www.epa.gov
May 2017
EPA 402-R16-003
Revision 0
Rapid Method for Sodium Hydroxide Fusion
of Asphalt Roofing Material Matrices Prior to
Americium, Plutonium, Strontium, Radium,
and Uranium Analyses
U.S. Environmental Protection Agency
Office of Air and Radiation
Office of Radiation and Indoor Air
National Analytical Radiation Environmental Laboratory
Montgomery, AL 36115
Office of Research and Development
National Homeland Security Research Center
Cincinnati, OH 45268

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Sodium Hydroxide Fusion of Asphalt Roofing Material Matrices
Revision History
Revision 0 Original release.
05-01-2017
This report was prepared for the National Analytical Radiation Environmental Laboratory of the Office of
Radiation and Indoor Air and the National Homeland Security Research Center of the U.S. Environmental
Protection Agency's (EPA) Office of Research and Development. It was prepared by Environmental
Management Support, Inc., of Silver Spring, Maryland, under contract EP-W-13-016, task order 014,
managed by Dan Askren. This document has been reviewed in accordance with EPA policy and approved
for publication. Note that approval does not signify that the contents necessarily reflect the views of the
Agency. Mention of trade names, products, or services does not convey EPA approval, endorsement, or
recommendation.

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Sodium Hydroxide Fusion of Asphalt Roofing Material Matrices
Rapid Method for Sodium Hydroxide Fusion of Asphalt Roofing Material
Matrices Prior to Americium, Plutonium, Strontium, Radium, and Uranium
Analyses
1. Scope and Application
1.1.	The method is applicable to the sodium hydroxide (NaOH) fusion of asphalt roofing
material samples, prior to the chemical separation procedures described in the
following procedures:
1.1.1.	Rapid Radiochemical Method for Americium-241 in Building Materials for
Environmental Remediation Following Radiological Incidents (Reference
16.1).
1.1.2.	Rapid Radiochemical Method for Plutonium-238 and Plutonium-239/240 in
Building Materials for Environmental Remediation Following Radiological
Incidents (Reference 16.2).
1.1.3.	Rapid Radiochemical Method for Radium-226 in Building Materials for
Environmental Remediation Following Radiological Incidents (Reference
16.3).
1.1.4.	Rapid Radiochemical Method for Total Radiostrontium (Sr-90) in Building
Materials for Environmental Remediation Following Radiological Incidents
(Reference 16.4).
1.1.5.	Rapid Radiochemical Method for Isotopic Uranium in Building Materials
for Environmental Remediation Following Radiological Incidents
(Reference 16.5).
1.2.	This general method applies to asphalt roofing material samples collected following a
radiological or nuclear incident. The term "asphalt roofing materials" is used in this
procedure to mean asphalt organic shingles or asphalt fiberglass shingles typically
used for residential or commercial roofs. This roofing material procedure was
validated with asphalt fiberglass shingles, which are likely more difficult to analyze
due to the presence of fiberglass. Other roofing types will need to be validated by the
laboratory.
1.2.1.	Asphalt fiberglass shingles have a base layer of glass fiber reinforcing mat.
The mat is made from wet, random-laid fiberglass bonded with urea-
formaldehyde resin. The mat is then coated with asphalt which contains
mineral fillers and makes the fiberglass shingle waterproof.
1.2.2.	Organic asphalt shingles generally have thicker organic (paper) matting
saturated with asphalt to make it waterproof, then a top coating of adhesive
asphalt is applied and ceramic granules are then embedded. This method
should work with asphalt organic shingles and other bitumen-based
membrane roofing materials, but this will have to be tested and validated by
the laboratory. The organic asphalt shingles aliquants will likely have less
residual ash than fiberglass shingles after the furnace heating step that
destroys the organic components in the aliquant. The fusion method is
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expected to process the smaller organic shingles residue successfully. It is
recommended that labs validate the method for organic asphalt shingles as
well.
1.3.	The fusion method is rapid and rigorous, effectively digesting refractory radionuclide
particles that may be present on asphalt roofing material samples. Asphalt roofing
material samples should be cut into very small subsample pieces (<0.25 g) to get a
representative as-received sample of 100 - 250 g prior to taking a representative
aliquant for furnace heating and fusion. The asphalt roofing material sample should
be cut into pieces small enough so that representative subsamples can be taken and
analyzed. Material sampling techniques to combine asphalt roofing subsamples that
represent a larger roof surface area may be appropriate.
1.4.	Asphalt roofing material samples should be cut into very small pieces to get a
representative as-received sample of 100 - 250 g prior to taking a representative
aliquant for furnace heating and fusion. The asphalt roofing material sample should
be cut into pieces small enough so that representative subsamples can be taken and
analyzed. Material sampling techniques to combine asphalt roofing subsamples that
represent a larger roof surface area may be appropriate.
1.5.	After a homogeneous subsample is obtained, the asphalt roofing material aliquant is
heated to destroy organics in the sample matrix. After heating, the sample aliquant is
fused to digest the asphalt roofing material and sample matrix. Matrix removal steps
are employed to collect and preconcentrate the radionuclides from the alkaline fusion
matrix.
1.5.1.	A subsample (-25 g or larger) of asphalt roofing material sample is taken to
facilitate representative sampling of a larger roofing material surface area (a
25 g sample represents approximately a 15 x 5 x 0.06 cm surface area). The
25 g sample subsample is ashed in a furnace and homogenized as well as
possible. A smaller representative aliquant of the ashed roofing material is
taken for analysis.
1.5.2.	As this method is a sample digestion and pretreatment technique to be used
prior to other separation and analysis methods, the user should refer to those
individual methods and any project-specific requirements for the
determination of applicable measurement quality objectives (MQOs).
1.6.	Application of this method by any laboratory should be validated by the laboratory
using the protocols provided in Method Validation Guide for Qualifying Methods
Used by Radioanalytical Laboratories Participating in Incident Response Activities
(Reference 16.6), or the protocols published by a recognized standards organization
for method validation.
1.6.1. In the absence of project-specific guidance, MQOs for asphalt roofing
samples may be based on the analytical action levels (AALs), required
method uncertainty (wmr), and the required relative method uncertainty ((pmr)
found in the Radiological Sample Analysis Guide for Incidents of National
Significance  Radionuclides in Soil (Reference 16.7).
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2.	Summary of Method
2.1.	The method is based on ashing a 25 g subsample of asphalt roofing material sample
in a furnace to remove organic components, followed by taking a representative
aliquant from the ashed sample. The 1-1.5 g aliquant of ashed sample is fused using
NaOH fusion at 600 C.
2.2.	Plutonium (Pu), uranium (U), and americium (Am) are separated from the alkaline
matrix using an iron (Fe)/titanium hydroxide precipitation (enhanced with calcium
phosphate precipitation) followed by a lanthanum fluoride matrix removal step.
2.3.	Strontium (Sr) is separated from the alkaline matrix using a phosphate precipitation,
followed by a calcium fluoride precipitation to remove silicates.
2.4.	Radium (Ra) is separated from the alkaline matrix using a carbonate precipitation.
2.5.	The resulting solutions are subsequently processed using the methods referred to in
Steps 1.1.1-1.1.5.
