Page:NIOSH Manual of Analytical Methods - 8317.pdf/1

 ANILINE and @-TOLUIDINE in urine (1) Aniline: C6 H7 N (2) @-Toluidine: C7 H9 N

MW: 93.13 MW: 107.16

METHOD: 8317, Issue 1

CAS: 62-53-3 CAS: 95-53-4

8317 RTECS: BW6650000 RTECS: XU2975000

EVALUATION: PARTIAL

Issue 1: 15 March 2003

BIOLOGICAL INDICATOR OF: exposure to (1) aniline and (2) @-toluidine ACGIH BEI: none SYNONYMS: (1) (2)

aniline: benzeneamine; aminobenzene; phenylamine @-toluidine: 2-aminotoluene SAMPLING

MEASUREMENT

SPECIMEN:

Urine

TECHNIQUE:

HPLC with electrochemical detection

VOLUME:

At least 4 mL of sample

ANALYTE:

Aniline and @-toluidine

TREATMENT:

Base hydrolysis and liquid-liquid extraction

PRESERVATIVE: 5 g citric acid SHIPMENT:

SAMPLE STABILITY: CONTROLS:

Freeze urine; ship on dry ice in an insulated container

Sample stable for over 6 months at -65 o C Collect urine from non-occupationally exposed workers

INJECTION VOL.: 50 :L MOBILE PHASE: 37:53 methanol-phosphate buffer (pH 3.3), containing - 67 mg/L sodium dodecyl sulfate. FLOW RATE:

0.8 mL/min

GUARD CELL:

1000 mV

DETECTOR:

Dual electrode coulometric electrochemical monitored at 600 mV.

COLUMN:

Highly endcapped C1 8 -RP column (Waters NovaPak), 300-mm x 4.6-mm, heated to 30 o C with 0.2 :m inline filter and guard column of same sorbent.

CALIBRATION:

Analyte in mobile phase.

QUALITY CONTROL:

Analyte in urine at 0, 4, 20, 100 ng/mL.

RANGE:

1.4 to 1200 ng/mL

ESTIMATED LOD: Aniline 1.4 ng/mL @-Toluidine 0.6 ng/mL PRECISION ( þ r ):

Aniline Acetanilide @-Toluidine n-Acetyltoluidine

0.17 [4] 0.16 @ 18 ng/mL 0.20 0.17 @ 16 ng/mL; 0.10 @ 200 ng/mL

APPLICABILITY: This method, monitors the parent compounds and their acetyl metabolites to remove the ambiguity from the aminophenol’s origin. INTERFERENCES: No interferences were observed for aniline or @-toluidine OTHER METHODS: El Bayoumy developed a biological monitoring method for aniline and @-toluidine in 1986 [3], in which each liter of sample spiked with internal standard was lyophilized, reconstituted, concentrated, liquid/liquid extracted 3 times, evaporated to dryness, reflux hydrolyzed for 2.5 hrs, liquid/liquid again extracted 3 times, evaporated to dryness, reacted with pentafluoropropionic acid, before being analyzed by GC-ECD.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition