Page:NIOSH Manual of Analytical Methods - 5504.pdf/1

 ORGANOTIN COMPOUNDS (as Sn) Table 1

MW: Table 1 CAS: Table 1 RTECS: Table 1

METHOD: 5504, Issue 2

OSHA : NIOSH: ACGIH:

5504

EVALUATION: FULL

0.1 mg/m3 0.1 mg/m3 (skin) 0.1 mg/m3

Issue 1: 15 August 1987 Issue 2: 15 August 1994

PROPERTIES: Table 1

SYNONYMS: Table 1 SAMPLING

MEASUREMENT

SAMPLER:

FILTER + SORBENT (glass fiber + XAD-2, 80 mg/40 mg)

TECHNIQUE:

HPLC/ATOMIC ABSORPTION, GRAPHITE FURNACE

FLOW RATE:

1 to 1.5 L/min

ANALYTE:

tin

VOL-MIN: -MAX: 500 L

50 L

DESORPTION:

10 mL 0.1% acetic acid/CH3CN; ultrasonic, 30 min

SHIPMENT:

ship assembled sampler in dry ice

SEPARATION:

HPLC (cation exchange)

SAMPLE STABILITY:

stable 7 days @ 0 EC [1]

GRAPHITE FURNACE:

FIELD BLANKS:

2 to 10 field blanks per set

MEDIA BLANKS:

12 per sample set ACCURACY

RANGE STUDIED:

0.07 to 0.2 mg/m3 [1] (300-L samples)

BIAS:

see EVALUATION OF METHOD

dry 30 sec @ 80 EC; atomize 5 sec @ 2750 EC (gas interrupt mode)

INJECTION VOLUME:

20 µL

WAVELENGTH:

286.3 nm, with background correction

CALIBRATION:

standard solutions of organotin compounds in acetic acid/CH3CN

RANGE:

5 to 50 µg Sn per sample

ESTIMATED LOD: 1 µg Sn per sample [1] PRECISION (þ r):

0.07 to 0.08 [1]

OVERALL PRECISION ( rT): 0.07 to 0.10 [1] ACCURACY:

see EVALUATION OF METHOD

APPLICABILITY: The working range is 0.015 to 1 mg/m3 (as Sn) for a 300-L air sample. The method was validated using TeBT, TBTC, TCHH, and BuIOMA as surrogates for the most important classes of organotin compounds [1]. If speciation of organotin compounds is not required and if inorganic tin compounds are absent, the HPLC separation may be deleted. Use special care to avoid losses of TeBT and other volatile tetra-substituted organotin compounds INTERFERENCES: Organotin compounds not separated chromatographically will mutually interfere. Other compounds with similar retention times will not interfere unless they contain tin.

OTHER METHODS: This replaces the colorimetric criteria document method [2].

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition, 8/15/94