National Institute of Standards & Technology

Certificate of Analysis
Standard Reference Material® 2709a
San Joaquin Soil
Baseline Trace Element Concentrations
This Standard Reference Material (SRM) is intended primarily for use in the analysis of soils, sediments, or other
materials of a similar matrix. A unit of SRM 2709a consists of 50 g of dried, powdered, agricultural soil.

Certified Values: The certified concentrations of elements, expressed as mass fractions [1] on a dry-mass basis, are
provided in Table 1. Certified values are based on results obtained from critically evaluated independent analytical
techniques. 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 [2]. The measurands are the total
concentrations of the elements reported in Table 1. Metrological traceability is to the SI unit of mass expressed as the
derived unit of mass fraction.

Reference Values: The reference values for elements, expressed as mass fractions on a dry-mass basis, are provided
in Table 2. The reference values are based on results obtained from a single NIST analytical method. Reference
values are non-certified values that are the best estimate of the true value; however, the values do not meet NIST
criteria for certification and are provided with associated uncertainties that may not include all sources of
uncertainty [2]. The measurands are the total concentrations of the elements reported in Table 2. Metrological
traceability is to the SI unit of mass expressed as the derived unit of mass fraction.

Information Values: Information values for elements based on results obtained from one NIST method, are provided
in Table 3. Particle size measurements are provided in Figure 1. 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 or only a limited number of analyses were performed [2]. Information values cannot be used to establish
metrological traceability.

Expiration of Certification: The certification of SRM 2709a is valid, within the measurement uncertainties
specified, until 01 November 2028, provided the SRM is handled in accordance with the instructions given in this
certificate (see “Instructions for 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 or register online) will facilitate notification.

E.A. Mackey and R.R. Greenberg, formerly of the NIST Analytical Chemistry Division, and S.E. Long of the NIST
Chemical Sciences Division were responsible for coordination of the technical measurements.

Statistical analyses were performed by J.H. Yen of the NIST Statistical Engineering Division.

Support aspects involved in the issuance of this SRM were coordinated through the NIST Office of Reference
Materials.

Carlos A. Gonzalez, Chief

Chemical Sciences Division

Gaithersburg, MD 20899 Steven J. Choquette, Director

Certificate Issue Date: 02 November 2018 Office of Reference Materials
Certificate Revision History on Page 6
SRM 2709a Page 1 of 7
INSTRUCTIONS FOR USE

Sampling: The SRM should be thoroughly mixed by repeatedly inverting and rotating the bottle horizontally before
removing a test portion for analysis. A minimum mass of 250 mg (dry mass - see Drying) should be used for analytical
determinations to be related to the mass fraction values in this Certificate of Analysis.

To obtain the certified values, sample preparation procedures should be designed to effect complete dissolution. If
volatile elements (i.e., arsenic, mercury, selenium) are to be determined, precautions should be taken in the dissolution
of SRM 2709a to avoid volatilization losses.

Drying: To relate measurements to the certified, reference, and information values that are expressed on a dry-mass
basis, users should determine a drying correction at the time of each analysis. The recommended drying procedure is
oven drying for 2 h at 110 °C. Note that analytical determination of volatile elements (i.e., arsenic, mercury, selenium)
should be determined on samples as received; separate samples should be dried as previously described to obtain a
correction factor for moisture. Correction for moisture is to be made to the data for volatile elements before comparing
them to the certified values. This procedure ensures that these elements are not lost during drying. The mass loss on
drying for this material as bottled was approximately 3 %, but this value may change once the bottle is opened and
the soil is exposed to air.

SOURCE, PREPARATION, AND ANALYSIS

Source and Preparation of Material(1): The U.S. Geological Survey (USGS), under contract to NIST, collected and
processed the soil for SRM 2709a with assistance from the U.S. Bureau of Reclamation’s Sacramento CA office. The
agricultural soil used to produce SRM 2709a was collected from a fallow field, in the central California San Joaquin
Valley. Three separate collection sites were used to obtain the necessary amount of material. Each collection site
covered an area of approximately 4 m2. Prior to sample collection the area was scraped clean of surface vegetation.
Collected material was transferred to 20 plastic-lined five-gallon plastic buckets and shipped to the USGS laboratory
for processing. At USGS, the SRM 2709a soil was dried at room temperature, disaggregated, and sieved to remove
coarse material (≥2 mm). The resulting soil was ball-milled in 50 kg portions, and then the entire batch of soil was
transferred to a cross-flow V-blender for mixing. The blended soil was radiation sterilized prior to bottling. In the
final preparation step the blended material was split into containers using a custom-designed spinning riffler, which
was used to divide the material into smaller batches, and then used to apportion approximately 50 g into each
pre-cleaned bottle.

Every 100th bottle was set aside for chemical analyses designed to assess material homogeneity using X-ray
fluorescence spectrometry (XRF), inductively coupled plasma optical emission spectrometry (ICP-OES), and
inductively coupled plasma mass spectrometry (ICP-MS) at the USGS. Homogeneity assessments were performed at
NIST as well, and results indicated that additional processing was needed to achieve optimum homogeneity. The
material from all bottles was combined, and then ground in batches between stainless steel plates for a time sufficient
to produce a powder of which ≥95 %, by mass, passed through a 200 mesh (74 µm) sieve. The resulting powder was
blended, and 50 g portions were dispensed into bottles using the spinning riffler. Results from additional analyses
indicated material homogeneity was acceptable (see below).

Homogeneity Testing: The homogeneity was assessed for elements in the bottled material using X-ray fluorescence
spectrometry and instrumental neutron activation analysis. In a few cases, statistically significant differences were
observed, and the variance due to material inhomogeneity is included in the expanded uncertainties of the certified
values. The estimated relative standard deviation for material inhomogeneity for most elements is ≤1 %, for calcium
it is approximately 2 %, and for chromium it is approximately 3 %. Significant material heterogeneity was observed
for mercury, for which a reference value with a prediction interval is provided; see Table 2.

Analysis: Analyses of this material were performed at NIST and at the USGS (Denver, CO). Results from NIST
were used to provide the certified, reference, and information values shown in Tables 1, 2, and 3 respectively. Results
from the USGS were used to confirm those values. The analytical techniques used for each element are listed in
Table 4; the analysts are listed in Tables 5 and 6.

Particle Size Measurements: Particle size measurements for SRM 2709a were made using a Malvern Mastersizer
3000 laser-based light scattering system and the particle size distribution is shown in Figure 1.

(1)
Certain commercial equipment, instruments, or materials are identified in this certificate in order to specify adequately
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 2709a Page 2 of 7
 Table 1. Certified Values(a) (Dry-Mass Basis) for Elements in SRM 2709a

Element Mass Fraction Coverage Element Mass Fraction Coverage

(%) Factor, k (mg/kg) Factor, k
Aluminum (Al) 7.37 ± 0.16 2.04 Antimony (Sb) 1.55 ± 0.06 2.36
Calcium (Ca) 1.91 ± 0.09 2.05 Barium (Ba) 979 ± 28 2.57
Iron (Fe) 3.36 ± 0.07 2.23 Cadmium (Cd) 0.371 ± 0.002 2
Magnesium (Mg) 1.46 ± 0.02 2.02 Chromium (Cr) 130 ± 9 2.05
Phosphorus (P) 0.0688 ± 0.0013 2.12 Cobalt (Co) 12.8 ± 0.2 2.45
Potassium (K) 2.11 ± 0.06 2.45 Lead (Pb) 17.3 ± 0.1 2
Silicon (Si) 30.3 ± 0.4 2.57 Manganese (Mn) 529 ± 18 2.16
Sodium (Na) 1.22 ± 0.03 2.02 Strontium (Sr) 239 ± 6 2.26
Titanium (Ti) 0.336 ± 0.007 2.26 Vanadium (V) 110 ± 11 2.10
Zirconium (Zr) 195 ± 46 2.10

