Designation: C1001 − 11

Standard Test Method for

Radiochemical Determination of Plutonium in Soil by Alpha
Spectroscopy1
This standard is issued under the fixed designation C1001; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope D3084 Practice for Alpha-Particle Spectrometry of Water

1.1 This test method covers the determination of plutonium D3648 Practices for the Measurement of Radioactivity
in soils at levels of detection dependent on count time, sample D7282 Practice for Set-up, Calibration, and Quality Control
size, detector, background, and tracer yield. This test method of Instruments Used for Radioactivity Measurements
describes one acceptable approach to the determination of 3. Summary of Test Method
plutonium in soil.
3.1 Plutonium is extracted from the soil with a mixture of
1.2 This test method is designed for 10 g of soil, previously nitric, hydrofluoric, and hydrochloric acids in the presence of
collected and treated as described in Practices C998 and C999, 242
Pu or 236Pu isotopic tracer (See Appendix for purification
but sample sizes up to 50 g may be analyzed by this test and standardization of 236Pu tracer). Plutonium is isolated by
method. This test method may not be able to completely anion exchange, then electrodeposited onto a polished metal
dissolve all forms of plutonium in the soil matrix. disk for determination by alpha spectrometry. As an option, the
1.3 The values stated in SI units are to be regarded as plutonium may be prepared for alpha spectrometry measure-
standard. The values given in parentheses are for information ment by using coprecipitation with neodymium fluoride. The
only. range of chemical yield is between 40 and 90 %. The test
1.4 This standard does not purport to address all of the method is based on a published procedure (1).3
safety concerns, if any, associated with its use. It is the
4. Significance and Use
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 4.1 A soil sampling and analysis program provides a direct
bility of regulatory limitations prior to use. Specific hazard means of determining the concentration and distribution of
statements are given in Section 9. radionuclides in soil. A soil analysis program has the most
significance for the preoperational monitoring program to
2. Referenced Documents establish baseline concentrations prior to the operation of a
2.1 ASTM Standards:2 nuclear facility. Soil analysis, although useful in special cases
C859 Terminology Relating to Nuclear Materials involving unexpected releases, is a poor technique for assess-
C998 Practice for Sampling Surface Soil for Radionuclides ing small incremental releases and is therefore not recom-
C999 Practice for Soil Sample Preparation for the Determi- mended as a method for routine monitoring releases of
nation of Radionuclides radioactive material. Nevertheless, because soil is an integrator
C1163 Practice for Mounting Actinides for Alpha Spectrom- and a reservoir of long-lived radionuclides, and serves as an
etry Using Neodymium Fluoride intermediary in several of the plutonium pathways of potential
C1284 Practice for Electrodeposition of the Actinides for importance to humans, knowledge of the concentration of
Alpha Spectrometry plutonium in soil is essential.
D1193 Specification for Reagent Water
5. Apparatus
1
5.1 Electrodeposition Apparatus (2), see Practice C1284.
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of 5.2 Alpha Spectrometer, capable of 40 to 50 keV resolution
Test. on actual samples electrodeposited on a flat, mirror-finished
Current edition approved Feb. 15, 2011. Published February 2011. Originally
approved in 1983. Last previous edition approved in 2005 as C1001 – 05. DOI:
metal planchet, and a fractional counting efficiency greater
10.1520/C1001-11. than 17 %, and a background less than 0.010 cpm over each
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to the list of references at the end of
the ASTM website. this standard.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 C1001 − 11
designated energy region. Resolution is defined as the full 6.13 Iron Carrier solution (10 g Iron (III)/L)—Dissolve 10.0
width half maximum (FWHM) in keV, the distance between g iron metal in HCl (1.7M) and dilute to 1 L with HCl (1.7M).
those points on either side of the alpha peak where the count is 6.14 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
equal to one-half the maximum count. Also see Practices (HNO3).
D3084 and D3648.
6.15 Nitric Acid (8M)—Add 500 mL of concentrated HNO3
NOTE 1—A regular program of measurement control operations should
be conducted for the alpha spectrometry system, such as regular back-
(sp gr 1.42) to 400 mL of water, mix, and dilute to 1.0 L with
ground checks, source check to determine system stability, control water.
charting, and careful handling of samples during changing. See Practice 6.16 Nitric Acid (1.8M)—Add 112 mL of concentrated
D7282.
HNO3 (sp gr 1.42) to 500 mL of water, mix, and dilute to 1.0
5.3 PTFE-polytetrafluoroethylene beakers, 250-mL. L with water.
6. Reagents 6.17 Octyl alcohol.
6.1 Purity of Reagents—Reagent grade chemicals shall be 6.18 Sodium Bisulfite (NaHSO3).
used in all tests. Unless otherwise indicated, it is intended that 6.19 Sodium Hydroxide (50 %)—Dissolve 500 g of NaOH
all reagents shall conform to the specifications of the Commit- in 500 mL water. A 50 % NaOH solution is available commer-
tee on Analytical Reagents of the American Chemical Society, cially.
where such specifications are available (3). Other grades may
be used, provided it is first ascertained that the reagent is of 6.20 Sodium Nitrite (NaNO2).
sufficiently high purity to permit its use without lessening the 6.21 Thymol Blue Indicator, Sodium Salt, 0.02 % Solution.
accuracy of the determination.
6.22 National Standard Traceable Plutonium-236 Reagent.4
6.2 Purity of Water—Unless otherwise indicated, references
6.23 National Standard Traceable Plutonium-242 Reagent.4
to water shall be understood to mean reagent water as defined
in Specification D1193, Type III.
7. Sampling
6.3 Reagent blanks should be run to determine their contri-
bution to the sample result. 7.1 Collect the sample in accordance with Practice C998.
6.4 Ammonium Hydroxide (sp gr 0.90)—Concentrated am- 7.2 Prepare the sample for analysis in accordance with
monium hydroxide (NH4OH). Practice C999.
6.5 Ammonium Iodide (NH4I) (1 M)—Dissolve 14.5 g of 7.3 Samples consisting of 10 to 50 g of soil can be readily
NH4I in 100 mL water. analyzed by the procedure. In order to obtain more represen-
tative samples, as well as lowering the minimum detectable
6.6 Ammonium Iodide, Hydrochloric Acid Solution(NH4I-
concentration, the analyses of large soil samples is desirable. In
HCl)—Add 25 mL 1 M ammonium iodide to 500 mL concen-
general, it is poor practice to use less than 10 g of sample,
trated hydrochloric acid. Prepare fresh prior to use.
unless replicate analyses are performed, because of needed
6.7 Analytical Grade Anion Exchange Resin Type 1, 8 % sensitivity to determine lower levels of activity.
cross-linked, 100 to 200 mesh, chloride form4—Store the resin
in water in a wash bottle, transfer sufficient resin to a 1.3-cm ID 8. Calibration and Standardization
ion exchange column to give a 10-cm bed of settled resin.
8.1 The fractional counting efficiency of the alpha spec-
Convert the resin to the nitrate form by passing 100 mL of
trometer is used to determine the chemical yield. The fractional
HNO3 (8M) through the column at maximum flow rate.
efficiency of the alpha spectrometer is determined as the ratio
6.8 Boric Acid (H3BO3). of the observed count rate to the known disintegration rate.
6.9 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro- 8.2 The quantity of the tracer to be used should be in the
chloric acid (HCl). expected range (but not less than 0.17 Bq) of the isotopic
6.10 Hydrochloric Acid (3M)—Add 250 mL of concentrated activity being determined so that the statistical uncertainty in
HCl (sp gr 1.19) to 500 mL of water, mix, and dilute to 1.0 L the chemical yield determination will not be larger than that of
with water. the nuclide being determined.
6.11 Hydrochloric Acid (1.7M)—Add 142 mL of concen-
trated HCl (sp gr 1.19) to 500 mL of water, mix, and dilute to 9. Precautions
1.0 L with water. 9.1 Adequate laboratory facilities, such as fume hoods and
6.12 Hydrofluoric Acid (48 to 51 %)—Concentrated hydro- controlled ventilation, along with safe techniques, must be used
fluoric acid (HF). in this procedure. Extreme care should be exercised in using
hydrofluoric and other hot, concentrated acids. Use of proper
gloves is recommended. Refer to the laboratory’s chemical
4
hygiene plan and other applicable guidance for handling
Plutonium-236 is available from NBL and is traceable to NIST. Plutonium-242
is available as a Standard Reference Material from the National Institute of chemical and radioactive materials and for the management of
Standards and Technology, Gaithersburg, MD 20899. radioactive, mixed, and hazardous waste.

