Page:NIOSH Manual of Analytical Methods - Chapter K.pdf/6

 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

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NIOSH Manual of Analytical Methods