Page:NIOSH Manual of Analytical Methods - 9110.pdf/5

 BERYLLIUM in Surface Wipes: METHOD 9110, Issue 1 dated 06 April 2007 – Page � of 6 EVALUATION OF METHOD: The method was evaluated [7] in accordance with published guidelines [8]. Experiments were conducted using an Ocean Optics® portable fluorescence device with the following components: USB 200 spectrometer with spectral grating #2 (UV/Vis 600), LS-1 lamp (380 nm) in LS-450 housing, UV-2 casting, OFLV linear filter 200-850, L2 collection lens and slit-200. Tests were carried out in relative irradiance mode using 2- or 5-second integration times. The method was evaluated using beryllium oxide spiked onto Whatman #541 cellulose and nylon filters at levels of (0, 0.02, 0.1, 0.2, 0.3, 0.4, 1.5, 3.0, and 6.0) µg (five samples at each level). The method was also field-tested using real-world samples (collected using Whatman #541 cellulose and nylon filters) obtained at U.S. Department of Energy sites suspected to be contaminated with beryllium. Field samples measured by portable fluorometry were also analyzed using hot-plate digestion and ICPAES analysis. The latter served as a reference analytical method. Observed sample loadings ranged from below the detection limit (<0.02 µg per sample) to ≈12 µg per sample. Long-term stability of samples was verified from spikes (number [n] = 30) of 0.1 µg Be on Whatman #541 cellulose and nylon filters. Samples were analyzed at day one (n = 12) and then one week (n = 6), ten days (n = 3), two weeks (n = 3), three weeks (n = 3), and one month (n = 3) after spiking. No diminution of fluorescence signal was observed from samples prepared and analyzed after having been stored for up to thirty days. Interference tests were carried out using solutions of 0 nmol/L, 100 nmol/L, and 1.0 µmol/L Be in the presence of 0.4 mmol/L Al, Ca, Co, Cu, Fe, Ti, Li, Ni, Pb, Sn, U, V, W, or Zn (separate experiments were carried out for each potential interferant). An interlaboratory evaluation of the method was also performed [9]. REFERENCES: [1]	Agrawal A, Cronin J, Tonazzi J, McCleskey TM, Ehler DS, Minogue EM, Whitney G, Brink C, Burrell AK, Warner B, Goldcamp MJ, Schlecht PC, Sonthalia P, Ashley K [2006]. Validation of a standardized portable fluoresence method for determining trace beryllium in workplace air and wipe samples. J Environ Monit 2006 (8): 619- 624. [2]	Ashley K, Agrawal A, Cronin J, Tonazzi J, McCleskey TM, Burrell AK, Ehler DS [2007]. Ultra-trace determination pf beryllium in occupational hygiene samples by ammonium bifluoride extraction and fluorescence detection using hydroxybenzoquinoline sulfonate. Analytica Chimica Acta 584 (2007): 281-286.	 [3]	NIOSH [1994]. Elements by ICP (nitric/perchloric acid ashing): Method 7300 (supplement issued 3/15/03). In: NIOSH manual of analytical methods. 4th ed. Cincinnati, OH: U.S. Department of Health and Human Services, Public Health Service, Centers for Disease Control and Prevention, National Institute for Occupational Safety and Health, DHHS (NIOSH) Publication No. 94–113. [4]	ASTM [2006]. D7202 Standard test method for determination of beryllium in the workplace using field-based extraction and fluorescence detection. West Conshohocken, PA: ASTM International. [5]	Matsumiya H, Hoshino H, Yotsuyanagi T [2001]. A novel fluorescence reagent, 10-hydroxy­ben­ zo[h]quinoline-7-sulfonate, for selective determination of beryllium(II) ion at pg cm−3 levels. Analyst 126:2082–2086.	 [6]	ASTM [2003]. D6966 - Standard practice for wipe sampling of surfaces for subsequent determination of metals. West Conshohocken, PA: ASTM International. NIOSH Manual of Analytical Methods (NMAM), 5th Edition (Electronic)

Updated: 04/06/2007