(a) Certified values for all elements except cadmium and lead are the equally weighted means of results from two or three analytical
methods. The uncertainty listed with each value is an expanded uncertainty about the mean. The expanded uncertainty is
calculated as U = kuc, where uc is intended to represent, at the level of one standard deviation, the combined effect of
between-method and within-method components of uncertainty, following the ISO/JCGM Guide [3,4]. A component for
material heterogeneity is incorporated into the uncertainties of aluminum, calcium, chromium, manganese, and sodium. The
coverage factor (k) is determined from the Student's t-distribution corresponding to the appropriate associated degrees of freedom
and approximately 95 % confidence for each analyte.
The certified values for cadmium and lead are each results from a single NIST method (isotope dilution (ID)-ICP-MS, see
Table 4) for which a complete evaluation of all sources of uncertainty has been performed. The uncertainty provided is an
expanded uncertainty about the mean to cover the measurand with approximately 95 % confidence, consistent with the
ISO/JCGM Guide [4]. The expanded uncertainty is calculated as U = kuc, where uc is the combined uncertainty that incorporates
within-method uncertainty and Type B uncertainty components related to the analysis, and k is the coverage factor corresponding
to approximately 95 % confidence for each analyte.

Table 2. Reference Values(a) (Dry-Mass Basis) for Elements in SRM 2709a

Element Mass Fraction

(mg/kg)
Arsenic (As) 10.5 ± 0.3
Cerium (Ce) 42 ± 1
Cesium (Cs) 5.0 ± 0.1
Copper (Cu) 33.9 ± 0.5
Europium (Eu) 0.83 ± 0.02
Gadolinium (Gd) 3.0 ± 0.1
Lanthanum (La) 21.7 ± 0.4
Mercury (Hg)(b) 0.9 ± 0.2
Nickel (Ni) 85 ± 2
Rubidium (Rb) 99 ± 3
Scandium (Sc) 11.1 ± 0.1
Thallium (Tl) 0.58 ± 0.01
Thorium (Th) 10.9 ± 0.2
Uranium (U) 3.15 ± 0.05
Zinc (Zn) 103 ± 4
(a) Reference values for all elements are based on results from one analytical method at NIST. Uncertainty values represent the
expanded uncertainties about the mean to cover the measurand with approximately 95 % confidence, consistent with the
ISO/JCGM Guide [4]. The expanded uncertainty is calculated as U = kuc, where uc is the combined uncertainty that incorporates
within-method uncertainty and type B uncertainty components related to the analysis, and k is the coverage factor (k = 2)
corresponding to approximately 95 % confidence for each analyte.
(b) The reference value for mercury represents the average value from analysis of portions from six bottles using ID-cold

vapor (CV)-ICP-MS. Results indicate significant material heterogeneity; values ranged from 0.8 mg/kg to 1.1 mg/kg. The
uncertainty for this reference value is in the form of a prediction interval.

SRM 2709a Page 3 of 7

 Table 3. Information Values(a) (Dry Mass Basis) for Elements in SRM 2709a

Element Mass Fraction

(mg/kg)
Boron (B) 74
Dysprosium (Dy) 3
Hafnium (Hf) 4
Lutetium (Lu) 0.3
Neodymium (Nd) 17
Samarium (Sm) 4
Selenium (Se) 1.5
Tantalum (Ta) 0.7
Terbium (Tb) 0.5
Ytterbium (Yb) 2
(a) Information values are based on results from one analytical method at NIST.

SUPPLEMENTAL INFORMATION FOR SRM 2709a

Particle Size Measurements: Particle size measurements for SRM 2709a were made using a Malvern Mastersizer
3000 laser-based light scattering system. Approximately 0.5 g of SRM 2709a material was measured using water as
the dispersant (refractive index: 1.330). Sample was introduced into the measurement cell before ten individual
measurements were made at an obscuration of 14 % – 18 % of the laser beam. The information values calculated
10th (Dv10), 50th (Dv50) and 90th (Dv90) percentile particle sizes are Dv(10) = 2.62 µm, Dv(50) = 12.6 µm, and
Dv(90) = 71.7 µm. The volume fraction of material smaller than 10.1 µm in diameter is approximately 44 %. The
particle size distribution is shown in Figure 1.