3.	Definitions, Abbreviations and Acronyms
3.1.	Discrete Radioactive Particles (DRPs or "hot particles"). Particulate matter in a
sample of any matrix where a high concentration of radioactive material is present as
a very small particle (
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Sodium Hydroxide Fusion of Asphalt Roofing Material Matrices
roofing material are effectively digested, including refractory radionuclide particles.
A small amount of mineralized granules may remain after the fusion.
4.2.	Information regarding the elemental composition of the sample may be helpful. For
example, asphalt roofing materials may have native concentrations of U, Ra, thorium,
stable Sr, or stable barium (Ba), all of which may have an effect on the chemical
separations used following the fusion of the sample. In some cases (e.g., Sr analysis),
elemental analysis of the digestate prior to chemical separations may be necessary to
determine native concentrations of carrier elements present in the sample.
Note: In those samples where native constituents are present that could interfere with the
determination of the chemical yield (e.g., Sr for 90Sr analysis) or with the creation of a sample
test source (e.g., Ba for 226Ra analysis by alpha spectrometry), it may be necessary to determine
the concentration of these native constituents in advance of chemical separation (using a separate
aliquant of fused material) and make appropriate adjustments to the yield calculations or
amount of carrier added.
4.3.	The native stable Sr in asphalt shingles may have an impact on the Sr-90 method.
Asphalt shingles may contain enough stable Sr to have a slight, yet significant impact
on the Sr carrier chemical yield measurement used in the Sr-90 method. This will
cause Sr carrier yields that are biased high and therefore Sr-90 measurements that are
biased low. While a higher level Sr carrier (7 milligram [mg]) is used to mitigate this
effect, the digestion and analysis of samples to determine stable Sr content or analysis
of several shingle aliquots with no Sr carrier added may be needed to make reliable Sr
carrier chemical yield measurements. The analysis of representative shingles aliquots
with no carrier added may be the approach with the least impact on the laboratory
during an emergency and the most efficient way to correct for the small amount of
stable Sr in the asphalt shingle samples.
4.4.	Matrix blanks for these matrices may not be practical to obtain. Efforts should be
made to obtain independent, analyte-free materials that have similar composition as
the samples to be analyzed. These blanks will serve as process monitors for the
fusion, and as potential monitors for cross contamination during batch processing.
4.5.	Uncontaminated asphalt roofing material may be acceptable blank material for Pu,
Am, and Sr analyses, but this material will contain background levels of naturally
occurring U and Ra isotopes.
4.5.1.	If analyte-free blank material is not available and an empty crucible is used
to generate a reagent blank sample, it is recommended that -100-150 mg
calcium (Ca) per sample aliquant be added as calcium nitrate (Ca(N03)2) to
the empty crucible as blank simulant. This step facilitates strontium
phosphate and radium carbonate precipitations from the alkaline fusion
matrix.
4.5.2.	Tracer yields may be slightly lower for reagent blank matrices, since asphalt
roofing material matrix components, such as Ca, typically enhance
recoveries across the precipitation steps since Ca in the native asphalt
materials facilitates analyte precipitation across the preconcentration steps
used.
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4.6.	Samples with elevated activity or samples that require multiple analyses from a single
aliquant may need to be split after dissolution. In these cases the initial digestate and
the split fractions should be carefully measured to ensure that the sample aliquant for
analysis is accurately determined.
4.6.1.	Tracer or carrier amounts (added for yield determination) may be increased
where the split allows for the normal added amount to be present in the
subsequent aliquant. For very high activity samples, the addition of the
tracer or carrier may need to be postponed until following the split, in which
case special care must be taken to ensure that the process is quantitative
until isotopic exchange with the yield monitor is achieved. This deviation
from the method should be thoroughly documented and reported in the case
narrative.
4.6.2.	When this method is employed and the entire volume of fused sample is
processed in the subsequent chemical separation method, the original
sample size and units are used in all calculations, with the final results
reported in the units requested by the project manager.
4.7.	Batch blank samples, laboratory control samples (LCSs), and sample duplicates
should be created as early in the process as possible, following the same tracer/carrier
additions, digestion process, and sample splitting used for the field samples. In this
method, quality control (QC) samples should be initiated at the point samples are
aliquanted into crucibles for the fusion.
4.8.	Zirconium crucibles used in the furnace ashing and fusion process may be reused.
4.8.1.	Before reuse, the crucibles should be cleaned very well using soap and
water, followed by warm nitric acid, HNO3 (multiple rinses), and then
water. Blank measurements should be monitored to ensure effective
cleaning and control against cross-contamination.
4.8.2.	Segregation of crucibles used for low and high activity samples is
recommended to minimize the risk of cross-contamination while
maximizing the efficient use of crucibles.
4.9.	Centrifuge speeds of 3500 revolutions per minute (rpm) are recommended but lower
rpm speeds may be used if 3500 rpm is not available. Longer centrifuge times may be
needed with lower speeds.
4.10.	Aluminum nitrate reagent typically contains trace levels of U contamination and may
have a slight impact on the U isotopic method at very low levels. To achieve the
lowest possible blanks for isotopic U measurements, some labs have removed the
trace U by passing -250 mL of the 2M aluminum nitrate reagent through ~7 mL TRU
Resin, but this will have to be tested and validated by the laboratory.
4.11.	It is very important to withdraw a representative subsample from as homogeneous
and representative a sample aliquant of the asphalt roofing material as possible to
allow reliable assessment of radiological contamination of the samples taken. The
asphalt roofing sample, as received, is cut into small pieces (0.25 g or less if
possible), combined, and pieces of the sample are randomly taken to comprise a 25 g
sample aliquant (nominally 100-125 pieces, representing approximately a 15 x 5 x
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0.06 cm surface area) for analysis. A 1-1.5 g subsample aliquant of the ashed sample
is taken for analysis. The mass used for calculation of results is corrected based on the
relative mass of the ashed and as-received sample (i.e., percent ash). Enough shingles
sample should be collected in the field so that 100-250 g of the asphalt shingles may
be collected for sub-sampling and analysis. Replicate samples may be taken to
minimize concerns about representative sampling.
4.12. The asphalt shingles should be cut into as small a pieces as possible (0.2 g or less) to
facilitate homogenizing the residual ash for subsampling, in particular to minimize
the size of the residual fiberglass so it can be effectively blended with the ash.
5. Safety
5.1.	General
5.1.1.	Refer to your laboratory' s safety manual for concerns of contamination
control, personal exposure monitoring and radiation dose monitoring.
5.1.2.	Refer to your laboratory's chemical hygiene plan (or equivalent) for general
safety rules regarding chemicals in the workplace.
5.2.	Radiological
5.2.1. Hot particles (DRPs)
5.2.1.1.	Hot particles, also termed "discrete radioactive particles" (DRPs),
will likely be small, on the order of 1 mm or less. DRPs typically
are not evenly distributed in the media and their radiation
emissions are not uniform in all directions (anisotropic).
5.2.1.2.	Asphalt roofing material media should be individually surveyed
using a thickness of the solid sample that is appropriate for
detection of the radionuclide decay particles.
