ASTM D7035-2004 Standard Test Method for Determination of Metals and Metalloids in Airborne Particulate Matter by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES)《.pdf

1、Designation: D 7035 04Standard 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 D 7035; the number immediately following the designation indicate

2、s 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method specifies a procedure for co

3、llection,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 t

4、o areasampling.1.3 This method specifies a number of alternative methodsfor preparing test solutions from samples of airborne particu-late matter. One of the specified sample preparation methods isapplicable to the measurement of soluble metal or metalloidcompounds. Other specified methods are appli

5、cable to themeasurement of total metals and metalloids.1.4 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 dissolu

6、tion 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 Y

7、ttriumCobalt Rhodium ZincCopper Selenium ZirconiumHafnium Silver1.5 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.1.6 This test method contains notes that are explanatory andare n

8、ot part of the mandatory requirements of the method.1.7 The values stated in SI units are to be regarded as thestandard.1.8 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-pr

9、iate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1356 Terminology Related to Atmospheric SamplingD 4185 Practice for Measurement of Metals in WorkplaceAtmosphere

10、 by Atomic Absorption SpectrophotometryD 4840 Practice for Sampling Chain-of-Custody Proce-duresD 5011 Practices for Calibration of Ozone Monitors UsingTransfer StandardsD 6062 Guide for Personal Samplers of Health-RelatedAerosol FractionsD 6785 Test Method for Determination of Lead in Work-place Ai

11、r Using Flame or Graphite Furnace Atomic Ab-sorption SpectrometryE 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1370 Guide for Air Sampling Strategies for Worker andWorkplace ProtectionE 1613 Test Method for the Analysis of Digested or Ex-tracted Samples for L

12、ead by Inductively Coupled PlasmaAtomic Emission Spectrometry (ICP-AES), Flame AtomicAbsorption Spectrometry (FAAS), or Graphite FurnaceAtomic Absorption Spectrometry (GFAAS) TechniquesE 1728 Practice for Field Collection of Settled DustSamples Using Wipe Sampling Methods for Lead Deter-mination1Thi

13、s test method is under the jurisdiction of ASTM Committee D22 onSampling and Analysis of Atmospheres and is the direct responsibility of Subcom-mittee D22.04 on Workplace Atmospheres.Current edition approved October 1, 2004. Published October 2004.2For referenced ASTM standards, visit the ASTM websi

14、te, 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United State

15、s.2.2 ISO and European Standards:ISO 1042 Laboratory GlasswareOne-mark VolumetricFlasks3ISO 3585 Glass Plant, Pipelines and FittingsProperties ofBorosilicate Glass3ISO 6879 Glass Plant, Pipelines and FittingsProperties ofBorosilicate Glass3ISO 7708 Particle Size Definitions for Health-Related Sam-pl

16、ing3ISO 8655 Piston-Operated Volumetric Instruments (6parts)3ISO 12235 ChemistryGeneral Guidelines for InductivelyCoupled Plasma-Atomic Emission Spectrometry (2parts)3ISO 15202 Workplace AirDetermination of Metals andMetalloids in Airborne Particulate Matter by InductivelyCoupled Plasma Atomic Emiss

17、ion 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, seeTerminology D 1356.3.2 Definitions:3.2.

18、1 analytical recoveryratio of the mass of analytemeasured to the known mass of analyte in the sample,expressed as a percentage. D 67853.2.2 area samplera device, not attached to a person, thatis used to sample air in a particular location.3.2.3 atomic emissioncharacteristic radiation emitted byan el

19、ectronically 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 theirexcited states are then meas

20、ured at specific wavelengths.3.2.4 axial plasmaa horizontal inductively coupledplasma that is viewed end-on (versus radially).3.2.5 background correctionthe process of correcting theintensity at an analytical wavelength for the intensity due to theunderlying spectral background of a blank. ISO 15202

21、3.2.6 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)samples that are collected or processed toget

22、her at the sametime using the same reagents and equipment. E 16133.2.8 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 breathing zonethe space around a workers facefrom where he or she takes his or her bre

23、ath. For technicalpurposes a more precise definition is as follows: A hemisphere(generally accepted to be 0.3 m in radius) extending 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 lary

24、nx. The definition is not applicablewhen respiratory protective equipment is used. EN 15403.2.10 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 pr

25、oduced intentionally andwhether or not placed on the market. EN 15403.2.11 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

26、.ISO 152023.2.12 field blanksampling media (for example, an airfilter) 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). D 67853.2.12.1 DiscussionAnalysis results from field blanksprovide information on t

27、he analyte background level in thesampling media, combined with the potential contaminationexperienced by samples collected within the batch resultingfrom handling.3.2.13 inductively coupled plasma (ICP)a high-temperature discharge generated by a flowing conductive gas,normally argon, through a magn

28、etic field induced by a load coilthat surrounds the tubes carrying the gas. ISO 152023.2.14 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 152023.2.15 in

29、halable fractionthe total airborne particle massfraction inhaled through the nose and mouth, that is, whichenters the respiratory system. D 60623.2.16 injector tubethe innermost tube of an inductivelycoupled plasma torch, usually made of quartz or ceramicmaterials, through which the sample aerosol i

