ASTM D7439-08
(Test Method)Standard Test Method for Determination of Elements in Airborne Particulate Matter by Inductively Coupled Plasma–Mass Spectrometry
Standard Test Method for Determination of Elements in Airborne Particulate Matter by Inductively Coupled Plasma<span class='unicode'>–</span>Mass Spectrometry
SIGNIFICANCE AND USE
The health of workers in many industries is at risk through exposure by inhalation to toxic metals and metalloids. Industrial hygienists and other public health professionals need to determine the effectiveness of measures taken to control workplace exposure. This is generally achieved by making workplace air measurements. This test method has been developed to make available a standard methodology for valid exposure measurements for a wide range of metals and metalloids that are used in industry. It will be of benefit to agencies concerned with health and safety at work; analytical laboratories; industrial hygienists and other public health professionals; industrial users of metals and metalloids and their workers; and other groups.
This standard test method specifies a generic method for determination of the concentration of metals and metalloids in workplace air samples using ICP-MS. For many metals and metalloids, analysis by ICP-MS may be advantageous, when compared to methods such as ICP atomic emission spectrometry, due to its sensitivity and the presence of fewer spectral interferences.
The analysis results can be used for the assessment of workplace exposures to metals and metalloids in workplace air.
SCOPE
1.1 This standard test method specifies a procedure for sample preparation and analysis of airborne particulate matter for the content of metals and metalloids in workplace air samples using inductively coupled plasma–mass spectrometry (ICP-MS).
1.2 This standard test method assumes that samples will have been collected in accordance with Test Method D 7035.
1.3 This standard test method should be used by analysts experienced in the use of ICP-MS, the interpretation of spectral and matrix interferences and procedures for their correction.
1.4 This standard test method specifies a number of alternative methods for preparing test solutions from samples of airborne particulate matter. One of the specified sample preparation methods is applicable to the measurement of soluble metal or metalloid compounds. Other specified methods are applicable to the measurement of total metals and metalloids.
1.5 It is the user's 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 the sample dissolution methods specified 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 vapor state.
1.8 No detailed operating instructions are provided because of differences among various makes and models of suitable ICP-MS instruments. Instead, the analyst shall follow the instructions provided by the manufacturer of the particular instrument. This test method does not address comparative accuracy of different devices or the precision between instruments of the same make and model.
1.9 The values 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 responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D7439 − 08
StandardTest Method for
Determination of Elements in Airborne Particulate Matter by
Inductively Coupled Plasma–Mass Spectrometry
This standard is issued under the fixed designation D7439; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.9 The values stated in SI units are to be regarded as
standard.
1.1 This standard test method specifies a procedure for
sample preparation and analysis of airborne particulate matter 1.10 This standard test method contains notes that are
for the content of metals and metalloids in workplace air explanatory and are not part of the mandatory requirements of
samples using inductively coupled plasma–mass spectrometry the method.
(ICP-MS).
1.11 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.2 This standard test method assumes that samples will
responsibility of the user of this standard to establish appro-
have been collected in accordance with Test Method D7035.
priate safety and health practices and determine the applica-
1.3 This standard test method should be used by analysts
bility of regulatory limitations prior to use.
experiencedintheuseofICP-MS,theinterpretationofspectral
and matrix interferences and procedures for their correction.
2. Referenced Documents
1.4 This standard test method specifies a number of alter-
2.1 ASTM Standards:
native methods for preparing test solutions from samples of
D1193Specification for Reagent Water
airborne particulate matter. One of the specified sample prepa-
D1356Terminology Relating to Sampling and Analysis of
ration methods is applicable to the measurement of soluble
Atmospheres
metal or metalloid compounds. Other specified methods are
D4185Practice for Measurement of Metals in Workplace
applicable to the measurement of total metals and metalloids.
Atmospheres by Flame Atomic Absorption Spectropho-
1.5 Itistheuser’sresponsibilitytoensurethevalidityofthe
tometry
standard method for filters of untested matrices.
