1、Designation: D7439 08D7439 14Standard Test Method forDetermination of Elements in Airborne Particulate Matter byInductively Coupled PlasmaMass Spectrometry1This standard is issued under the fixed designation D7439; the number immediately following the designation indicates the year oforiginal adopti
2、on 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 standard test method specifies a procedure for sample preparation and
3、 analysis of airborne particulate matter for thecontent of metals and metalloids in workplace air samples using inductively coupled plasmamass spectrometry (ICP-MS). Thistest method can be used for other air samples provided the user ensures the validity of the test method (by ensuring that appropri
4、atedata quality objectives can be achieved).1.2 This standard test method assumes that samples will have been collected in accordance with Test Method D7035.1.3 This standard test method should be used by analysts experienced in the use of ICP-MS, the interpretation of spectral andmatrix interferenc
5、es and procedures for their correction.1.4 This standard test method specifies a number of alternative methods for preparing test solutions from samples of airborneparticulate matter. One of the specified sample preparation methods is applicable to the measurement of soluble metal or metalloidcompou
6、nds. Other specified methods are applicable to the measurement of total metals and metalloids.1.5 It is the users responsibility to ensure the validity of the standard method for filters of untested matrices.1.6 Table 1 provides a non-exclusive list of metals and metalloids for which one or more of
7、the sample dissolution methodsspecified in this document is applicable.1.7 This standard test method is not applicable to compounds of metals and metalloids that are present in the gaseous or vaporstate.1.8 No detailed operating instructions are provided because of differences among various makes an
8、d models of suitable ICP-MSinstruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This testmethod does not address comparative accuracy of different devices or the precision between instruments of the same make andmodel.1.9 The valu
9、es stated in SI units are to be regarded as standard.1.10 This standard test method contains notes that are explanatory and are not part of the mandatory requirements of the method.1.11 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the r
10、esponsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1356 Terminology Relating to Sampling and Analysis of
11、AtmospheresD4185 Practice for Measurement of Metals in Workplace Atmospheres by Flame Atomic Absorption SpectrophotometryD4840 Guide for Sample Chain-of-Custody ProceduresD5011 Practices for Calibration of Ozone Monitors Using Transfer Standards1 This test method is under the jurisdiction of ASTM Co
12、mmittee D22 on Air Quality and is the direct responsibility of Subcommittee D22.04 on Workplace Air Quality.Current edition approved April 1, 2008Jan. 15, 2014. Published May 2008May 2014. Originally approved in 2008. Last previous edition approved in 2008 as D7439 - 08.DOI: 10.1520/D7439-08.10.1520
13、/D7439-14.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intend
14、ed only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current
15、 versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D6785 Test Method for Determination of Lead in Workplace Air Using Flame or Graphite Furnace Atomic
16、 AbsorptionSpectrometryD7035 Test Method for Determination of Metals and Metalloids in Airborne Particulate Matter by Inductively Coupled PlasmaAtomic Emission Spectrometry (ICP-AES)D7202 Test Method for Determination of Beryllium in the Workplace by Extraction and Optical Fluorescence DetectionD744
17、0 Practice for Characterizing Uncertainty in Air Quality MeasurementsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE882 Guide for Accountability and Quality Control in the Chemical Analysis LaboratoryE1613 Test Method for Determination of Lead by In
18、ductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES),FlameAtomicAbsorption Spectrometry (FAAS), or Graphite FurnaceAtomicAbsorption Spectrometry (GFAAS) Techniques2.2 ISO and European Standards:ISO 1042 Laboratory GlasswareOne-Mark Volumetric Flasks3ISO 3585 Borosilicate Glass 3.3Properti
19、es3ISO 8655 Piston-Operated Volumetric Apparatus (6 parts)3ISO 15202 Workplace AirDetermination of Metals and Metalloids in Airborne Particulate Matter by Inductively CoupledPlasma Atomic Emission Spectrometry (3 parts)3ISO 17294 Water QualityApplication of Inductively Coupled Plasma Mass Spectromet
20、ry (ICP-MS) (2 parts)3EN 1540 Workplace AtmospheresTerminology33. Terminology3.1 DefinitionsFor definitions of other terms used in this standard test method, refer to Terminology D1356.3.2 Definitions of Terms Specific to This Standard:3.2.1 analytical recoveryratio of the mass of analyte measured t
21、o the known mass of analyte in the sample, expressed as apercentage. D67853.2.2 batcha group of field or quality control (QC) samples that are collected or processed together at the same time usingthe same reagents and equipment. E16133.2.3 blank solutionsolution prepared by taking a reagent blank,
22、laboratory blank or field blank through the same procedureused for sample dissolution. ISO 152023.2.3.1 DiscussionA blank solution may need to be subjected to further operations, such as addition of an internal standard, if the sample solutionsare subjected to such operations in order to produce tes
23、t solutions that are ready for analysis.3.2.4 calibration blank solutioncalibration solution prepared without the addition of any stock standard solution or workingstandard solution. ISO 152023.2.4.1 Discussion3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor,
24、New York, NY 10036, http:/www.ansi.org.TABLE 1 Applicable Metals and MetalloidsElement Symbol CASRNA Element Symbol CASRNA Element 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
25、7440-43-9 Calcium Ca 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 GermaniumB Ge 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 Mer
26、curyB Hg 7439-97-6 Molybdenum Mo 7439-98-7Nickel Ni 7440-02-0 NiobiumB Nb 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 7440-31-5Tungste
27、n W 7440-33-7 Uranium U 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 NumberB For the elements in italics, there is insufficient information available on the effectiveness of the sample dissolution procedures in
28、 Annex A1 through Annex A4.D7439 142The concentration of the analyte(s) of interest in the calibration blank solution is taken to be zero.3.2.5 calibration curvea plot of instrument response versus concentration of standards (1).43.2.6 calibration solutionsolution prepared by dilution of the stock s
29、tandard solution(s) or working standard solution(s),containing the analyte(s) of interest at a concentration(s) suitable for use in calibration of the analytical instrument. ISO 152023.2.6.1 DiscussionThe technique of matrix matching is normally used when preparing calibration solutions.3.2.7 chemic
30、al 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 waste, by any work activity, whether or not produced intentionally and whetheror not placed on the market. EN 1540/ISO 152023.2.8 collision/reaction
31、systemany system, such as a transmission collision cell, to which an oscillating radio frequencypotential is applied that is used for charge exchange neutralization of interfering ions in inductively coupled plasma massspectrometry (2).3.2.8.1 DiscussionSome collision systems also have one or more r
32、eaction modes that can further reduce selected interferences.3.2.9 continuing calibration blank (CCB)a solution containing no analyte added, that is used to verify blank response andfreedom from carryover. E16133.2.9.1 DiscussionThe CCB must be analyzed after the CCV (see 3.2.10). The measured conce
33、ntration of the CCB should not exceed 10 % of theapplicable occupational exposure limit or minimum level of concern.3.2.10 continuing calibration verification (CCV)a solution (or set of solutions) of known analyte concentration used to verifyfreedom from excessive instrumental drift; the concentrati
34、on is to be near the mid-range of a linear calibration curve. E16133.2.10.1 DiscussionThe CCV must be matrix matched to the acid content present in sample digestates or extracts. The CCV must be analyzed beforeand after all samples and at a frequency of not less than every ten samples. The measured
35、value is to fall within 610 % of theknown value.3.2.11 field blanksampling media (for example, an air filter) that is taken through the same handling procedure as a sample,except that no sample is collected (that is, no air is purposely drawn through the sampler), and is then returned to the laborat
