Page:NIOSH Manual of Analytical Methods - 2543.pdf/1

 HEXACHLOROBUTADIENE

Cl2C:CClCCl:CCl2

MW: 260.74

METHOD: 2543, Issue 2

2543

CAS: 87-68-3

RTECS: EJ0700000

EVALUATION: FULL

OSHA : no PEL NIOSH: 0.02 ppm (skin); carcinogen ACGIH: 0.02 ppm (skin); carcinogen (1 ppm = 10.67 mg/m 3 @ NTP)

PROPERTIES:

Issue 1: 28 June 1979 Issue 2: 15 August 1994

clear, colorless liquid with a mild odor; d = 1.675 (15.5 °C); VP 2.9 kPa (22 mm Hg) @ 100 C°; B.P. 220 °C

SYNONYMS: 1,3-hexachlorobutadiene; HCBD; perchlorobutadiene; DOLEN-PUR

SAMPLING SAMPLER:

SOLID SORBENT TUBE (XAD-2; 100 mg/50 mg)

FLOW RATE:

0.05 to 0.2 L/min

VOL-MIN: -MAX:

1L 100 L @ 0.2 L/min

SHIPMENT:

routine, but store in dark

SAMPLE STABILITY:

7 days @ 25 °C; 28 days @ 0 °C in dark

BLANKS:

2 to 10 field blanks per set

ACCURACY RANGE STUDIED:

0.01 to 2 mg/m 3 [1] (100-L samples)

BIAS:

+ 0.5%

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY/ECD

ANALYTE:

hexachlorobutadiene (HCBD)

EXTRACTION:

2 mL hexane; ultrasonic bath 1 h

INJECTION VOLUME:

1 µL

TEMPERATURE-INJECTOR: -DETECTOR: -COLUMN:

150 °C 250 °C 135 °C

COLUMN:

Nukol or Stabilwax-DA

CARRIER GAS:

Ar, 30 mL/min

DETECTOR:

ECD

PURGE GAS:

He or N 2, 80 mL/min

CALIBRATION:

standard solutions of hexachlorobutadiene in hexane

RANGE:

0.06 µg to 6 µg per sample [1]

ESTIMATED LOD:

0.02 µg per sample [1]

PRECISION (Sr):

0.03 [1]

ˆ ): 0.09 [1] OVERALL PRECISION (S rT ACCURACY:

± 18.1%

APPLICABILITY: The working range is 0.01 to 2.0 mg/m 3 for a 100-L sample [1]. An alternate column, DB-210, may be used with appropriate changes in instrumental conditions.

INTERFERENCES: Conditions of high humidity (>90%) may reduce capacity. Any compound with overlapping or similar retention times, or any sample containing chloroform may interfere[2].

OTHER METHODS: This revises method P&CAM 307 [1].

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