EPA 402-R-12-008
www.epa.gov/narel
October 2012
Revision 0
Rapid Method for Sodium Carbonate Fusion of
Glass-Fiber and Organic/Polymeric Composition
Filters and Swipes Prior to Isotopic Uranium,
Plutonium, Americium, Strontium, and Radium
Analyses for Environmental Remediation
Following Homeland Security Events
U.S. Environmental Protection Agency
Office of Air and Radiation
Office of Radiation and Indoor Air
National Air and Radiation Environmental Laboratory
Montgomery, AL 36115
Office of Research and Development
National Homeland Security Research Center
Cincinnati, OH 45268
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Rapid Method for Sodium Carbonate Fusion of Glass-Fiber and Organic/Polymeric Composition Filters and Swipes
Revision History
Revision 0 | Original release. | 10/22/2012 |
This report was prepared for the National Air and Radiation Environmental Laboratory of the Office of
Radiation and Indoor Air and the National Homeland Security Research Center of the Office of Research
and Development, United States Environmental Protection Agency. It was prepared by Environmental
Management Support, Inc., of Silver Spring, Maryland, under contract EP-W-07-037, work assignments
B-41 and 1-41, all managed by David Carman. Mention of trade names or specific applications does not
imply endorsement or acceptance by EPA.
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RAPID METHOD FOR SODIUM CARBONATE FUSION OF GLASS-FIBER AND
ORGANIC/POLYMERIC COMPOSITION FILTERS AND SWIPES PRIOR TO ISOTOPIC URANIUM,
PLUTONIUM, AMERICIUM, STRONTIUM, AND RADIUM ANALYSES
1. Scope and Application
1.1. The method will be applicable to the fusion digestion of air particulate filters,
removable contamination swipes and smears, and other similar sample matrices, prior
to the chemical separation procedures described in the following procedures (see
Reference 16.3l):
1.1.1. Rapid Radiochemical Method for Americium-241 in Water for Environmental
Remediation Following Homeland Security Events.
1.1.2. Rapid Radiochemical Method for Plutonium-238 and Plutonium-239/240 in
Water for Environmental Remediation Following Homeland Security Events.
1.1.3. Rapid Radiochemical Method for Isotopic Uranium in Water for Environmental
Remediation Following Homeland Security Events.
1.1.4. Rapid Radiochemical Method for Radium-226 in Water for Environmental
Remediation Following Homeland Security Events
1.1.5. Rapid Radiochemical Method for Total Radiostrontium (Sr-90) in Water for
Environmental Remediation Following Homeland Security Events.
1.2. The method is specific for the fusion of glass-fiber and organic/polymeric composition
filters, swipes, and smears, and the associated particulate deposition collected during air
sampling events and removable contamination surveys following a radiological or
nuclear incident. An alternate method using inorganic acids is presented separately
in the document, Rapid Method for Acid Digestion of Glass-Fiber and Organic/
Polymeric Composition Filters and Swipes Prior to Isotopic Uranium, Plutonium,
Americium, Strontium, and Radium Analyses. Generally, the sodium carbonate fusion
technique should be chosen when refractory constituents are suspected in the sampled
particulates or when the acidic digestion procedure is otherwise deemed to be
ineffective. The Incident Commander (or designee, 1C) should be involved in the
selection of the appropriate digestion technique.
1.3. 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 (see
Reference 16.1), or the protocols published by a recognized standards organization for
method validation.
1.3.1. In the absence of project-specific guidance, measurement quality objectives
(MQOs) for air particulate samples may be based on the Analytical Action
Levels (AALs) and Required Method Uncertainties (zv) found in the
1 Revision 0.1 for all five rapid methods in water were released in October 2011 and are available at www.epa.gov/
erln/radiation.html and www.epa.gov/narel/incident guides.html. These revisions addressed typographical errors,
improved wording consistency with other methods, and clarified some examples. There were no substantive changes
to any of the methods.
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Rapid Method for Sodium Carbonate Fusion of Glass-Fiber and Organic/Polymeric Composition Filters and Swipes
Radiological Sample Analysis Guide for Incidents of National Significance —
Radionuclides in Air., Appendix I (see Reference 16.2).
1.3.2. In the absence of project-specific guidance, measurement quality objectives
(MQOs) for swipe samples may be based on the Analytical Action Levels
(AALs) derived from the Removable Contamination Values found in 10 CFR
835, Appendix D, with a default Required Method Uncertainty (WMR) of not more
than 13% at the AAL.