D6785TestMethodforDeterminationofLeadinWorkplace
Air Using Flame or Graphite FurnaceAtomicAbsorption
1.6 Table 1 provides a non-exclusive list of metals and
Spectrometry
metalloids for which one or more of the sample dissolution
D7035Test Method for Determination of Metals and Met-
methods specified in this document is applicable.
alloids in Airborne Particulate Matter by Inductively
1.7 This standard test method is not applicable to com-
Coupled Plasma Atomic Emission Spectrometry (ICP-
poundsofmetalsandmetalloidsthatarepresentinthegaseous
AES)
or vapor state.
D7202Test Method for Determination of Beryllium in the
1.8 No detailed operating instructions are provided because
Workplace Using Field-Based Extraction and Optical
of differences among various makes and models of suitable
Fluorescence Detection
ICP-MS instruments. Instead, the analyst shall follow the
E882Guide for Accountability and Quality Control in the
instructions provided by the manufacturer of the particular
Chemical Analysis Laboratory
instrument. This test method does not address comparative
E1613Test Method for Determination of Lead by Induc-
accuracy of different devices or the precision between instru-
tively Coupled Plasma Atomic Emission Spectrometry
ments of the same make and model.
(ICP-AES), Flame Atomic Absorption Spectrometry
This test method is under the jurisdiction of ASTM Committee D22 on Air
Quality and is the direct responsibility of Subcommittee D22.04 on WorkplaceAir For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Quality. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved April 1, 2008. Published May 2008. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D7439-08. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7439 − 08
TABLE 1 Applicable Metals and Metalloids
A A A
Element Symbol CASRN Element Symbol CASRN Element Symbol CASRN
Aluminum Al 7429-90-5 Antimony Sb 7440-36-0 Arsenic As 7440-38-2
Barium Ba 7440-39-3 Beryllium Be 7440-41-7 Bismuth Bi 7440-69-9
Boron B 7440-42-8 Cadmium Cd 7440-43-9 Calcium Ca 7440-70-2
Cesium Cs 7440-46-2 Chromium Cr 7440-47-3 Cobalt Co 7440-48-4
B
Copper Cu 7440-50-8 Gallium Ga 7440-55-3 Germanium Ge 7440-56-4
Hafnium Hf 7440-58-6 Indium In 7440-74-6 Iron Fe 7439-89-6
Lead Pb 7439-92-1 Lithium Li 7439-93-2 Magnesium Mg 7439-95-4
B
Manganese Mn 7439-96-5 Mercury Hg 7439-97-6 Molybdenum Mo 7439-98-7
B
Nickel Ni 7440-02-0 Niobium Nb 7440-03-1 Phosphorus P 7723-14-0
Platinum Pt 7440-06-4 Potassium K 7440-09-7 Rhodium Rh 7440-16-6
Selenium Se 7782-49-2 Silver Ag 7440-22-4 Sodium Na 7440-23-5
Tellurium Te 13494-80-9 Thallium Tl 7440-28-0 Tin Sn 7440-31-5
Tungsten W 7440-33-7 Uranium U 7440-61-1 Vanadium V 7440-62-2
Yttrium Y 7440-65-5 Zinc Zn 7440-66-6 Zirconium Zr 7440-67-7
A
CASRN = Chemical Abstracts Service Registry Number
B
For the elements in italics, there is insufficient information available on the effectiveness of the sample dissolution procedures in Annex A1 through Annex A4.
(FAAS), or Graphite Furnace Atomic Absorption Spec- 3.2.5 calibration curve—a plot of instrument response ver-
trometry (GFAAS) Techniques sus concentration of standards (1).
2.2 ISO and European Standards:
3.2.6 calibration solution—solution prepared by dilution of
ISO 1042Laboratory Glassware—One-Mark Volumetric
the stock standard solution(s) or working standard solution(s),
Flasks
containing the analyte(s) of interest at a concentration(s)
ISO 3585Borosilicate Glass 3.3—Properties
suitable for use in calibration of the analytical instrument.
