1、Designation: F2980 13 (Reapproved 2017)Standard Test Method forAnalysis of Heavy Metals in Glass by Field Portable X-RayFluorescence (XRF)1This standard is issued under the fixed designation F2980; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e 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 field portable X-ray fluores-cence (XRF) spectrometric procedures f
3、or analyses of arsenicand lead in glass compositions using field portable energydispersive XRF spectrometers.1.2 The mass fraction range of arsenic within which this testmethod is quantitative is given in Table 1. Scope limits weredetermined from the interlaboratory study results using theapproach g
4、iven in Practice E1601.1.3 The mass fraction range for which lead was tested isgiven in Table 1. However, lead results cannot be consideredquantitative on the basis of single-sample results because theprecision performance is not good enough to allow laboratoriesto compare results in a quantitative
5、manner.NOTE 1The performance of this test method was evaluated usingresults based on single-sample determinations from specimens composedof glass beads. One laboratory has determined that performance can besignificantly improved by basing reported results on the mean of deter-minations from multiple
6、 samples to overcome inherent heterogeneity ofelements in glass beads, especially the element lead. Additional informa-tion is provided in Section 17 on Precision and Bias.1.3.1 To obtain quantitative performance, lead results mustconsist of the average of four or more determinations.1.4 The values
7、stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety
8、, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Some specific hazards statements are given in Section 7 onHazards.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization
9、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 ASTM Standards:2D75/D75M Practice for Sampling AggregatesD6299 Practice fo
10、r Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related
11、 MaterialsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1361 Guide for Correction of Interelement Effects inX-Ray Spectrometric AnalysisE1601 Practice for Conducting an Interla
12、boratory Study toEvaluate the Performance of an Analytical MethodE1621 Guide for Elemental Analysis by Wavelength Disper-sive X-Ray Fluorescence SpectrometryF2576 Terminology Relating to Declarable Substances inMaterials2.2 ANSI Standard:3N43.2 Radiation Safety for X-Ray Diffraction and Fluores-cenc
13、e Analysis Equipment2.3 AASHTO Standard:4TP-97-11 Test Method for Glass Beads used in PavementMarkings1This test method is under the jurisdiction of ASTM Committee F40 onDeclarable Substances in Materials and is the direct responsibility of SubcommitteeF40.01 on Test Methods.Current edition approved
14、 Nov. 1, 2017. Published November 2017. Originallyapproved in 2013. Last previous edition approved in 2013 as F29180-13. DOI:10.1520/F2980-13R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards
15、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.4Available from American Association of State Highway and TransportationOfficials (AASHTO
16、), 444 N. Capitol St., NW, Suite 249, Washington, DC 20001,http:/www.transportation.org.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
17、on standardization established 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.13. Terminology3.1 DefinitionsDefinitions of terms applying to X-rayfluorescence (
18、XRF) and declarable substances appear in Ter-minologies E135 and F2576, respectively.3.2 Compton-matrix correction, nmeasured intensity ofCompton or incoherent scattered radiation may be used directlyto compensate for matrix effects or indirectly for the determi-nation of the effective mass absorpti
19、on coefficient to correct formatrix effects.53.2.1 DiscussionThe compensation for matrix effects isbased on a combination of sample preparation and experimen-tal intensity data.3.3 Compton scatter, ninelastic scattering of an X-rayphoton through its interaction with the bound electrons of anatom.3.3
20、.1 DiscussionThis process is also referred to as inco-herent scatter.3.4 fundamental parameters, FP, model, nmodel for cali-bration of X-ray fluorescence response, including the correc-tion of matrix effects, based on the theory describing thephysical processes of the interactions of X-rays with mat
21、ter.63.5 Acronyms:3.5.1 EDXRFEnergy dispersive X-ray fluorescence3.5.2 QCQuality control3.5.3 XRFX-ray fluorescence4. Summary of Test Method4.1 Portable handheld instruments are used to measure glassspheres, ground glass, cullet, fiberglass, and sheet glass fortheir contents of arsenic and lead. Sam
22、ples of sheet glass canbe measured directly. Samples that are not in sheet form aremeasured as is or after pulverizing to an appropriate particlesize.4.2 The samples of glass spheres or powders may be placedinto disposable cups with a polymer film supporting the glass.The filled cup is measured from
