Page:NIOSH Manual of Analytical Methods - 5526.pdf/1

 METHYLTIN CHLORIDES Formula: Table 1

MW: Table 1

METHOD: 5526, Issue 1

CAS: Table 1

RTECS: Table 1

EVALUATION: FULL

Issue 1: 15 March 2003

PROPERTIES: See Table 1

OSHA : See Table 1 NIOSH: See Table 1 ACGIH: See Table 1 SYNONYMS:

5526

Methyltin Trichloride: Trichloromethylstannane, Monomethyltin trichloride Dimethyltin Dichloride: Dichlorodimethylstannane, Dichlorodimethyltin Trimethyltin Chloride: Chlorotrimethylstannane, Chlorotrimethyltin, Trimethylstannyl chloride SAMPLING

SAMPLER:

FILTER + SORBENT TUBE (OVS Tube: 13-mm glass fiber filter; XAD-2, 270/140 mg)

FLOW RATE:

0.25 to 1 L/min

VOL -MIN: -MAX:

15L 75L

SHIPMENT:

Ship assembled sampler cold

SAMPLE STABILITY:

14 days @ 4 °C

FIELD BLANKS:

2 to 10 field blanks per set

ACCURACY

MEASUREMENT TECHNIQUE:

GAS CHROMATOGRAPHY, FPD (tinspecific filter)

ANALYTE:

Sodium tetraethylborate derivatives of the analytes

DESORPTION:

2 mL 1% acetic acid in acetonitrile

INJECTION VOLUME:

1 :L

TEMPERATURE -INJECTION: -DETECTOR: -COLUMN:

Cool-on-column 250 °C 50 °C (3min), 12°C/min to 200°C (1min)

CARRIER GAS:

He, 6 mL/min

COLUMN:

Capillary, fused silica, 30m x 0.53mm ID, 1.5-:m film, 5% phenyl, 95% methyl silicone, DB-5 or equivalent.

RANGE STUDIED:

Table 2

BIAS:

Table 2

CALIBRATION:

Analytes in hexane

OVERALL PRECISION (Ö r T ):

Table 2

RANGE:

0.01 to 15 :g/sample (as tin) [1]

ACCURACY:

Table 2

ESTIMATED LOD: 0.01 :g [1] PRECISION ( þ r ):

0.065 [1]

APPLICABILITY: This method was developed for air monitoring of methyltin chlorides.[1]

INTERFERENCES: None were identified.

OTHER METHODS: NMAM 5504 is another method for the measurement of organotin compounds using a filter with a sorbent tube for collection and HPLC/AA for analysis [3].

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition