1、Designation: D7035 10Standard 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 The method is applicable to personal sampling of theinhalable or respirable fraction of airborne particles and to a
4、reasampling.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 method specifies a number of alternative methodsfor preparing test solutions from samples of airborne part
5、icu-late matter. One of the specified sample preparation methods isapplicable to the measurement of soluble metal or metalloidcompounds. Other specified methods are applicable to themeasurement of total metals and metalloids.1.5 It is the users responsibility to ensure the validity of thestandard me
6、thod for filters 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 dissolution methods for
7、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 YttriumCobalt Rhod
8、ium ZincCopper Selenium ZirconiumHafnium Silver1.7 The method is not applicable to the sampling of elemen-tal mercury, or to inorganic compounds of metals and metal-loids that are present in the gaseous or vapor state.1.8 No detailed operating instructions are provided becauseof differences among va
9、rious 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 the same make and mod
10、el.1.9 This test method contains notes that are explanatory andare not part of the mandatory requirements of the method.1.10 The values stated in SI units are to be regarded as thestandard.1.11 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It i
11、s 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:2D1193 Specification for Reagent WaterD1356 Terminology Relating to Sampling and An
12、alysis ofAtmospheresD4185 Practice for Measurement of Metals in WorkplaceAtmospheres by Flame Atomic Absorption Spectropho-tometryD4840 Guide for Sample Chain-of-Custody ProceduresD5011 Practices for Calibration of Ozone Monitors UsingTransfer StandardsD6062 Guide for Personal Samplers of Health-Rel
13、atedAerosol FractionsD6785 Test Method for Determination of Lead in Work-place Air Using Flame or Graphite Furnace Atomic Ab-sorption SpectrometryD7202 Test Method for Determination of Beryllium in the1This test method is under the jurisdiction of ASTM Committee D22 on AirQuality and is the direct r
14、esponsibility of Subcommittee D22.04 on Workplace AirQuality.Current edition approved April 1, 2010. Published June 2010. Originallyapproved in 2004. Last previous edition approved in 2004 as D7035 - 04. DOI:10.1520/D7035-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcon
15、tact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Workplace Using Field
16、-Based Extraction and Fluores-cence DetectionD7439 Test Method for Determination of Elements inAirborne Particulate Matter by Inductively CoupledPlasmaMass SpectrometryD7440 Practice for Characterizing Uncertainty in Air Qual-ity MeasurementsE882 Guide for Accountability and Quality Control in theCh
17、emical 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 Spec
18、-trometry (GFAAS) TechniquesE1728 Practice for Collection of Settled Dust SamplesUsing Wipe Sampling Methods for Subsequent LeadDetermination2.2 ISO and European Standards:ISO 1042 Laboratory GlasswareOne-mark VolumetricFlasks3ISO 3585 Glass Plant, Pipelines and FittingsProperties ofBorosilicate Gla
19、ss3ISO 6879 Glass Plant, Pipelines and FittingsProperties ofBorosilicate Glass3ISO 7708 Particle Size Definitions for Health-Related Sam-pling3ISO 8655 Piston-Operated Volumetric Instruments (6parts)3ISO 15202 Workplace AirDetermination of Metals andMetalloids in Airborne Particulate Matter by Induc
20、tivelyCoupled PlasmaAtomic Emission Spectrometry (3 parts)3EN 482 Workplace AtmospheresGeneral Requirementsfor the Performance of Procedures for the Measurement ofChemical Agents4EN 1540 Workplace AtmospheresTerminology43. Terminology3.1 For definitions of pertinent terms not listed here, seeTermino
21、logy D1356.3.2 Definitions:3.2.1 analytical recoveryratio of the mass of analytemeasured to the known mass of analyte in the sample,expressed as a percentage. D67853.2.2 area samplera device, not attached to a person, thatis used to sample air in a particular location.3.2.3 atomic emissioncharacteri
22、stic radiation emitted byan electronically excited atomic species.3.2.3.1 DiscussionIn atomic (or optical) emission spec-trometry, a very high-temperature environment, such as aplasma, is used to create excited state atoms. For analyticalpurposes, characteristic emission signals from elements in the
23、irexcited states are then measured at specific wavelengths.3.2.4 axial plasmaa horizontal inductively coupledplasma that is viewed end-on (versus radially; see 3.2.43).3.2.5 background correctionthe process of correcting theintensity at an analytical wavelength for the intensity due to theunderlying
24、 spectral background of a blank. ISO 152023.2.6 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 152023.2.7 batcha group of field or quality control (QC)sam
25、ples that are collected or processed together at the sametime using the same reagents and equipment. E16133.2.8 biasconsistent deviation of the results of a measure-ment process from the true value of the air quality character-istic itself. ISO 68793.2.9 blank solutionsolution prepared by taking a r
26、eagentblank or field blank through the same procedure used forsample dissolution.3.2.10 breathing zonethe space around a workers facefrom where he or she takes his or her breath. For technicalpurposes a more precise definition is as follows: A hemisphere(generally accepted to be 0.3 m in radius) ext
27、ending in front ofthe human face, centered on the midpoint of a line joining theears; the base of the hemisphere is a plane through this line, thetop of the head and the larynx. The definition is not applicablewhen respiratory protective equipment is used. EN 15403.2.11 calibration blank solutioncal
28、ibration solution pre-pared without the addition of any stock standard solution orworking standard solution. ISO 152023.2.11.1 DiscussionThe concentration of the analyte(s) ofinterest in the calibration blank solution is taken to be zero.3.2.12 calibration curvea plot of instrument responseversus co
29、ncentration of standards (1)5.3.2.13 calibration solutionsolution prepared by dilutionof the stock standard solution(s) or working standard solu-tion(s), containing the analyte(s) of interest at a concentra-tion(s) suitable for use in calibration of the analytical instru-ment. ISO 152023.2.13.1 Disc
30、ussionThe technique of matrix matching isnormally used when preparing calibration solutions.3.2.14 chemical agentany chemical element or com-pound, on its own or admixed as it occurs in the natural stateor as produced, used or released including release as waste, byany work activity, whether or not
31、produced intentionally andwhether or not placed on the market. EN 15403.2.15 continuing calibration blank (CCB)a solution con-taining no analyte added, that is used to verify blank responseand freedom from carryover. E16133.2.15.1 DiscussionThe measured concentration of theCCB is to be (at most) les
32、s than five times the instrumentaldetection limit.3.2.16 continuing calibration verification (CCV)a solu-tion (or set of solutions) of known analyte concentration usedto verify freedom from excessive instrumental drift; the con-centration is to be near the mid-range of a linear calibration3Available
33、 from American National Standards 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.5The boldface numbers in parentheses refer to the list of references at the end ofthis standard.D7
34、035 102curve. E16133.2.16.1 DiscussionThe CCV must be matrix matched tothe acid content present in sample digestates or extracts. TheCCV must be analyzed before and after all samples and at afrequency of not less than every ten samples. The measuredvalue is to fall within 610 % of the known value.3.