1.4. As this method is a gross pre-treatment 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.
1.5. The dissolution of glass-fiber filters, or similar swipes, by this method is expected to
take approximately one hour. This is based on a sample consisting of one 47-mm
diameter filter, loaded with approximately 10 mg of particulate material. For organic
filter or swipe matrices, an additional fifteen minutes is expected for charring the sample
prior to fusion. For the dissolution of larger filters, or filters loaded with significantly
more parti culate material, additional time and proportionately larger volumes of reagents
may be required.
2. Summary of Method
2.1. The method is based on the complete dissolution of both the filter or swipe material and
the deposited particulates.
2.2. In the case of glass-fiber media, the media and the deposited particulates are destroyed
by fusion with molten sodium carbonate in a nickel or platinum crucible. The resulting
fusion cake is dissolved in hydrochloric acid in preparation for the ensuing chemical
separation techniques.
2.3. For media composed of organic matrices, such as cellulose or polypropylene, the sample
is charred in a crucible prior to fusion.
3. Definitions, Abbreviations and Acronyms
3.1. Discrete Radioactive Particles (DRPs or "hot particles"). Parti culate matter in a sample
of any matrix where a high concentration of radioactive material is contained in a tiny
particle (um range).
3.2. Multi-Agency Radiological Analytical Laboratory Protocol (MARLAP) Manual (see
Reference 16.4).
3.3. The use of specific terminology, such as "filter," "swipe," "smear," etc., throughout this
method is not intended to be limiting or prescriptive, and the terms may be used
interchangeably. In cases where the distinction is important, the specific issues related
to a particular sample type will be discussed.
4. Interferences and Limitations
4.1. Samples that contain large amounts of parti culate material may result in persistent
undissolved particulates in the fusion melt during Step 11.7. These samples may require
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additional time in the hot fusion process to cause a complete dissolution of the
particulates.
4.2. In some cases particulate material may become dislodged during shipping or handling
and may be found loose in the shipping envelope or container. For these samples, care
should be taken to ensure a quantitative transfer of the sample to the digestion vessel. In
some cases, it may become necessary to include the envelope for ashing and digestion,
to ensure a quantitative transfer of material. Irregularities in sample processing such as
these should be thoroughly documented and reported in the case narrative.
4.3. Most glass-fiber filters and swipes contain significant amounts of barium, which may
ultimately interfere with the separation and analysis of radium, where that analyte is
required. Initial characterization of the filter matrix to determine the content of
elemental barium may help the laboratory make decisions about the optimum sample
aliquant that the separation method will successfully process.
4.4. Some media, particularly glass-fiber filters and swipes, contain measurable quantities
of naturally occurring radionuclides, such as uranium. The radionuclides native to the
filter matrix should be measured and this activity should be considered in the
assessment of the particulate results.
Matrix blanks, prepared with new, uncontaminated filters or swipes should be requested
by the incident commander to assess the concentration of radionuclides native to the
filter material. This may be done outside the scope of the initial background
determination for the project, especially if the manufacture or lot number changes
during the project.
4.4.1. In the preparation and analysis of matrix blanks the laboratory should verify
with the incident commander that a sufficient number of blank samples are
provided for analysis, and that those samples are of the same manufacture and
lot (if practicable) as those used in the incident sampling.
4.4.2. In the absence of specific direction from the incident commander or in the
project specifications, at least three uncontaminated blank samples should be
processed at the beginning of each project and the results of these analyses
should be properly identified and reported to the incident commander.
4.5. In the analysis of air filters, where the available sample is limited and irreplaceable, the
laboratory is strongly encouraged to reserve an aliquant of the sample digestate to allow
for unforeseen analysis requirements, and to guard against the loss of sample through
failure of the method or laboratory error. It is acknowledged that the creation of a
reserve aliquant may not be possible in all cases, particularly where very low detection
limits are required and the entire sample must be used.
4.6. Samples for which the creation of a reserve aliquant is appropriate, as well as samples
with elevated activity and samples that require multiple analyses from a single filter,
may need to be split after dissolution. In these cases care should be taken to carefully
measure the initial digestate and the split fractions to ensure that the sample aliquant for
analysis is accurately determined. The creation of multiple aliquants of a sample should
be thoroughly documented and reported in the case narrative.