Note: The information regarding DRPs should accompany the samples
during processing as well as be described in the case narrative that
accompanies the sample results.
5.2.1.3.	It is assumed that radiological activity from surface deposition
onto the asphalt roofing material is primarily in the homogenized
ash material and not in any strands or clumps of fiberglass from
the shingle matting remaining with the ash. Small amounts of the
fiberglass may be analyzed, however, if desired.
5.3.	Procedure-Specific Non-Radiological Hazards:
5.3.1. The furnace ashing and NaOH fusion are performed in a furnace at -550 C
and 600 C, respectively. The operator should exercise extreme care when
using the furnace and when handling the hot crucibles. Long tongs are
recommended. Thermal protection gloves are also recommended when
performing this part of the procedure. The fusion furnace should be used in
a well-ventilated area (hood, trunk exhaust, etc.).
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5.3.2. Particular attention should be paid to the use of hydrofluoric acid (HF). HF is
an extremely dangerous chemical used in the preparation of some of the
reagents and in the microprecipitation procedure. Appropriate personal
protective equipment (PPE) must be used in strict accordance with the
laboratory safety program specification.
6.	Equipment and Supplies
6.1.	Adjustable temperature laboratory hotplates.
6.2.	Balance, top loading or analytical, readout display of at least  0.01 g.
6.3.	Beakers, Pyrex, 600 mL, 100 mL, 150 mL capacity.
6.4.	Centrifuge able to accommodate 225 mL tubes. (250 mL tubes are acceptable)
6.5.	Centrifuge tubes, 50 mL and 225 mL capacity.
6.6.	Crucibles, 250 mL, zirconium, with lids.
6.7.	100 microliters (|jL), 200 [j,L, 500 [xL, and 1 mL pipets or equivalent and appropriate
plastic tips.
6.8.	1-10 mL electronic/manual pipet(s).
6.9.	Hot water bath or dry bath equivalent.
6.10.	Metal snips or shears
Note: See Appendix A for a method for cutting and homogenization of asphalt roofing material
samples.
6.11.	Muffle furnace capable of reaching at least 600 C.
6.12.	Tongs for handling crucibles (small and long tongs).
6.13.	Tweezers or forceps.
6.14.	Vortex stirrer.
7.	Reagents and Standards
Notes: Unless otherwise indicated, all references to water should be understood to mean Type I
reagent water (ASTM D1193; Reference 16.10).
All reagents are American Chemical Society grade or equivalent unless otherwise specified.
7.1.	Type I reagent water as defined in ASTM Standard D1193 (Reference 16.10).
7.2.	Aluminum (Al) nitrate solution, A1(N03)3 (2M): Add 750 g of aluminum nitrate
nonahydrate (A1(N03)3  9H20) to -700 mL of water and dilute with water to 1 L.
7.3.	Ammonium hydrogen phosphate (3.2M): Dissolve 106 g of (NH/^HPC^ in 200 mL
of water, heat on low to medium heat on a hot plate to dissolve and dilute with water
to 250 mL.
7.4.	Boric Acid, H3BO3.
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7.5.	Calcium nitrate, Ca(NC>3)2, (1.25M): Dissolve 147 g of calcium nitrate tetrahydrate
(Ca(N03)2  4H2O) in 300 mL of water and dilute with water to 500 mL.
7.6.	Fe carrier (50 mg/mL): Dissolve 181 g of ferric nitrate (Fe(N03)3  9H20) dissolved
in 300 mL water and dilute with water to 500 mL. This carrier does not need to be
standardized.
7.7.	Hydrochloric acid, HC1 (12M): Concentrated HC1.
7.7.1.	HC1 (0.01M): Add 0.83 mL of concentrated HC1 to 800 mL of water and
dilute with water to 1 L.
7.7.2.	HC1 (1.5M): Add 125 mL of concentrated HC1 to 800 mL of water and
dilute with water to 1 L.
7.8.	Hydrofluoric acid, HF (28M): Concentrated HF.
3_i_
7.9.	Lanthanum (La) carrier (1.0 mg La /mL): Add 1.56 g lanthanum (III) nitrate
hexahydrate (La(NC>3)3  6H20) in 300 mL water, dilute with water to 500 mL. This
carrier does not need to be standardized.
7.10.	Nitri c aci d, HN03(16M): C oncentrated HNO3.
7.10.1.	HNO3 (3M): Add 191 mL of concentrated HNO3 to 700 mL of water and
dilute with water to 1 L.
7.10.2.	HNO3 (3M)- H3BO3 (0.25M) solution: Add 15.4 g of H3BO3 and 190 mL of
concentrated HNO3 to 500 mL of water, heat to dissolve, and dilute with
water to 1 L.
7.10.3.	HNO3 (7M): Add 443 mL of concentrated HNO3 to 400 mL of water and
dilute with water to 1 L.
7.10.4.	HNO3 (8M): Add 506 mL of concentrated HNO3 to 400 mL of water and
dilute with water to 1 L.
7.11.	Sodium carbonate, Na2CC>3 (2M): Dissolve 212 g anhydrous Na2CC>3 in 800 mL of
water, then dilute with water to 1 L.
7.12.	NaOH pellets.
7.13.	Titanium (III) chloride solution (TiCh), 10 percent by mass (wt%) solution in 20-30
wt% HC1. (This reagent is typically available commercially in this concentration.)
7.14.	Radioactive tracers/carriers (used as yield monitors) and spiking solutions. A
radiotracer is a radioactive isotope of the analyte that is added to the sample to
measure any losses of the analyte. A carrier is a stable isotope form of a radionuclide
(usually the analyte) added to increase the total amount of that element so that a
measureable mass of the element is present. A carrier can be used to determine the
yield of the chemical process and/or to carry the analyte or radiotracer through the
chemical process. Refer to the chemical separation method(s) to be employed upon
completion of this dissolution technique. Tracers/carriers that are used to monitor
radiochemical/chemical yield should be added to a 1-1.5 g aliquant of the ashed
sample. This allows for monitoring and correction of chemical losses in the combined
digestion process, as well as in the chemical separation method. Carriers used to
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prepare sample test sources but not used for chemical yield determination (e.g.,
cerium added for microprecipitation of Pu or U), should be added where indicated.
8.	Sample Collection, Preservation, and Storage
Not Applicable.
9.	Quality Control
9.1.	Where the subsequent chemical separation technique requires the addition of carriers
and radioactive tracers for chemical yield determinations, these are to be added prior
to beginning the fusion procedure, unless there is good technical justification for
doing otherwise (e.g., significantly elevated activity).
9.2.	Quality control samples are generally specified in the laboratory's quality manual or
in a project's analytical protocol specifications (APS). At the very minimum, the
following are suggested:
9.2.1.	A LCS, which consists solely of the reagents used in this procedure and a
known quantity of radionuclide spiking solution, shall be run with each
batch of samples. The concentration of the LCS should be at or near the
action level or level of interest for the project.
9.2.2.	One reagent blank shall be run with each batch of samples. The blank
should consist solely of the reagents used in this procedure (including tracer
or carrier from the analytical method added prior to the fusion process).
