1、Designation: D 7439 08Standard Test Method forDetermination of Elements in Airborne Particulate Matter byInductively Coupled PlasmaMass Spectrometry1This standard is issued under the fixed designation D 7439; the number immediately following the designation indicates the year oforiginal adoption or,
2、 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 standard test method specifies a procedure forsample preparation and analy
3、sis of airborne particulate matterfor the content of metals and metalloids in workplace airsamples using inductively coupled plasmamass spectrometry(ICP-MS).1.2 This standard test method assumes that samples willhave been collected in accordance with Test Method D 7035.1.3 This standard test method
4、should be used by analystsexperienced in the use of ICP-MS, the interpretation of spectraland matrix interferences and procedures for their correction.1.4 This standard test method specifies a number of alter-native methods for preparing test solutions from samples ofairborne particulate matter. One
5、 of the specified sample prepa-ration methods is applicable to the measurement of solublemetal or metalloid compounds. Other specified methods areapplicable to the measurement of total metals and metalloids.1.5 It is the users responsibility to ensure the validity of thestandard method for filters o
6、f untested matrices.1.6 Table 1 provides a non-exclusive list of metals andmetalloids for which one or more of the sample dissolutionmethods specified in this document is applicable.1.7 This standard test method is not applicable to com-pounds of metals and metalloids that are present in the gaseous
7、or vapor state.1.8 No detailed operating instructions are provided becauseof differences among various makes and models of suitableICP-MS instruments. Instead, the analyst shall follow theinstructions provided by the manufacturer of the particularinstrument. This test method does not address compara
8、tiveaccuracy of different devices or the precision between instru-ments of the same make and model.1.9 The values stated in SI units are to be regarded asstandard.1.10 This standard test method contains notes that areexplanatory and are not part of the mandatory requirements ofthe method.1.11 This s
9、tandard 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 and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.
10、1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1356 Terminology Relating to Sampling and Analysis ofAtmospheresD 4185 Practice for Measurement of Metals in WorkplaceAtmospheres by Flame Atomic Absorption Spectropho-tometryD 6785 Test Method for Determination of Lead in Work-place Air Usin
11、g Flame or Graphite Furnace Atomic Ab-sorption SpectrometryD 7035 Test Method for Determination of Metals and Met-alloids in Airborne Particulate Matter by InductivelyCoupled Plasma Atomic Emission Spectrometry (ICP-AES)D 7202 Test Method for Determination of Beryllium in theWorkplace Using Field-Ba
12、sed Extraction and Fluores-cence DetectionE 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1613 Test Method for Determination of Lead by Induc-tively Coupled Plasma Atomic Emission Spectrometry(ICP-AES), Flame Atomic Absorption Spectrometry(FAAS), or Graphite Fu
13、rnace Atomic Absorption Spec-trometry (GFAAS) Techniques2.2 ISO and European Standards:ISO 1042 Laboratory GlasswareOne-Mark VolumetricFlasks3ISO 3585 Borosilicate Glass 3.3Properties3ISO 8655 Piston-Operated Volumetric Apparatus (6 parts)31This test method is under the jurisdiction of ASTM Committe
14、e D22 on AirQuality and is the direct responsibility of Subcommittee D22.04 on Workplace AirQuality.Current edition approved April 1, 2008. Published May 2008.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of
15、ASTMStandards 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Con
16、shohocken, PA 19428-2959, United States.ISO 15202 Workplace AirDetermination of Metals andMetalloids in Airborne Particulate Matter by InductivelyCoupled Plasma Atomic Emission Spectrometry (3 parts)3ISO 17294 Water QualityApplication of InductivelyCoupled Plasma Mass Spectrometry (ICP-MS) (2 parts)
17、3EN 1540 Workplace AtmospheresTerminology33. Terminology3.1 DefinitionsFor definitions of other terms used in thisstandard test method, refer to Terminology D 1356.3.2 Definitions of Terms Specific to This Standard:3.2.1 analytical recoveryratio of the mass of analytemeasured to the known mass of an
18、alyte in the sample,expressed as a percentage. D 67853.2.2 batcha group of field or quality control (QC)samples that are collected or processed together at the sametime using the same reagents and equipment. E 16133.2.3 blank solutionsolution prepared by taking a reagentblank, laboratory blank or fi