23、 below through the polymerfilm.4.3 The glass specimen may be analyzed in situ by using ahandheld spectrometer positioned in contact with sheet glass orthe contents of a larger container, for example, a bulk shippingcontainer.4.4 The handheld XRF may be used while the operator isholding the unit or b
24、y being mounted in a stand for safer, moreconvenient laboratory use. The two measurement options arediscussed throughout this test method.5. Significance and Use5.1 Waste glass is currently recycled into various consumerproducts. This test method has been developed as a tool forevaluation of heavy m
25、etals in glass to satisfy reporting require-ments for maximum allowable content for some applications.5.2 The ranges within which this test method is quantitativeare given in Table 1.5.3 For amounts of the analyte elements outside the rangesin Table 1, this test method provides screening results. Th
26、at is,it provides an unambiguous indication that each element can bedescribed as present in an amount greater than the scope upperlimit or that the amount of the element can be described as lessthan the scope lower limit with a high degree of confidence.NOTE 2In general, when a quantitative result i
27、s obtained, the analystcan make a clear decision as to whether a material is suitable for theintended purpose. When the contents of elements of interest are outsidethe quantitative range, the analyst can still make a decision whether theamount is too high or whether additional analyses are required.
28、5.4 These methods can be applied to glass beads, plateglass, float glass, fiber glass, or ground glass. This test methodhas been validated for the ranges of matrix compositions thatare summarized in Table 2.5.5 Detection limits, sensitivity, and element ranges willvary with matrices, detector type,
29、and other instrument condi-tions and parameters.5.6 All analytes are determined as the element and reportedas such. These include all elements listed in Table 1. This testmethod may be applicable to other glass matrices, additionalelements, and wider concentration ranges provided the labora-tory is
30、able to validate the broadened scope of this test method.6. Interferences6.1 Spectral InterferencesThese can occur for some ele-ments as a result of partial or total line overlaps. These lineoverlaps can result from scattered characteristic lines from thetarget of the X-ray tube or by X-ray fluoresc
31、ence from atoms inthe specimen. Spectral interference can also be the result ofescape peaks from the solid-state detector. See Guide E1621for a full discussion of models used to correct for these effects.In this particular case, the most obvious line overlap is theoverlap of As K-L2,3(As K1,2; 10.53
32、 keV) on Pb L3-M5(PbL1; 10.55 keV) and vice versa. The energy difference betweenthese two lines is about 0.02 keV, which cannot be resolvedwith the detectors used. The emission lines of these twoelements will appear as a single peak. However, both As andPb have alternative lines that can be used for
33、 analysis. For Pb,5Andermann, G. and Kemp, J. W., “Scattered X-rays as Internal Standards inX-Ray Spectroscopy,” Analytical Chemistry, Vol 20, No. 8, 1958.6The algorithm used for the procedure is usually implemented in the instrumentmanufacturers software. Third-party software is available and may b
34、e used.TABLE 1 Scope Ranges for Quantitative ResultsElement Scope Lower Limit (mg/kg)Scope Upper Limit (mg/kg)Arsenic 240 2000Lead 120 500TABLE 2 Matrix Components and RangesOxide Scope Lower Limit, % Scope Upper Limit, %SiO258 80Al2O3110Na2O3 15CaO 6 20MgO 1 5F2980 13 (2017)2the use of the doublet
35、Pb L2,3-M4,N5(Pb L1,2; 12.61 keV) ishighly recommended. This line has virtually the same sensi-tivity as the Pb L3-M5line. For As, the As K-M2,3(As K1,3;11.72 keV) can be used; its sensitivity is about 20 % of themore intense As K-L2,3line. It is possible to determine the netintensity of Pb L3-M5bas
36、ed on the intensity of Pb L2,3-M4,N5(this implies determining a proportionality factor between thetwo lines on specimens with no or varying amounts of As).This can then be used to calculate the intensity of As K-L2,3.6.2 In EDXRF, the possibility exists that two photons areseen and treated as a sing
37、le one by the counting electronics.When that happens, they appear as a single photon with anenergy corresponding to the sum of the energies of theindividual photons. This phenomenon is called the sum-peak.For this effect to be significant, the total count rate must behigh; and (at least) one element
38、 must be present at a relativelyhigh level; and the element concerned must have a high yield.In the current method, the presence of e.g. iron at high levelscould lead to a sum-peak of 2 Fe K-L3 (6.4 keV) photons, withan energy of about 12.6- 12.8 keV - this corresponds to theenergy of Pb L2,3-M4,N5.
