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ACETALDEHYDE by HPLC
3507
CH3CHO
MW: 44.05
CAS: 75-07-0
RTECS: AB1925000

METHOD: 3507, Issue 2
EVALUATION: FULL
Issue 1: 15 August 1987

Issue 2: 15 August 1994


OSHA: 200 ppm
PROPERTIES: liquid; d 0.78 g/mL @ 20 °C; BP 20.4 °C; MP
NIOSH: carcinogen; lowest feasible
−123 °C; VP 100 kPa (750 mm Hg; 99% v/v) @
ACGIH: C 25 ppm; suspect carcinogen
20 °C; explosive range 4 to 60% in air
(1 ppm = 1.801 mg/m³ @ NTP)

SYNONYMS: ethanal; acetic aldehyde


SAMPLING
MEASUREMENT

SAMPLER: LIQUID IN BUBBLER
(midget bubbler containing 15 mL Girard T
solution @ pH 4.5)

FLOW RATE: 0.1 to 0.5 L/min

VOL-MIN: 6 L @ 200 ppm

-MAX: 60 L

SHIPMENT: seal bubblers to prevent leakage before

shipping; protect from light

SAMPLE STABILITY: 1 week @ 25 °C in dark [1]

FIELD BLANKS: 2 to 10 field blanks per set


ACCURACY

RANGE STUDIED: 170 to 670 mg/m³ [1] (60-L samples)

BIAS: 1.2%

OVERALL PRECISION (ŜrT): 0.053 [1]

ACCURACY: ±14.4%

TECHNIQUE: HPLC, UV

ANALYTE: Girard T derivative

SAMPLE
PREPARATION: dilute 5 mL sample to 100 mL with HPLC

mobile phase

INJECTION
VOLUME: 50 µL

COLUMN: 50 cm × 2-mm ID SS, Zipax SCX

DETECTOR: UV @ 245 nm for acetaldehyde

MOBILE PHASE: Na2HPO4/NaH2PO4 buffer, 0.75 mL/min

CALIBRATION: standard solutions of acetaldehyde in

Girard T reagent

RANGE: 2 to 60 mg per sample [1]

ESTIMATED LOD: 0.1 mg per sample [1]

PRECISION (Ŝr): 0.024 @ 11 to 43 mg per sample [1]


APPLICABILITY: The working range is 18 to 372 ppm (33 to 670 mg/m³) for a 60-L air sample. The method is sensitive enough for short-term exposure sampling and can be used to measure lower concentrations by diluting samples to less than the recommended 100 mL.


INTERFERENCES: Other volatile aldehydes and ketones (e.g., acetone, acrolein, benzaldehyde, formaldehyde, furfural, methyl ethyl ketone, and propionaldehyde) compete for the Girard T reagent which should be kept at a two-fold molar excess over aldehyde concentration. Chromatographic conditions may be adjusted to resolve acetaldehyde from other aldehydes [1].


OTHER METHODS: This revises S345 [2]. Method 2538 is an adaptation of OSHA Method 68, which uses solid sorbent collection and GC analysis. Other reported methods for acetaldehyde use collection in 2,4-dinitrophenylhydrazine solution [3,4].


NIOSH Manual of Analytical Methods (NMAM), Fourth Edition