National Institute of Standards & Technology

Certificate of Analysis
Standard Reference Material® 2783
Air Particulate on Filter Media
This Standard Reference Material (SRM) is an air particulate sample reduced in particle size to simulate PM2.5 air
particulate matter (particles with an aerodynamic equivalent diameter of 2.5 µm) and deposited on a polycarbonate
filter membrane. It is primarily intended for use in the evaluation and calibration of methods of analysis for
common and toxic elements contained in various fractions of airborne particulate matter collected on filter media.
A unit of SRM 2783 includes two loaded filters and two blank filters.

Certified Values: The certified values for elemental content of the SRM, expressed as mass of element deposited
on the filter membrane, are provided in Table 1. A NIST certified value is a value for which NIST has the highest
confidence in its accuracy in that all known or suspected sources of bias have been investigated or taken into
account [1]. The certified values for all elements are based on results of NIST methods and results from
collaborating laboratories using independent and complementary analytical methods.

Reference Values: The reference values for elemental content, expressed as mass of element deposited on the filter
membrane, are provided in Table 2. Reference values for selected elements in blank filters are provide in Table 4.
Reference values are noncertified values that are the best estimate of the true value; however, the values do not meet
the NIST criteria for certification and are provided with associated uncertainties that may reflect only measurement
precision, may not include all sources of uncertainty, or may reflect a lack of sufficient statistical agreement among
multiple analytical methods [1].

Information Values: Supplementary information values for average deposit area and mass loading per loaded
filter are provided in Table 3. Information values for blank filters are provided in Table 5. An information value is
considered to be a value that will be of use to the SRM user, but insufficient information is available to assess the
uncertainty associated with the value.

Expiration of Certification: The certification of SRM 2783 is valid, within the measurement uncertainty
specified, until 01 September 2021, provided the SRM is handled and stored in accordance with the instructions
given in this certificate (see “Instructions for Handling, Storage, and Use”). This certification is nullified if the
SRM is damaged, contaminated, or otherwise modified.

Maintenance of SRM Certification: NIST will monitor this SRM over the period of its certification. If
substantive technical changes occur that affect the certification before the expiration of this certificate, NIST will
notify the purchaser. Registration (see attached sheet) will facilitate notification.

This SRM has been developed in cooperation with the International Atomic Energy Agency (IAEA) Laboratories,
Seibersdorf, Austria and collaborating laboratories in several countries.

The material was prepared by R. Oflaz and R.L. Zeisler of the NIST Analytical Chemistry Division. The
coordination of the technical measurements leading to certification was performed by R.L. Zeisler.

Stephen A. Wise, Chief

Analytical Chemistry Division

Gaithersburg, MD 20899 Robert L. Watters, Jr. Chief

Certificate Issue Date: 13 December 2011 Measurement Services Division
Certificate Revision History on Last Page

SRM 2783 Page 1 of 6

Analytical measurements at NIST were performed by R. Oflaz, M.E. Howard, A.P. Lindstrom, K.E. Murphy,
J.R. Sieber, L.J. Wood, L.L. Yu, R.L. Zeisler of the NIST Analytical Chemistry Division.

Results were also provided by analysts at other collaborating laboratories: M. Bogovac, A. Mendoza,
A. Markowicz at IAEA Laboratories Seibersdorf, Austria; I. Orlic at ANSTO, Australia; W. Maenhaut at Ghent
University, Belgium; P. Artaxo at University of São Paulo, Brazil; M. Jakšiç at Rudjer Boškoviç Institute; Croatia;
J. Kučera at Nuclear Physics Institute, Czech Republic; M. Gallorini; E. Rizzio at University of Pavia; Italy;
J. Weinstein at U.S. EPA, Research Triangle Park, NC, USA.

Statistical analyses leading to certified and reference values were performed by S.D. Leigh of the NIST Statistical
Engineering Division.

Support aspects involved in the issuance of this SRM were coordinated through the NIST Measurement Services
Division.

INSTRUCTIONS FOR HANDLING, STORAGE, AND USE(1)

Handling: Please note that no fixation or surface coating was used on the filters, therefore they should be handled
with care to avoid material loss or contamination. The filter membranes are mounted in Millipore PetriSlide
containers (Figure 1). These containers are holding the filter membranes in place by means of a plastic ring inside
the lid. To remove the filter from the container, grasp the lid with the thumb and finger of one hand at the grip,
while holding the slide, i.e., bottom portion of the casing, with the other hand. The lid is then opened with a slight
twisting upward motion. Users are cautioned to use care when opening the container because electrostatic
charges may cause the filter membrane to move. The filter membrane can be picked up at the notched side of the
casing with round-tipped (blunt) forceps.

Storage: The material should be kept in its original container and stored at temperatures less than 30 °C and away
from sources of light.

