Page:NIOSH Manual of Analytical Methods - 1015.pdf/1

 VINYLIDENE CHLORIDE

CH2=CCl2

MW: 96.94

METHOD: 1015, Issue 2

CAS: 75-35-4

1015

RTECS: KV9275000

EVALUATION: FULL

OSHA : no PEL NIOSH: lowest feasible; carcinogen ACGIH: 5 ppm; STEL 20 ppm; carcinogen (1 ppm = 3.96 mg/m 3 @ NTP)

PROPERTIES:

Issue 1: 15 August 1987 Issue 2: 15 August 1994

liquid; d 1.213 g/mL @ 20 °C; BP 31.7 °C; MP -122.5 °C; flammable

SYNONYMS: 1,1-dichloroethene; 1,1-dichloroethylene.

SAMPLING SAMPLER:

SOLID SORBENT TUBE (coconut shell charcoal, 100 mg/50 mg)

FLOW RATE:

0.01 to 0.2 L/min

VOL-MIN: -MAX:

2.5 L @ 1 ppm 7L

SHIPMENT:

routine

SAMPLE STABILITY:

BLANKS:

7 days @ 25 °C 21 days @ 5 °C [2]

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY, FID

ANALYTE:

vinylidene chloride

DESORPTION:

1 mL CS 2; stand 30 min

INJECTION VOLUME:

5 µL

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

150 °C 200 °C 65 °C

CARRIER GAS:

He or N 2, 30 mL/min

COLUMN:

silanized glass, 3 m x 6-mm OD packed with Durapak OPN 100/120 mesh or equivalent

CALIBRATION:

standard solutions of vinylidene chloride in CS 2

RANGE:

10 to 100 µg per sample

2 to 10 field blanks per set

ACCURACY RANGE STUDIED:

7.6 to 10 mg/m 3 [2]

BIAS:

- 0.05

ˆ ): 0.069 OVERALL PRECISION (S rT

ESTIMATED LOD: 7 µg per sample [2]

ACCURACY:

PRECISION (Sr):

± 18.6%

0.048 @ 12 to 85 µg per sample [2]

APPLICABILITY: The working range is 0.5 to 5 ppm (2 to 20 mg/m 3) for a 5-L air sample. The capacity of charcoal for vinylidene chloride decreased rapidly with increasing relative humidity and was also found to be a function of concentration.

INTERFERENCES: The GC column will not separate vinyl chloride and carbon disulfide. Other GC packings that separate vinyl chloride and CS 2 may not separate vinylidene chloride and CS 2. If determination of both of these monomers is to be performed, a capillary column such as a 105 meter Rtx® 502.2 would be required.

OTHER METHODS: The revises P&CAM 266 [1].

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