1、Designation: D7035 16Standard Test Method forDetermination of Metals and Metalloids in AirborneParticulate Matter by Inductively Coupled Plasma AtomicEmission Spectrometry (ICP-AES)1This standard is issued under the fixed designation D7035; 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 test method specifies a procedure for colle
3、ction,sample preparation, and analysis of airborne particulate matterfor the content of metals and metalloids using inductivelycoupled plasma-atomic emission spectrometry (ICP-AES).1.2 This test method is applicable to personal sampling ofthe inhalable or respirable fraction of airborne particles an
4、d toarea sampling.1.3 This test method should be used by analysts experiencedin the use of ICP-AES, the interpretation of spectral and matrixinterferences, and procedures for their correction.1.4 This test method specifies a number of alternativemethods for preparing test solutions from samples of a
5、irborneparticulate matter. One of the specified sample preparationmethods is applicable to the measurement of soluble metal ormetalloid compounds. Other specified methods are applicableto the measurement of total metals and metalloids.1.5 It is the users responsibility to ensure the validity of this
6、test method for sampling materials of untested matrices.1.6 The following is a non-exclusive list of metals andmetalloids for which one or more of the sample dissolutionmethods specified in this document is applicable. However,there is insufficient information available on the effectivenessof dissol
7、ution methods for those elements in italics.Aluminum Indium SodiumAntimony Iron StrontiumArsenic Lead TantalumBarium Lithium TelluriumBeryllium Magnesium ThalliumBismuth Manganese TinBoron Molybdenum TitaniumCadmium Nickel TungstenCalcium Phosphorus UraniumCesium Platinum VanadiumChromium Potassium
8、YttriumCobalt Rhodium ZincCopper Selenium ZirconiumHafnium Silver1.7 This test method is not applicable to the sampling ofelemental mercury, or to inorganic compounds of metals andmetalloids that are present in the gaseous or vapor state.1.8 No detailed operating instructions are provided becauseof
9、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 t
10、he same make and model.1.9 This test method contains notes that are explanatory andare not part of the mandatory requirements of this test method.1.10 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.11 This standard does not p
11、urport 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 and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2
12、D1193 Specification for Reagent WaterD1356 Terminology Relating to Sampling and Analysis ofAtmospheresD4185 Practice for Measurement of Metals in WorkplaceAtmospheres by Flame Atomic Absorption Spectropho-tometryD4840 Guide for Sample Chain-of-Custody ProceduresD6062 Guide for Personal Samplers of H
13、ealth-RelatedAero-sol Fractions1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct responsibility of Subcommittee D22.04 on Workplace AirQuality.Current edition approved Oct. 1, 2016. Published October 2016. Originallyapproved in 2004. Last previous edit
14、ion approved in 2010 as D7035 10. DOI:10.1520/D7035-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyri
15、ght ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D6785 Test Method for Determination of Lead in WorkplaceAir Using Flame or Graphite Furnace Atomic AbsorptionSpectrometryD7202 Test Method for Determination of Beryllium in theWorkplace by Ext
16、raction and Optical Fluorescence Detec-tionD7439 Test Method for Determination of Elements in Air-borne Particulate Matter by Inductively Coupled Plasma-Mass SpectrometryD7440 Practice for Characterizing Uncertainty in Air Qual-ity MeasurementsE882 Guide for Accountability and Quality Control in the
17、Chemical Analysis LaboratoryE1370 Guide for Air Sampling Strategies for Worker andWorkplace ProtectionE1613 Test Method for Determination of Lead by Induc-tively Coupled Plasma Atomic Emission Spectrometry(ICP-AES), Flame Atomic Absorption Spectrometry(FAAS), or Graphite Furnace Atomic Absorption Sp
18、ec-trometry (GFAAS) TechniquesE1728 Practice for Collection of Settled Dust Samples UsingWipe Sampling Methods for Subsequent Lead Determi-nation2.2 ISO and European Standards:ISO 1042 Laboratory GlasswareOne-mark VolumetricFlasks3ISO 3585 Glass Plant, Pipelines and FittingsProperties ofBorosilicate
19、 Glass3ISO 7708 Particle Size Definitions for Health-Related Sam-pling3ISO 8655 Piston-Operated Volumetric Instruments (6 parts)3ISO 15202 Workplace AirDetermination of Metals andMetalloids in Airborne Particulate Matter by InductivelyCoupled PlasmaAtomic Emission Spectrometry (3 parts)3ISO 18158 Wo