30、s introduced tothe plasma. ISO 152023.2.17 interelement correctiona spectral interference cor-rection technique in which emission contributions from inter-fering elements that emit radiation at the analyte wavelengthare subtracted from the apparent analyte emission after mea-suring the interfering e

31、lement concentrations at other wave-lengths. ISO 152023.2.18 inner (nebulizer) argon flowthe 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 152023.2.19 internal standarda non-analyte elem

32、ent, present inall calibration, blank, and sample solutions, the signal fromwhich is used to correct for non-spectral interference orimprove analytical precision. ISO 152023.2.20 intermediate (auxiliary) argon flowthe flow ofargon gas that is contained between the intermediate and center3Available f

33、rom American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.4Available from CEN Central Secretariat: rue de Stassart 36, B-1050 Brussels,Belgium.D7035042(injector) tubes of an inductively coupled plasma torch; typi-cally 0.1 L/min 2 L/min. ISO 152023.2.21 instrumen

34、tal detection limit (IDL)an instrumentalmeasurement value that is used to provide a lower concentra-tion limit for reporting optimum quantitative analysis data fora given instrument. E 16133.2.21.1 DiscussionThe IDL pertains to the maximumcapability of an instrument and should not be confused with t

35、hemethod detection limit (MDL).3.2.22 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 152023.2.23 load coila length of metal tubing (typically cop-per) which is woun

36、d around the end of an inductively coupledplasma torch and connected to the radio frequency generator.ISO 152023.2.23.1 DiscussionThe load coil is used to inductivelycouple energy from the radiofrequency generator to the plasmadischarge.3.2.24 matrix interferenceinterference of a non-spectralnature

37、which is caused by the sample matrix. ISO 152023.2.25 matrix matchinga technique used to minimize theeffect of the test solution matrix on the analytical results.ISO 152023.2.25.1 DiscussionMatrix matching involves preparingcalibration solutions in which the concentrations of acids andother major so

38、lvents and solutes are matched with those in thetest solutions.3.2.26 measuring procedureprocedure for sampling andanalyzing one or more chemical agents in the air, includingstorage and transportation of the sample(s). ISO 152023.2.27 method detection limit (MDL)the minimum con-centration of an anal

39、yte measured in the sample matrix whichgives a mean signal of at least three times the standarddeviation of the mean blank signal (1).53.2.28 method quantitation limit (MQL)the minimumconcentration of an analyte that can be measured with accept-able precision, ordinarily taken to be at least ten tim

40、es thestandard deviation of the mean blank signal (1).3.2.29 nebulizera device used to create an aerosol from aliquid. ISO 152023.2.30 outer (plasma) argon flowthe flow of argon gasthat is contained between the outer and intermediate tubes of aninductively coupled plasma torch; typically 7 to 15 L/m

41、in.ISO 152023.2.31 overall uncertainty (of a measuring procedure or ofan instrument)quantity used to characterize as a whole theuncertainty of a result given by an apparatus or measuringprocedure. It is expressed as a percentage by a combination ofbias and precision, usually in accordance with the f

42、ormula:? xref? 1 2s! / xref# 3 100, where is the mean value ofresults of a number of repeated measurements; xrefis the true oraccepted reference value of concentration, and s is the standarddeviation of repeated measurements. EN 4823.2.32 personal samplera device attached to a person thatsamples air

43、 in the breathing zone. EN 15403.2.33 pneumatic nebulizera nebulizer that uses high-speed gas flows to create an aerosol from a liquid.ISO 152023.2.34 primary standardan acceptable reference sampleor device used for establishing measurement of a physicalquantity, directly defined and established by

44、some authority,against which all secondary standards are compared. D 50113.2.35 radial plasmaan inductively coupled plasma thatis viewed from the side (versus end-on).3.2.36 reference periodthe specified period of time statedfor the exposure limit of a specific chemical agent. D 67853.2.36.1 Discuss

45、ionExamples of exposure limits havingdifferent reference values include short-term and long-termexposure limits, such as those established by the ACGIH (2).3.2.37 respirable fractionthe mass of inhaled particlespenetrating to the unciliated airways. ISO 77083.2.38 sample dissolutionthe process of ob

46、taining a solu-tion containing the analyte(s) of interest from a sample. Thismay or may not involve complete dissolution of the sample.D 67853.2.39 sample preparationall operations carried out on asample, after transportation and storage, to prepare it foranalysis, including transformation of the sa

47、mple into a mea-surable state, where necessary. D 67853.2.40 sampling device; samplerfor purposes of this stan-dard, a device for collecting airborne particles.3.2.40.1 DiscussionDevices used to collect airborne par-ticles are often referred to by a number of other terms, such assampling heads, filt

48、er holders, filter cassettes, and so forth.3.2.41 sampling locationa specific area within a samplingsite that is subjected to sample collection. E 17283.2.41.1 DiscussionMultiple sampling locations are com-monly designated for a single sampling site.3.2.42 sampling sitea local geographic area that c

49、ontainsthe sampling locations. E 17283.2.42.1 DiscussionAsampling site is generally limited toan area that is easily covered by walking.3.2.43 secondary standardan acceptable reference sampleor device used for establishing measurement of a physicalquantity, used as a means of comparison, but checked againsta primary standard. D 50113.2.44 spectral interferencean interference caused by theemission from a species other than the analyte of interest.ISO 152023.2.45 spray chambera device placed between a nebulizerand a