gHK DETERMINATION OP COUMARIN 301 TOBACCO AND ...

More documents

Recommendations

Info

APPENDIX I THE MEASUREMENT OF <strong>COUMARIN</strong> iff APPARATUS PARK DRIVE CIGARETTE SMOKE Gas chromatograph : Pye 104 vith FIB detectors. Columns ; Two |" 1 9' stainless steel columns packed vith 10% Carbovax 20M-TPA on Chromosorb WAW-DMCS, 60-100 mesh. Top drive macerator and flask. Baohner funnel (9cm diameter). Buchner flask (300ml) Cambridge filter pads (9cm diameter) Graduated cylinders (1 x 23ml, 2 x 50ml,, 1 x 100ml) Conical flask (11) vith stopper. Beakers (1 x 50ml, 2 x 50ml) Glass funnelB (1 large, 1 small). Separatory funnel (500ml) vith stopper. Round bottomed flask (1 x 1l). Rotary evaporator. Chromatography columns (Two, height 30cm, diameter 1cm). Pear shaped flasks (3 x 50ml) Volumetric flasks, REAGENTS Lead acetate (E & V GPR, 8% solution). Celite Analytical Filter Aid' (BDH, supplied by Hyde and Entvhistle), Dichloromethane (H & W GPR)..; Petroleum Spirit 40-60° (May & Baker). Diethyl Ether (H & W GPR) Solvent mixture A (20% ether/80% petroleum spirit) Solvent mixture B (10% ether/90% petroleum spirit) Sodium bicarbonate (H & V Analar, 4% solution). Magnesium sulphate, anhydrous (H & W) Silicic acid (for resolution of basic or neutral mixtures, