Page:NIOSH Manual of Analytical Methods - 5503.pdf/1

 POLYCHLOROBIPHENYLS

mixture:

C12H10-x Clx [where x = 1 to 10]

MW: ca. 258 (42% Cl ; C12H7Cl3); ca. 326 (54% Cl ; C12H5Cl5)

METHOD: 5503, Issue 2

CAS: Table 1

EVALUATION: PARTIAL

OSHA : 1 mg/m3 (42% Cl); 0.5 mg/m3 (54% Cl) NIOSH: 0.001 mg/m3/10 h (carcinogen) ACGIH: 1 mg/m3 (42% Cl) (skin) 0.5 mg/m3 (54% Cl) (skin)

5503

RTECS: Table 1

Issue 1: 15 February 1984 Revision #1: 15 August 1987 Issue 2: 15 August 1994

PROPERTIES: 42% Cl: BP 325 to 366 °C; MP -19 °C; d 1.38 g/mL @ 25 °C; VP 0.01 Pa (8 x 10-5 mm Hg; 1 mg/m3) @ 20 °C 54% Cl: BP 365 to 390 °C; MP 10 °C; d 1.54 g/mL @ 25 °C; VP 0.0004 Pa (3 x 10-6 mm Hg; 0.05 mg/m3) @ 20 °C

SYNONYMS: PCB; 1,1'-biphenyl chloro; chlorodiphenyl, 42% Cl (Aroclor 1242); and 54% Cl (Aroclor 1254)

SAMPLING SAMPLER:

FILTER + SOLID SORBENT (13-mm glass fiber + Florisil, 100 mg/50 mg)

FLOW RATE: 0.05 to 0.2 L/min or less VOL-MIN: -MAX:

1 L @ 0.5 mg/m3 50 L

SHIPMENT:

transfer filters to glass vials after sampling

SAMPLE STABILITY:

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY, ECD (6 3Ni)

ANALYTE:

polychlorobiphenyls

DESORPTION:

filter + front section, 5 mL hexane; back section, 2 mL hexane

INJECTION VOLUME:

unknown for filters; 2 months for Florisil tubes [1]

4-µL with 1-µL backflush

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN: CARRIER GAS:

BLANKS:

250 to 300 °C 300 to 325 °C 180 °C

N2, 40 mL/min

2 to 10 field blanks per set COLUMN:

glass, 1.8 m x 2-mm ID, 1.5% OV-17/1.95% QF-1 on 80/100 mesh Chromosorb WHP

ACCURACY RANGE STUDIED:

not studied

BIAS:

none identified

ˆ ): not evaluated OVERALL PRECISION (S rT ACCURACY:

not determined

CALIBRATION:

standard PCB mixture in hexane

RANGE:

0.4 to 4 µg per sample [2]

ESTIMATED LOD: 0.03 µg per sample [2] PRECISION (Sr):

0.044 [1]

APPLICABILITY: The working range is 0.01 to 10 mg/m3 for a 40-L air sample [1]. With modifications, surface wipe samples may be analyzed [3,4].

INTERFERENCES: Chlorinated pesticides, such as DDT and DDE, may interfere with quantification of PCB. Sulfur-containing compounds in petroleum products also interfere [5].

OTHER METHODS: This method revises methods S120 [6] and P&CAM 244 [1]. Methods S121 [7] and P&CAM 253 [8] for PCB have not been revised.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94