Page:NIOSH Manual of Analytical Methods - 2559.pdf/2

 DEC ABR OM OD IPHEN YL OX IDE: ME TH OD 2559, Issue 1, dated 1 5 Ma rch 2003 - Page 2 of 4 REAGENTS:

EQUIPMENT:

1. Me than ol, HP LC grad e.* 2. Dim ethyl Su lfoxide (DM SO ), HP LC grad e.* 3. Decabromodiphenyl oxide, 98%. Sold as Pentabromophenyl ether (Sigma-Aldrich, Milwa ukee, W I., or equivalen t).* 4. Potassium dihydrogen phosphate (KH 2PO 4). (Sigm a-Aldrich, Milwaukee, W I., or equivalent). 5. Disodium hydrogen phosphate (Na 2HPO 4). (Sigm a-Aldrich, Milwaukee, W I., or equivalent). 6. Mobile phase buffer: 1.509 g KH 2PO 4 and 2.477 g Na2HPO 4 in 1 L deionized water.

1. Sam pler: quartz fiber filter, 37-m m diame ter, 0.45 mm thick (SKC, Eighty Four, PA, or equivalent), backed by a cellulose support pad 37-mm OD, in a two part, 37-mm cassette filter holder. 2. For calibration and QC sam ples, filter spacer rings are u sed instea d of a sup port p ad. Space r Ring, 37 m m (SKC, Eighty Four, PA). 3. Personal sampling pump capable of operating for 8 hr at 2 L/min., with flexible connecting tube. 4. Lab qua ke rotary shak er or equ ivalent. 5. Vials, Autosampler, glass with PTFE lined crimp or screw top cap. 6. Forceps. 7. Syringes, glass: 5-µL, 10-µL, 1-mL, other sizes as needed. 8. Liquid Chromatograph: Shimadzu LC-10ADvp pum p, SIL-10AD vp auto injector, and SPD 10AVvp UV detector (or equivalent), Alltech Alltima C -18 5µ, 150 X 2.1 m m colum n (or equivalent).


 * See SPECIAL PRECAUTIONS

SPECIAL PRECAUTIONS: Decabromodiphenyl Oxide is a cancer suspect agent and irritant. Methanol is a flamm able liquid, toxic. DMSO is an irritant, wear protective clothing as it can penetrate the skin.

SAMPLING: 1. Calibrate each personal sampling pump with a representative sampler in line. 2. Sam ple at an accurately known flow rate of 1.0 to 2.0 L/min for a volume of 48 to 960 L. 3. After the sa m ple is c olle cte d, p lace the plastic plugs in the tubing connector stubs on the sampling cassette.

SAMPLE PREPARATION: 4. Extract Filters: a. Re m ove the filter fro m the cass ette with a pair of forceps, discard the support pad, fold the filter and transfer to an autos am pler vial. b. Add 1.5 mL of DMSO and cap the vial with the appropriate top. c. Place the vial on the labquak e rotary shaker (VW R Sc ientific, Batavia, IL). Rotate the samples for a m inim um of 2 h ours. Place sam ples in an ultrasonic ba th for 3 0 m inutes. NOTE: Decabrom odiphenyl oxide is not a highly soluble com pound. T o insure com plete s olubility, both m anual agitation and sonication are used on the samples to solubilize the decabromodiphenyl oxide. 5. Prepare the filter extract for analysis. a. Carefully remove the septum cap from the vial containing the extracted filter. b. Using a transfer pipette, remove as m uch liquid extract from the extraction vial as possible and trans fer to a n au tosa m pler vial. Cap the vial with an app ropriate se ptum cap.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition