EPA 402-R-12-009
www.epa.gov/narel
October 2012
Revision 0
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 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 Acid Digestion 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 ACID DIGESTION 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 digestion of air particulate filters, removable
contamination swipes and smears, and other similar sample matrices that may contain
non-refractory materials or the matrix substrate is not refractory, 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 rapid dissolution of glass-fiber or organic composition
filters, and the associated particulate deposition collected during air sampling events
following a radiological or nuclear incident. An alternate method for sodium
carbonate fusion is presented separately in the document, 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. 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 because of
refractory residuals or constituents. 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 to an air particulate filter sample must 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). In the absence of project-specific guidance,
measurement quality objectives (MQOs) may be based on the Analytical Action Levels
(AALs) and Required Method Uncertainties (MMR) found in the Radiological Sample
Analysis Guide for Incidents of National Significance — Radionuclides in Air.,
Appendix I (see Reference 16.2).
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/incidentguides.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 Acid Digestion of Glass-Fiber and Organic/Polymeric Composition Filters and Swipes
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 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 airborne particulate material. For organic filter matrices, an
additional one and one-half hours is expected for dry ashing the sample prior to
dissolution. 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 material and the
deposited particulates.
2.2. In the case of glass-fiber filters, the siliceous filter as well as deposited silicates are
dissolved with direct application of hydrofluoric acid. The addition of nitric and
hydrochloric acids facilitates the dissolution of the remaining solids. The sample
digestate is taken to dryness and re-dissolved in nitric acid in preparation for the
ensuing chemical separation techniques.
2.3. For filters composed of organic materials, such as cellulose or polypropylene, the
preliminary step of dry ashing in a 450 °C muffle furnace is taken to destroy the
organic filter material. Dissolution of the organic material in the sample is essential to
the success of the subsequent ion-exchange chromatography analytical separation
methodologies.
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 (M ARL AP) Manual (See
Reference 16.4).
4. Interferences and Limitations
4.1. Filters that contain large amounts of parti culate material may result in persistent
undissolved particulates in the digestion process during Step 11.2.5. These samples
may require repeated application of the digestion procedure 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.
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4.3. Most glass-fiber filters 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 aliquot that the
separation method will successfully process.
4.4. Some filters, particularly glass-fiber filters 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 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 filters are
provided for analysis, and that those filters 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 filter blanks will be
processed at the beginning of each project and the results of these analyses will
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.
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, 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.
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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 results 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.
4.9. In some cases the 1C may provide air volumes to be assigned to each filter and may
request that the results are reported in units of activity per volume of air.
4.9.1. In cases where the entire filter is used for analysis, the volume of air volume,
generally in liters or cubic meters, is used in place of the "1 filter" sample size
described above.
4.9.2. When the sample is split prior to analysis, the sample size must reflect the
product of the total sample volume 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.
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
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 filed samples.
4.15. This procedure uses hydrofluoric acid (HF) to digest glass filters and any siliceous
material in the sample. Do not use glass beakers in this method. The use of HF in glass
beakers will damage the beakers and could result in catastrophic failure of the beakers
during use, as well as the introduction of uranium and other radioactive constituents of
glass into the sample. Only PTFE (Teflon®) beakers, or others impervious to HF, are to
be used with this procedure.
4.16. Depending on the specific composition and manufacture, the PTFE beakers used in the
acid digestion portion of this procedure may have a melting point as low as 400 °C,
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with a recommended performance temperature as low as 200 °C. Care should be taken
to perform this portion of the procedure at operating temperatures of 200 °C or lower.
4.17. During the dry-ashing portion (Step 11.1.5) of this procedure, care should be taken to
ensure that the glass beakers and the ribbed watch glasses are sufficiently durable to
withstand the furnace temperature of 450 °C.
4.18. 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
5.3.1. Particular attention should be paid to addressing issues surrounding the use and
handling of hydrofluoric acid (HF). HF is an extremely dangerous chemical
used in this procedure. Appropriate PPE must be obtained and used in strict
accordance with the laboratory safety program specification. The laboratory is
strongly encouraged to consider having an appropriate topical binding agent,
such as calcium gluconate gel, immediately available in the laboratory area.
5.3.2. The acid digestion process alternately generates siliceous fluoride fumes and
strong acidic vapors, which present extreme respiratory hazards, as well as other
heath risks. The entire digestion process should be carried out in a laboratory
fume hood.
