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Expertise in Sample Preparation

Application Note: 602

Beryllium Analysis-Matrix Removal
for more reliable ICP-AES analysis

Introduction: Beryllium metal, alloys and salts have been used widely in industry for decades.
Beryllium is particularly valuable in specific areas of nuclear technology. Its ability to reflect
neutrons and its efficiency in the production of neutrons when exposed to alpha emitters has led
to its use in nuclear reactors and nuclear weapons. However, the use of Be carries with it someserious health hazards, the most serious of which is chronic beryllium disease (CBD). Chronic
beryllium disease is caused by the inhalation of beryllium compounds, particularly the oxide, andscarring of the lung tissue. Because of the seriousness of CBD, the United States Department ofEnergy promulgated in 1999 the CBD prevention program, 10CFR Part 850, to protect DOE
workers from exposure to beryllium contaminated dust.
The Problem: Due to the incidence of Chronic Beryllium Disease, analysis of surface wipes
and air filters by ICP-AES is widely practiced at U.S. DOE sites to monitor potential exposure toberyllium. However, several elements, including uranium, vanadium, cerium, zirconium andniobium can interfere with the determination of beryllium by ICP-AES, especially at the low
detection limits required under 10 CFR 850.
The Solution: A beryllium sample preparation method has been developed to remove allspectrally interfering elements and many other matrix elements from samples prior to analysis byICP-AES. The method was developed for samples containing sufficient amounts of spectrallyinterfering elements that correction by ICPAES software is unreliable. The method
involves the use of a chelating diphosphonicacid extractant sorbed onto acrylic ester
beads and is marketed under the trade name,
Beryllium Resin. Figure 1 shows theseparation of beryllium from a number ofspectrally interfering elements using
Beryllium Resin. It highlights the simplicityof the method in three steps;
1: Adjust the digested filter wipe to pH 1
to 2 with sodium acetate and load on a 2mL Beryllium Resin cartridge,
2: Rinse with 0.2 M nitric acid, and
3: Strip beryllium with 4M nitric acid.
The three step method is compatible with any
digestion technique. Should hydrofluoric acidbe used, 0.1 M boric acid must be added to theload solution. Samples are processed in about
an hour using a vacuum box which serves as asample collector using 50 ml disposable
centrifuge tubes.
01/06/2006

Figure 1. Elution of Be, Ce, U, Zr, and Nb on a 2 mL
dry packed cartridge of Beryllium Resin, 50-100 µm
particle size, flow rate 2mL/min, 22(1)°C, Load: 5.5 cm
ashless filter spiked with 140 µg Be, Ce, U, Zr and Nb,digested with H2SO4 and H2O2, diluted to 10mL withHNO3 and neutralized to pH 1 with 3.4 M sodium
acetate.

Application Note: 602

Data: The method has been tested at BWXT Y-12 on filter wipe samples which had yieldedunacceptable results by ICP-AES measurement alone. Y-12 digests their samples with sulfuric
acid and hydrogen peroxide. This is followed up by nitric acid. Analysis of samples containing
between 75 and 500 ppm U of various enrichment all produced negative Be results. These dirty
samples required re-testing by ICP-MS resulting in costly maintenance and turn around timeissues.
These same samples run through the Beryllium Resin compared well with the ICP-MS results.
Yields ranged from 94 to 111%, using the ICP-MS values as the standard. Beryllium values
ranged from 0.0428 to 0.1452 micrograms per 100 square cm filter. By comparison, DOE has
set 0.2 micrograms Be per 100 sq. cm as the limit for releasing equipment to non-beryllium
areas.
Table 1.
Unlike U, vanadium tends to create a high bias. Twostandards were created one containing 80 ppm
vanadium and 0.001 ppm Be and the second containing
Standard 10.001 ppm Be, 80 ppm V, 400 ppm Cr, 800 ppm Fe, 2ppm Sc and 100 ppm each of Mo, Nb, Th, Ti, U, Y, andStandard 2Zr. Ten ml of 0.3 M oxalic acid was added to thesamples. Virtually all interferences were removed.
The results are shown in Table 1.

Recoveryw/ cartridge
99.9%

Recovery w/ocartridge
2010%

67.8%

4160%

Y-12 has implemented this method on samples showing negative Be or high U during an ICPAES scan. Because of the consistency of the Beryllium Resin processed samples, no internal
standard is necessary. The method is fast, reliable, robust and simple and can be used toconcentrate beryllium. This provides a tool to address new lower measurement requirements
being considered by ACGIH. Additionally, the method continues to be developed to look at theeffect of even higher concentrations of interfering metals. Different resins can be paired with theBeryllium Resin to handle virtually any matrix combination.
References:
T. P. Taylor, et al., J. Environ. Sci., A38 (2003) 439-469.
E. P. Horwitz & D. R. McAlister, Solvent Ext. Ion Exchange. 23(5), 611-629 (2005)
D. R. McAlister & E. P. Horwitz, Talanta, 67(5), 873-879, (2005)

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01/06/2006

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