AN-1408

Rapid Determination of Actinides
in Animal Tissue Samples

Summary of Method Uranium, Plutonium, and Americium-Curium are separated and concentrated from up to 200g
tissue samples. Samples are digested with aqua regia, wet ashed with HNO3-H2O2 and muffled over night at 550°C todestroy organic content. Actinides are separated from matrix impurities and potentially interfering radionuclides in thesample using stacked 2mL cartridges of Eichrom TEVA, TRU and DGA Resin. Actinides are measured via alpha
spectrometry following cerium fluoride microprecipitation onto Eichrom Resolve® Filters. Average chemical recoveries ofPu for 100-200g samples are 93-101%. Typical americium recoveries are 93-105%. Typical uranium recoveries are 8296%. A single operator can complete the sample preparation for 12-24
Figure 1. Sample Preparation
samples, including 16 hours for muffling, in less than 24 hours.
Up to 200g Tissue in 600mL glass beaker
Reagents
TEVA Resin, 2mL Cartridges (Eichrom TE-R50-S)
Add tracers
TRU Resin, 2mL Cartridges (Eichrom TR-R50-S)
DGA Resin, 2mL Cartridges (Eichrom DN-R50-S)
Add 80mL 70% HNO3,
Hydrofluoric Acid (49%) or Sodium Fluoride
and 20mL 37% HCl.
Iron Carrier (50mg/mL Fe, as ferric nitrate)
Digest on hotplate medium setting
242Pu (or 236Pu if meas. Np), 243Am and 232U tracers
until complete dryness.
Oxalic acid/Ammonium oxalate
Nitric Acid (70%)
Hydrochloric Acid (37%)
Remove from hot plate and cool.
Hydrogen Peroxide (30%)
Deionized Water
Cerium Carrier (1mg/mL)
2M Al(NO3)3
Carefully add 3mL 70% HNO3 andSodium nitrite
Sulfamic acid
3mL 30% H2O2 (Foaming may occur).
Ascorbic acid10% (w:w) TiCl3
Evaporate to dryness on hot plate.
Denatured Ethanol
Muffle at 200°C for 10 minutes, 300°C
for 1 hour, and 550°C over night.
Equipment
Vacuum Box (Eichrom AR-24-BOX or AR-12-BOX)
Cartridge Reservoir, 20mL (Eichrom AR-200-RV20)
Inner Support Tubes-PE (Eichrom AR-1000-TUBE-PE)
Yellow Outer Tips (Eichrom AR-1000-OT)
Resolve Filters in Funnel (Eichrom RF-DF25-25PP01)
Muffle Furnace
Hot Plate
Analytical Balance
600mL Glass Beakers
Stainless Steel planchets with adhesive
Vacuum Pump
Alpha Spectrometry System
Heat Lamp

Remove samples from muffle oven and cool.
Wet ash samples with 5mL 70% HNO3
and 5mL 30% H2O2, until residue is white.
Additional muffling at 550°C may be necessary.
Dissolve residue in 12mL 6M HNO3 and12mL 2M Al(NO3)3. Add 3M HNO3 as
necessary to complete dissolution.
Adjust valence states of actinides by adding(mix between each addition):
0.5mL 1.5M Sulfamic acid, 10uL 50mg/mL
Fe carrier, 1.25mL 1M Ascorbic acid,1mL 3.5M NaNO2, and 1.5mL 70% HNO3.

Figure 2. Actinide Separation on TEVA - TRU - DGA*
(13) Strip Am and Cm from DGA with
(1) Precondition stacked 2mL(23) Draw vacuum until filter is dry.
10mL 0.25M HCl.
(24) Remove filter from funnel
TEVA, TRU, DGA withTEVA
assembly and mount filter on
10mL 3M HNO3.
(14) Rinse TRU cartridge with 15mL
(2) Load sample solution.
stainless steel planchet with 24M HCl-0.2M HF-0.002M TiCl3.
(3) Rinse sample tube withsided tape.
(15) Strip U from TRU with 15mL of5mL 6M HNO3.** AddTRU
0.1M ammonium bioxalate.
tube rinse to cartridges.
(16) Add 0.5mL 10% TiCl3 to U samples,(4) Rinse cartridges with 10mL
0.5mL 30% H2O2 to Pu and 0.2mL
3M HNO3.
DGA
30% H2O2 to Am/Cm samples.
(5) Separate TEVA, TRU, and(17) Add 50-100ug Ce carrier to all
DGA cartridges.
samples. Mix well. Add 1mL 49%(6) Rinse TEVA cartridge with:
HF. Mix well. Wait 15-20 minutes.
-10mL 3M HNO3(18) Set up Resolve® Filter Funnel on-20mL 9M HCl( remove Th)(25) Dry filter under heat lamp forvacuumbox.
-5mL 3M HNO33-5 minutes.
(19)Wetfilterwith(7) Strip Pu(Np) from TEVA with 20mL(26) Measure actinides by alpha3mL
80%
0.1M HCl-0.05MHF-0.01M TiCl3.
spectrometry.
ethanolfollowed(8) Rinse DGA with 8mL 0.1M HNO3.
by 3mL DI(9) Place TRU cartridge above DGA .
water.
(10) Strip Am/Cm from TRU onto DGA(20) Filter sample.
with 15mL 3M HCl.
(21) Rinse sample(11) Separate TRU and DGA. Set
tube with 5mL DI
TRU aside for U recovery.
water and add to(12) Rinse DGA with:-5mL 3M HCl(22) Rinse filter funnel with 3mL DI-3mL 1M HNO3water and 2mL 100% ethanol.
-15mL 0.05M HNO3
*Radiostrontium may also be measured by adding a 2mL + 1mL Sr Resin cartridge below DGA and following separation
scheme in Eichrom application note AN-1407, “Rapid Determination of Sr in Animal Tissue Samples.”**Adding 50uL of 30% H2O2 to tube rinse can improve U recoveries and decontamination in Pu/Np samples.
Method Performance for 100-200g Tissue Samples% Tracer Recovery
Samplemass, g replicatesPu-236Am-243
U-232
97.1 + 8.4
93.4 + 4.7
Beef100
698.7 + 5.7
93.4 + 10
90.4 + 8.0
Deer
100
59
99.3 + 12
Fish-Bass
200
7296.2 + 14
102 + 1395.1 + 8.1
Fish-Bream
100
57
96.6 + 12
98.4 + 7.7
91.1 + 6.3
103.7 + 7.6
89 + 12
Fish-Catfish
200
69
98.3 + 12
96.4 + 9.7
86 + 15Hog
100
1793 + 20
Shelfish100
5101.3 + 2.2 97.4 + 7.1
81.7 + 3.2

Reference Sherrod L. Maxwell, Donald M. Faison, “Rapid column extraction method for actinides and strontium infish and other animal tissue samples,” J. Radioanal. Nucl. Chem., 275(3), 605-612 (2007).
1955 University Lane Lisle, IL 60532, USA+1 (630)963-0320

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