20、rkplace AtmospheresTerminology3EN 482 Workplace AtmospheresGeneral Requirementsfor the Performance of Procedures for the Measurement ofChemical Agents43. Terminology3.1 For definitions of pertinent terms not listed here, seeTerminology D1356.3.2 Definitions:3.2.1 atomic emissioncharacteristic radiat
21、ion emitted byan electronically excited atomic species.3.2.1.1 DiscussionIn atomic (or optical) emissionspectrometry, a very high-temperature environment, such as aplasma, is used to create excited state atoms. For analyticalpurposes, characteristic emission signals from elements in theirexcited sta
22、tes are then measured at specific wavelengths.3.2.2 axial plasmaa horizontal inductively coupledplasma that is viewed end-on (versus radially; see 3.2.30).3.2.3 background correctionthe process of correcting theintensity at an analytical wavelength for the intensity due to theunderlying spectral bac
23、kground of a blank. ISO 152023.2.4 background equivalent concentrationthe concentra-tion of a solution that results in an emission signal ofequivalent intensity to the background emission signal at theanalytical wavelength. ISO 152023.2.5 batcha group of field or quality control (QC)samples that are
24、 collected or processed together at the sametime using the same reagents and equipment. E16133.2.6 blank solutionsolution prepared by taking a reagentblank or field blank through the same procedure used forsample dissolution.3.2.7 calibration blank solutioncalibration solution pre-pared without the
25、addition of any stock standard solution orworking standard solution. ISO 152023.2.7.1 DiscussionThe concentration of the analyte(s) ofinterest in the calibration blank solution is taken to be zero.3.2.8 calibration solutionsolution prepared by dilution ofthe stock standard solution(s) or working sta
26、ndard solution(s),containing the analyte(s) of interest at a concentration(s)suitable for use in calibration of the analytical instrument. ISO152023.2.8.1 DiscussionThe technique of matrix matching isnormally used when preparing calibration solutions.3.2.9 continuing calibration blank (CCB)a solutio
27、n con-taining no analyte added, that is used to verify blank responseand freedom from carryover. E16133.2.9.1 DiscussionThe measured concentration of theCCB is to be (at most) less than five times the instrumentaldetection limit.3.2.10 excitation interferencesnon-spectral interferencesthat manifest
28、as a change in sensitivity due to a change ininductively coupled plasma conditions when the matrix of acalibration or test solution is introduced into the plasma. ISO152023.2.11 field blanksampling media (for example, an airfilter) that is exposed to the same handling as field samples,except that no
29、 sample is collected (that is, no air is purposelydrawn through the sampler). D67853.2.11.1 DiscussionAnalysis results from field blanks pro-vide information on the analyte background level in thesampling media, combined with the potential contaminationexperienced by samples collected within the bat
30、ch resultingfrom handling.3.2.12 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. ISO 152023.2.13 inductively coupled plasma (ICP) torcha device
31、consisting of three concentric tubes, the outer two usuallymade from quartz, that is used to support and introduce sampleinto an ICP discharge. ISO 152023.2.14 injector tubethe innermost tube of an inductivelycoupled plasma torch, usually made of quartz or ceramic3Available from American National St
32、andards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Available from CEN Central Secretariat: rue de Stassart 36, B-1050 Brussels,Belgium.D7035 162materials, through which the sample aerosol is introduced tothe plasma. ISO 152023.2.15 inner (nebulizer) argon flo
33、wthe flow of argon gasthat is directed through the nebulizer and carries the sampleaerosol through the injector and into the plasma; typically 0.5L/min 2 L/min. ISO 152023.2.16 instrumental detection limit (IDL)the lowest con-centration at which the instrumentation can distinguish analytecontent fro
34、m the background generated by a minimal matrix.E16133.2.16.1 DiscussionThe IDL pertains to the maximumcapability of an instrument and should not be confused with themethod detection limit (MDL).3.2.17 interelement correctiona spectral interference cor-rection technique in which emission contribution