2
 C1001 − 11
9.2 Hydrofluoric acid is a highly corrosive acid that can decanting the supernate, and then completing the separation by
severely burn skin, eyes, and mucous membranes. Hydroflu- centrifugation on a smaller scale.
oric acid is similar to other acids in that the initial extent of a 10.11 Add 1.0 mL of iron carrier solution (10 mg Fe
burn depends on the concentration, the temperature, and the (III)/mL) to each centrifuge bottle and mix (Note 4).
duration of contact with the acid. Hydrofluoric acid differs
from other acids because the fluoride ion readily penetrates the NOTE 4—It may not be necessary to add the iron carrier if a sufficient
amount of iron is present in the soil.
skin, causing destruction of deep tissue layers. Unlike other
acids that are rapidly neutralized, hydrofluoric acid reactions 10.12 Add NaOH (50 %) with mixing to each bottle to a pH
with tissue may continue for days if left unattended. Due to the of about 9 (using pH paper) to precipitate ferric hydroxide. Add
serious consequences of hydrofluoric acid burns, prevention of 5 to 10 mL excess NaOH and mix for 1 min.
exposure or injury of personnel is the primary goal. Utilization 10.13 Centrifuge for approximately 5 min, decant, and
of appropriate laboratory controls (hoods) and wearing ad- discard the supernate.
equate personal protective equipment to protect from skin and
10.14 Dissolve each precipitate with about 30 mL HNO3
eye contact is essential.
(8M) (60 mL total) saturated with boric acid. (Approximately
7 g of boric acid/30 mL HNO3 (8M).) Digest in a hot water
10. Procedure
bath for 10 min.
10.1 Weigh a 10.0 6 0.1 g soil aliquot into a 250 mL PTFE
10.15 Cool and centrifuge for approximately 5 min. Decant
beaker.
the supernate into the original 250 mL PTFE beaker and save.
10.2 Wet sample with distilled water and add a known
10.16 Wash each residue with approximately 10 to 20 mL
quantity of 236Pu or 242Pu tracer.
(20 to 40 mL total) of HNO3 (8M) saturated with boric acid.
10.3 Add concentrated HNO3 (sp gr 1.42) a few drops at a Centrifuge for 5 min and combine the supernates with that in
time as fast as the frothing and vigor of the reaction will permit 10.15. Discard the undigested soil.
until the entire sample is covered. 10.17 Heat the supernate on a hotplate and evaporate to
10.4 Add 60 mL more of the concentrated HNO3 (sp gr approximately 5 mL.
1.42) and 30 mL of concentrated HF (48 to 51 %) and digest on 10.18 Add approximately 30 mL water and heat to dissolve
a hotplate with frequent stirring (TFE fluorocarbon stirring rod) the salts. Cool and transfer into a centrifuge tube.
for about 1 h (Note 2 and Note 3).
10.19 Add concentrated ammonium hydroxide dropwise
NOTE 2—For organic soils, first add the nitric acid only in small with mixing to a pH of approximately 9 (using pH paper) to
portions while stirring. If the solution threatens to overflow as a result of