Use: The filters should be used as received; the surface with the deposit shall NOT be touched or brought into
contact with implements. Filters can be used for multiple non-destructive assays; the filter membranes should be
stored in the Millipore PetriSlide containers after use; the deposit (shiny) side of the filter must face upward. If a
filter is partitioned for analysis or not analyzed in whole due to the analytical technique used, a minimum sample
area of 1 cm2 should be used for analytical determinations to be related to elemental mass loading values provided.
The value of the total deposit area should be determined for the filter being measured because the deposited area is
smaller than the filter area. The deposited area can be determined directly, or the information value for average
deposited area in Table 3 may be used.

Blanks: Blank filters are supplied to augment the assays of the aerosol loaded filters with the determination of
analytical blanks associated with the filter matrix. A heterogeneous distribution of bromine in the filter lots
prevented a value assignment for this element. A significant amount of chromium and nickel is found by techniques
that assay the whole filter, i.e., matrix and aerosol loading together, such as instrumental neutron activation
analysis (INAA). Reference and information values established for several elements are listed in Table 4 and
Table 5.

PREPARATION, HOMOGENEITY, AND ANALYSIS

Source and Preparation of Material: The aerosol material deposited on the filters is intended to represent a
material of PM2.5 particle size distribution with elemental concentrations typical of those of an urban industrial area.
A special collection of PM2.5 material for this project from an EPA national monitoring site in Baltimore, MD, had
yielded sufficient contemporary material [2], however controlled deposit on filter membranes was not achievable
because of variable retention of ultra-fine particles. Therefore an earlier prepared and successfully tested batch of
urban particulate matter [3] was used. This urban dust was collected by the IAEA Laboratories from the air intake
system of the Vienna General Hospital (AKH), in Vienna, Austria. The hospital is located in a mixed industrial
urban area, with several nearby major highways. The dust was collected with vacuum cleaners from the
electrostatic filters of the hospital air intake ducts. Approximately 9 kg of material was collected in three batches
over the period September 1994 to December 1995. The batches of material were combined and sieved to particle
sizes below 70 µm to eliminate coarse materials. The sieved sample was homogenized with a V-shaped blender for

(1)
Certain commercial equipment, instruments or materials are identified in this certificate to adequately specify the
experimental procedure. Such identification does not imply recommendation or endorsement by the National Institute of
Standards and Technology, nor does it imply that the materials or equipment identified are necessarily the best available for the
purpose.
SRM 2783 Page 2 of 6
4 h. A portion of this material was then successively air-jet milled three times to obtain a more homogeneous
distribution of smaller particles that simulates the respirable fractions of an urban aerosol. The material has a
median particle size of 3.2 µm and a size range (full width at half maximum) of 2.5 µm. The air-jet milled material
was designated IAEA-396a/m. Small sample analysis studies have demonstrated a high degree of homogeneity for
this material [4].

All preparation for the deposit on the filter membranes and handling of the filters was carried out in the NIST
Specimen Bank clean room. Batches of 700 mL to 900 mL each of air particulate matter suspensions were prepared
by weighing appropriate portions of bulk air particulate matter into 1 L Erlenmeyer flasks, adding the appropriate
mass of pure water containing a mass fraction of 0.1 % Triton X-100, and placing the flask in an ultra-sonicating
bath. A 140 µg/mL starting ratio yielded a 100 µg/mL particulate suspension for deposit after 1 h of
ultra-sonication, followed by 15 h equilibration and an additional 1 h of ultra-sonication. During the subsequent
dispension, the particulate was kept in suspension by vigorous stirring. Each of these batches was prepared for one
day of filter preparation (about 150 filters each); a total of 15 batches were prepared yielding 2200 individual filters.

Two Millipore filtration units were used for the preparation. The filters were Nuclepore polycarbonate membrane
filters, 0.4 µm pore size (Corning, Lots 8265024 and 8265025). After mounting the filters into the filtration
assembly, the filters were covered with about 40 mL of pure water, then 5 mL aliquots of the suspension were
pipetted on top with a 5 mL adjustable pipette. Because two staff members were preparing the SRM filters, the
pipettes were calibrated to deliver the same volume by mass. This calibration was controlled before and during the
preparation of each SRM batch. After dispension into the filtration apparatus, vacuum was applied and the aerosol
matter was deposited on the filters. After filtering to dryness, the filters were removed from the filtration apparatus
and allowed to air dry under Class 10 clean air flow.

