Page:NIOSH Manual of Analytical Methods - 2536.pdf/1

 VALERALDEHYDE

CH3(CH2)3CH=O

M.W.: 86.13

METHOD: 2536, Issue 2

CAS: 110-62-3

EVALUATION: FULL

OSHA : no standard NIOSH: 50 ppm ACGIH: 50 ppm (1 ppm = 3.52 mg/m 3 @ NTP)

2536

PROPERTIES:

RTECS: YV3600000 Issue 1: 15 May 1989 Issue 2: 15 August 1994

liquid; d 0.810 g/mL @ 20 °C; BP 103 °C; VP 6.7 kPa (50 mm Hg) @ 25 °C; vapor density (air = 1) 3.0; flash point = 12.2 °C

SYNONYMS: pentanal; amyl aldehyde.

SAMPLING SAMPLER:

SOLID SORBENT TUBE (10% 2-(hydroxymethyl)piperidine on XAD-2, 120 mg/60 mg)

FLOW RATE:

0.01 to 0.04 L/min

VOL-MIN: -MAX:

0.5 L@ 50 ppm 10 L

SHIPMENT:

routine

SAMPLE STABILITY:

at least 4 weeks @ 25 °C [1]

FIELD BLANKS:

2 to 10 field blanks per set

MEDIA BLANKS:

18 per set

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY, FID

ANALYTE:

valeraldehyde oxazolidine (9-butyl-1aza-8-oxabicyclo[4.3.0]nonane)

DESORPTION:

2 mL toluene, 60 min ultrasonic

INJECTION VOLUME:

1 µL splitless

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

250 °C 280 °C 0.5 min @ 70°C; 50 °C/min to 120°C, hold 4 min; 20°C/min to 170°C, hold 7 min

CARRIER GAS:

He, 27 cm/sec linear velocity makeup flow 29 mL/min

COLUMN:

capillary, 15 m x 0.32-mm, 5% phenyl, 95% methyl polysiloxane, 1-µm film (DB-5 or equivalent)

CALIBRATION:

standard solutions of valeraldehyde on sorbent

OVERALL PRECISION (SrT): 0.073 [1]

RANGE:

4 to 3900 µg per sample [1]

ACCURACY:

ESTIMATED LOD: 2 µg per sample [1]

ACCURACY RANGE STUDIED:

9 to 374 mg/m 3 [1] (12-L samples)

BIAS:

0.12%

± 14.4%

PRECISION (Sr):

0.066 @ 2 to 508 µg per sample [1]

APPLICABILITY: The working range is 0.11 to 110 ppm (0.4 to 390 mg/m 3) for a 10-L air sample. The method is also suitable for determination of furfural and glutaraldehyde in a mixture [2].

INTERFERENCES: None have been observed; an alternate capillary column, 15 m x 0.32-mm cyanopropylphenyl dimethylpolysiloxane, 1-µm film (DB-1301) can be used.

OTHER METHODS: The method of Lipari and Swarin [3] uses 2,4-dinitrophenylhydrazine for the collection of valeraldehyde.

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