1	Application of a beryllium specific resin at the Y-12 National Security Complex Darrin K. Mann, D.H. “Bo” Bowman, Thomas J. Oatts, and Vicki F. Belt Analytical Chemistry Organization Y-12 National Security Complex P.O. Box 2009, MS 8189 Oak Ridge, TN 37831-8189
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3	Be: Why we use it Discovered in 1798 Not widely used in Industry until 1940s and 50s Lighter then Aluminum, Stiffer then Steel 2^nd 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
4	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
5	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
6	Overview of Y-12 Be Program Over 50K Samples Analyzed in 04. Average 53 +/- 79 samples/day Average 2625 +/- 876 samples/month Average turnaround time is 24 hours.
7	Typical Workloads Associated with Be Program
8	Breakdown of Be Smears at Y-12
9	Basic Flow Chart for Analysis of Be Smear Program
10	The Problem? The Internal Standard (IS) works great correcting interferences to a point: High Concentrations of Interfering Elements Some elements are very spectral rich Uranium Shift depends on enrichment Some elements overlap spectrally Vanadium, Cesium and Zirconium are examples Dilution not useful for these elements Possible Solutions Dilution May lose Be signal Increase in MDL Run samples by ICPMS Expensive (relative to an OES) Not as rugged as OES (can’t handle 500 samples/day) Remove/Concentrate Be
11	Method using Eichrom Be resin Elegantly simplistic Usually use 5 ml of sample left over from ICPOES analysis Adjust sample pH to between 1-2 with 4 M Sodium Acetate 2% Crystal Violet used as indicator (3-4 drops) Load sample onto Be cartridge (usually 10 mL) and pass through at 2 ml/min Rinse cartridge with 10 ml of 0.2 M HNO₃ at 2 ml/min Elute Be with 10 ml of 4M HNO₃ at < 1 ml/min Sample can be re-run within a few hours.
12	Vacuum System with Be cartridges and 10 ml Reservoirs
13	How clean are the Samples?
14	Comparison of Be data using Be Resin and ICPMS Analysis
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16	Be recovery Conc. Before and After Be cartridge ICP Analysis Represents “Normal” Analysis
17	Percent Recovery of Be vs. Initial Concentration ICPMS and ICPOES Results
18	So Where is the Be Going? ICPMS data appears acceptable, so Be is there. Recovery of Be in ICV and CCV is fine Colored samples may cause pH problem Yellow Samples are a particular problem Answer may lie in looking at IS Scandium Signal is being suppressed RSD is very poor (5-10%)
19	Recovery of IS Scandium 2 mg/L standard added
20	Why is IS Signal being Suppressed? Doesn’t seem to correct in same ratio as Be Very large suppression at times, up to 75% of signal. Only source of suppression can come from column Doesn’t seem to be acid concentration based An organic from the resin may be complexing with Sc and pulling it out of solution Need to remove organic after it passes through initial column.
21	Recovery of Sc IS using Post Organic Resin Cartridge 2 ug/L Sc added
22	Conclusion/Future Work Eichrom’s Be resin seems to be a fast and reliable method to remove spectral interferences from samples when analyzing for Beryllium Need to better understand the effects of residual organics on the recovery of Internal Standards such as Sc. A post organic filter seems to solve the problem Filter could be used to Lower MDL ACGIH has recently issued a Notice of Intended Change (NIC) to lower the Threshold Limit Value (TLV) for airborne beryllium to 0.02 micrograms per cubic meter, or one-tenth of the current DOE action level. Concentrate sample onto column, elate with smaller volume Need to quicken the process Reduce number of sample Customer knowledge??