froth generation, add a few drops of octyl alcohol and stir. Digest on a
precipitate ferric hydroxide.
hotplate until the evolution of reddish-brown fumes is reduced to a barely 10.20 Centrifuge and discard the supernate.
visible level. Cool to room temperature before carefully adding the
concentrated hydrofluoric acid (48 to 51 %) and digesting for an hour. 10.21 Dissolve the precipitate with a volume of concen-
NOTE 3—For larger soil aliquots, larger amounts of the acids (in the trated nitric acid approximately equal to the volume of the
same proportions) should be used. For example, for a 50 g sample, use 200 precipitate and transfer using nitric acid (8M) into a 250-mL
mL concentrated. HNO3 and 100 mL HF, etc., with appropriately sized beaker. Add nitric acid (8M) to a total volume of approximately
containers.
75 mL. If the volume of the hydroxide precipitate is consider-
10.5 Remove from the hotplate and cool somewhat before ably greater than should be expected from the 10 mg of Fe(III)
adding 30 mL concentrated HNO3 (sp gr 1.42) and 30 mL added, the final volume should be brought up to approximately
concentrated HF (48 to 51 %). Digest on the hotplate with 100 mL with nitric acid (8M) or, alternatively, the dissolved
intermittent stirring for an additional 1 h. hydroxides should be evaporated to salts before the addition of
10.6 Remove from the hotplate and cool. Carefully add 20 the nitric acid (8M) solution. The final nitric acid molarity of
mL concentrated HCl (sp gr 1.19) and stir. Heat on hotplate for the solution is not extremely critical, but should be in the range
45 min with occasional stirring. of 7 to 9.
10.7 Add about 5 g of powdered boric acid and digest for an 10.22 Add approximately 200 mg of sodium nitrite crystals
additional 15 min with occasional stirring. and stir with a stirring rod. Bring to a quick gentle boil on a
hotplate and cool. Avoid prolonged heating.
10.8 Add approximately 200 mg of sodium bisulfite and
continue heating until the solution has evaporated to a liquid 10.23 Prepare an anion-exchange column as described in
volume of approximately 20 mL. 6.7.
10.9 Add 50 mL of water and digest on a hotplate while 10.24 Pass the sample (at maximum flow rate) through the
stirring for 10 min to dissolve soluble salts. anion-exchange resin column.
10.10 Cool and transfer approximately equal parts of the 10.25 When the solution just drains to the top of the resin
total sample into centrifuge bottles with a minimum of water bed, wash the column with six column volumes of
from a wash bottle. If equipment for large volume centrifuga- HNO3 (8M). A column volume is approximately 9.5 mL.
tion is not available, the two precipitations in 10.11-10.21 may 10.26 Wash the resin column with six column volumes of
be performed in a beaker, allowing the precipitate to settle, concentrated HCl.