9.2.3.	A sample duplicate that is equal in size to the original aliquant should be
analyzed with each batch of samples. This provides assurance that the
laboratory's sample size reduction and subsampling processes are
reproducible.
9.3.	Batch quality control results shall be evaluated and meet applicable APS prior to
release of unqualified data. In the absence of project-defined APS or a project-
specific quality assurance project plan (QAPP), the quality control sample acceptance
criteria defined in the laboratory's Quality Manual and procedures shall be used to
determine acceptable performance for this method.
10.	Calibration and Standardization.
10.1. Refer to the individual chemical separation and analysis methods for calibration and
standardization protocols.
11.	Procedure
11.1. Fusion
11.1.1. In accordance with the data quality obj ectives (DQOs) and sample
processing requirements stated in the project plan documents, remove
extraneous materials from the asphalt roofing material sample using a clean
forceps or tweezers.
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11.1.2.	Weigh a labeled 250 mL (or 400 mL) glass beaker. Record the tare weight.
11.1.3.	Weigh out a representative -25 g (or larger) subsample into a 250 ml or 400
mL glass beaker and record the beaker plus sample weight. See Appendix A
for the asphalt roofing materials sampling procedure.
11.1.4.	Place the labeled beakers in a furnace at -200 C using tongs, ramp
temperature to 350 C for -30 minutes, ramp to 450 C for -15 minutes, and
ramp to 550 C-600 C and heat for -3 hours (or until black tar color is gone
and a grey ash remains).
11.1.5.	Remove the beakers using tongs and allow to cool.
11.1.6.	Weigh each beaker and record the final weight.
11.1.7.	Transfer the ashed sample to a small plastic sample container. Using a
Teflon or stainless steel spatula or equivalent, loosen and transfer the ashed
solids, scraping the beaker as needed to transfer the solids.
Note: Transfer the fiberglass that is present into the sample tube or container and
mix well with the ashed solids. The sample container should have enough space so that
effective mixing can occur when vortexing.
11.1.8.	Cap and mix well with a vortex mixer to homogenize sample. Use a spatula
(pressing and twisting) to grind up the fiberglass into the ash as well as
possible.
11.1.9.	Weigh out a representative 1-1.5 g aliquant of the ashed asphalt roofing
sample into a 250 mL zirconium crucible.
Note: The weight loss on ashing will be used to calculate the equivalent weight of pre-
ashed sample to allow the proper sample aliquant calculations. For example, if 1.5 g of
ash is taken for assay and the weight loss was about 20%, the ashed samples will
represent ~1.8 g of as received asphalt shingle. For Sr and Ra analyses, a reagent
blank of 150 mg Ca (prepared by evaporating 3 mL of 1.25M Ca(N03)2 for each
sample) should be added to the crucible as a blank simulant to ensure the blank
behaves like the asphalt roofing samples during the precipitation steps.
11.1.10.	Add the proper amount of tracer or carrier appropriate for the method being
used and the number of aliquants needed.
11.1.11.	Place crucibles on a hot plate and heat to dryness on medium heat.
Note: Heat on medium heat to dry quickly but not so high as to cause splattering.
11.1.12.	Add the following amounts of NaOH based on the aliquant size/analysis
required.
1.5 g for Pu, Am, U, Sr: 15 g NaOH
1 g for Ra:	10 g NaOH
11.1.13.	Place the crucibles with lids in the 600 C furnace using tongs.
11.1.14.	Fuse samples in the crucibles for -20 minutes.
Note: Longer times may be needed for larger particles.
11.1.15.	Remove hot crucibles from furnace very carefully using tongs, and transfer
to hood.
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11.1.16.	Add -25-50 mL of water to each crucible ~8 to 10 minutes (or longer) after
removing crucibles from furnace, and heat on hotplate to loosen and
dissolve solids.
11.1.17.	If necessary for dissolution, add more water and warm as needed on a
hotplate.
11.1.18.	Proceed to Section 11.2 for the actinide preconcentration procedure, 11.3 for
Sr preconcentration, or 11.4 for Ra preconcentration steps.
11.2. Preconcentration of Actinides (Pu, U, or Am) from Hydroxide Matrix
11.2.1.	Pipet 1 mL of Fe carrier (50 mg/mL) into a labeled 225 mL centrifuge tube
for each sample.
11.2.2.	Pipet 1 mg La/mL to each tube as follows:
Pu, U: 5 mL, 1 mg, La/mL
Am: 3 mL, 1 mg, La/mL
11.2.3.	Transfer each fused sample to a 225 mL centrifuge tube, rinse crucibles well
with water, and transfer rinses to each tube.
Note: A final rinse of 5 mL 3M HN03 may be added to rinse each crucible and then
added to tube.
11.2.4.	Dilute each sample to ~180 mL with water.
11.2.5.	Cool the 225 mL centrifuge tubes in an ice bath to approximately room
temperature.
11.2.6.	Pipet 1 mL 1.25M Ca(NC>3) 2 and 5 mL 3,2M (NLL^HPC^ into each tube.
11.2.7.	Cap tubes and mix well.
11.2.8.	Pipet 10 mL of 10 wt% TiCh into each tube, and cap and mix immediately.
11.2.9.	Cool 225 mL centrifuge tubes in an ice bath for approximately 10 minutes.
11.2.10.	Centrifuge tubes for approximately 6 minutes at 3500 rpm or more or as
needed.
11.2.11.	Pour off the supernatant and discard to waste.
11.2.12.	Add 1,5M HC1 to each tube to redissolve each sample in a total volume of
-60 mL.
11.2.13.	Cap and shake each tube to dissolve solids as well as possible.
11.2.14.	Dilute each tube to -170 mL with 0.01M HC1.
11.2.15.	Pipet 1 mL of 1.0 mg La/mL into each tube. Cap and mix.
11.2.16.	Pipet 5 mL of 10 wt% TiCh into each tube. Cap and mix.
11.2.17.	Add -25 mL of concentrated HF into each tube. Cap and mix well.
11.2.18.	Cool in ice bath for approximately 10 minutes to facilitate the precipitation.
11.2.19.	Centrifuge for approximately 5 to 10 minutes at 3500 rpm or more or as
needed.
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11.2.20.	Pour off supernatant, and discard to waste.
11.2.21.	Pipet 6 mL of 3M HNO3 - 0.25M H3BO3 into each tube.
11.2.22.	Cap, mix and transfer contents of the tube into a labeled 50 mL centrifuge
tube.
11.2.23.	Pipet 7 mL of 7M HNO3 and 8 mL of 2M A1(N03)3 into each tube, cap and
mix (shake or use a vortex stirrer), and transfer rinse to 50 mL centrifuge
tube.
11.2.24.	Pipet 3 mL of 3M HNO3 directly into the 50 mL centrifuge tube.
11.2.25.	Warm each 50 mL centrifuge tube in a hot water bath (or dry hot block) for
a few minutes, swirling to dissolve.
11.2.26.	Allow each 50 mL centrifuge tube to cool to room temperature
11.2.27.	Centrifuge the 50 mL centrifuge tubes at 3500 rpm for 5 minutes to remove
any traces of solids (may not be visible prior to centrifuging), and transfer
solutions to labeled beakers or tubes for further processing. Discard any
solids.
