Page:NIOSH Manual of Analytical Methods - 2517.pdf/1

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OSHA:  

no standard

NIOSH:  

handle with caution

ACGIH:  

no standard (1 ppm = 8.27 mg/m³ @ NTP)

PROPERTIES:  

liquid; d 1.671 g/mL @ 25 °C; BP 162 °C; VP 450 Pa (3.4 mm Hg; 4500 ppm) @ 20 °C

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SYNONYMS:  

Pentalin; ethane pentachloride.

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SAMPLING

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SAMPLER:  

SOLID SORBENT TUBE
(Porapak R, 70 mg/35 mg)

FLOW RATE:  

0.01 to 0.2 L/min

VOL-MIN:  

1 L @ 0.1 mg/m³

10:  

10 L

SHIPMENT:  

routine

SAMPLE STABILITY:  

stable ≥ 7 days @ 25 °C;
≥ 21 days @ 0 °C in the dark

BLANKS:  

2 to 10 field blanks per set

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ACCURACY

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RANGE STUDIED:  

0.014 to 5.37 mg/m³[1]
(3-L samples)

BIAS:  

not significant [1]

OVERALL PRECISION (${\hat {S}}_{rT}$^[1]):  

0.075 [1]

ACCURACY:  

± 15%

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MEASUREMENT

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MEASUREMENT:  

GAS CHROMATOGRAPHY,⁶³Ni ECD

ANALYTE:  

pentachloroethane

DESORPTION:  

2 mL hexane; 30 min ultrasonic

TEMPERATURE-INJECTION:  

240 °C

-DETECTOR:  

250 °C

-COLUMN:  

70 °C

INJECTION VOLUME:  

5 µL

CARRIER GAS:  

5% methane, 95% argon; 30 mL/min

DETECTOR PURGE GAS:  

5% methane, 95% argon if required; 80 mL/min

COLUMN:  

nickel, 2-mm ID x 2 m, packed with 3% OV-17 on 100/120 mesh Chromosorb WHP

CALIBRATION:  

standard solutions of pentachloroethane in hexane

RANGE:  

0.04 to 40 µg per sample

ESTIMATED LOD:  

0.004 µg per sample [2]

PRECISION (${\hat {S}}_{r}$^[2]):  

0.019 [1]

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APPLICABILITY: The working range is 0.01 to 20 mg/m³ (0.001 to 2.4 ppm) for a 5-L air sample.

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INTERFERENCES: 1,2,2,3-Tetrachloropropane interferes with the analyte GC peak but is not likely to be present in most samples. Large concentrations of 1,1,2,2-tetrachloroethane may obscure the analyte GC peak.

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OTHER METHODS: This revises P&CAM 335 [2].

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

1. Estimate of overall precision including pump error. Formerly ${\hat {C}}V_{T}$
2. Pooled relative standard deviation. Formerly ${\hat {C}}V$