3
 C1001 − 11
10.27 Elute the plutonium with four column volumes of 11.2 Most of the available plutonium-236 and some of the
freshly prepared NH4I-HCl solution, and collect in a 150-mL available plutonium-242 contain significant impurities of the
beaker. isotopes being sought. Thus a correction must be made to
10.28 Evaporate the solution to approximately 5 mL on a account for contaminant contributions to the analyte regions.
hotplate. Rinse down the sides of the beaker dropwise with 1 to The correction must take into account a predetermined ratio of
2 mL of concentrated HNO3. Add six drops of concentrated the net count rate of the tracer to that of the respective
HCl and evaporate to near dryness. contaminant isotopes activity to ensure that is adequately
reflects the changing contribution based on varying chemical
10.29 Add 50 mL of HNO3 (8M) and repeat steps yield of the tracer in the sample. This interference must also be
10.22-10.27, using a fresh anion-exchange resin column. reflected in the statistics reported in association with the result.
10.30 Continue heating the final plutonium elution just to
11.3 The activity of each plutonium isotope is calculated as
dryness on the hotplate. Rinse down the sides of the beaker
follows:
with a few mL of concentrated HCl, and evaporate to approxi-
mately 0.5 mL. See Note 5. Assemble the electrodeposition cell X i 5 ~ C iA t! / ~ C tW s! (1)
as described in Practice C1284. where:
NOTE 5—Plutonium can also be prepared for alpha spectrometry by
coprecipitation with neodymium fluoride, see Practice C1163. If samples Xi = concentration of a plutonium isotope in Bq/g,
are determined by coprecititation, then the counting standards must be At = activity of the tracer added in Bq,
prepared is a similar manner. Ci = net sample counts in the energy region of the pluto-
10.31 Add 1.5 to 2 mL of HCl (3M) solution into the beaker, nium isotope being measured,
rinse as above, and add the rinses to the plating cell. Ct = net sample counts in the energy region of the pluto-
nium yield tracer (Pu-236 or Pu-242), and
10.32 Add three drops of thymol blue indicator solution and Ws = the sample weight in g.
then add concentrated NH4OH dropwise until the color
changes to yellow. 11.4 The fractional counting efficiency of the alpha
spectrometer, E, must be determined if it is desired to calculate
10.33 Add HCl (1.7M) dropwise to a salmon pink endpoint. the chemical yield for the plutonium analysis. Calculate the
10.34 Electroplate at 1.5 amps for 20 min. See Note 6. fractional efficiency as follows:
NOTE 6—Caution: The electrodeposition should be performed in a E 5 R s /A std (2)
fume hood due to the chlorine gas evolved during the electrodeposition.
where:
10.35 At the end of 20 min, quickly add 2 to 3 mL of
Rs = net counting rate of the standard source in the region
concentrated NH4OH and leave the current on for another 20 s.
of the alpha emitter of interest in cps, and
10.36 Turn off the current, rinse out the solution into a Astd = activity of the standard source in Bq at the time of the
beaker with water, and dismantle the cell. Rinse the disk with count.
water and dry it in a clean planchet on a hotplate at medium
heat for 5 min, or flame with a burner. 11.5 Calculate the fractional chemical yield for plutonium
as follows:
10.37 Count the sample in an alpha spectrometer long
Y 5 ~ C t ! / ~ TAt E ! (3)
enough to obtain the desired sensitivity (see Table 1).
where:
TABLE 1 Decay Characteristics (4)
T = counting time in s,
Ct = the net sample counts in the energy region of the
Iso- Maximum Alpha Energy,
tope
Half-life
MeV (Abundance)
plutonium tracer (Pu-236 or Pu-242),
236
Pu 2.851 years 5.768 (68.1 %), 5.721 (31.7 %)
At = activity of the yield tracer added in Bq, and
238
Pu 87.74 years 5.499 (71.6 %), 5.456 (28.3 %) E = absolute counting efficiency of the alpha spectrometer.
239
Pu 2.411 × 104 years 5.155 (73.2 %), 5.143 (15.1 %), 5.105
(10.6 %) 11.6 Refer to Practice D3084 for the Minimum Detectable
240
Pu 6.570 × 103 years 5.159 (75.5 %), 5.115 (24.4 %) Concentration (MDC), critical level, and uncertainty calcula-
242
Pu 3.763 × 105 years 4.901 (78 %), 4.856 (22.4 %)
tions.