39、 The software provided by themanufacturer must correct for this effect; otherwise the inten-sity (and thus the contents) of Pb L2,3-M4,N5is overestimated.6.3 Matrix InterferencesSome of the X-rays generatedwithin the sample will interact with atoms in the matrix. As aresult of such interactions, the
40、 emitted intensity of the analytedepends on the amount of the analyte in the sample and, to alesser, but measurable degree, on the amounts of other ele-ments. The magnitude of such matrix interferences is mostpronounced for elements that are present in high concentra-tions. Several mathematical mode
41、ls, such as the fundamentalparameter model, exist for the correction of such effects; seeGuide E1361 for a full discussion. Typically, these matrixcorrection models require that the net intensities are free fromline overlap effects. In practice, the approach chosen dependsupon the manufacturer.6.4 F
42、loat glass is heterogeneous because one side is coatedwith tin. Differential absorption can bias the results.7. Apparatus7.1 EDXRF Spectrometerdesigned for X-ray fluorescenceanalysis with energy dispersive selection of radiation. AnyEDXRF spectrometer can be used if its design incorporates thefollow
43、ing features.7.1.1 Source of X-Ray Excitationcapable of exciting therecommended lines, typically an X-ray tube. The recom-mended lines are shown in Table 3.7.1.2 X-Ray DetectorAn energy resolution of better than250 eV at Mn K-L2,3has been found suitable for use in this testmethod.7.1.3 Signal condit
44、ioning and data-handling electronics in-clude the functions of X-ray counting and peak processing.7.2 The following spectrometer features and accessories areoptional.7.2.1 Beam Filtersused to make the excitation moreselective and reduce background count rates.7.2.2 Drift Correction Monitor(s)Because
45、 of instability ofthe measurement system, the sensitivity and background of thespectrometer may drift with time. Drift correction monitorsmay be used to correct for this drift. The optimum driftcorrection monitor specimens are permanent materials that arestable with time and repeated exposure to X-r
46、ays.7.3 Reference Materials:7.3.1 Purchased certified reference materials, and7.3.2 In-house reference materials that were analyzed by atleast two independent methods.7.4 Consumables:7.4.1 Disposable latex or nitrile gloves,7.4.2 Methanol or isopropyl alcohol,7.4.3 Deionized water,7.4.4 XRF sample c
47、ups,7.4.5 Lint-free wipes, and7.4.6 Polymer film, including, but not limited to polyimide,polyester, and polypropylene.8. Hazards8.1 Safety practices shall conform to applicable local, state,and national regulations. For example, personal monitoringdevices and periodic radiation surveys may be requi
48、red.8.2 Dust MaskWhen this test method is performed onpowder samples, it may be advisable to use a dust mask.8.3 GlovesThe use of powder-free polymer gloves isrecommended to prevent contamination of sample surfaces bybody oils and other substances.9. Sampling9.1 Users should develop plans to determi
49、ne if the measuredspecimens are representative of a larger quantity of material.Refer to AASHTO TP-97-11 or Practice D75/D75M forexamples of sampling procedures for quantities greater than 45kg.9.2 For laboratories having small quantities of material,three replicate measurements may be taken to obtain informa-tion on homogeneity. If the range of three results is greater thanthe repeatability limit of this standard test method, there maybe evidence for statistically significant heterogeneity. Theanalyst may measure more samples and note standard devia-tion.10