6. Equipment and Supplies
For samples with elevated activity concentrations of these radionuclides, labware should be
used only once due to potential for cross contamination. The laboratory safety manual should
provide guidance for making these decisions.
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6. 1 . Adjustable temperature laboratory hotplates.
6.2. Dispensing pipette, 5 mL delivery volume. Alternately, a bottle-top dispenser, small
volume graduated cylinder, or any other device for delivering nominal 5 mL volumes
of reagents into the sample beaker.
6.3. Teflon beakers, 250 mL capacity.
6.4. Teflon spatula or rubber policeman.
6.5. Tweezers or forceps.
6.6. For organic filter matrices, the following equipment will also be needed:
6.6. 1 . Muffle furnace, for heating to 450 °C.
6.6.2. Beakers, 250 mL capacity, Pyrex or equivalent.
6.6.3. Watch glasses, ribbed. These should be large enough to cover the beakers
during dry ashing.
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).
7. 1 . Boric Acid, HaBOs, available commercially.
7.2. Water.
7.3. Hydrochloric acid (12 M), Concentrated HC1, available commercially.
7.4. Hydrofluoric acid (28 M), Concentrated HF, available commercially.
7.5. Nitric acid (16 M), Concentrated HNCb, available commercially.
7.6. (For samples requiring Sr analysis) Nitric acid (8 M): Add 500 mL of concentrated
to 400 mL of water and dilute to 1 L with water.
7.7. 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 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., lanthanum 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 dissolution procedure, unless there is good technical
justification for doing otherwise.
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9.2. Batch quality control results shall be evaluated and meet applicable analytical project
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.
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 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.
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.
9.5. In the case of organic-matrix filters, precaution should be taken to ensure that the
tracers, carriers, and spiking solutions used in the QC samples remain soluble and do
not preferentially adhere to the vessel during the dry-ashing process (Step 11.1). For
samples that need to be dry-ashed, the tracers, carriers, and spiking solutions used in the
QC samples should be spiked onto an analyte-free material, such as ashless filter paper.
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 organic filter matrices, the preliminary step of destroying the filter by dry ashing is
necessary prior to dissolution of the particulate material. For glass-fiber filters, skip to
Step 11.2.
11.1.1. Remove the filter from its container or sleeve, using a clean forceps if
necessary, and transfer the filter into a 250-mL glass beaker.
11.1.2. If any loose particulate material is present transfer that material to the beaker
as well.
11.1.3. Add any necessary tracers or carriers, as prescribed in the subsequent
chemical separation methods, adding the solution directly onto the filter
material. The tracer solution should be absorbed into the filter material, if
possible.
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11.1.4. If the total volume of tracers used exceeds 2 mL, dry the sample on a hotplate
before proceeding. Otherwise, proceed directly to the next step.
11.1.5. Cover the beaker with a ribbed watch glass and heat in a muffle furnace at
450 °C for one hour, or until the sample is completely ashed.
11.1.6. Remove from furnace to cool, approximately 15 minutes.
11.1.7. When the beaker is cool, add 5 mL concentrated nitric acid and heat gently on
a hot plate to dissolve the ashed material. Use a spatula or rubber policeman,
if necessary, to dislodge the ashed material from the surface of the beaker.
11.1.8. Transfer the sample to a Teflon beaker.
11.1.9. Rinse the glass beaker and watch glass into the Teflon beaker using small
portions of an additional 5 mL rinse of concentrated nitric acid.
11.1.10. Rinse the glass beaker again into the Teflon beaker using a 5 mL rinse of
concentrated hydrochloric acid.
11.1.11. Add 5 mL concentrated HF to the Teflon beaker.
11.1.12. Go to Step 11.2.6.
11.2. For glass-fiber filters.
11.2.1. Remove the filter from its container or sleeve, using a clean forceps if
necessary, and transfer the filter into a 250-mL Teflon beaker.
11.2.2. If any loose particulate material is present transfer that material to the beaker
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 filter
material. The tracer solution should be absorbed into the filter material, if
possible.
11.2.4. In a fume hood, carefully add 5 mL concentrated hydrofluoric acid. The
reaction will be vigorous and will immediately destroy the glass filter
material.
11.2.5. Add 5 mL each of concentrated nitric acid and concentrated hydrochloric acid.
11.2.6. Heat the beaker on a hotplate to a maximum of 200° C, taking the sample to
dryness.
