TR IPHEN YL TIN CH LOR IDE: ME TH OD 5527, Issue 1, dated 1 5 Ma rch 2003 - Page 2 of 5 REAGENTS:
EQUIPMENT:
1. Tropolone (2-Hydroxy-2,4,6cycloheptatrienone) min. 99% pure. 2. Glacial Ac etic Acid, T race M etal G rade .* 3. Me than ol, HP LC Grade .* 4. Triphenyl tin chloride*, 95% pure. 5. Deionized, distilled water. 6. Mobile Phase: 0.020%(w/v)tropolone, 22%(v/v) water, 6.0% (v/v) acetic acid, 72% (v/v) m etha nol [3]. 7. De sorbing solution: 0.020% (w/v)tropo lone, 22%(v/v) w ate r, 78% (v/v) m eth anol. 8. Triphenyl tin chloride standard solution, 200 µg/m L (as tin) with m etha nol as solve nt. 9. Ca libration c urve solutions: P ipet approp riate am ounts of triphenyl tin chloride standard solution into 1 0-m L volum etric flas ks to prepare solutions that are 1, 5, 15, 25, 35, and 45 µg/mL (as tin). Add desorbing solution to the m ark . 10. Argon. 11. Ox ygen.
1. Sam pler: po lyvinyl chloride filter with su ppo rt pad s (3-µm , 5-µm obtainable from SKC, Inc ., Eighty Four, PA 15330 , Cat. No. 225-8-01-1) in cassette filter holder. 2. Personal sa m pling pum p, 1 to 4 L/m in, with flexible connecting tubing. 3. High performance liquid chromatograph (HPLC) with reverse phase column (Kingsorb 5 C 18, 250 x 4.60-mm , 5-micron, or equivalent), guard column (Alltima 10 mm X 4.60-m m C 18, 5-m icron) an d 50-µL sam ple loop injector. 4. Ind uctively coupled arg on plasm a-ato m ic emission spectrometer equipped for analysis of organic com pounds (See AP PEN DIX). 5. Regulators for argon and for oxygen. 6. Bea kers : Griffin, 50-m L. ** 7. Volum etric flasks : 10-, 100- a nd 10 00-m L.** 8. Syringe, 100-µL. 9. Ultrasonic bath. 10. Pipets, various sizes for standard preparation. 11. Polystyrene (8-m L) round bottom tubes with caps. 12. Pla stic film . 13. Forceps.
- See SPECIAL PRECAUTIONS
- Clean all glasswa re with conc. nitric acid
and rinse thorough ly with distilled water.
SPECIAL PRECAUTIONS: Triphenyl tin chloride is highly toxic and readily absorbed through skin. Avoid bre ath ing dust a nd wear gloves when workin g with it and its solution s. C oncentrate d acetic acid is corrive, and a skin and eye irritant. Methanol is flamm able and toxic.
SAMPLING: 1. Calibrate each personal sampling pump with a representative sampler in line. 2. Sam ple at a n ac curately kn own flow ra te betwee n 1 and 4 L/m in for a total sam ple size of 10 0 to 1000 L.
SAMPLE PREPARATION: 3. Open the cassette filter holders and, with tweezers, transfer the samples and blanks to clean beakers. 4. Ad d 5 m L of de sorbing solution. C over with plastic film . 5. Agitate be akers in an u ltrasonic ba th for 5 m in. 6. Transfer the solutions to polystyrene tubes. Cap.
CALIBRATION AND QUALITY CONTRO L: 7. Calibrate with six working standards in the range of 5 to 225 µg as tin per sample. a. Pipet kno wn a m oun ts of triphen yl tin chloride stoc k solution into 10-m L volum etric flas ks . Dilute NIOSH Manual of Analytical Methods (NMAM), Fourth Edition