35、2.17 excitation interferencesnon-spectral interferencesthat manifest 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.ISO 152023.2.18 field blanksampling media (for example, an airfilter)
36、 that is exposed to the same handling as field samples,except that no sample is collected (that is, no air is purposelydrawn through the sampler). D67853.2.18.1 DiscussionAnalysis results from field blanksprovide information on the analyte background level in thesampling media, combined with the pot
37、ential contaminationexperienced by samples collected within the batch resultingfrom handling.3.2.19 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
38、gas. ISO 152023.2.20 inductively coupled plasma (ICP) torcha deviceconsisting of three concentric tubes, the outer two usuallymade from quartz, that is used to support and introduce sampleinto an ICP discharge. ISO 152023.2.21 inhalable fractionthe total airborne particle massfraction inhaled throug
39、h the nose and mouth, that is, whichenters the respiratory system. D60623.2.22 injector tubethe innermost tube of an inductivelycoupled plasma torch, usually made of quartz or ceramicmaterials, through which the sample aerosol is introduced tothe plasma. ISO 152023.2.23 inner (nebulizer) argon flowt
40、he 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 152023.2.24 instrumental detection limit (IDL)the lowest con-centration at which the instrumentation can distinguish analytecontent from
41、the background generated by a minimal matrix.E16133.2.24.1 DiscussionThe IDL pertains to the maximumcapability of an instrument and should not be confused with themethod detection limit (MDL; see 3.2.35).3.2.25 interelement correctiona spectral interference cor-rection technique in which emission co
42、ntributions 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 other wave-lengths. ISO 152023.2.26 intermediate (auxiliary) argon flowthe flow ofargon gas that is contain
43、ed between the intermediate and center(injector) tubes of an inductively coupled plasma torch; typi-cally 0.1 L/min 2 L/min. ISO 152023.2.27 internal standarda non-analyte element, present inall calibration, blank, and sample solutions, the signal fromwhich is used to correct for non-spectral interf
44、erence orimprove analytical precision. ISO 152023.2.28 laboratory blankunused sample media (for ex-ample, an air filter), taken from the same batch used forsampling, that does not leave the laboratory. ISO 152023.2.29 limit valuereference figure for concentration of achemical agent in air. ISO 15202
45、3.2.30 linear dynamic rangethe range of concentrationsover which the calibration curve for an analyte is linear. Itextends from the detection limit to the onset of calibrationcurvature. ISO 152023.2.31 load coila length of metal tubing (typically cop-per) which is wound around the end of an inductiv
46、ely coupledplasma torch and connected to the radio frequency generator.ISO 152023.2.31.1 DiscussionThe load coil is used to inductivelycouple energy from the radio frequency generator to the plasmadischarge.3.2.32 matrix interferenceinterference of a non-spectralnature which is caused by the sample
47、matrix. ISO 152023.2.33 matrix matchinga technique used to minimize theeffect of the test solution matrix on the analytical results.ISO 152023.2.33.1 DiscussionMatrix matching involves preparingcalibration solutions in which the concentrations of acids andother major solvents and solutes are matched
48、 with those in thetest solutions.3.2.34 measuring procedureprocedure for sampling andanalyzing one or more chemical agents in the air, includingstorage and transportation of the sample(s). ISO 152023.2.35 method detection limit (MDL)the minimum con-centration of an analyte that can be reported with
49、a 99 %confidence that the value is above zero. D13563.2.35.1 DiscussionThe MDL is also known as the limitof detection (LOD) (2).3.2.36 method quantitation limit (MQL)the minimumconcentration of an analyte that can be measured with accept-able precision, ordinarily taken to be at least ten times thestandard deviation of the mean blank signal (2).3.2.36.1 DiscussionThe MQL is also known as the limitof quantitation.3.2.37 nebulizera device used to create an aerosol from aliquid. ISO 152023.2.38 outer (plasma) argon flowthe fl