11.2.7. If the sample is to be analyzed for actinides, add approximately 0.5 g HsBOs,
otherwise skip to Step 11.2.8.
11.2.8. Add 5 mL concentrated HNCb and continue heating to re-dissolve the residue
and to effect a complete conversion to a nitrate environment.
11.2.9. Once the sample is dissolved, heat gently to dryness.
11.2.10. Proceed to the chemical separation methods. In all cases omit the initial
addition of tracers and carriers used for yield determinations, as those reagents
were added at the beginning of the digestion process.
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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.
11.2.10.1. For actinide analyses, proceed directly to any of those methods
listed in Steps 1.1.1, 1.1.2, or 1.1.3, proceeding directly to Step
11.2, "Actinide Separations using Eichrom resins"
11.2.10.2. For radium analysis, the sample will need to be converted to a
hydrochloric matrix before continuing. Proceed directly to the
method listed in Step 1.1.4, proceeding directly to Step 11.1.6,
"Reconstitute the sample with an additional 10 mL of hydrochloric
acid..."
11.2.10.3. For strontium analysis, dissolve sample residue in 5 mL 8 M
FDSTCb, then proceed directly to the method listed in Step 1.1.5,
proceeding directly to Step 11.11, "Set up a vacuum box for Sr-
Resin columns.."
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.
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 selection of equipment for volumetric and gravimetric measurements
should reflect the analytical requirements; the uncertainty of the measurement should
be controlled at a level that is consistent with the analysis Measurement Quality
Objectives (MQOs). 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:
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 11.2.10 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
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(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. The laboratory should ensure that the additional uncertainty associated with splitting
the sample is included in the calculation of the standard uncertainty of the sample
volume, generally referred to as u(Va) in the associated chemical separation methods
described in Section 1.1 above. The laboratory should also note in the case narrative, or
appropriate documentation, that this additional uncertainty has been incorporated into
the final combined standard uncertainty (CSU) calculation.
13. Method Performance
13.1. Method validation results may be found in the attached appendices.
13.2. Expected turnaround time per batch:
13.2.1. For 47-mm diameter glass-fiber filters, the digestion should add
approximately one hour to the time specified in the individual chemical
separation methods.
13.2.2. For 47-mm organic matrix filters requiring dry ashing and digestion,
approximately two and one-half hours should be required, in addition to the
time specified in the individual chemical separation methods.
14. Pollution Prevention: This method utilizes the smallest volumes of inorganic acids that are
reasonably expected to perform the required dissolution in the samples. This approach
significantly reduces the acid volumes and the energy required for drying, as compared to
conventional techniques that are standard in the industry.
15. Waste Management
15.1. For each sample analyzed, 20 - 25 mL concentrated inorganic acids, including nitric,
hydrochloric, and hydrofluoric, are dried completely and the volatilized vapors are
exhausted through the laboratory fume hood. The fume hood should be equipped with a
water scrubber or other means for removing the acid vapors from the exhaust air. The
resulting acidic effluent water should be evaluated to ensure that all local, state, and
federal disposal requirements are met.
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.
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.
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16.3. U.S. Environmental Protection Agency (EPA). 2010. RapidRadiochemical 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
Flow Chart of the Acid Digestion of Particulate Air Filters and Swipes
Elapsed Time
(hours)
Start
1.25 h
1.75 h
2.5 h
Organic Filters (Step 11.1)
Sample Transfer
1. Transfer sample to glass beaker.
2. Add tracers, dry on hotplate, if
necessary.
Dry Ash ing
1. Muffle at450°C.
Cooling
1. Remove sample from furnace to
cool.
Sample Transfer
1. Add5mLHNO3.
2. Heat on hotplate.
3. Transfer to Teflon beaker.
4. Rinse glass beaker with 5 ml
eachofHN03andHCI,
transferring rinses to Teflon
beaker.
ReagentAddition
1. Add 5 ml HF to Teflon beaker.
Glass Filters (Step 11.2)
Sample Transfer
1. Transfer sample to Teflon
beaker.
2. Add tracers.
ReagentAddition
1. AddSmLeachofHF, HNO3and
HCIto Teflon beaker.
Digestion
1. H eat at 200 °C to dry ness.
Acid Conversion
1. Add5mLHN03.
2. Heatto dryness.
Proceed to chemical separation
method
Elapsed Time
(hours)
Start
1 h
10-22-2012
12
Revision 0
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