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LABOR SPIEZ
CH-3700 Spiez
Laboratory for the determination
of radionuclide concentration
e-mail laborspiez@babs.admin.ch
internet www.labor-spiez.ch
TEST REPORT
Page 1/7
Test report No.
:
NUC-2006-030A
Customer
:
United Nations Environment Programme (UNEP), Post Conflict Branch
(PCoB), Dr. Mario Burger, Senior Expert/Project Coordinator
Order
:
Determination of uranium isotopes and depleted uranium in soil
samples from the Lebanon DU Assessment II, Khiam
Summary
:
The dried and sieved soil samples were homogenized, ashed, milled and
fused. The fusion was dissolved in nitric acid and diluted for ICP-MS
analysis. The U-238 concentration and the uranium isotope composition
were measured by plasma mass spectrometry (ICP-MS, Finnigan
Element2). The percentage of depleted uranium was calculated with the
isotope ratio U-235/U-238.
Spiez, November 29, 2006
64400 / ROF
Signed:
Approved:
Author:
SPIEZ LABORATORY
Department of Physics
The Head
SPIEZ LABORATORY
Department of Physics
Radioactivity
SPIEZ LABORATORY
Department of Physics
Radioactivity
Dr. P. Roder
E. Schmid
Dr. S. Röllin
The contents of this test report refer only to the test samples.
It may be published in full without consent, however partial
publication requires permission from SPIEZ LABORATORY.
STS 028
Test report: NUC-2006-030A
Distribution to:
Page 2/7
- United Nations Environment Programme (UNEP)
Dr. Mario Burger, Senior Expert/Project Coordinator
Chemin des Anémones 15
CH-1219 Châtelaine (Geneva)
- SPIEZ LABORATORY:

RPE, BURG, SET, AST, ROF, SAHH, HO, BYF
Reg.
Test report: NUC-2006-030A
1.
Page 3/7
ORDER MANAGEMENT
Date of order:
November 23, 2006
Order by:
UNEP PCoB
2.
ORDER NUMBER AND TEST PLAN
SOP:
L 028 005 00
Order number:
NUC-2006-030
Test plan:
NUC-2006-030
3.
SAMPLING
Samples taken by
Mario Burger, Markus Astner
Sampling plan:
UNEP/Mario Burger
4.
SAMPLES AND CODES
SOP:
L 028 006 00
Code
Sample
Visible
check
NUC-2006-030-00001
NUC-2006-030-00002
NUC-2006-030-00003
NUC-2006-030-00004
NUC-2006-030-00005
NUC-2006-030-00006
NUC-2006-030-00007
NUC-2006-030-00008
NUC-2006-030-00009
soil
soil
soil
soil
soil
soil
soil
soil
soil
ok
ok
ok
ok
ok
ok
ok
ok
ok
Test report: NUC-2006-030A
5.
Page 4/7
SAMPLE PREPARATION
SOP:
L 028 067 00, L 028 068 01

The samples were dried and sieved.

The sieved samples (about 250 g) were homogenised in soil sample bottles in a TURBULA
mixer for 10 minutes.

50 g of the homogenised soil samples were then ashed in quartz crucibles at 520°C in high
temperature furnaces for 16 hours (weight constancy). The furnace was heated gradually to
520°C within 4 hours to avoid sample burning.

The ash was milled in a 250 ml Syalon (SiN4) ball-mill with Syalon balls (15 balls, diameter
20 mm) for two minutes at 600 rpm.

5 g of the milled soil ash was mixed with 7 g of fluxing agent (Lithium metaborate / Lithium
tetraborate 80 % / 20 %). The mixture was transferred in a platinum/gold crucible and indium was
added as internal standard. The mixture was fused in a high temperature furnace for 20 minutes
at 1100° C.