19、eld blank through the sameprocedure used for sample dissolution. ISO 152023.2.3.1 DiscussionA blank solution may need to be sub-jected to further operations, such as addition of an internalstandard, if the sample solutions are subjected to such opera-tions in order to produce test solutions that are
20、 ready foranalysis.3.2.4 calibration blank solutioncalibration solution pre-pared without the addition of any stock standard solution orworking standard solution. ISO 152023.2.4.1 DiscussionThe concentration of the analyte(s) ofinterest in the calibration blank solution is taken to be zero.3.2.5 cal
21、ibration curvea plot of instrument response ver-sus concentration of standards (1).43.2.6 calibration solutionsolution prepared by dilution ofthe stock standard solution(s) or working standard solution(s),containing the analyte(s) of interest at a concentration(s)suitable for use in calibration of t
22、he analytical instrument.ISO 152023.2.6.1 DiscussionThe technique of matrix matching isnormally used when preparing calibration solutions.3.2.7 chemical agentany chemical element or compound,on its own or admixed as it occurs in the natural state or asproduced, used or released including release as
23、waste, by anywork activity, whether or not produced intentionally andwhether or not placed on the market. EN 1540/ISO 152023.2.8 collision/reaction systemany system, such as atransmission collision cell, to which an oscillating radiofrequency potential is applied that is used for charge exchangeneut
24、ralization of interfering ions in inductively coupled plasmamass spectrometry (2).3.2.8.1 DiscussionSome collision systems also have oneor more reaction modes that can further reduce selectedinterferences.3.2.9 continuing calibration blank (CCB)a solution con-taining no analyte added, that is used t
25、o verify blank responseand freedom from carryover. E 16133.2.9.1 DiscussionThe CCB must be analyzed after theCCV (see 3.2.10). The measured concentration of the CCBshould not exceed 10 % of the applicable occupational expo-sure limit or minimum level of concern.3.2.10 continuing calibration verifica
26、tion (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 calibrationcurve. E 16133.2.10.1 DiscussionThe CCV must be matrix matched tothe acid content present in sampl
27、e 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.3.2.11 field blanksampling media (for example, an airfilter) that is taken through the same handling proce
28、dure as asample, except that no sample is collected (that is, no air ispurposely drawn through the sampler), and is then returned tothe laboratory for analysis. ISO 15202/D 70353.2.11.1 DiscussionAnalysis results from field blanksprovide information on the analyte background level in thesampling med
29、ia, combined with the potential contaminationexperienced by samples collected within the batch resultingfrom handling.3.2.12 inductively coupled plasma (ICP)a high-temperature discharge generated by a flowing conductive gas,4The boldface numbers in parentheses refer to the list of references at the
30、end ofthis standard.TABLE 1 Applicable Metals and MetalloidsElement Symbol CASRNAElement Symbol CASRNAElement Symbol CASRNAAluminum Al 7429-90-5 Antimony Sb 7440-36-0 Arsenic As 7440-38-2Barium Ba 7440-39-3 Beryllium Be 7440-41-7 Bismuth Bi 7440-69-9Boron B 7440-42-8 Cadmium Cd 7440-43-9 Calcium Ca
31、7440-70-2Cesium Cs 7440-46-2 Chromium Cr 7440-47-3 Cobalt Co 7440-48-4Copper Cu 7440-50-8 Gallium Ga 7440-55-3 GermaniumBGe 7440-56-4Hafnium Hf 7440-58-6 Indium In 7440-74-6 Iron Fe 7439-89-6Lead Pb 7439-92-1 Lithium Li 7439-93-2 Magnesium Mg 7439-95-4Manganese Mn 7439-96-5 MercuryBHg 7439-97-6 Moly
32、bdenum Mo 7439-98-7Nickel Ni 7440-02-0 NiobiumBNb 7440-03-1 Phosphorus P 7723-14-0Platinum Pt 7440-06-4 Potassium K 7440-09-7 Rhodium Rh 7440-16-6Selenium Se 7782-49-2 Silver Ag 7440-22-4 Sodium Na 7440-23-5Tellurium Te 13494-80-9 Thallium Tl 7440-28-0 Tin Sn 7440-31-5Tungsten W 7440-33-7 Uranium U
33、7440-61-1 Vanadium V 7440-62-2Yttrium Y 7440-65-5 Zinc Zn 7440-66-6 Zirconium Zr 7440-67-7ACASRN = Chemical Abstracts Service Registry NumberBFor the elements in italics, there is insufficient information available on the effectiveness of the sample dissolution procedures in Annex A1 through Annex A
34、4.D7439082normally 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 deviceused to support and introduce sample into an ICP discharge.ISO 152023.2.14 initial calibration blank (ICB)a standard conta
