Development Of A Method For The Sampling And Analysis Of Organotin Compounds.
Gutknecht-WF; Grohse-PM; Homzak-CA; Tronzo-C; Ranade-MB; Damle-A
NIOSH 1982 Apr:137 pages
A technique for sampling and analysis of organotin compounds was developed and tested. Samples were collected on a glass fiber filter/XAD-2 resin system and were then extracted with 0.1 percent by volume acetic-acid in acetonitrile. Separation of organotin species prior to measurement was accomplished using high performance liquid chromatography (HPLC) with a strong cation exchange column. The test compounds were measured using an electrothermal atomization atomic absorption spectrometer connected directly to the HPLC. Atomization was accomplished on a zirconium coated graphite tube furnace. Recovery and collection/recovery tests were performed using tetrabutyltin (1461252) (TBT), tributyltin-chloride (1461229), and tricyclohexyltin-hydroxide (13121705). These compounds were chosen as representative of the classes of organotins most important with regard to health effects or production/use volumes. Recovery tests were performed by spiking glass fiber filters and XAD-2 resin with and then extracting, separating, and measuring the compounds. Aerosols and vapors of the test compounds with the same concentration range were generated using a nebulizer system. The compounds were collected with collection systems composed of glass fiber filters and XAD-2 solvent resin tubes connected in series. Samples were extracted, separated, and measured. All recovery values exceeded 95 percent except for TBT at 0.01mg/m3 which exceeded 90 percent recovery. All collection/recovery values exceeded 90 percent. Overall method precision was 10.8 percent for TBT, 6.0 percent for tributyltin-chloride, and 6.6 percent for tricyclohexyltin-hydroxide in the 0.05 to 0.2mg/m3 concentration range. Filter samples were stable under refrigeration or freezing for up to 7 days after collection. The authors conclude that the method meets NIOSH criteria for collection/recovery efficiencies and precision over the 0.05 to 0.2mg/m3 concentration range for the test compounds.
NIOSH-Contract; Decomposition-products; Organic-compounds; Analytical-chemistry; Chromatographic-analysis; Testing-equipment; Research; Analytical-methods; Contract-210-80-0066;
1461-25-2; 1461-22-9; 13121-70-5;
NTIS Accession No.
Division of Physical Sciences and Engineering, NIOSH, U.S. Department of Health and Human Services, Cincinnati, Ohio, NTIS PB83-180-737