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THIOPHANATE-METHYL in air
5606
C12H14N4O4S2 MW: 342.40 CAS: 23564-05-8 RTECS: BA3675000

METHOD: 5606, Issue 1
EVALUATION: PARTIAL
Issue 1: 15 March 2003


OSHA: N/A

NIOSH: N/A

ACGIH: N/A

PROPERTIES: colorless prisms; MP 181.5–182.5 °C; soluble in acetone, methanol, chloroform, acetonitrile, slightly soluble in other organics, insoluble in water



SYNONYMS: Topsin-M; [1,2-phenylenebis(iminocarbonothioyl)]bisdimethyl ester carbamic acid



SAMPLING


SAMPLER: FILTER/SOLID SORBENT TUBE (OVS-2 tube: 11 mm quartz fiber filter; XAD-2, 270 ing/140 ing)
FLOW RATE: 0.1 L/min to 1 L/min
VOL-MIN: 20 L @ 0.1 L/min [see Evaluation of Method, Note 1.]
-MAX: 480 L
SHIPMENT: 4 °C
SAMPLE STABILITY: at least 28 days at 4 °C
BLANKS: 2 to 10 field blanks per set

ACCURACY


RANGE STUDIED: not determined
BIAS: not determined
OVERALL PRECISION (Ŝ): not determined
ACCURACY: not determined

MEASUREMENT


TECHNIQUE: HPLC, UV detector
ANALYTE: thiophanate-methyl
EXTRACTION: 2 mL 40% isopropanol: 60% acetonitrile
INJECTION VOLUME: 5 µL
MOBILE PHASE: A = 2% n-propanol in water, 0.02 M TEA-PO4, pH adjusted to 7.0 ± 0.1 using phosphoric acid; B = 2% n-propanol in acetonitrile; gradient from 20% B to 70% B (20 min), decreasing to 20% B (2 min), hold at 20% B (5 min)
COLUMN: reversed phase C-18, 4 µm, 250 × 2.00 mm (or equivalent)
DETECTOR: UV @ 200 nm [see Evaluation of Method, Note 2.]
CALIBRATION: solutions prepared in extraction solvent
RANGE: 5 to 650 µg/sample
ESTIMATED LOD: 0.76 µg/sample
PRECISION (Sr): 0.0318



APPLICABILITY: This method was developed for the determination of thiophanate-methyl in air samples for a fungicide field study of orchard workers, and was meant to be used in conjunction with NMAM 5601 for the determination of carbendazim and captan as well. Recoveries of thiophanate-methyl may be lower when carbendazim, thiophanate-methyl, and captan are present in the same sample due to chemical interactions. The working range for this method is 0.025–5.67 ing/m³ based on a 100-L sample.


INTERFERENCES: Potential interferences to the analysis of thiophanate-methyl include other organic compounds, in particular other pesticides or fungicides that have the same retention time on a C-18 column. Positive identification may be confirmed by dual column chromatography using an appropriate alternative LC column. NOTE: It is possible to see a peak at the retention time for carbendazim, 9.8 minutes, since carbendazim is a decomposition product of thiophanate-methyl.


OTHER METHODS: This method is based in part on NMAM 5601 [1] for the development work. As such, several of the compounds listed in NMAM 5601can also be analyzed in conjunction with thiophanate-methyl using this method.


NIOSH Manual of Analytical Methods (NMAM), Fourth Edition