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4.7. Samples that require the creation of multiple aliquants, or samples that require analyses
for which the addition of tracers and carriers necessary for other tests may be an
interferent (e.g., gross alpha/beta analyses), may necessitate the addition of those tracers
and carriers to the individual split fractions of the sample, after dissolution. This
necessary addition of tracers or carriers after the sample dissolution should be
thoroughly documented and reported in the case narrative.
4.8. The subsequent chemical separation methods for water samples, which are referenced in
Section 1.1 above, specify a sample size (in liters), which is used in the associated
calculation of activity, uncertainty, etc.
4.8.1. When this method is employed and the entire volume of digestate is processed
in the subsequent chemical separation method, a sample size of "1 filter" is used
in lieu of the water volume in all calculations, with the final result reported in
units of activity per filter, rather than activity per liter.
4.8.2. In cases where the filter digestate is split prior to analysis the fractional aliquant
of the filter is used for the sample size. The calculation of the appropriate
sample size used for analysis is described in Section 12, below.
4.9. In some cases, the 1C may provide air volumes or areal sample sizes to be assigned to
each filter or swipe and may request that the results are reported in units of activity per
volume of air or activity per area.
4.9.1. In cases where the entire filter sample is used for analysis, the volume of air,
generally in liters or cubic meters, is used in place of the "1 filter" sample size
described above.
4.9.2. In cases where the entire swipe is used for analysis, the areal sample size,
generally in square centimeters or square meters, is used in place of the "1
filter" sample size described above.
4.9.3. When the sample is split prior to analysis, the sample size used for analysis
must reflect the product of the total sample size times the fractional aliquant of
the filter used for analysis.
4.10. Where volumetric or areal sample sizes are provided by the 1C and used in the
calculation of sample activity concentrations, the laboratory should note in the case
narrative whether the uncertainties associated with these volumetric or areal
measurements are included in the calculated combined standard uncertainty using this
method.
4.11. As with any analytical method, QC requirements may be superseded by the 1C and the
project specifications. Nonetheless, this method attempts to address QC requirements
and considerations, particularly those associated with the unique nature of air filters and
swipes.
4.12. Duplicate analyses are not generally possible in air filters. Consequently, this procedure
does not address the preparation of duplicate samples for analysis.
4.13. Similarly, matrix spikes are not generally possible, nor are they required in this
procedure. At the direction of the incident commander, a specific sample may be
requested for spiking and analysis. While the 1C may use these results to evaluate
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potential matrix effects in the sample, this is not considered a matrix spike by the
laboratory, and the laboratory will not correct or control a batch of samples based on
the results.
4.14. In the preparation of blank samples and LCSs, care should be taken to create these QC
samples as early in the process as possible, and to follow the same tracer/carrier
additions, digestion process, and sample splitting used for the field samples.
4.15. Although this method is applicable to a variety of subsequent chemical separation
procedures, it is not appropriate where the analysis of volatile constituents such as
iodine or polonium is required. The user of this method must ensure that analysis is not
required for any radionuclide that may be volatile under these sample preparation
conditions, prior to performing this procedure.
5. Safety
5.1. General
5.1.1. Refer to your laboratory safety manual for concerns of contamination control,
personal exposure monitoring and radiation dose monitoring.
5.1.2. Refer to the laboratory 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 will be small, on the order of 1 mm or less. Discrete
radioactive particles are typically not evenly distributed in the media and
their radiation emissions are not uniform in all directions (anisotropic).
5.2.1.2. Filter media should be individually surveyed for the presence of these
particles, and this information should accompany the samples during
processing.
5.3. Procedure-Specific Non-Radiological Hazards:
This procedure employs molten salts generated under high temperatures (~ 1,000 °C) in
an open flame. The operator should exercise extreme care when using the burners and
when handling the hot crucibles. Thermal protection gloves and a face shield are
recommended when performing this part of the procedure. The entire fusion process
should be carried out in a laboratory fume hood.
6. Equipment and Supplies
6.1. Adjustable temperature laboratory hotplates.
6.2. Balance, top loading or analytical, readout display of ± 0.1 g or less.
6.3. Beakers, 250 mL capacity.
6.4. Crucibles, minimum 50 mL capacity, nickel or platinum.
6.5. Dispensing pipette, 10 mL delivery volume. Alternately, a bottle-top dispenser, small
volume graduated cylinder, or any other device for delivering nominal 10 mL volumes
of reagent into a beaker or disposable cup.