Figure 1. Particle size distribution in SRM 2709a

SRM 2709a Page 4 of 7

 Table 4. Methods(a,b) Used for the Analysis of SRM 2709a

Element Methods Element Methods

Al INAA; XRF Na NAA; XRF

As INAA Nd INAA
B PGAA Ni ICP-MS
Ba ICP-OES; INAA: XRF P ICP-OES; XRF
Ca INAA; XRF Pb ID-ICP-MS
Cd ID-ICP-MS; PGAA Rb INAA
Ce INAA Sb INAA; ICP-MS
Co INAA; ICP-OES Sc INAA
Cr INAA; XRF Se CCT-ICP-MS
Cs INAA Si PGAA; XRF
Cu ICP-MS Sm INAA
Dy INAA Sr INAA; ICP-OES; XRF
Eu INAA Ta INAA
Fe INAA; PGAA; XRF Tb INAA
Gd PGAA Th INAA
Hf INAA Ti INAA; PGAA; XRF
Hg CV-ID-ICP-MS Tl ICP-MS
K INAA; PGAA; XRF U ICP-MS
La INAA V INAA; XRF
Lu INAA Yb INAA
Mg INAA; XRF Zn INAA
Mn INAA; PGAA; XRF Zr INAA; XRF
(a) NIST Methods of Analysis:
CCT-ICP-MS Collision Cell Inductively Coupled Plasma Mass Spectrometry
CV ID-ICP-MS Cold Vapor Isotope Dilution Inductively Coupled Plasma Mass Spectrometry
ICP-MS Inductively Coupled Plasma Mass Spectrometry
ICP-OES Inductively Coupled Plasma Optical Emission Spectrometry
ID-ICP-MS Isotope Dilution Inductively Coupled Plasma Mass Spectrometry
INAA Instrumental Neutron Activation Analysis
PGAA Prompt Gamma-Ray Activation Analysis
XRF X-ray Fluorescence Spectrometry
(b) USGS Methods of Analysis (used to confirm results from certification methods).

WD-XRF Wavelength Dispersive X-ray Fluorescence Spectrometry

ICP-OES Inductively Coupled Plasma Optical Emission Spectrometry
ICP-MS Inductively Coupled Plasma Mass Spectrometry

Table 5. Participating NIST Analysts:

S.J. Christopher A.F. Marlow S.A. Rabb B.E. Tomlin

D.L. Ellisor K.E. Murphy J.R. Sieber L.J. Wood
R.M. Lindstrom J.M. Ness R.O. Spatz L.L. Yu
S.E. Long R.L. Paul R.S. Popelka-Filcoff R. Zeisler
E.A. Mackey

Table 6. Participating USGS Laboratory and Analysts

Laboratory Analysts

U.S. Geological Survey Branch of M.G. Adams; Z.A. Brown; P.L. Lamothe;
Geochemistry (Denver, CO) J.E. Taggart; S.A. Wilson

SRM 2709a Page 5 of 7

 REFERENCES

[1] Thompson, A.; Taylor, B.N.; Guide for the Use of the International System of Units (SI), NIST Special Publication
811 (2008); available at https://www.nist.gov/pml/special-publication-811 (accessed Nov 2018).
[2] May, W.E.; Gills, T.E.; Parris, R.; Beck, II, C.M.; Fassett, J.D.; Gettings, R.J.; Greenberg, R.R.; Guenther, F.R.;
Kramer, G.; MacDonald, B.S.; Wise, S.A.; Definitions of Terms and Modes Used at NIST for Value-Assignment of
Reference Materials for Chemical Measurements; NIST Special Publication 260-136 (1999); available at
https://www.nist.gov/sites/default/files/documents/srm/SP260-136.PDF (accessed Nov 2018).
[3] 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).
[4] JCGM 100:2008; Evaluation of Measurement Data - Guide to the Expression of Uncertainty in Measurement; (GUM
1995 with Minor Corrections), Joint Committee for Guides in Metrology (JCGM) (2008); available at
https://www.bipm.org/utils/common/documents/jcgm/JCGM_100_2008_E.pdf (accessed Nov 2018); 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
https://www.nist.gov/pml/nist-technical-note-1297 (accessed Nov 2018).