12. Precision and Bias

11. Calculation of Plutonium Concentration 12.1 Reference samples and standards were sent to 15
11.1 Because alpha spectrometry cannot distinguish be- laboratories. Analytical data were returned by six laboratories
tween plutonium-239 and plutonium-240, when plutonium-239 (2). It is not known if these six laboratories are typical of the
is mentioned, the alpha activity due to the plutonium-240 is laboratories that will use this test method. The responses of two
also included. of the laboratories were judged as outliers and excluded from

4
 C1001 − 11
the analyses. Thus, the following estimates are based on twelve 13. Keywords
measurements per sample, three at each of four laboratories: 13.1 alpha spectrometry; plutonium; radiochemistry; soil
Summary of Plutonium Results
Percent Relative
Known No. of X̄ Absolute Standard Deviation
Value Laboratories Percent Within Between
(Bq/g) (Bq/g) Bias Laboratory Laboratories

0.00188 4 0.0023 26 6.7 17.0

0.0023 4 0.0026 13 8.1 15.2
0.0150 4 0.0170 12 7.7 13.4
0.0172 4 0.0203 18 7.7 17.2
0.150 4 0.172 15 3.6 16.9

APPENDIXES

(Nonmandatory Information)

X1. PURIFICATION OF THE PLUTONIUM-236 TRACER (5)

X1.1 In order to accurately calibrate the plutonium-236 X1.1.8 Wash the resin column at maximum flow rate with
tracer by 2p counting and alpha spectrometry, it will be six column volumes of HCl (sp gr 1.19) using the same
necessary to ensure the absence of plutonium-236 progeny technique. Discard the hydrochloric acid washes.
(uranium-232, thorium-228, radium-224, etc.) in the tracer.
The following purification must be performed just prior to the X1.1.9 Elute the plutonium with four column volumes of
initial calibration and annually thereafter if additional calibra- freshly prepared ammonium iodide-hydrochloric acid solution
tions are desired. and collect in a 150-mL beaker.
X1.1.1 Add approximately 4.2 × 102 Bq of plutonium-236 X1.1.10 Evaporate the solution to approximately 5 mL on a
to a 250-mL beaker containing 25 mL of nitric acid (sp gr hotplate. Rinse down the sides of the beaker dropwise with 1 to
1.42). 2 mL of HNO3 (sp gr 1.42). Add six drops of HCl (sp gr 1.19)
X1.1.2 Evaporate the solution on a hotplate to a volume of and evaporate just to dryness on the hotplate.
approximately 10 mL. X1.1.11 Add 5 mL each of HCl (sp gr 1.19) and HNO3 (sp
X1.1.3 Remove from the hotplate and add 25 mL of HNO3 gr 1.42) to the beaker and evaporate to about 2 mL.
(8M) and 10 mL of distilled water to adjust the HNO3
concentration to 8 M. X1.1.12 Add 15 mL of HNO3 (sp gr 1.42) and boil down to
about 5 mL to ensure complete dissolution of the plutonium
X1.1.4 Add ;200 mg of sodium nitrite crystals and stir with
and complete oxidation of chlorides as indicated by the
a glass stirring rod. Bring the solution to a quick gentle boil on
absence of color or fumes of chlorine oxide or nitrogen oxide,
a hotplate and cool. Avoid prolonged heating.
or both.
X1.1.5 Pass through an anion-exchange resin column (ni-
trate form) prepared as described in 6.7 at maximum flow rate. X1.1.13 Cool, add 25 mL of distilled water and filter the
X1.1.6 When the solution just drains to the top of the resin solution through a DM-450 membrane filter in a filtering
bed, add two column volumes of HNO3 (8M) to the column chimney. Wash the flask and filter with enough distilled water
reservoir and wash the resin column at the maximum flow rate. to give a final volume of 50 mL.
Discard the effluents from the sample and washes. X1.1.14 Dilute aliquots of the 8.3 Bq/mL stock solution
X1.1.7 Repeat Step 6 twice until the resin column has been with HNO3 (8M) to give concentrations desired for use. Store
washed with a total of six column volumes of HNO3 (8M). all tracers in tightly capped TFE-fluorocarbon FEP bottles.

5
 C1001 − 11

X2. STANDARDIZATION OF THE PLUTONIUM-236 TRACER (5)

