Page:NIOSH Manual of Analytical Methods - 2010.pdf/1

 AMINES, ALIPHATIC (1) Diethylamine: (C2H5)2NH (2) Dimethylamine: (CH3)2NH

MW: 73.14 45.08

METHOD: 2010, Issue 2

2010

CAS: 109-89-7 124-40-3

RTECS: HZ8750000 IP8750000

EVALUATION: PARTIAL

OSHA : See Table 1 NIOSH: See Table 1 ACGIH: See Table 1

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

PROPERTIES: See Table 1

SYNONYMS: (1) DEA; N,N-diethamine; N-ethylethanamine; (2) N-methylmethanamine; DMA SAMPLING

MEASUREMENT

SAMPLER:

SOLID SORBENT TUBE (silica gel, 150 mg / 75 mg)

FLOW RATE:

0.01 to 1.0 L/min

VOL-MIN: -MAX:

3 L @ OSHA standards (Table 1) 30 L

SHIPMENT:

refrigerated

SAMPLE STABILITY:

not determined

FIELD BLANKS:

2 to 10 field blanks per set

TECHNIQUE:

GAS CHROMATOGRAPHY, FID

ANALYTE:

amines listed above

DESORPTION:

1 mL dilute H 2SO 4 in 10% (v/v) aqueous methanol, 3 h ultrasonic

INJECTION VOLUME:

1 µL

COLUMN:

1.8 m x 4-mm ID glass, 4% Carbowax 20M + 0.8% KOH on Carbosieve B (60/80 mesh)

CARRIER GAS:

nitrogen, 30 mL/min

CALIBRATION:

standard solutions of analyte in dilute sulfuric acid

RANGE:

(1) 0.5 to 11 mg per sample [1] (2) 0.15 to 2.6 mg per sample [1]

ACCURACY RANGE STUDIED: see EVALUATION OF METHOD BIAS:

(1) -5.0%; (2) 0.8%

ˆ ): OVERALL PRECISION (S rT METHOD ACCURACY:

see EVALUATION OF

ESTIMATED LOD: 0.02 mg per sample PRECISION (Sr):

see EVALUATION OF METHOD

(1) ±16.0%; (2) ±12.5%

APPLICABILITY: The working ranges for 20-L air samples are 8 to 183 ppm (25 to 550 mg/m 3) for diethylamine and 4 to 71 ppm (7.5 to 130 mg/m 3) for dimethylamine. A nitrogen-specific detector instead of an FID will greatly increase sensitivity. This alternative detector has been used for amines with a 30 m x 0.25-mm x 0.25-µm film DB-5 fused-silica capillary column, w ith column temperature 60 °C for 1 min, programmed to 300 °C at 10°/min; detector, 300 °C and injector, 250 °C.

INTERFERENCES: This method has been evaluated only in dry air [1]. Silica gel may have a reduced capacity at high humidity. The methanol peak could interfere in low-level analyses.

OTHER METHODS: This revises and combines Methods S139 and S142 [2]. The methods for other aliphatic amines are similar [3,4,5,6]. To avoid possible sample instability on silica gel, OSHA developed a method (OSHA 34) which employs XAD-7 coa ted with 7-chloro-4-nitrobenzo-2-oxa-1,3-diazole for sampling followed by HPLC of the derivative [7].

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