35、in-ing no analyte that is used for the initial calibration. E 16133.2.14.1 DiscussionThe ICB must be matrix matched tothe acid content of sample extracts and digestates. The ICBmust be measured during and after calibration. The measuredconcentration of the ICB should not exceed 10 % of theapplicable
36、 occupational exposure limit or minimum level ofconcern.3.2.15 initial calibration verification (ICV)a solution (orset of solutions) of known analyte concentration used to verifycalibration standard levels; the concentration of analyte is to benear the mid-range of the calibration curve that is made
37、 froma stock solution having a different manufacturer or manufac-turer lot identification than the calibration standards. E 16133.2.15.1 DiscussionThe ICV must be matrix matched tothe acid content of sample extracts or digestates. The ICV mustbe measured after calibration and before measuring any sa
38、mpledigestates or extracts. The measured value is to fall within610 % of the known value.3.2.16 instrumental detection limit (IDL)the lowest con-centration at which the instrumentation can distinguish analytecontent from the background generated by a minimal matrix.E 16133.2.16.1 DiscussionThe IDL c
39、an be determined fromblank, acidified, deionized, or ultrapure water as the matrix andfrom the same calculation methods used to determine a methoddetection limit (see 3.2.25).3.2.17 instrumental QC standardsthese provide informa-tion on measurement performance during the instrumentalanalysis portion
40、 of the overall analyte measurement process.They include CCBs, CCVs, ICB, and ICVs. E 16133.2.18 internal standardnon-analyte element, present inall solutions analyzed, the signal from which is used to correctfor matrix interferences or improve analytical precision.ISO 152023.2.18.1 DiscussionThe in
41、ternal standard is added inknown and constant amount(s) to all analyzed solutions. This isused to correct for instrument drift and some matrix effects bymeasuring the relative instrument response of the internalstandard(s) to the other analytes that are components of thesame solution. The element(s)
42、 selected for use as an internalstandard must be initially absent from the sample solution.3.2.19 laboratory blankunused sample media (for ex-ample, an air filter), taken from the same batch used forsampling, that does not leave the laboratory. ISO 152023.2.20 limit valuereference figure for concent
43、ration of achemical agent in air. ISO 152023.2.20.1 DiscussionAn example of a limit value would bea Permissible Exposure Limit (PEL) such as those establishedby the U.S. Occupational Safety and Health Administration.3.2.21 linear dynamic rangethe range of concentrationsover which the calibration cur
44、ve for an analyte is linear. Itextends from the detection limit to the onset of calibrationcurvature. ISO 152023.2.22 load coila length of metal tubing (typically cop-per) which is wound around the end of an inductively coupledplasma torch and connected to the radio frequency generator.ISO 152023.2.
45、23 matrix interferenceinterference of a non-spectralnature which is caused by the sample matrix. ISO 152023.2.24 matrix matchinga technique used to minimize theeffect of the test solution matrix on the analytical results.ISO 152023.2.24.1 DiscussionMatrix matching involves preparingcalibration solut
46、ions in which the concentrations of acids andother major solvents and solutes are matched with those in thetest solutions.3.2.25 method detection limit (MDL)the minimum con-centration of an analyte that can be reported with a 99 %confidence that the value is above zero. D 13563.2.25.1 DiscussionThe
47、MDL is also known as the limitof detection (LOD) (1).3.2.26 method quantitation limit (MQL)the minimumconcentration of an analyte that can be measured with accept-able precision. D 70353.2.26.1 DiscussionThe MQL is also known as the limitof quantitation (1).3.2.27 nebulizera device used to create an
48、 aerosol from aliquid. ISO 152023.2.28 reagent blanksolution containing all reagents usedin sample dissolution, in the same quantities used for prepara-tion of blank and sample solutions. ISO 152023.2.28.1 DiscussionThe reagent blank is used to assesscontamination from the laboratory environment and
49、 to charac-terize spectral background from the reagents used in samplepreparation.3.2.29 sample dissolutionthe process of obtaining a solu-tion containing the analyte(s) of interest from a sample. Thismay or may not involve complete dissolution of the sample.D 6785/ISO 152023.2.30 sample preparationall operations carried out on asample after transportation and storage to prepare it foranalysis, including transformation of the sample into a mea-surable state, where necessary. ISO 152023.2.31 sample solutionsolution prepared from a
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