Certificate Revision History: 02 November 2018 (Updated uncertainty calculation information; added particle size distribution; change of
expiration date; editorial changes); 07 April 2009 (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) 948-3730; e-mail
srminfo@nist.gov; or via the Internet at https://www.nist.gov/srm.

SRM 2709a Page 6 of 7

 Appendix A

Leachable Concentrations Determined Using USEPA Methods 200.7 and 3050B

The mass fraction values contained in the NIST Certificate of Analysis for SRM 2709a represent the total element
content of the material. The measurement results used to provide the certified, reference, or information values are
obtained from methods that require complete sample decomposition, or from nondestructive analytical methods such
as instrumental neutron activation analysis or prompt gamma-ray activation analysis. Where complete sample
decomposition is required, it can be accomplished by digestion with mixed acids or by fusion. For mixed-acid
decomposition, hydrofluoric acid must be included in the acid mixture used to totally decompose siliceous materials
such as soils and sediments.

In its monitoring programs, the U.S. Environmental Protection Agency (USEPA) has established a number of leach
methods for the preparation of soil samples for the determination of extractable elements. Eight laboratories
participated, seven of which used USEPA Method 200.7; the remaining laboratory used USEPA SW-846
Method 3050B for preparation of soil samples. All elements were determined in leachates by inductively coupled
plasma optical emission spectrometry. Six of the eight laboratories provided individual results from duplicate
portions, and these results were averaged together to provide one result for each element from each participating
laboratory. Results rejected as outliers by the USEPA Contract Laboratory Program (CLP) officials were not included.
Results are summarized in Table A1. The ranges of mass fraction values, median values (to two significant figures),
and the number of results included for each are given for 23 elements. The percent recovery values based on the ratios
of the median values to the total element content (from the certified, reference, or information values in the Certificate
of Analysis) are listed in the last column of Table A1. Note that the certified values provided as total mass
fractions in the Certificate of Analysis are the best estimate of the true mass fraction values for this material.

This USEPA CLP Study was coordinated by Clifton Jones, Quality Assurance and Technical Support Program, Shaw
Environmental & Infrastructure Group (Las Vegas, NV) under the direction of J. Nebelsick, USEPA, Analytical
Services Branch. The participating laboratories are listed below the table.

Table A1. Results from Laboratories Participating in the EPA Contract Laboratory Program Study.

Element n Range Median Recovery

(mg/kg) (mg/kg) (%)
Aluminum 7 13000 – 17000 16000 22
Antimony 2 1.2 – 1.5 1.4 88
Arsenic 8 6.4 – 10 7.8 74
Barium 8 350 – 400 380 39
Beryllium 7 0.50 – 0.72 0.61 ––
Cadmium 5 0.33 – 0.66 0.40 110
Calcium 8 12000 – 14000 12000 65
Chromium 8 46 – 67 53 41
Cobalt 8 8.2 – 13 10 81
Copper 7 24 – 28 27 81
Iron 8 22000 – 26000 24000 70
Lead 7 8.1 – 11 9.2 53
Magnesium 7 9700 – 11000 10000 71
Manganese 8 380 – 450 420.0 79
Mercury 8 0.79 – 0.92 0.87 97
Nickel 8 59 – 71 66 77
Potassium 8 2600 – 4000 2900 14
Selenium 5 0.69 – 1.9 0.95 63
Silver 4 0.14 – 4.1 0.64 ––
Sodium 7 460 – 610 500 4
Thallium 2 0.74 – 1.6 1.2 200
Vanadium 8 43 – 71 48 44
Zinc 8 69 – 87 79 77

List of CLP and non–CLP Participating Laboratories: A4 Scientific, Inc.; Bonner Analytical Testing Co.; Chem Tech
Consulting Group; Datachem Laboratories, Inc.; Liberty Analytical Corporation; MSE Laboratory Services; Shealy
Environmental; SVL Analytical Inc.

SRM 2709a Page 7 of 7