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6.6. Fisher blast burner or Meeker burner.
Note: Ordinary Bunsen burners will not achieve the high temperatures needed for fusion.
6.7. pH paper.
6.8. Ring stand with ceramic triangle (optional).
6.9. Teflon spatula or glass rod.
6.10. Tongs for handling crucibles. Should be tipped with platinum if platinum crucibles are
used.
6.11. Transfer pipette.
6.12. Tweezers or forceps.
7. Reagents and Standards
Note: Unless otherwise indicated, all references to water should be understood to mean Type I Reagent
water (ASTM D1193, see Reference 16.5).
Note: All reagents are ACS grade or equivalent unless otherwise specified.
7.1. Sodium Carbonate, anhydrous. Note that anhydrous sodium carbonate should be
stored in a desiccator.
7.2. Hydrochloric acid (6 M). Carefully add 500 mL of concentrated HC1 to 400 mL of
water and dilute to 1 L with water.
7.3. Radioactive tracers/carriers (used as yield monitors) and spiking solutions. Refer to
the chemical separation method(s) to be employed upon completion of this
dissolution technique. Any tracers/carriers that are used to monitor radiochemical/
chemical yield should be added at the beginning of this procedure. This allows for the
monitoring of chemical losses in the digestion process, as well as in the chemical
separation method. Carriers used to prepare sample test sources but not used for
chemical yield determination (e.g., neodymium added for uranium fluoride
precipitation), should be added where indicated.
8. Sample Collection, Preservation, and Storage
There are no special collection, preservation, or storage considerations for this method.
9. Quality Control
9.1. In all cases, 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.
9.2. Batch quality control results shall be evaluated and meet applicable analytical project
specifications (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 quality manual and
procedures shall be used to determine acceptable performance for this method.
9.3. A laboratory control sample (LCS), which consists solely of the reagents used in this
procedure and a known quantity of radionuclide spiking solution, shall be run with
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each batch of samples. The concentration of the LCS should be at or near the action
level or level of interest for the project
9.4. One reagent blank shall be run with each batch of samples. The reagent blank should
consist solely of the reagents used in this procedure. The reagent blank should not
include a blank filter or swipe.
9.5. The purpose and use of matrix blanks is described in Section 4.4. At the discretion of
the 1C, when matrix blanks are analyzed with each batch and the native filter
constituents are sufficiently well characterized so that incidents of laboratory
contamination may be differentiated from native blank filter activity, the use of
reagent blanks described in this section may be omitted.
9.6. This method does not define quality control parameters or acceptance criteria. Those
quality control factors are defined in the individual separation methods that follow
this technique.
10. Calibration and Standardization.
10.1. Refer to the individual chemical separation and analysis methods for calibration and
standardization protocols.
11. Procedure
11.1. For glass-fiber sampling media, proceed to Step 11.3.
11.2. For organic sampling media, the sample should first be charred in the crucible to
minimize violent reaction during the fusion process.
11.2.1. Remove the filter from its container or sleeve, using clean forceps if
necessary, and transfer the filter into a nickel or platinum crucible.
11.2.2. If any loose particulate material is present transfer that material to the
crucible as well.
11.2.3. Add any necessary tracers or carriers, as prescribed in the subsequent
chemical separation methods, adding the solution directly onto the sample
material. The tracer solution should be absorbed into the sample material, if
possible.
11.2.4. Gradually warm the uncovered crucible over the low flame of a Meeker or
Fisher blast burner to dry the tracer and carrier solutions. The crucible may
be held over the flame with tongs or supported on a ring stand with a
ceramic triangle.
11.2.5. Increase the flame, heating the crucible gradually until the sample begins to
char. Care should be taken to avoid open combustion (flaming) of the
sample, which could result in the loss of analyte in the escaping ash and
fume. Rather, the sample should be slowly charred. In addition, the crucible
lid should be readily available and the crucible should be covered and
removed from the heat if open combustion appears to be imminent.
11.2.6. Maintain this heat and continue until the sample appears to be completely
charred.
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11.2.7. Remove the crucible from the heat and allow it to cool for approximately
two minutes.
11.2.8. Add 2 g anhydrous Na2CC>3 to the crucible.
11.2.9. Thoroughly mix the sample with the added Na2CC>3 using a Teflon spatula
to avoid damage to the crucible.
