) using an aqueous leachant. If the nuclearwaste material is radioactive, a suitably contained and shieldedICP-AES spectrometer system with a filtered exit-gas systemmust be used, but no other changes in the practice are required.The leachant may be deionized water or an
32、y aqueous solutioncontaining less than 1 % total solids.5.2 This practice as written is for the analysis of solutionscontaining 1 % (v/v) nitric acid. It can be modified to specifythe use of the same or another mineral acid at the same orhigher concentration. In such cases, the only change needed in
33、this practice is to substitute the preferred acid and concentra-tion value whenever 1 % nitric acid appears here. It isimportant that the acid type and content of the reference andcheck solutions closely match the leachate solutions to beanalyzed.4The boldface numbers in parentheses refer to the lis
34、t of references at the endof this standard.C1109 10 (2015)25.3 This practice can be used to analyze leachates fromstatic leach testing of waste forms using Test Method C1220.6. Apparatus6.1 Ordinary laboratory apparatus are not listed, but areassumed to be present.6.2 Glassware, volumetric flasks co
35、mplying 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 rinsingthoroughly with water.6.3 Filters, inert membrane, having pore size of 0.45 m orsmaller.6.4 Piston-operat
36、ed Volumetric Pipettors and Dispensers,complying with the requirements of ISO 8655, for pipettingand dispensing of solutions, acids, and so forth.6.5 Bottles, tetrafluoroethylene or polyethylene, for storageof calibration and check solutions.6.6 Disposable Gloves, impermeable, for protection fromcor
37、rosive substances. Polyvinyl chloride (PVC) gloves aresuitable.6.7 Inductively Coupled Plasma-Atomic EmissionSpectrometer, computer controlled, with a spectral bandpass of0.05 nm or less, is required to provide the necessary spectralresolution.NOTE 1The spectrometer may be of the simultaneous multie
38、lement 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 instrument.NOTE 2An autosampler having a flowing rinse is recommended.7. Reagents and Materials7.1 Purity of ReagentsReagent
39、grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.5Other grades may be used,provided it is first ascertain
40、ed that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type I of Specification D1193 or water exceeding thesespecif
41、ications.7.3 Nitric Acid (specific gravity 1.42)Concentrated nitricacid (HNO3).7.4 Nitric Acid, High-PurityNitric acid of higher puritythan reagent grade, specially prepared to be low in metalliccontaminants. The acid may be prepared by sub-boiling distil-lation (4), or purchased from commercial sou
42、rces.7.5 Stock SolutionsMay be purchased or prepared frommetals or metal salts of known purity. Stock solutions shouldcontain known concentrations of the element of interest rang-ing from 100 to 10 000 mg/L.7.6 Calibration Blank Solution, 1 % (v/v) HNO3.7.7 Calibration Reference Solutions, Instrumen
43、t CheckSolutions, and Linearity Check Solutions:7.7.1 Prepare single-element or multielement calibrationreference solutions by combining appropriate volumes of thestock solutions in acid-rinsed volumetric flasks. To establishthe calibration slope accurately, provide at least one solutionwith element
44、 concentration that is a minimum of 100 times theLDfor each element.Add sufficient nitric acid to bring the finalsolution to 1 % HNO3. Prior to preparing the multielementsolutions, analyze each stock solution separately to check forstrong spectral interference and the presence of impurities (5).Take
45、 care when preparing the multielement solutions to verifythat the components are compatible and stable (they do notinteract to cause precipitation) and that none of the elementspresent exhibit mutual spectral interference. Transfer the cali-bration reference solutions to acid-leached FEP TFE-fluoroc
46、arbon or polyethylene bottles for storage. Calibrationreference solutions must be verified initially using a qualitycontrol sample and monitored periodically for stability.NOTE 3Solutions in polyethylene bottles are subject to transpirationlosses that may affect the assigned concentration values.7.7
47、.2 Prepare the instrument check solution(s) and linearitycheck solutions in a similar manner.7.7.3 Fresh solutions should be prepared as needed with therealization that concentrations can change over time. Therecommended maximum shelf life for calibration referencesolutions, instrument check solutio
48、ns, and linearity checksolutions is one month.8. Sample Preparation8.1 If necessary to remove solids or suspended colloids,filter the leachate through a clean filter, using an inert filtersupport (avoid the use of fritted glass supports). Examine thefiltered leachate to verify the absence of visible
49、 solids orsuspended colloids. The deposit on the filter may be analyzedseparately if required.8.2 Prepare filtered and unfiltered aliquots of a calibrationblank solution, and compare the results of these aliquots todetermine whether the filter membrane contributes to the blanklevel of the filtered solution.NOTE 4Step 8.2 may be omitted if none of the samples requiresfiltration.8.3 Add sufficient high-purity concentrated nitric acid tobring the leachate sample solution to volume 1 % HNO3.Iftheleachate is known to be a chloride solution, or nitric aci
