Page:NIOSH Manual of Analytical Methods - 2539.pdf/1

 ALDEHYDES, SCREENING Table 1

MW: Table 1

METHOD: 2539, Issue 2

2539

CAS: Table 1

RTECS: Table 1

EVALUATION: PARTIAL

PROPERTIES:

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

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

Table 1

COMPOUNDS: acetaldehyde; acrolein; butyraldehyde ; crotonaldehyde; formaldehyde; furfural; hepta nal; hexanal; isobutyraldehyde; isovaleraledhyde; propionaldehyde; valeraldehyde. SYNONYMS: Table 1 SAMPLING SAMPLER:

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

FLOW RATE:

0.01 to 0.05 L/min

VOLUME:

5L

SHIPMENT:

@ 25 °C or lower

SAMPLE STABILITY:

at least 1 week @ 25 °C

FIELD BLANKS:

2 to 10 field blanks per seat

MEDIA BLANKS:

6 per set

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY, FID & GC/MS

ANALYTE:

oxazolidine prepared from aldehyde

DESORPTION:

1 mL toluene; 60 min ultrasonic

INJECTION VOLUME:

1:L splitless; split vent time 30 sec

TEMPERATURE-INJECTION: -DETECTOR: -COLUMN:

CARRIER GAS:

He, 0.5 mL/min; makeup flow, 29 mL/min

COLUMN:

capillary, 15 m x 0.32-mm, 1.0-:m film 6% cyanopropyl-phenyl, DB-1301 or equivalent

CALIBRATION:

standard solutions of aldehydes spiked on sorbent

ACCURACY RANGE STUDIED:

not studied

BIAS:

not determined

OVERALL PRECISION (Ö r T ):

not determined

ACCURACY:

not determined

250 °C 280 °C 1 min @ 70 °C, 6 °C/min to 100 °C for 2 min; 30 °C/min to 260 °C

RANGE AND PRECISION:

not determined

ESTIMATED LOD: 2 :g aldehyde per sample APPLICABILITY: This is a screening technique to determine the presence of aldehydes and should not be used for quantitation. Further confirmation of aldehyde identification should be performed by gas chromatography/ mass spectrometry (See Table 2 fo r structural ion dat a). Methods fo r quantitation of some aldeh ydes listed in th is method are available in the NIOSH Manual of Analytical Methods (See OTHER METHODS). All aldehydes tested have detected by this method in bulk field samples. INTERFERENCES: High-boiling naphtha mixtures, such as kerosene and mineral spirits may have components with retention times similar to the oxazolidines and may be interferences in the gas chromatographic analysis. A second column (DB -5, DB-WAX ) may be neede d to separate so me of the earlie r C 3 -C 4 aldehydes from excess HMP reagent. OTHER METHODS: This method incorporates sampling technology used in NIOSH methods 2501 (acrolein), 2541 (formaldehyde), 2529 (furfural), 2531 (glutaraldehyde) [1], and 2526 (valeraldehyde), and OSHA methods 68 (acetaldehyde) and 52 (acrolein/formaldehyde) [2].

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition