Page:NIOSH Manual of Analytical Methods - 5504.pdf/5

 Organotin Compounds (as Sn): Method 5504, Issue 2 dated 15 August 1994 - Page 5 of 6 REFERENCES: [1] Gutknecht, W.F., P.M. Grohse, C.A. Homzak, C. Tronzo, M.H. Ranade, and A. Damle. Development of a Method for the Sampling and Analysis of Organotin Compounds, NIOSH Contract 210-80-0066, Research Triangle Institute, Research Triangle Park, NC 27709, available through NTIS, Springfield, VA 22161, as PB83-180737 (May, 1982). [2] Criteria for a Recommended Standard...Occupational Exposure to Organotin Compounds, U.S. Department of Health, Education, and Welfare, Publ. (NIOSH) 77-157 (1976).

METHOD WRITTEN (REVISED) BY: Eugene R. Kennedy, Ph.D., NIOSH/DPSE

APPENDIX: PREPARATION OF Zr-COATED GRAPHITE FURNACE TUBE AND PLATFORM 1. Zirconium coating: soak pyrolytic graphite tubes and platforms overnight in 4.5% (w/v) zirconium acetate oxide solution; then dry in a muffle furnace for 2 h at 200 EC. 2. Pyrolytic zirconium-coated graphite furnace tubes are acceptable for measurements of all organotin compounds. However, a pyrolytic zirconium-coated graphite platform (e.g., L'vov platform) is recommended for better precision at low levels and improved atomization response for volatile species such as TeBT. Platforms may be purchased commercially or prepared from pyrolytic graphite tubes, as shown in Fig. 2. Special care must be exercised during placement of the platform in the tube (Fig. 3) and in optical alignment.

Table 1. Formulae and Physical Properties [3]. Compound/ RTECS

Formula

M.W.

% Sn

Synonym

C28H56O4S2Sn

639.57

18.6

BulIOMA; CAS #25168-24-5

Tetrabutyltin WH8605000

C16H36Sn

347.16

34.2

Stannane, tetrabutyl-; TEBT; CAS #1461-25-2

Tributyltin chloride WH6820000

C12H27ClSn

325.49

36.5

Stannane, chlorotributyl-; TBTC; CAS #1461-22-9

Tricyclohexyltin hydroxide WH8750000

C18H34OSn

385.16

30.8

Stannane, tricyclohexylhydroxy-; TCHH; Pilctran; Dowco213; CAS #13121-70-5

Dibutyltin bis(isooctyl mercaptoacetate) WH6719000

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