36、oryfor analysis. ISO 15202/D70353.2.11.1 DiscussionAnalysis results from field blanks provide information on the analyte background level in the sampling media, combined with thepotential contamination experienced by samples collected within the batch resulting from handling.3.2.12 inductively coupl
37、ed plasma (ICP)a high-temperature discharge generated by a flowing conductive gas, normally argon,through a magnetic field induced by a load coil that surrounds the tubes carrying the gas. ISO 152023.2.13 inductively coupled plasma (ICP) torcha device used to support and introduce sample into an ICP
38、 discharge.ISO 152023.2.14 initial calibration blank (ICB)a standard containing no analyte that is used for the initial calibration. E16133.2.14.1 DiscussionThe ICB must be matrix matched to the acid content of sample extracts and digestates. The ICB must be measured during and aftercalibration. The
39、 measured concentration of the ICB should not exceed 10 % of the applicable occupational exposure limit orminimum level of concern.4 The boldface numbers in parentheses refer to the list of references at the end of this standard.D7439 1433.2.15 initial calibration verification (ICV)a solution (or se
40、t of solutions) of known analyte concentration used to verifycalibration standard levels; the concentration of analyte is to be near the mid-range of the calibration curve that is made from astock solution having a different manufacturer or manufacturer lot identification than the calibration standa
41、rds. E16133.2.15.1 DiscussionThe ICV must be matrix matched to the acid content of sample extracts or digestates. The ICV must be measured after calibrationand before measuring any sample digestates or extracts. The measured value is to fall within 610 % of the known value.3.2.16 injector tubethe in
42、nermost tube of an inductively coupled plasma torch, usually made of quartz or ceramic materials,through which the sample aerosol is introduced to the plasma. ISO 152023.2.17 inner (nebulizer) argon flowthe flow of argon gas that is directed through the nebulizer and carries the sample aerosolthroug
43、h the injector and into the plasma; typically 0.5 L/min 2 L/min. ISO 152023.2.18 instrumental detection limit (IDL)the lowest concentration at which the instrumentation can distinguish analyte contentfrom the background generated by a minimal matrix. E16133.2.18.1 DiscussionThe IDL can be determined
44、 from blank, acidified, deionized, or ultrapure water as the matrix and from the same calculationmethods used to determine a method detection limit (see 3.2.253.2.28).3.2.19 instrumental QC standardsthese provide information on measurement performance during the instrumental analysisportion of the o
45、verall analyte measurement process. They include CCBs, CCVs, ICB, and ICVs. E16133.2.20 intermediate (auxiliary) argon flowthe flow of argon gas that is contained between the intermediate and center(injector) tubes of an inductively coupled plasma torch; typically 0.1 L/min 2 L/min. ISO 152023.2.21
46、internal standardnon-analyte element, present in all solutions analyzed, the signal from which is used to correct formatrix interferences or improve analytical precision. ISO 152023.2.21.1 DiscussionThe internal standard is added in known and constant amount(s) to all analyzed solutions. This is use
47、d to correct for instrumentdrift and some matrix effects by measuring the relative instrument response of the internal standard(s) to the other analytes thatare components of the same solution. The element(s) selected for use as an internal standard must be initially absent from thesample solution.3
48、.2.22 laboratory blankunused sample media (for example, an air filter), taken from the same batch used for sampling, thatdoes not leave the laboratory. ISO 152023.2.23 limit valuereference figure for concentration of a chemical agent in air. ISO 152023.2.23.1 DiscussionAn example of a limit value wo
49、uld be a Permissible Exposure Limit (PEL) such as those established by the U.S. OccupationalSafety and Health Administration.3.2.24 linear dynamic rangethe range of concentrations over which the calibration curve for an analyte is linear. It extendsfrom the detection limit to the onset of calibration curvature. ISO 152023.2.25 load coila length of metal tubing (typically copper) which is wound around the end of an inductively coupled plasmatorch and connected to the radio frequency generator. ISO 152023.2.26 matrix interferencein