Homogeneity: The average mass loadings and homogeneity of the deposition procedure for the lot was determined
by gravimetry using ten preweighed filters per batch and weighing the prepared filters after drying and conditioning.
The pooled relative standard deviation of this procedure was 5.5 %. Considering the difficulties of these mass
determinations, the loaded filters were accepted as a homogeneous lot. The homogeneity of elemental mass
loadings was determined by INAA on 30 filters, 2 from each batch selected at random. Twenty elements ranging
from several nanograms to tens of microgram amounts exhibited a relative standard deviation attributable to
heterogeneity of less than 2.5 %. The within-filter homogeneity was determined from micro-beam energy
dispersive x-ray fluorescence (EDXRF) and micro-beam proton-induced x-ray emission (PIXE) data.
Variances in elemental mass loading not exceeding 4 % relative standard deviation were observed for sampling
areas ranging from 1 mm2 to 30 mm2. A sampling area of 1 cm2 is deemed necessary for any certified value in
Table 1 to be valid within the stated uncertainty.

VALUE ASSIGNMENT
The analytical techniques used for measurement of each element are listed in Table 6.
Certified Values: Certified values are weighted means of results from two or more analytical methods [5]. The
uncertainty listed with each value is an expanded uncertainty, with coverage factor 2 (approximately 95 %
confidence), calculated by combining a between-source variance incorporating inter-method bias with a pooled
within-source variance, and a component of variance for material heterogeneity following the ISO Guide [6].

Table 1. Certified Mass Loading Values for Selected Elements

Elements ng(a) Elements ng(a)

Al 23210  530 Mg 8620  520

As 11.8  1.2 Mn 320  12
Ba 335  50 Na 1860  100
Ca 13200  1700 Ni 68  12
Co 7.7  1.2 Pb 317  54
Cr 135  25 Sb(b) 71.8  2.6
Cu 404  42 Ti 1490  240
Fe 26500  1600 V 48.5  6.0
K 5280  520 Zn 1790  130
(a)
Conversion to ng/cm2 must use area of deposit (not total filter membrane).
(b)
Expanded uncertainty calculated according to BOB, “Type B On Bias” [7]. Although this method has been discontinued
since the original certification, the numerical value of the uncertainty assessment is valid.

SRM 2783 Page 3 of 6

Reference Values: Reference values are based on weighted means of results from one method determined in
several collaborating laboratories or from two or more analytical methods performed by selected collaborating
laboratories. The uncertainty listed with each value is an expanded uncertainty, with coverage factor 2
(approximately 95 % confidence), calculated by combining a between-source variance incorporating inter-method
or inter-procedure bias with a pooled within-source variance, and a component of variance for material
heterogeneity following the ISO Guide [6]. These results do not fulfill the criteria for certification since a full
estimate of method bias or results from NIST methods are not available.

Table 2. Reference Mass Loading Values for Selected Elements

Elements ng(a) Elements ng(a)

Ce 23.4  3.5 Si 58600  1600

Rb 24.0  5.5 Sm 2.04  0.15
S 1050  260 Th 3.23  0.59
Sc 3.54  0.28 U(b) 1.234  0.024
W 5.0  1.8
(a)
Conversion to ng/cm2 must use area of deposit (not total filter membrane).
(b)
Data from a single source only; uncertainty does not include an estimate for between-source variance.

Table 3. Supplementary Information Values

Average deposit area per filter: 9.96 cm2 (1 s = 0.04 cm2)

Average mass loading per filter: 485 g (1 s = 10 g)

Reference Values for Blank Filters: Reference values are based on weighted means of results from one method
determined in several collaborating laboratories or from two or more analytical methods performed by selected
collaborating laboratories. The uncertainty listed with each value is an expanded uncertainty, with coverage
factor 2 (approximately 95 % confidence), calculated by combining a between-source variance incorporating
inter-method or inter-procedure bias with a pooled within-source variance, and a component of variance for material
heterogeneity following the ISO Guide [6]. These results do not fulfill the criteria for certification since a full
estimate of method bias or results from NIST methods are not available. The uncertainty for the nickel reference
value does not include an estimate for between-source variance because nickel data are from a single source only.

Table 4. Reference Values for Selected Elements in Blank Filters(b)

Elements ng(a)

Ni 8  2
Cr 70  4
(a)
Conversion to ng/cm2 must use area of deposit (not total filter membrane).
(b)
Only found by techniques that include complete filter matrix in analysis.

Information Values for Blank Filters: Information values are given for SRM 2783 blank filters to assist
users in the determination of the components of their procedural blank that are from the blank filter alone.
Information values are based on results that did not allow complete assessment of Type A and Type B components
of uncertainty, hence, only an estimated mean without an uncertainty is given for each element. For all blank filters
analyzed, only elements for which blank values were observed above the detection limit of the method used are
reported. These limits of detection are generally lower than 1 % relative of the certified or reference value in the
loaded filter.

