Page:NIOSH Manual of Analytical Methods - 2008.pdf/1

 CHLOROACETIC ACID

ClCH2COOH

MW: 94.50

METHOD: 2008, Issue 2

CAS: 79-11-8

2008

RTECS: AF8575000

EVALUATION: FULL

OSHA : no PEL NIOSH: no REL ACGIH: no TLV (1 ppm = 3.87 mg/m 3 @ NTP)

PROPERTIES:

Issue 1: 15 May 1989 Issue 2: 15 August 1994

solid; MP 61 to 63 °C; BP 189 °C; VP 0.1 kPa (0.75 mm Hg) @ 20 °C; flash point 126 °C; lower explosive limit in air 8% v/v

SYNONYMS: chloroethanoic acid; monochloroacetic acid

SAMPLING

MEASUREMENT

SAMPLER:

SOLID SORBENT TUBE (silica gel, 100 mg/50 mg)

TECHNIQUE:

ION CHROMATOGRAPHY, CONDUCTIVITY DETECTION

FLOW RATE:

0.05 to 0.2 L/min

ANALYTE:

chloroacetate ion

VOL-MIN: -MAX:

1 L @ 0.25 ppm 100 L

DESORPTION:

2 mL deionized water

SHIPMENT:

routine

INJECTION LOOP VOLUME:

500 µL

ELUENT:

1.5 mM NaHCO 3; 1.0 mL/min

COLUMNS:

Ion Pac AS4A Separator, AG4A Guard, micromembrane suppressor (see OTHER METHODS)

CALIBRATION:

standard solutions of chloroacetic acid in deionized water

RANGE:

1 to 80 µg per sample [1]

SAMPLE STABILITY:

BLANKS:

at least 7 days @ 25 °C; 32 days refrigerated [1] 2 to 10 field blanks per set

ACCURACY RANGE STUDIED:

BIAS:

0.35 to 29 mg/m 3 [1,2] (3-L samples)

ESTIMATED LOD: 0.04 µg per sample [2]

- 2.0%

PRECISION (Sr):

0.016 [1]

ˆ ): 0.08 [1] OVERALL PRECISION (S rT ACCURACY:

± 17.7%

APPLICABILITY: The working range is 0.09 to >85 ppm (0.3 to 30 mg/m 3) for a 3-L air sample.

INTERFERENCES: Chloroacetyl chloride is a positive interferent since it is hydrolyzed to monochloroacetic acid by the measurement procedure and is efficiently collected by silica gel [3]. Particulate salts of the acid are positive interfe rents. The chromatographic conditions given will separate acetate, chloride, dichloroacetate, fluoride, glycolate, and trichloroace tate ions from chloroacetate ion.

OTHER METHODS: This revises P&CAM 332 [2]. The columns used in P&CAM 332 are no longer available. The newer columns indicated here show improvements in the analytical range and sensitivity.

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