11.2.28.	Proceed directly to the Am, Pu, or U methods listed in Steps 1.1.1, 1.1.2, or
1.1.5.
11.3. Preconcentration of 90Sr from Hydroxide Matrix
11.3.1.	Transfer each fused sample to a 225 mL centrifuge tube, rinse crucibles well
with water, and transfer rinses to each tube.
11.3.2.	Dilute each sample to -150 mL with water.
11.3.3.	Cool the 225 mL centrifuge tubes in an ice bath to approximately room
temperature.
11.3.4.	Pipet 1.5 mL 1.25M Ca(NC>3)2 ,1 mL 50 mg/mL Fe carrier and 5 mL 3.2M
(NH4)2HP04 into each tube.
11.3.5.	Cap tubes and mix well.
11.3.6.	Allow 225 mL centrifuge tubes to sit for approximately 10 minutes.
11.3.7.	Centrifuge tubes for approximately 6 minutes at 3500 rpm or more or as
needed.
11.3.8.	Pour off the supernatant and discard to waste.
11.3.9.	Add 1.5M HC1 to each tube to redissolve each sample in a total volume of
-60 mL.
11.3.10.	Cap and shake each tube to dissolve solids as well as possible.
11.3.11.	Dilute sample aliquant in 225 mL tube to -170 mL with 0.01M HC1.
11.3.12.	Cap and mix tubes.
11.3.13.	Add -25 mL of concentrated HF into each tube. Cap and mix well.
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11.3.14.	Allow 225 mL tubes to sit for approximately 10 minutes.
11.3.15.	Centrifuge for approximately 5 to 10 minutes at 3500 rpm or more or as
needed.
11.3.16.	Pour off supernatant and discard to waste.
11.3.17.	Pipet 5 mL of concentrated HNO3 and 5 mL of 3MHNO3- O.25MH3BO3
into each 225 mL centrifuge tube to dissolve precipitate.
11.3.18.	Cap and mix well. Transfer contents of the tube into a labeled 50 mL
centrifuge tube.
11.3.19.	Pipet7 mL of 3M HNO3 and 7 mL of 2M A1(N03)3 into each tube, cap tube
and mix.
11.3.20.	Transfer the rinse solutions to 50 mL centrifuge tubes and mix well (shake
or use vortex stirrer).
11.3.21.	Centrifuge the 50 mL tubes at 3500 rpm for 5 minutes to remove any traces
of solids.
11.3.22.	Transfer solutions to labeled beakers or new 50 mL centrifuge tubes for
further processing.
11.3.23.	If solids remain, add 5 mL 3M HNC^to each tube, cap and mix well by
shaking or vortex stirrer, centrifuge for 5 minutes, and add the supernatant
to the sample solution. Discard any residual solids.
11.3.24.	Set aside for 90Sr analysis using Rapid Radiochemical Methodfor Total
Radiostrontium (Sr-90) in Building Materials for Environmental
Remediation Following Radiological Incidents (Step 1.1.4).
11.4. Preconcentration of 226Ra from Hydroxide Matrix
11.4.1.	Transfer each sample to a 225 mL centrifuge tube, rinse crucibles well with
water, and transfer rinses to each tube.
11.4.2.	Dilute to-150 mL with water.
11.4.3.	Add 15 mL concentrated HC1 to each tube.
11.4.4.	Cap and mix each tube well.
11.4.5.	Pipet 1 mL 1.25M Ca(N03)2into each tube.
11.4.6.	Add 10 mL 2M Na2CC>3 to each tube.
11.4.7.	Cap tubes and mix.
11.4.8.	Allow tubes to stand for approximately 10 minutes.
11.4.9.	Centrifuge tubes for 6 minutes at 3500 rpm.
11.4.10.	Pour off the supernatant and discard to waste.
11.4.11.	Pipet 10 mL 1,5M HC1 into each tube to dissolve precipitate. Cap and mix.
11.4.12.	Transfer sample solution to a 50 mL centrifuge tube.
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11.4.13.	Pipet 10 mL 1.5M HC1 into each 225 mL centrifuge tube to rinse. Cap and
rinse well.
11.4.14.	Transfer rinse solution to 50 mL tube and mix well by shaking well or
vortex stirrer.
Note: Typically, the HC1 added to dissolve the carbonate precipitate is sufficient to
acidify the sample. If the precipitate was unusually large and suspended solids remain,
additional acid may be needed. The pH can be checked to verify it is pH 1 or less. To
acidify the pH <1, add 1 or 2 mL of concentrated hydrochloric acid to the solution and
get it to clear. Tubes may be warmed in a water bath to help dissolve samples.
11.4.15.	If solids remain, add 5 mL 1.5M HC1 to each tube, cap and mix well,
centrifuge for 5 minutes and add the supernatant liquid to the sample
solution. Discard any residual solids.
11.4.16.	Set aside for 226Ra analysis using Rapid Radiochemical Methodfor Radium-
226 in Bitumen Aggregate, Stone or other Solid Samples for Environmental
Remediation Following Radiological Incidents (Step 1.1.3).
12. Data Analysis and Calculations
12.1.	Equations for determination of final result, combined standard uncertainty, and
radiochemical yield (if required) are found in the corresponding chemical separation
and analysis methods, with the units being provided by the project manager.
12.2.	An asphalt roofing subsample (-25 g) is ashed in a furnace at 550 C. A 1-1.5 g
aliquant of the ashed sample is taken for dissolution and analysis. The weight loss of
the subsample is used to determine the amount of as-received sample contained in the
1 -1.5 g ashed aliquant. Tracers are not added until the 1-1.5 g sample aliquant is
taken.
12.3.	The following calculation is performed to determine the amount of as-received (or
dried sample; see A12.1) asphalt roofing sample contained in the 1-1.5 g ashed
aliquant.
M = M x M' ~Mfa	(1)
Ma-M,
Mb = empty beaker tare weight (g)
Mi = total weight of initial as-received sample weight + beaker (g)
Ma = total weight of ashed sample + beaker (g)
Ms = aliquant of ash taken for analysis (g)
Mc = aliquant corrected for weight loss (g)
12.3.1. If the sample aliquants taken for analysis are split or serially diluted during
the fusion sample preparation method, the initial activity of tracer added to
the sample aliquant is used for calculations. The aliquant size used for
calculations, however, must be the effective amount of sample in the
aliquant into which the tracer is added. It is calculated as follows:
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Wa=Wsxdlxd2xd3
(2)
Where
d, = ^-,d0 =^^,and d, =
D D
(3)
and
Wa = sample aliquant size, used for analysis, in the units designated by the
project manager (e.g., kg, g, etc.).
Ws = initial size of the sample aliquant taken for fusion in the units designated
in analytical protocol specifications (e.g., kg, g, etc.).
Da# = mass or volume of the aliquant taken (i.e., the redissolved fusion cake or
subsequent dilution thereof) where # denotes the respective number of the
serial dilution from i to n, (e.g., 5.0 mL, etc.).
Ds# = mass or volume of the digestate from which Da# is taken, where # denotes
the number of the respective serial dilution from i to n (e.g., 20 mL, etc.).