ISO 8655Piston-Operated Volumetric Apparatus (6 parts)
ISO 15202
ISO 15202Workplace Air—Determination of Metals and
3.2.6.1 Discussion—The technique of matrix matching is
Metalloids in Airborne Particulate Matter by Inductively
normally used when preparing calibration solutions.
CoupledPlasmaAtomicEmissionSpectrometry(3parts)
3.2.7 chemical agent—any chemical element or compound,
ISO 17294 Water Quality—Application of Inductively
on its own or admixed as it occurs in the natural state or as
Coupled Plasma Mass Spectrometry (ICP-MS) (2 parts)
produced, used or released including release as waste, by any
EN 1540Workplace Atmospheres—Terminology
work activity, whether or not produced intentionally and
whether or not placed on the market. EN 1540/ISO 15202
3. Terminology
3.2.8 collision/reactionsystem—anysystem,suchasatrans-
3.1 Definitions—For definitions of other terms used in this
mission collision cell, to which an oscillating radio frequency
standard test method, refer to Terminology D1356.
potential is applied that is used for charge exchange neutral-
3.2 Definitions of Terms Specific to This Standard:
ization of interfering ions in inductively coupled plasma mass
3.2.1 analytical recovery—ratio of the mass of analyte
spectrometry (2).
measured to the known mass of analyte in the sample,
3.2.8.1 Discussion—Some collision systems also have one
expressed as a percentage. D6785
or more reaction modes that can further reduce selected
interferences.
3.2.2 batch—a group of field or quality control (QC)
samples that are collected or processed together at the same
3.2.9 continuing calibration blank (CCB)—a solution con-
time using the same reagents and equipment. E1613
taining no analyte added, that is used to verify blank response
and freedom from carryover. E1613
3.2.3 blank solution—solution prepared by taking a reagent
3.2.9.1 Discussion—The CCB must be analyzed after the
blank, laboratory blank or field blank through the same
CCV (see 3.2.10). The measured concentration of the CCB
procedure used for sample dissolution. ISO 15202
3.2.3.1 Discussion—A blank solution may need to be sub- should not exceed 10% of the applicable occupational expo-
sure limit or minimum level of concern.
jected to further operations, such as addition of an internal
standard, if the sample solutions are subjected to such opera-
3.2.10 continuing calibration verification (CCV)—a solu-
tions in order to produce test solutions that are ready for
tion (or set of solutions) of known analyte concentration used
analysis.
to verify freedom from excessive instrumental drift; the con-
centration is to be near the mid-range of a linear calibration
3.2.4 calibration blank solution—calibration solution pre-
pared without the addition of any stock standard solution or curve. E1613
3.2.10.1 Discussion—The CCV must be matrix matched to
working standard solution. ISO 15202
3.2.4.1 Discussion—The concentration of the analyte(s) of the acid content present in sample digestates or extracts. The
CCV must be analyzed before and after all samples and at a
interest in the calibration blank solution is taken to be zero.
3 4
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St., Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
4th Floor, New York, NY 10036, http://www.ansi.org. this standard.
D7439 − 08
frequency of not less than every ten samples. The measured used to correct for instrument drift and some matrix effects by
value is to fall within 610% of the known value. measuring the relative instrument response of the internal
standard(s) to the other analytes that are components of the
3.2.11 field blank—sampling media (for example, an air
same solution. The element(s) selected for use as an internal
filter) that is taken through the same handling procedure as a
standard must be initially absent from the sample solution.
sample, except that no sample is collected (that is, no air is
purposely drawn through the sampler), and is then returned to 3.2.19 laboratory blank—unused sample media (for
the laboratory for analysis. ISO 15202/D7035 example, an air filter), taken from the same batch used for
sampling, that does not leave the laboratory. ISO 15202
3.2.11.1 Discussion—Analysisresultsfromfieldblankspro-
vide information on the analyte background level in the
3.2.20 limit value—reference figure for concentration of a
sampling media, combined with the potential contamination
chemical agent in air. ISO 15202
experienced by samples collected within the batch resulting
3.2.20.1 Discussion—An example of a limit value would be
from handling.
a Permissible Exposure Limit (PEL) such as those established
by the U.S. Occupational Safety and Health Administration.
