The Determination of Be in an Enriched Uranium Matrix
YGG-01-0419
Darrin K. Mann, D.H. “Bo” Bowman, Thomas J. Oatts, and Vicki F. Belt
Analytical Chemistry OrganizationY-12 National Security Complex
P.O. Box 2009, MS 8189Oak Ridge, TN 37831-8189
Outline
Short review of Be, or why we use it
Problems associated with handling of Be– Physical
– Health
Be program at Y-12 national Security Complex
Current Method– Problems with current method
– New method
Data from new method
Conclusions/Future Work
Be: Why we use it
Discovered in 1798– Not widely used in Industry until 1940s and 50s
Lighter then Aluminum, Stiffer then Steel– 2nd lightest metal– 6 times stiffer then steel
High heat absorption– One pound absorbs as much heat as 6 pounds of copper
Be Metals, Alloys, Salts and Oxides are used for a wide variety of Industries– Structures in high-speed aircraft (space shuttle)– Satellite mirrors and space telescopes– Golf clubs and bicycle frames– Neutron moderators or reflectors in nuclear reactors– Nuclear Weapons components
Problems Associated with Be
Physical Problems– Expensive
– Brittleness
• Increases toxicity
Health Hazard– Most Significant disadvantage for industrial use
– Causes Chronic Beryllium Disease (CBD)
• No known cure, can only be treated
– Produces scaring of lung tissue
• Chronic, may take years to develop
– Average latency period is 10-15 years
• 2-5 % of population Be sensitive
• Over 100 current and former DOE employees have CBD
Be program at Y-12 National Security Complex
Controlled by US Dept. of Energy’s Chronic Beryllium Disease Prevention Program
– 10 CFR Part 850
– Promulgated in 1999 to protect DOE workers from CBD
– Requires Be surface and air monitoring to determine health risk
– Rule greatly increased the need for Be analysis in the DOE complex
– Current analytical methods include ICPOES and GFAA
Overview of Y-12 Be Program
0
1000
2000
3000
4000
5000
6000
Oct Feb June
FY03FY04
Almost 40K samples analyzed in 03.
Averaging 50% more samples in 04
Some months topping 5000 SAMPLES
Average turnaround time is 24 hours.
Typical Workloads Associated with Be Program
FY 2004 Beryllium Filters Analyzed
5070
3585
4968
3510
4244
2725
0
500
1000
1500
2000
2500
3000
3500
4000
4500
5000
5500
6000
6500
7000
7500
Oct
No
v
Dec
Jan
Feb
Mar
Ap
r
May
Jun
Jul
Au
g
Sep
Month
# o
f sa
mp
les
FY 04 Monthly Be samples FY 03 Monthly Be samples FY 01 Monthly Be samples
FY 00 Monthly Be samples FY 99 Monthly Be samples FY 02 Monthly Be samples
Breakdown of Be Smears at Y-12
Breathing Zone (BZ) 24 hr deadline12.5%
Routine Large area wipes from special projects/areas (LAW5D) 5
day deadline15.9%
Rush Large area wipes from special projects/areas (LAW24) 24
hr deadline7.0%
General housekeeping smears (HSKEEP) 3 day deadline
6.0%
Movement of items from area to area (PMOVE) 24 hr deadline
2.4%
Non-routine smears (NRS) 5 day deadline
23.9%
Be Site characterization smears (Be-Site) TBD deadlines
1.2%
Operations needed special attention (SPECIAL) 24 hr deadline
0.1%
Downposting of area smears, cleanup work (DNPOST) 24 hr
deadline0.5%
Respirator smears (RESP) 5 day deadline
1.2%
Permanent Air filters (PA) 10 day deadline
1.3%
QA Samples (daily)0.3%
Routine smears (RS) 10 day deadline
11.6%
Non-routine next day smears (NRS-ND) 24 hr deadline
16.2%
Others0.0%
Current Method for Be Analysis
Microwave Digest samples– H2SO4 and H2O2
– Diluted to volume with HNO3
– Final solution is 10% HNO3/6% H2SO4
Samples counted using ICPOES– Use Scandium as Internal Standard
– Look at 313.107 and 313.034 lines
Interfering lines corrected using Inter Element Correction or IEC– Corrects for most spectral interferences, such as Uranium
The Problem? The IEC works great correcting for uranium, to a point:
– High Concentrations of Natural Uranium• Uranium very spectral rich• Require Dilution for Be Quantitation
– Enriched Uranium causes spectral shift• Dependent on Enrichment
Possible Solutions– Dilution
• May lose Be signal• Increase in MDL
– Determine Enrichment for all Samples• Expensive• Time consuming
– Remove/Concentrate Be– Remove Uranium
Method using Eichrom UTEVA
Elegantly simplistic
Prepare column with 10% HNO3/6% H2SO4
Load sample onto column (usually 10 mL)
Collect sample– No rinsing, we do not want to dilute solution
Internal Scandium Standard adjusts for any loss
Sample re-run within the hour
Spiked Sample Recovery0.0005 mg/L Be and 500 mg/L U
Average RSD 7.4%
0
20
40
60
80
100
120
140
160
1 2 3 4 5 6 7 Avg
Samples
Be
reco
vere
d (%
)
Be3130a Be3130b
Decontamination of U0.0005 mg/L Be and 500 mg/L U
>99% Uranium Removal
80
85
90
95
100
105
1 2 3 4 5 6 7
Samples
U R
emov
ed (
% o
f T
otal
)
U367a U367b U367c
So Where is the “REAL” Data
Real Samples yet to be processed– Sample Backlog
– Procedure Approval
Sample will be split
Analysis to be done by ICP-MS and Eichrom Extraction Method
Expect data to statistically be the same
Conclusion/Future Work
UTEVA seems to be fast and reliable method to remove the enriched uranium interference from samples when analyzing for Be
Can also be used to remove high levels of natural uranium from samples
Need to quicken the process– Vacuum Box– Prepacked column– Reduce number of sample
• Customer knowledge??
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