SRM 2783 Page 4 of 6

 Table 5. Information Values for Selected Elements in Blank Filters

Elements ng(a)

Al 30
Na 15
Ba 0.4
Co 0.04
Pb 0.4
S 100
Zn 50
(a)
Conversion to ng/cm2 must use area of deposit (not total filter membrane).

Table 6. Analytical Techniques Used for Value Assignment

Element Methods Element Methods

Al INAA, EDXRF, ICP-MS, PIXE Pb EDXRF, ID-ICP-MS, PIXE

As INAA, PIXE Rb INAA, EDXRF
Ba INAA, EDXRF, ID-ICP-MS, PIXE S EDXRF, PIXE
Ca INAA, EDXRF, PIXE Sb INAA, EDXRF, ID-ICP-MS
Ce INAA Sc INAA
Co INAA, ICP-MS Si INAA, EDXRF, PIXE
Cr INAA, EDXRF, PIXE Sm INAA
Cu INAA, EDXRF, ID-ICP-MS, PIXE Th INAA
Fe INAA, EDXRF, PIXE Ti INAA, EDXRF, PIXE
K INAA, EDXRF, PIXE U ID-ICP-MS
Mg INAA, PIXE V INAA, ICP-MS, PIXE
MN INAA, EDXR, PIXE W INAA
Na INAA, ICP-MS, PIXE Zn INAA, EDXRF, PIXE
Ni EDXRF, ID-ICP-MS, PIXE

Key to Methods:

INAA Instrumental neutron activation analysis

EDXRF Energy-dispersive X-ray fluorescence, including micro-EDXRF
ID-ICP-MS Isotope dilution inductively coupled plasma mass spectrometry
ICP-MS Inductively coupled plasma mass spectrometry
PIXE Proton-induced X-ray emission analysis, including micro-PIXE

SRM 2783 Page 5 of 6

 Figure 1. Millipore PetriSlide container

REFERENCES

[1] May, W.; Parris, R.; Beck, C.; Fassett, J.; Greenberg, R.; Guenther, F.; Kramer, G.; Wise, S.; Gills, T.;
Colbert, J.; Gettings, R.; MacDonald, B.; Definitions of Terms and Modes Used at NIST for
Value-Assignment of Reference Materials for Chemical Measurements; NIST Special Publication 260-136,
U.S. Government Printing Office: Gaithersburg, MD (2000); available at
[Link] (accessed Dec 2011)
[2] Heller-Zeisler, S.F.; Ondov, J.M.; Zeisler, R.; Collection and Characterization of a Bulk PM2.5 Air
Particulate Matter Material for the Preparation of Standard Reference Materials; Biol. Trace Elem. Res.,
Vol. 71-72, pp. 195–202 (1999).
[3] Heller-Zeisler, S.F.; Fajgelj, A.; Bernasconi, G.; Tajani, A.; Zeisler, R.; Examination of a Procedure for the
Production of a Filter-Based Air Particulate Matter Reference Material; Fresenius J. Anal. Chem.,
Vol. 360, pp. 435–438 (1998).
[4] Zeisler, R.; Reference Materials for Small Sample Analysis; Fresenius J. Anal. Chem., Vol. 360,
pp. 376-379 (1998).
[5] Ruhkin, A.L.; Vangel, M.G.; Estimation of a Common Mean and Weighted Means Statistics; J. Am. Statist.
Assoc., Vol. 93, pp. 303–308 (1998).
[6] JCGM 100:2008; Evaluation of Measurement Data  Guide to the Expression of in Measurement (ISO
GUM 1995 with Minor Corrections); Joint Committee for Guides in Metrology (JCGM) (2008); available at
[Link] (accessed Dec 2011); see also
Taylor, B.N.; Kuyatt, C.E.; Guidelines for Evaluating and Expressing the Uncertainty of NIST Measurement
Results; NIST Technical Note 1297; U.S. Government Printing Office: Washington, DC (1994); available at
[Link] (accessed Dec 2011).
[7] Levenson, M.S.; Banks, D.L.; Eberhardt, K.R.; Gill, L.M.; Guthrie, W.F.; Liu, H.-K.; Vangel, M.G.;
Yen, J.H.; Zhang, N.F.; An Approach to Combining Results from Multiple Methods Motivated by the ISO
GUM; J. Res. Natl. Inst. Stand. Technol., Vol. 105, pp. 571–579 (2000).

Certificate Revision History: 13 December 2011 (Editorial changes); 19 July 2011 (Extension of the certification period; editorial changes);
02 January 2002 (This revision reflects an editorial correction to Table 1); 19 November 2001 (Original certificate date).

Users of this SRM should ensure that the Certificate of Analysis in their possession is current. This can be
accomplished by contacting the SRM Program: telephone (301) 975-2200; fax (301) 926-4751;
e-mail srminfo@[Link]; or via the Internet at [Link]

SRM 2783 Page 6 of 6