35、s 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. ISO 152023.2.18 intermediate (auxiliary) argon flowthe flow ofargon gas that is contained between t
36、he intermediate and center(injector) tubes of an inductively coupled plasma torch; typi-cally 0.1 L/min 2 L/min. ISO 152023.2.19 internal standarda non-analyte element, present inall calibration, blank, and sample solutions, the signal fromwhich is used to correct for non-spectral interference orimp
37、rove analytical precision. ISO 152023.2.20 limit valuereference figure for concentration of achemical agent in air. ISO 152023.2.21 linear dynamic rangethe range of concentrationsover which the calibration curve for an analyte is linear. Itextends from the detection limit to the onset of calibration
38、curvature. ISO 152023.2.22 load coila length of metal tubing (typically copper)which is wound around the end of an inductively coupledplasma torch and connected to the radio frequency generator.ISO 152023.2.22.1 DiscussionThe load coil is used to inductivelycouple energy from the radio frequency gen
39、erator to the plasmadischarge.3.2.23 matrix interferenceinterference of a non-spectralnature which is caused by the sample matrix.3.2.23.1 DiscussionMatrix matching involves preparingcalibration solutions in which the concentrations of acids andother major solvents and solutes are matched with those
40、 in thetest solutions. ISO 152023.2.24 measuring procedureprocedure for sampling andanalyzing one or more chemical agents in the air, includingstorage and transportation of the sample(s). ISO 152023.2.25 method quantitation limit (MQL)the minimumconcentration of an analyte that can be measured with
41、accept-able precision, ordinarily taken to be at least ten times thestandard deviation of the mean blank signal (1).53.2.25.1 DiscussionThe MQL is also known as the limitof quantitation.3.2.26 nebulizera device used to create an aerosol from aliquid. ISO 152023.2.27 outer (plasma) argon flowthe flow
42、 of argon gasthat is contained between the outer and intermediate tubes of aninductively coupled plasma torch; typically 7 to 15 L/min. ISO152023.2.28 personal samplera device attached to a person thatsamples air in the breathing zone. ISO 181583.2.29 pneumatic nebulizera nebulizer that uses high-sp
43、eed gas flows to create an aerosol from a liquid. ISO 152023.2.30 radial plasmaan inductively coupled plasma that isviewed from the side (versus axial).3.2.31 respirable fractionthe mass of inhaled particlespenetrating to the unciliated airways. ISO 77083.2.32 sample dissolutionthe process of obtain
44、ing a solu-tion containing the analyte(s) of interest from a sample. Thismay or may not involve complete dissolution of the sample.D67853.2.33 sample preparationall operations carried out on asample, after transportation and storage, to prepare it foranalysis, including transformation of the sample
45、into a mea-surable state, where necessary. ISO 152023.2.34 sampling locationa specific area within a samplingsite that is subjected to sample collection. E17283.2.34.1 DiscussionMultiple sampling locations are com-monly designated for a single sampling site.3.2.35 sampling sitea local geographic are
46、a that containsthe sampling locations. E17283.2.35.1 DiscussionAsampling site is generally limited toan area that is easily covered by walking.3.2.36 spectral interferencean interference caused by theemission from a species other than the analyte of interest. ISO152023.2.37 spray chambera device pla
47、ced between a nebulizerand an inductively coupled plasma torch whose function is toseparate out aerosol droplets in accordance with their size, sothat only very fine droplets pass into the plasma, and largedroplets are drained or pumped to waste. ISO 152023.2.38 stock standard solutionsolution used
48、for prepara-tion of working standard solutions and/or calibration solutions,containing the analyte(s) of interest at a certified concentra-tion(s) traceable to primary standards (National Institute ofStandards and Technology or international measurement stan-dards).3.2.39 transport interferencenon-s
49、pectral interferencecaused by a difference in viscosity, surface tension, or densitybetween the calibration and test solutions (for example, due to5The boldface numbers in parentheses refer to a list of references at the end ofthis standard.D7035 163differences in dissolved solids content, type and concentrationof acid, and so forth). ISO 152023.2.39.1 DiscussionSuch differences produce a change innebulizer efficiency and hence in the amount of analytereaching the plasma.3.2.40 ultrasonic nebulizera nebulizer in which