3.2.12 inductively coupled plasma (ICP)—a high-
temperature discharge generated by a flowing conductive gas,
3.2.21 linear dynamic range—the range of concentrations
normallyargon,throughamagneticfieldinducedbyaloadcoil
over which the calibration curve for an analyte is linear. It
that surrounds the tubes carrying the gas. ISO 15202
extends from the detection limit to the onset of calibration
3.2.13 inductively coupled plasma (ICP) torch—a device curvature. ISO 15202
used to support and introduce sample into an ICP discharge.
3.2.22 load coil—alengthofmetaltubing(typicallycopper)
ISO 15202
which is wound around the end of an inductively coupled
plasma torch and connected to the radio frequency generator.
3.2.14 initial calibration blank (ICB)—a standard contain-
ISO 15202
ing no analyte that is used for the initial calibration. E1613
3.2.14.1 Discussion—The ICB must be matrix matched to
3.2.23 matrix interference—interference of a non-spectral
the acid content of sample extracts and digestates. The ICB
nature which is caused by the sample matrix. ISO 15202
must be measured during and after calibration. The measured
3.2.24 matrix matching—a technique used to minimize the
concentration of the ICB should not exceed 10% of the
effect of the test solution matrix on the analytical results.
applicable occupational exposure limit or minimum level of
ISO 15202
concern.
3.2.24.1 Discussion—Matrix matching involves preparing
3.2.15 initial calibration verification (ICV)—a solution (or
calibration solutions in which the concentrations of acids and
set of solutions) of known analyte concentration used to verify
other major solvents and solutes are matched with those in the
calibrationstandardlevels;theconcentrationofanalyteistobe
test solutions.
near the mid-range of the calibration curve that is made from
3.2.25 method detection limit (MDL)—the minimum con-
a stock solution having a different manufacturer or manufac-
centration of an analyte that can be reported with a 99%
turer lot identification than the calibration standards. E1613
confidence that the value is above zero. D1356
3.2.15.1 Discussion—The ICV must be matrix matched to
3.2.25.1 Discussion—The MDL is also known as the limit
theacidcontentofsampleextractsordigestates.TheICVmust
of detection (LOD) (1).
bemeasuredaftercalibrationandbeforemeasuringanysample
3.2.26 method quantitation limit (MQL)—the minimum
digestates or extracts. The measured value is to fall within
concentration of an analyte that can be measured with accept-
610% of the known value.
able precision. D7035
3.2.16 instrumental detection limit (IDL)—the lowest con-
3.2.26.1 Discussion—The MQL is also known as the limit
centration at which the instrumentation can distinguish analyte
of quantitation (1).
content from the background generated by a minimal matrix.
3.2.27 nebulizer—a device used to create an aerosol from a
E1613
liquid. ISO 15202
3.2.16.1 Discussion—The IDL can be determined from
blank,acidified,deionized,orultrapurewaterasthematrixand
3.2.28 reagent blank—solution containing all reagents used
fromthesamecalculationmethodsusedtodetermineamethod in sample dissolution, in the same quantities used for prepara-
detection limit (see 3.2.25).
tion of blank and sample solutions. ISO 15202
3.2.28.1 Discussion—The reagent blank is used to assess
3.2.17 instrumental QC standards—these provide informa-
contamination from the laboratory environment and to charac-
tion on measurement performance during the instrumental
terize spectral background from the reagents used in sample
analysis portion of the overall analyte measurement process.
preparation.
They include CCBs, CCVs, ICB, and ICVs. E1613
3.2.29 sample dissolution—the process of obtaining a solu-
3.2.18 internal standard—non-analyte element, present in
tion containing the analyte(s) of interest from a sample. This
all solutions analyzed, the signal from which is used to correct
may or may not involve complete dissolution of the sample.
for matrix interferences or improve
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