BERYLLIUM in Surface Wipes: METHOD 9110, Issue 1 dated 06 April 2007 – Page � of 6 REAGENTS: 1. Ammonium bifluoride.* 2. Ethylenediaminetetraacetic acid (EDTA), disodium salt, dihydrate. 3. 10-Hydroxybenzo[h]quinoline-7-sulfonate (HBQS) [5]. 4. L-Lysine monohydrochloride. 5. Sodium hydroxide.* 6. Water, deionized. 7. Dissolution solution:* aqueous ammonium bifluoride, 10 g/L (prepared by dissolving ammonium bifluoride in deionized water). 8. Detection solution:* 63.4 µmol/L HBQS, 2.5 mmol/L EDTA, and 50.8 mmol/L lysine monohydrochloride; pH adjusted to 12.85 with 10 mol/L NaOH). 9. Beryllium standard solution,* 1,000 mg/L (commercially available). 10. Beryllium-spiked media* (commercially available).
- See SPECIAL PRECAUTIONS.
EQUIPMENT: 1. Sampler: wipe, cellulosic, 47 mm diameter minimum. Note: Polyvinyl alcohol (PVA) media are unsuitable for this method. 2. Template, disposable/reusable, 100 cm2 minimum area. 3. Tape, masking. 4. Portable ultraviolet/visible (UV/Vis) fluoro meter, with excitation lamp (λ = 380 nm) and time-integrating visible detector (400 nm to 700 nm, λmax ≈ 475 nm) or optical filters for appropriate wavelengths (excitation of 360 nm to 390 nm; emission of ≈475 nm, with full width at half maximum of less than ±10 nm). 5. Mechanical agitator, shaker, or rotator. 6. Hot block (for beryllium oxide extraction). 7. Fluorescence cuvettes, disposable, 10 mm diameter, transparent to UV/Vis radiation. 8. Centrifuge tubes, plastic, 15 mL. 9. Syringe filters, nylon, 0.45 µm pore size, 13- or 25-mm diameter, in plastic housings. NOTE: Polytetrafluoroethylene (PTFE) filters are unsuitable for this method. 10. Pipettors, mechanical, of assorted sizes. 11. Pipet tips, plastic, disposable, of assorted sizes. 12. Labware, plastic (e.g., beakers, flasks, graduated cylinders), of assorted sizes as needed. 13. Tweezers, plastic or plastic-coated. 14. Laboratory wipes. 15. Personal protective wear (e.g., respirators, gloves, lab coats, safety eyewear) as needed.
SPECIAL PRECAUTIONS: Wear appropriate personal protection during sampling activities and analysis. It is essential that suitable gloves, eye protection, laboratory coat, etc., be used when working with the chemicals. Perform sample preparation and analysis in a clean, well-ventilated area that is well removed from any possible beryllium contamination. Any area affected by the dissolution or detection solutions must be immediately washed with plenty of water. Ammonium bifluoride will etch glass, so it is essential that all ammonium bifluoride solutions be contained in plastic labware. Avoid exposure by contact with skin or eyes, or by inhalation of vapor. SAMPLING [6]: 1. Don a clean pair of gloves. 2. Demarcate the sampling area (100 cm2 minimum) using a clean template or tape. If a template is used, tape the outside edges of the template to the surface to prevent its moving during sampling. 3. Wet a clean wipe with 0.2 mL of deionized water and wipe the surface to be sampled with firm pressure, using 3 to 4 vertical S-strokes. Fold the exposed side of the wipe in and wipe the area with 3 to 4 horizontal S-strokes. Fold the wipe once more and wipe the perimeter of the area. 4. Fold the wipe sample, exposed side in, and place into a labeled 15 mL plasic centrifuge tube. Updated: 04/06/2007
NIOSH Manual of Analytical Methods (NMAM), 5th Edition (Electronic)
