TR IPHEN YL TIN CH LOR IDE: ME TH OD 5527, Issue 1, dated 1 5 Ma rch 2003 - Page 4 of 5
REFERENCES: [1] [2] [3]
Hopkins BM [2002] Backup data report for Triphenyl Tin Chloride, August 15, 2002, (unpublished report). NIOSH/DART. NIO SH [1994]. NIO SH Ma nua l of Analytical Metho ds, 4 th ed., Method 5504, DHHS(NIOSH) Publication 94-113 (August 1994) Dauchy X, Cottier R, Batel A, Jeannot R, Borsier M, Astruc A, Astruc M [1993]. Mobile phase composition based on speciation of butyltin compounds by high-performance liquid chromatography with inductively coupled plasma m ass spectrometry detection. J Chromatogr Sci 31: 416-421.
METHOD WRITTEN BY: Barbara M. Hopkins, Ph.D. NIOSH/DART
APP EN DIX : Ope ration of ICP -HPL C Instrum ent: ICP conditions refer specifically to the Spectroflame EOP. 1. Install torch and s pray cham ber for an alysis of orga nic com pou nds into ICP instrum ent. 2. Co nne ct inlet tub ing for organic ana lysis to sp ray cham ber a nd d irect IC P waste into a suitable was te container. 3. Once argon is flowing through instrument adjust gas pressures so that nebulizer pressure is 2.2 bar and auxiliary gas flow rate is 23 SKT. 4. Set valve for switching between pumping aqueous solutions and organic solvents to position for aqueous. Allow water to pump through system while following typical procedures for lighting the torch. Light torch and allow system to warm up for 30 minutes. 5. Start mobile phase pumping through HPLC instrument at a flow rate of 1 ml/min. Check for correct flow rate. 6. After warm-up period, profile the optics on the ICP using an aqueous solution that is 10 ppm Cd +2, 10 ppm Li +1, and 50 ppm Zn +2. 7. Following successful profiling, open the valve on the oxygen tank and then change certain settings on the ICP under INSTR UMEN T PARAM ETERS (a subset of OPERAT IONS) so that the following are applied: GENERATOR PARAMETERS Plasm a Powe r (W ) Pum p Step Coolant Step Auxiliary Step Nebulizer Step Heating SPECIAL VALVE Flush Step
1500 2 5 1 1 0
2
8. Change the position of the valve for switch ing betwe en pum ping aqueous solutions and organic solvents to the position for organic and connect the tubing from the ICP to the end of the HPLC column. Check the valve on the inside of the ICP side panel for leaks. 9. Allow mobile phase to run through ICP for about 10 min before injecting. 10. Plug in sample loop position controller being sure that it is in Position A. 11. In order to obtain a transient scan, select SCAN MANAGER, SCAN, TRANSIENT SCAN on ICP computer. Type in the name of the sample, the measure time (100), the interval time (600), and the num ber of points (999). Select the Sn line (189.9 nm ). 12. Inject a sample of methanol (about 70 :L) into the 50 :L sample loop. Simultaneously push the button on the sam ple injector and the STA RT button on the com puter. 13. After the sample loop controller has moved from Position B back to Position A, remove the syringe. 14. Upon com pletion of the scan, save the scan on a floppy disc. 15. Inject standards and unknowns in triplicate following procedures 11-14.
NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