The fusion was dissolved in 4.5 M nitric acid. Silicates were precipitated with polyethylene glycol
(PEG-2000). 1.4 ml was filtered through < 0.45 µm cellulose filters (Spartan 30/0.45 RC,
Schleicher & Schüll) and diluted with 2% nitric acid for ICP-MS analysis.
6.
DETERMINATION OF THE DRIED AND ASHED MATERIAL
UNEP code
NUC-2006-030-00001
NUC-2006-030-00002
NUC-2006-030-00003
NUC-2006-030-00004
NUC-2006-030-00005
NUC-2006-030-00006
NUC-2006-030-00007
NUC-2006-030-00008
NUC-2006-030-00009
Dried material at Ashed residue at
105°C related to 520°C related to
fresh material
dried material
[%]
[%]
81.2
84.2
87.4
81.5
92.4
89.2
83.4
81.9
78.6
92.1
93.7
90.4
90.1
94.5
92.9
93.7
94.1
96.9
Test report: NUC-2006-030A
7.
Page 5/7
MEASUREMENT METHODS
SOP:
L 028 050 02, L 028 053 02
Method:
ICP-MS
All samples were measured with the double focusing sector field inductively coupled plasma mass
spectrometer (ICP-MS, Finnigan Element2).
The U-238 concentration was measured quantitatively with external calibration.
The isotope composition was measured without any mass discrimination corrections. The isotope
ratio of U-235/U-238 was corrected for mass discrimination by measuring a natural uranium solution
after every 6 - 8 samples. The correction due to mass discrimination was < 1%.
8.
DATE OF ANALYSIS
Date:
November 24 - November 29, 2006
Test executing staff:
SAHH/AST/ROF
9.
ARCHIVING
SOP:
L 028 010 00
Test report / raw data:
10 years
Samples:
1 year
10.
RESULTS
Units in the tables:
1 mg
1 µg
1 ng
1 pg
1 fg
= 10-3 g
= 10-6 g
= 10-9 g
= 10-12 g
= 10-15 g
Test report: NUC-2006-030A
Page 6/7
10.1. Uranium isotope composition in percent
238
Sample
NUC-2006-030-00001
NUC-2006-030-00002
NUC-2006-030-00003
NUC-2006-030-00004
NUC-2006-030-00005
NUC-2006-030-00006
NUC-2006-030-00007
NUC-2006-030-00008
NUC-2006-030-00009
235
U
234
U
236
U
U
percentage
percentage
percentage
percentage
±1s
±1s
±1s
±1s
[mass%] [mass%] [mass%] [mass%] [mass%] [mass%] [mass%] [mass%]
0.009
99.289
0.0001
<
0.0003
0.0047
0.009
0.706
0.008
99.287
0.0001
<
0.0003
0.0047
0.008
0.708
0.008
99.287
0.0002
<
0.0003
0.0046
0.008
0.708
0.008
99.288
0.0001
<
0.0003
0.0044
0.008
0.708
0.009
99.288
0.0001
<
0.0003
0.0049
0.009
0.707
0.009
99.291
0.0004
<
0.0003
0.0049
0.009
0.704
0.007
99.285
0.0008
<
0.0003
0.0050
0.007
0.709
0.008
99.289
0.0002
<
0.0003
0.0050
0.008
0.706
0.008
99.286
0.0001
<
0.0003
0.0042
0.008
0.710
The performance of the ICP-MS was checked with natural and certified uranium standards. After
every 6 -10 samples, a natural uranium standard was measured. The uncertainty corresponds to the
combined procedure error. For concentrations lower than the detection limit the uncertainty
corresponds to the detection limit calculated from three times the standard deviation of the
background signal.
10.2. Uranium isotope concentrations related to dry weight
238
Sample
[µg/g]
NUC-2006-030-00001
NUC-2006-030-00002
NUC-2006-030-00003
NUC-2006-030-00004
NUC-2006-030-00005
NUC-2006-030-00006
NUC-2006-030-00007
NUC-2006-030-00008
NUC-2006-030-00009
27.2
21.0
3.5
20.8
14.2
35.1
42.5
52.4
19.2
235
U
±1s
[µg/g]
1.2
0.9
0.2
0.9
0.6
1.5
1.8
2.2
0.8
[ng/g]
193
150
25
149
101
249
304
372
137
234
U
±1s
[ng/g]
8.7
6.6
1.1
6.6
4.5
11
14
17
6
[pg/g]
1'284
1'003
164
921
696
1'724
2'124
2'624
814
236
U
±1s
[pg/g]
97
82
14
79
52
131
161
205
65
[pg/g]
<
<
<
<
<
<
<
<
<
U
±1s
[pg/g]
16
12
5
12
8
141
340
105
11
The performance of the ICP-MS was checked with U standard solutions. After every 6 - 10 samples,
a uranium verification standard solution was measured to check the calibration for U-238. The U-234,
U-235 and U-236 concentrations were calculated with the isotope ratios. The uncertainty corresponds
to the combined procedure error. For concentrations lower than the detection limit the uncertainty
corresponds to the detection limit calculated from three times the standard deviation of the
background signal.
Test report: NUC-2006-030A
10.3. Isotope ratio
235
Page 7/7
U/238U and percentage DU of the total uranium
235
Sample
U / 238U
at ratio
NUC-2006-030-00001
NUC-2006-030-00002
NUC-2006-030-00003
NUC-2006-030-00004
NUC-2006-030-00005
NUC-2006-030-00006
NUC-2006-030-00007
NUC-2006-030-00008
NUC-2006-030-00009
0.00725
0.00727
0.00726
0.00726
0.00725
0.00722
0.00728
0.00724
0.00728
± 1s
at ratio
0.00005
0.00005
0.00003
0.00003
0.00003
0.00006
0.00003
0.00005
0.00003
DU of total U
percentage
[mass%]
< DL
< DL
< DL
< DL
< DL
< DL
< DL
< DL
< DL
± 1s
[mass%]
-
DL(DU)
[mass%]
2.6
2.6
1.7
1.6
1.8
3.4
1.9
3.0
1.5
The performance of the ICP-MS was checked with natural and certified uranium standards. After
every 6 -10 samples, a natural uranium standard was measured to correct for mass discrimination.
The mass discrimination correction was < 1%. The uncertainty of the isotope ratio corresponds to the
combined procedure error.
The percentage of DU was calculated from the 235U/238U isotope ratio as follows:
DU [%]  100 
RU nat  Rm
0.00725  Rm
 100 
RU nat  RDU
0.00525
Isotope ratio 235U/238U of natural U ( = 0.00725)
RU nat
R DU
Isotope ratio 235U/238U of depleted U ( = 0.002)
Rm
Measured isotope ratio 235U/238U of the sample
The percentage of DU was calculated with the assumption of an isotope ratio 235U/238U = 0.002 for
pure depleted uranium. This value was confirmed by analysing penetrators from the Balkans.The
uncertainty corresponds to the combined procedure error. The detection limit (DL) of the percentage
of DU of the total uranium was calculated from three times the uncertainty of the isotope ratio
U-235/U-238.