X2.1 Transfer a 1-mL aliquot of the purified plutonium-236 X2.6.2 Evaporate carefully on a hotplate just to dryness.
stock tracer (;8.3 Bq/mL in nitric acid (1 + 1)) onto a polished Rinse down the sides of the beaker with a few millilitres of HCl
metal planchet with a calibrated silicone-treated pipet and (sp gr 1.19) and evaporate to approximately 0.5 mL.
slowly evaporate to near dryness under an infrared lamp to
minimize any loss. Keep the activity in the center of the X2.6.3 Treat and electrodeposit as described in 10.31-10.36.
planchet in an area limited to approximately 2 cm (3⁄4 in.) in X2.6.4 Count the electroplated source on an alpha spec-
diameter by alternately adding the tracer a few drops at a time trometer for 15 000 s over an energy range of 3 to 8 MeV.
and evaporating. The partially filled silicone-treated pipet can Determine the fraction of the total number of counts in the
be placed on its side between additions with no loss of solution. alpha spectrum that is due to plutonium-236 in the source. This
To ensure quantitative transfer of the tracer, carefully blow out fraction is the correction factor to be applied to the counting
the last few drops with a rubber bulb. rate of the plutonium-236 evaporated source in the 2p propor-
X2.2 When the last of the tracer has been transferred to the tional counter.
planchet and evaporated nearly to dryness, add 2 or 3 drops of
NOTE X2.1—Prolonged and repeated counting of high level plutonium-
HNO3 (sp gr 1.42) to help keep the activity spread as uniformly 236 sources on the alpha spectrometer should be avoided to minimize
as possible and evaporate to complete dryness. daughter recoil contamination of the alpha detector. Alternatively, such
contamination virtually can be eliminated by leaving a small amount of air
X2.3 Heat the dry planchet over a blast burner just to the in the counting chamber and applying a small negative potential to the
first dull red glow. Then quickly lower the temperature by source plate.
placing the planchet on a cold steel surface to minimize
oxidation of the plate. X2.7 Calculate the activity concentration of the plutonium-
236 tracer (Bq plutonium-236/mL) by dividing by the frac-
X2.4 Count in the 2p alpha counter immediately after tional detector efficiency and the volume of tracer used to
cooling to avoid any possibility of absorption of water vapor
prepare the evaporated sources.
from the air. Collect at least 5 × 104 counts for the standard to
ensure adequate statistical precision. X2.8 Typical conditions for method are as follows:
X2.5 Prepare and count a duplicate source by repeating CE ( %) = 25
CB (cps) = 0.00002
X2.1-X2.4. Y ( %) = 80
V (g) = 10
X2.6 The 2p counting rate of the plutonium-236 sources LLD = 2 400 s (Bq) 0.0017
must be corrected by determining the fraction of the total alpha LLD = 60 000 s (Bq) 0.00034
LLD = 300 000 s (Bq) 0.00015
activity due to plutonium-236. MDC = 2 400 s (Bq/g) 0.0002
X2.6.1 Transfer 2 mL of the purified ;8.3 Bq/mL MDC = 60 000 (Bq/g) 0.00004
MDC = 300 000 (Bq/g) 0.00002
plutonium-236 tracer to a 150-mL beaker and add 2 mL each of
HNO3 (sp gr 1.42) and HCl (sp gr 1.19).

REFERENCES

(1) “Measurements of Radionuclides in the Environment; Sampling and Chemicals and Standards,” by Joseph Rosin, D. Van Nostrand Co.,
Analysis of Plutonium in Soil,” Atomic Energy Commission Regula- New York, NY, and the “United States Pharmacopeia.”
tory Guide 4.5, May 1974 . (4) Browne, E., and Firestone, R. B., (Shirley, V. S., Ed.), Table of
(2) “Acid Dissolution Method for the Analysis of Plutonium in Soil,” Radioactive Isotopes, John Wiley and Sons, Inc., 1986.
Environmental Protection Agency 600/7-79-081, p. 30. (5) “Acid Dissolution Method for the Analysis of Plutonium in Soil,”
(3) “Reagent Chemicals, American Chemical Society Specifications,” Environmental Protection Agency 600/7-79-081, pp. 37–41.
Am. Chemical Soc., Washington, D.C. For suggestions on the testing (6) “Upgrading Environmental Radiation Data,” Environmental Protec-
of reagents not listed by the American Chemical Society, see “Reagent tion Agency, 520/1-80-012, pp. 6–24.

6
 C1001 − 11
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/
COPYRIGHT/).