11.2.10. Cover the mixed sample with another 2 g Na2CC>3.
11.2.11. Proceed to Step 11.4.
11.3. For glass-fiber media, the sample can be fused whole, without pretreatment.
11.3.1. Add 2 g anhydrous Na2CC>3 to the bottom of a nickel or platinum crucible.
11.3.2. Remove the filter from its container or sleeve, using forceps if necessary,
and transfer the filter into the crucible.
11.3.3. If any loose particulate material is present transfer that material to the
crucible as well.
11.3.4. Carefully and slowly add any necessary tracers or carriers, as prescribed in
the subsequent chemical separation methods, adding the solution directly
onto the sample material. The tracer solution should be absorbed into the
sample material, if possible.
11.3.5. Cover the sample with another 2 g Na2CC>3.
11.3.6. Proceed to Step 11.4.
11.4. Warm the crucible slowly over the low flame of a Meeker or Fisher blast burner. The
initial heating may produce a vigorous reaction, which may last approximately 5
minutes. It is important to perform this step very carefully to avoid losses due to
sample sputtering or boiling over the rim of the crucible.
11.5. After the initial reaction has subsided, increase the heat gradually over 5 minutes until
the Meeker or Fisher blast burner is at full flame.
11.6. Continue heating until the crucible glows bright red.
11.7. Continue heating over full flame for 5 minutes. The sample should be fully fused,
with a completely liquid and homogenous melt, and there should be no visible
reaction occurring in the melt. If this is not the case, continue heating over full flame
until the fusion process is complete.
11.8. Remove the crucible from the flame and swirl the contents so that the melt solidifies
on the sides of the crucible, approximately half-way up the sides. This will facilitate
the rapid dissolution of the cooled melt.
11.9. Allow the crucible and contents to cool approximately five minutes. The crucible
should be cool enough to handle and to allow for the addition of hydrochloric acid
without violent reaction.
11.10. When the crucible is moderately cool carefully add approximately 10 mL of 6 M HC1
by using a clean transfer pipette to wash the solid fusion cake down the inside walls
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of the crucible. The reaction may be vigorous and care should be taken to avoid
frothing the sample over the top of the crucible.
11.11. If necessary, heat the crucible gently on a hotplate and occasionally swirl the sample
to facilitate the dissolution of the fusion cake. Ensure that the entire fusion cake is
dissolved and that no solid material remains on the sides of the crucible.
11.12. If necessary, add additional 6 M HC1 in small (~1 mL) increments to facilitate the
complete dissolution of the fusion cake.
11.13. Transfer the dissolved sample to an appropriately sized beaker, rinsing the crucible
with 6 M HC1 to ensure a quantitative transfer of material.
11.14. Proceed to the chemical separation methods. In all cases omit the addition of tracers
and carriers, as those reagents were added at the beginning of the fusion process:
Note: The counting time stated in Section 1.4 of the applicable rapid water method must
be reevaluated for the required air filter or swipe MQOs as well as the expected
chemical yield, aliquanting of the sample, and for air filters a nominal sample volume.
11.14.1. For actinide analyses, proceed directly to any of those methods listed in
Sections 1.1.1, 1.1.2, or 1.1.3, proceeding directly to Step 11.1.4, "Calcium
phosphate coprecipitation option, " and following the calcium phosphate
coprecipitation to remove the excess sodium added during the fusion
process.
11.14.2. For radium analysis, proceed directly to the method listed in Section 1.1.4,
proceeding directly to Step 11.2, "Water Sample Preparation andPre-
concentration of Radium on MnO2 Resin. "
11.14.3. For strontium analysis, dilute the sample to 0.2 L with water and proceed
directly to the method listed in Section 1.1.5, proceeding directly to Step
11.1, "For each sample in the batch...." Note that if the sample is already at
a pH less than 2, no additional nitric acid will be added.
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 exception that the sample size is calculated as described
below, with the units being provided by the 1C, rather than liters of water.
12.2. In cases where the creation of a reserve aliquant is appropriate, as well as samples with
elevated activity and samples that require multiple analyses from a single filter, the
sample should be split after dissolution. In these cases care should be taken to carefully
measure the mass or volume of the entire final digestate, and the mass or volume of the
subsequent split fractions to ensure that the sample aliquant for analysis is accurately
determined. The creation of multiple aliquants of a sample should be thoroughly
documented and reported in the case narrative.
12.3. The sample aliquant size for analysis is calculated:
Va = Vsx(Da/Ds)
Where:
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r\
Vs = the original sample size, in the units designated by the 1C (e.g., 100 cm ,
68.5 m3, etc.)