Note: The Da# and Ds# must use the same units of mass or volume. If fewer than three
splits/dilutions are made, a factor of one (1) is substituted for the unneeded Da and Ds terms. If
no splits or dilutions are performed, Ws = Wa.
12.3.2. The actual activity of tracer added to the sample is used in the calculation of
the final sample results as described in Step 12.3.1. If the sample has been
split or diluted, the tracer activity used to calculate the radiochemical yield
must be modified to reflect the activity of tracer that would be present
theoretically in the final sample test source assuming 100% radiochemical
yield. It is calculated as follows:
At = activity of the tracer added to the sample aliquant at the reference
di, d2 and d3 are defined as described in Step 12.3.1.
Note: The Da# and Ds# must use the same units of mass or volume. If fewer than three
splits/dilutions are made, a factor of one (1) is substituted for the unneeded Da and Ds terms. If no
splits or dilutions are performed, At yid = At.
Where
theoretical activity in sample test source assuming 100%
radiochemical yield
(4)
date/time for the tracer
and
13. Method Performance
13.1.	Method validation results are to be reported.
13.2.	Expected turnaround time per sample.
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13.2.1.	For a representative 1 g aliquant of sample, the furnace heating and fusion
steps should add approximately 2 hours per batch to the time specified in the
individual chemical separation methods.
13.2.2.	The preconcentration steps should add approximately 2 to 2.5 hours per
batch.
Note: Processing times for the subsequent chemical separation methods are given in those
methods for batch preparations.
14.	Pollution Prevention
This method utilizes small volume (2 mL) extraction chromatographic resin columns. This
approach leads to a significant reduction in the volumes of load, rinse and strip solutions, as
compared to classical methods using ion exchange resins or solvent extraction techniques to
separate and purify the radionuclide fractions.
15.	Waste Management
15.1. Refer to the appropriate chemical separation methods for waste disposal information.
16.	References
Cited References
16.1.	EPA 2013. Rapid Radiochemical Methodfor Americium-241 in Building Materials for
Environmental Remediation Following Radiological Incidents. Office of Air and
Radiation, Washington, DC. EPA. Available here.
16.2.	EPA 2013. Rapid Radiochemical Methodfor Pu-238 and Pu-239/240 in Building
Materials for Environmental Remediation Following Radiological Incidents. Office
of Air and Radiation, Washington, DC. Available here.
16.3.	EPA. Improved Rapid Radiochemical Methodfor Radium-226 in Building Materials
for Environmental Remediation Following Radiological Incidents. Office of Air and
Radiation, Washington, DC. Not yet available.
16.4.	EPA 2013. Rapid Radiochemical Methodfor Total Radiostrontium (Sr-90) in Building
Materials for Environmental Remediation Following Radiological Incidents. Office
of Air and Radiation, Washington, DC. Available here
16.5.	EPA 2013. Rapid Radiochemical Methodfor Isotopic Uranium in Building Materials
for Environmental Remediation Following Radiological Incidents. Office of Air and
Radiation, Washington, DC. Available here.
16.6.	EPA 2009. Method Validation Guide for Qualifying Methods Used by Radiological
Laboratories Participating in Incident Response Activities. Revision 0. Office of Air
and Radiation, Washington, DC. EPA 402-R-09-006, June. Available here.
16.7.	EPA 2012. Radiological Laboratory Sample Analysis Guide for Incident Response 
Radionuclides in Soil. Revision 0. Office of Air and Radiation, Washington, DC. EPA
402-R-12-006, September. Available here. EPA 2004.
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16.8.	EPA 2004. Multi-Agency Radiological Laboratory Analytical Protocols Manual
(MARLAP). 2004. Volumes 1-3. Washington, DC: EPA 402-B-04-001A-C,
NUREG 1576, NTIS PB2004-105421, July. Available here.
16.9.	ASTM D228. "Standard Test Methods for Sampling, Testing, and Analysis of
Asphalt Roll Roofing, Cap Sheets, and Shingles Used in Roofing and Waterproofing"
ASTM Book of Standards 04.04, current version, ASTM International, West
Conshohocken, PA.
16.10.	ASTM D1193. "Standard Specification for Reagent Water" ASTM Book of
Standards 11.01, current version, ASTM International, West Conshohocken, PA.
16.11.	ASTMD2178. "Specification for Glass Felt Asphalt Shingles Used in Roofing and
Waterproofing" For Annual ASTM Book of Standards volume information, refer to
the standard's Document Summary page on ASTM website at www.astm.org.
16.12.	ASTM D3462. "Specification for Asphalt Shingles Made from Glass Felt and
Surfaced with Mineral Granules" For Annual ASTM Book of Standards volume
information, refer to the standard's Document Summary page on ASTM website at
www.astm.org.
16.13.	ASTMD4601. "Specification for Asphalt-Coated Glass Fiber Base Sheet Used in
Roofing" For Annual ASTM Book of Standards volume information, refer to the
standard's Document Summary page on ASTM website at www.astm.org.
16.14.	ASTM D4897. "Specification for Asphalt Shingles (Organic Felt) Surfaced with
Mineral Granules" For Annual ASTM Book of Standards volume information, refer
to the standard's Document Summary page on ASTM website at www.astm.org.
16.15.	ASTM D225. "Specification for Glass Felt Asphalt Shingles Used in Roofing and
Waterproofing" For Annual ASTM Book of Standards volume information, refer to
the standard's Document Summary page on ASTM website at www.astm.org.
16.16.	ASTM D2626. "Specification for Asphalt-Saturated and Coated Organic Felt Base
Sheet Used in Roofing" For Annual ASTM Book of Standards volume information,
refer to the standard's Document Summary page on ASTM website at www.astm.org.
16.17.	ASTM D6380. "Specification for Asphalt Roll Roofing (Organic Felt)" For Annual
ASTM Book of Standards volume information, refer to the standard's Document
Summary page on ASTM website at www.astm.org.
Other References
16.18.	EPA 2014. Rapid Methodfor Sodium Hydroxide Fusion of Concrete and Brick
Matrices Prior to Americium, Plutonium, Strontium, Radium, and Uranium Analyses
for Environmental Remediation Following Radiological Incidents. Office of Air and
Radiation. EPA-402-R-14-004, April. Revision 0 of rapid methods issued April 2014.
Available here.
16.19.	EPA 2010. Rapid Radiochemical Methods for Selected Radionuclides in Water for
Environmental Restoration Following Homeland Security Events, Office of Air and
Radiation. EPA 402-R-10-001, February. Revision 0.1 of rapid methods issued
October 2011. Available here.
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16.20. ASTM D3909. "Specification for Asphalt Roll Roofing (Glass Felt) Surfaced with
Mineral Granules" For Annual ASTM Book of Standards volume information, refer
to the standard's Document Summary page on ASTM website at www.astm.org.
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17. Tables, Diagrams, and Flow Charts
17.1. Fusion Flow Chart
Timeline for Rapid Fusion and Preparation of Asphalt
Roofing Samples for Precipitation and Analysis
Rapid Ashing and Fusion
1.	Add asphalt roofing sample aliquantto 250 mL or400 mL glass
beaker, (record beaker tare weight and sample weight) (11.1.2-
11.1.3).
