Reagent
NIOSH 5521
NIOSH 5522
NIOSH 2535
OSHA 42/47
PROPOSED NEW NIOSH1
MOPP in toluene
tryptamine in DMSO
nitro reagent 7d 25 C in dark
1-2PP 42 0.1 mg; 47 1 mg 6 mo 0 C sealed
MAP in butyl benzoate
Shelf Life
7d 0 C
6 mo 25 C in dark
Sampling Rate Volume
1 L/min 5-500 L
1-2 L/min 15-360 L
0.2-1 L/min 2-170 L
1 L/min 15 L
1-2 L/min 1-500 L
Personal
No
No
Yes
Yes
Yes
Vapor
Yes
Yes
Yes
Yes
Yes
Particles 2 µm
No
No
No
Yes
impinger: No filter: Yes
a) Slow-cure
Yes
Yes
No
No3
impinger: Yes filter: No3
b) Fast-cure4
Yes
Yes
No
No
impinger: Yes filter: No
Sample Stability
7d 25 C: 78% 7d 4 C: 88%
28d 25 C in dark: 95-104%
14d 25 C: 91%
15d 22 C: 42 80-86%; 47 94.8%
unknown
Laboratory Sample Preparation
impinger: evap/ redissolve in methanol
none
ultrasonic extraction in methanol
extraction in ACN/ DMSO, 9 /1
impinger: SPE filter: extract or SPE
Technique
HPLC/RP, isocratic
HPLC/RP, gradient
HPLC/RP, isocratic
HPLC/RP, isocratic
HPLC/RP, gradient
Detector 1 LOD5: a) amount injected b) 15 L air conc.
UV @ 242 nm/ PDA
UV @ 254 nm 14 pmol 0.9 ppb
FL ex 240 nm em 370 nm 0.2 - 1 pmol 0.06 - 0.1 ppb
UV @ 253 nm
14 pmol 1.2 ppb
FL ex 275 nm em 320 nm 0.7 pmol 0.9 ppb
Detector 2 LOD5: a) amount injected b) 15 L air conc
EC (+ 0.8V)
EC (+ 0.8V)
None
UV @ 254 nm
FL ex 250 nm em 409 nm est. ~ 5 fmol est. ~ 0.8 ppt
Identification
Monomer: Retention Time Aliphatic oligomers: PDA
Monomer: FL Retention Time Other isocyanate: EC confirmation
Retention Time
Retention Time
Monomer: Retention Time Other isocyanate: UV/FL ratio
unknown
Particles 2 µm
0.5 pmol 0.04 ppb
0.5 pmol 0.08 ppb
1
This method is under development; procedures may change somewhat pending validation. Determination possible; lacks validation data. Usually underestimates concentration. 4 Half-life under several minutes. 5 Instrumental limit of detection Abbreviations: ACN = acetonitrile; conc = concentration; d = days; DMSO = dimethyl sulfoxide; EC = electrochemical detector; em = emission; evap = evaporate; ex = excitation; FL = fluorescence detector; GFF = glass fiber filter; HPLC = high performance liquid chromatography; LOD = limit of detection; MAP = 1-(9anthracenylmethyl)piperazine; mo = months; MOPP = 1-(2-methoxyphenyl)piperazine; nitro reagent = N-[(4-nitrophenyl) methyl] propylamine; PDA = photodiode array detector; 1-2PP = 1-(2-pyridyl)piperazine; RP = reversed phase; SPE = solid phase extraction; UV = ultraviolet detector 2 3
1/15/98
120
NIOSH Manual of Analytical Methods