Ds = the mass or volume of the entire final digestate, created in Step 11.13 of this
procedure (e.g., 100 g, 50 mL, etc.).
Da = the mass or volume of the aliquant of digestate used for the individual
analyses, as described in the various parts of Step 11.14 of this procedure
(e.g., 25 g, 5.0 mL, etc.). Note that the values for Da must be in the same
units used in Ds.
Va = the sample aliquant size, used for analysis, in the units designated by the 1C
(e.g., 25 cm2, 6.85 m3, etc.).
12.4. In cases where the sample will not be split prior to analysis, the sample aliquant size is
simply equal to the original sample size, in the same units requested by the 1C.
13. Method Performance
13.1. Method validation results are to be reported.
13.2. Expected turnaround time per sample;
13.2.1. For 47-mm diameter glass-fiber filters, the fusion should add approximately
45 minutes to the time specified in the individual chemical separation
methods.
13.2.2. For 47-mm organic matrix filters, charring the sample and the subsequent
fusion should add approximately one hour to the time specified in the
individual chemical separation methods.
These expected turnaround times are for a single sample preparation, without regard to
batching efficiencies, if any. This process is generally not amenable to simultaneous
preparation of multiple samples. Turnaround times for the subsequent chemical
separation methods are given in those methods for batch preparations.
14. Pollution Prevention: With the exception of minute quantities of combustion products, this
method inherently produces no significant pollutants. The sample and fusion reagents are
retained in the final product and are carried into the ensuing chemical separation techniques,
which marginally increases the salt content of the effluent waste. It is noted that if the
sampled particulates include radionuclides which may be volatile under the fusion
conditions, these constituents will be exhausted through fume hood system.
15. Waste Management
15.1. Refer to the appropriate chemical separation methods for waste disposal information.
16. References
16.1. U.S. Environmental Protection Agency (EPA). 2009a. 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 at: www.epa.gov/narel/incident guides.html and
www.epa.gov/erln/radiation.html.
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16.2. U.S. Environmental Protection Agency (EPA). 2009b. Radiological Laboratory Sample
Analysis Guide for Incidents of National Significance-Radionuclides in Air. Revision 0.
Office of Air and Radiation, Washington, DC. EPA 402-R-09-007, June. Available at:
www.epa.gov/narel/incident guides.html and www.epa.gov/erln/radiation.html.
16.3. U.S. Environmental Protection Agency (EPA). 2010. Rapid Radiochemical Methods for
Selected Radionuclides in Water for Environmental Restoration Following Homeland
Security Events, Office of Air and Radiation, National Air and Radiation
Environmental Laboratory. EPA 402-R-10-001, February. Revision 0.1 of rapid
methods issued October 2011. Available at: www.epa.gov/narel/incident_guides.html
andwww.epa.gov/erln/radiation.html.
16.4. MARLAP. 2004. Multi-Agency Radiological Laboratory Analytical Protocols Manual.
Volumes 1-3. Washington, DC: EPA 402-B-04-001A-C, NUREG 1576, NTIS
PB2004-105421. July. Available at: www.epa.gov/radiation/marlap/.
16.5. ASTM Dl 193, "Standard Specification for Reagent Water" ASTM Book of Standards
11.01, current version, ASTM International, West Conshohocken, PA.
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17. Flowchart
Elapsed Time
(minutes)
Start
30 min.
50 min.
60 min.
Organic Media (Step 11.2)
Sample Transfer
1. Transfer sample to crucible.
2. Add tracers.
Charring
1. Char sample over Meeker
burner.
Reagent Addition
1. Add 2 g Na2C03 to crucible.
2. Mix with spatula.
3. Add additional
Glass Fiber Media (Step 11.3)
Reagent Addition
1. Add 2 g NaiCOs to crucible.
I
Sample Transfer
1. Transfer sample to crucible.
2. Add tracers.
Reagent Addition
1. Add additional 2 gNa2C03.
Fusion
1. Heat sample to clear, quiescent
melt.
2. Cool.
Dissolution of Fusion Cake
1. Add 10 ml 6 M HCI.
2. Heat on hotplate to aid
dissolution.
3. Transfer solution to beaker.
Proceed to chemical separation
method
Elapsed Time
(minutes)
Start
15 min.
35 min.
45 min.
10-22-2012
12
Revision 0
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