2.	Heat beaker in furnace at -200 C, ramp immediately to 350 C
for -30 min, to 450 C for -15 minutes, then ramp to 550-600 C
for~3 hours oruntil solids are grey (11.1..4).
3.	Remove beakers and allowto cool (11.1.5).
4.	Weigh beaker and ashed sample (11.1.6).
5.	Transfer ashed sample to sample container and mix well with
vortex to homogenize (11.1.7-11.1.8).
6.	Weigh 1-1.5 g of homogenized sample ash into a 250-mL Zr
crucible (11.1.9).
7.	Add tracer (11.1.10)
8.	Place crucible on hot plate and heat to dryness (11.1.11).
9.	Add 15g NaOH pellets (10g Ra) to crucible (11.1.12).
10.	Heat -20 min at 600 C (11.1.13-11.1.14)
11.	Removefrom furnace and allowto cool (11.1.15).
Continued on Appropriate
Procedure Chart
5% hours
Actinide
Precipitation
Procedure
Phosphate/Fluoride
Precipitations for Sr
Procedure
Carbonate
Precipitation for Ra
Procedure
Prepare for precipitations
1. Add - 20-25 mL water to crucibles -8-10 minutes to dissolve
fused sample as much as possible and transferto centrifuge
tubes. Warm on hotplate to dissolve/loosen solids (11.1.16).
Elapsed Time
5 hours
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17.2. Actinide Precipitation Flow Chart
Actinide Precipitation Procedure
\
t
Actinide

Precipitation

Procedure

	y	
Continued from 17.1 Fusion Flowchart
1.	Add Fe and La to each tube (11.2.1-11.2.2) .
2.	Transfer to 225 mL tube. Rinse crucibles and transfer to
tubes (11.2.3)
3.	Dilute to 180 mL with water (11.2.4).
4.	Cool to room temperature in ice bath (11.2.5)
5.	Add 1 mL Ca and (NH4)2HP04 to each tube. Cap and mix
(11.2.6-11.2.7).
6.	Add 10 mL TiCI3 to each tube. Cap and mix . Cool in ice
bath for- 10 minutes (11.2.8-11.2.9).
7.	Centrifuge for 6 min and pouroff supernate (11.2.10-
11.2.11).
8.	Redissolve in a total of 60 mL of 1.5M HCI. Cap and mix
(11.2.12-11.2.13)
9.	Dilute to 170 mLwith 0.01M HCI (11.2.14).
10.	Add 1 mL La, 5 mL TiCI3, and ~ 25 mL HF and cool in ice
bath for 10 min(11.2.15-11.2.18).
11.	Centrifuge for5-10 min and pouroff supernate (11.2.19-
11.2.20).
12.	Redissolve in 6-mL 3M HNO3-0.25M H3B03 . Cap, mix and
transfert 50 mL centrifuge (11.2.21-11.2.22).
13.	Pi pet 7 mL - 7M HN03 and 8 mL-2M AI(N03)3 Cap and
mix and transfer rinse to 50 mL centrifuge tube (11.2.23).
14.	Pipet 3mL-3M HN03, warming to dissolve in 50-mL
centrifuge tube . Allow to cool. (11.2.24-11.2.26).
15.	Centrifuge to remove any trace solids. Transfer sample
solutions to new tubes or beakers and discard in traces of
solids (11.2.27).
16.	Analyze sample solutions forspecific actinides using rapid
methods forspecific actinides in building materials.
Elapsed Time
v 73A hours
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17.3. Strontium Precipitation Flow Chart
Strontium Precipitation Procedure
Continued from 17.1 Fusion Flowchart
1.	Transfer to 225 mL tube. Rinse crucible and transfer
to tube (11.3.1)
2.	Dilute to 150 mL with water (11.3.2).
3.	Cool in ice bath to room temperature (11.3.3).
4.	Add 1.5 mL 1.25 M Ca(N03)2, 1 mL Fe, and 5 mL
3.2M (NH4)2HP04 to each tube . Cap and mix
(11.3.4-11.3.5).
5.	Allow 225-mL tubes to sitfor~10min (11.3.6).
6.	Centrifuge for 6 min and pour off supernate (11.3.7-
11.3.8).
7.	Redissolve in 1.5M HCI to a total of 60 mL. Cap and
mix (11.3.9-11.3.10).
8.	Dilute to 170 mLwith 0.01 M HCI. Cap and mix
(11.3.11-11.3.12).
9.	Add 25 mL concentrated HF and wait -10 min
(11.3.13-11.3.14).
10.	Centrifuge for 5-10 min and pour off supernate
(11.3.15-11.3.16).
11.	Redissolve in 5 mL 3M HNO3-0.25M H3B03 and 5
mL concentrated HN03. Cap, mix and transfer to 50
mL centrifuge tube (11.3.17-11.3.18)
12.	Pi pet 7 mL 2M AI(N03)3 + 7 mL-3M HN03. Cap and
mix well. Transfer rinse solution to 50 mL tubes and
mix well (11.3.19-.11.3.20).
13.	Centrifuge for 5 min and discard trace solids.
Transfer to 50 mL tubes (11.3.21-11.3.22).
14.	Analyze sample solutions for 90Sr using 90Sr method
for building materials.
Ca3(P04)2 I CaF2
Precipitation for Sr
Procedure
Elapsed Time
73A hours
v.	
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17.4. Radium Precipitation Flow Chart
Carbonate Precipitation for Radium Procedure

\


Carbonate
Precipitation for
Radium Procedure


Continued from 17.1 Fusion Flowchart
1.	Transfer to 225 mL tube. Rinse crucible and transfer
to tube (11.4.1)
2.	Dilute to 150 mL with water (11.4.2).
3.	Add 15 mL concentrated HCI. Cap and mix (11.4.3-
11.4.4).
4.	Add 1 mL-1.25M Ca(N03)2 and 10 mL-2M NaC03
to each tube. Cap and mix (11.4.5-11.4.7)
5.	Allow to stand 10 min (11.4.8).
6.	Centrifuge for6 min and pour off supernate (11.4.9-
11.4.10).
7.	Redissolvein 10 mL-1.5 M HCI. Cap and mix
(11.4.11).
8.	Transfer to 50-mL centrifuge tubes (11.4.12).
9.	Rinse 225-mL tube with 10 mL 1.5M HCI and
transferto 50-mL tube (11.4.13).
10.	Cap and mix using vortex stirrer (11.4.14).
11.	Centrifuge for 5 min and discard trace solids
(11.4.15).
12.	Analyze sample solutions for 226Ra using 226Ra
method forbuilding materials (11.4.16).
Elapsed Time
\tVA hours
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Appendix A:
Rapid Technique for Sampling Asphalt Roofing Material
A1. Scope and Application
A1.1. The goal is to obtain representative sample aliquants from the asphalt roofing
material received.
A1.2. This method describes one approach for the rapid preparation of asphalt roofing
materials samples to yield representative aliquants for radiochemical analysis of
non-volatile radionuclides.
A1.3. The method is designed to be used as a preparatory step for the attached methods
for furnace heating and fusion of asphalt roofing materials for measurement of
241 Am, 238Pu, 239/2V U, 90Sr, and^Ra.
A2. Summary of Methods
A2.1. This method uses disposable equipment or materials to contact the sample, where
possible, minimizing the risk of contamination and cross-contamination and
eliminating concerns about adequate cleaning of equipment.
A2.2. The asphalt roofing material, as-received is cut into as small pieces as possible to
allow a -25 g subsample to be taken, which will be ashed in a furnace,
homogenized, as well as possible, and a smaller aliquant of the ashed sample is
taken. Additional replicate analyses may also be performed to provide further
assurance that analytical results are representative of asphalt roofing material
samples received.
A3. Definitions, Abbreviations, and Acronyms
A3.1. Discrete Radioactive Particles (DRPs or "hot particles"). Particulate matter in a
sample of any matrix where a high concentration of radioactive material is present
as a very small particle (
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Sodium Hydroxide Fusion of Asphalt Roofing Material Matrices
A5. Safety
A5.1. General
A5.1.1. Refer to your laboratory's safety manual for concerns of contamination
control, personal exposure monitoring, and radiation dose monitoring.
A5.1.2. Refer to your laboratory's chemical hygiene plan (or equivalent) for
general safety rules regarding chemicals in the workplace.
A5.2. Radiological
A5.2.1. Refer to your radiation safety manual for direction on working with
known or suspected radioactive materials.
A5.2.2. This method has the potential to generate airborne radioactive
contamination. The process should be carefully evaluated to ensure that
airborne contamination is maintained at acceptable levels. This should
take into account the activity level, and physical and chemical form of
contaminants possibly present, as well as other engineering and
administrative controls available.
A5.2.3. Hot particles (DRPs)
A5.2.3.1. Hot particles, also termed "discrete radioactive particles"
(DRPs), will usually be small, on the order of 1 mm or less.
DRPs typically are not evenly distributed in the media and
their radiation emissions are not uniform in all directions
(anisotropic).
A6. Equipment and supplies
A6.1. Balance, top-loading, range to accommodate sample size encountered, readability
to 1%, or better.
A6.2. Drying oven, at 11010 C.
A6.3. Disposable scoop, scraper, tongue depressor or equivalent.
A6.4. Metal snips to cut the asphalt roofing material samples.
A6.5. Plastic bag.
A6.6. Steel paint cans and lids (pint, quart, 2 quart, 1 gallon, as needed), used to dry
asphalt roofing material if needed.
A7. Reagents and Standards
No reagents needed.
A8. Sample Collection, Preservation and Storage
A8.1. Samples should be collected in appropriately sized plastic bags or other
containers.
A9. Quality Control
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A9.1. Batch quality control results shall be evaluated and meet applicable analytical
protocol specifications (APSs) prior to release of unqualified data. In the absence
of project-defined APS or a project-specific quality assurance project plan
(QAPP), the quality control sample acceptance criteria defined in the laboratory
quality manual and procedures shall be used to determine acceptable performance
for this method.
A10. Procedure
A10.1. Prepare the asphalt roofing sample for subsampling.
Note: Asphalt roofing material samples do not typically contain large amounts of moisture.
Large pieces of asphalt roofing material will require cutting into smaller pieces.
A10.1.1. Spread a large piece of plastic in a hood (or alternate paper material
which can be discarded to waste later).
A10.1.2. Remove the asphalt roofing sample for the sample container.
A10.1.2.1. Take representative samples randomly from different areas of
the asphalt roofing material by cutting the asphalt shingle
material into smaller sections using metal snips (unless
already cut into smaller pieces).
A10.1.2.2. Cut enough of the asphalt roofing material from the sections
or larger pieces into very small subsample pieces (<0.5 g) to
get a representative as-received sample of 100-250 g.
Note: Clean the metal snips between use with different samples.
A10.2. If the asphalt roofing material is visibly wet (or if requested), place the cut pieces
of asphalt shingles into a can or other container that can be heated (without lid) in
an oven at 11010 C and dry the asphalt roofing material.
Notes: Asphalt roofing material samples will typically be dry enough such that drying prior
to taking the subsample aliquant is not required, however it may be received wet due to
weather conditions. In the event samples are received that contain moisture, the samples
may be dried in a drying oven at 11010 C prior to taking the aliquant. It may be difficult
to obtain a constant weight with continued volatility of organics upon heating.
A10.3. Weigh the combined mass of the can/container, sample, and lid. If the percent
solids are required calculations. Remove can from oven and allow to cool. Place
lid on can for storage and weigh with lid on container.
A10.4. Store the asphalt roofing material sample in a properly labeled sample can, jar, or
bag.
A11. Calibration and Standardization
A11.1. Balances used shall be calibrated using National Institute of Standards and
Technology (NIST)-traceable weights according to the process defined by the
laboratory's quality manual.
A12. Data Analysis and Calculations
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Sodium Hydroxide Fusion of Asphalt Roofing Material Matrices
Note: Drying of asphalt roofing materials is not required unless the material received is visibly wet
or damp due to weather conditions. It may be difficult to dry to a constant weight. It may be difficult
to obtain a constant weight with continued volatility of organics upon heating.
A12.1. The percent solids (dry-to-as-received mass ratio) for each sample is calculated
from data obtained during the preparation of the sample as follows:
Md - Mt
% Solids =	^	 x 100
Masrec  Mtare
where:
Mdry = mass of dry sample + labeled can + lid (g)
Mtare = tare mass of labeled can + lid (g)
Masrec = mass of sample as received + labeled can + lid (g)
A12.2. If dried, convert the equivalent mass of sample, as received, to dry mass. Dry
mass is calculated from a measurement of the total as received mass of the sample
received as follows:
~  ,  . ,	~	% Solids
Dry Sample Equivalent = MloLil_asrcc x
where:
Mtotai-as rec = total mass of sample, as received (g)
A12.3. Results Reporting
A12.3.1. The result for percent solids and the approximate total mass of sample as
received should be reported for each result.
A13. Method Performance
A13.1. Results of method validation performance are to be archived and available for
reporting purposes.
A13.2. Expected turnaround time for these sample preparation steps is about 3 hours for
an individual sample and about 4 hours per batch.
A14. Pollution Prevention.
Not applicable.
A15. W aste Management
A15.1. All radioactive and other regulated wastes shall be handled according to
prevailing regulations.
A16. References
A16.1. EPA 2004. Multi-Agency Radiological Laboratory Analytical Protocols Manual
(MARLAP). 2004. Volumes 1-3. Washington, DC: EPA 402-B-04-001A-C,
NUREG 1576, NTIS PB2004-105421, July. Available here.
A16.2. International Union of Pure and Applied Chemistry (IUPAC) 1997. Compendium
of Chemical Terminology, 2nd ed. (the "Gold Book"). Compiled by A. D.
McNaught and A. Wilkinson. Blackwell Scientific Publications, Oxford. XML
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Sodium Hydroxide Fusion of Asphalt Roofing Material Matrices
on-line corrected version: http://goldbook.iupac.org/C01265.html (2006-) created
by M. Nic, J. Jirat, B. Kosata; updates compiled by A. Jenkins. Last update: 2010-
12-22.
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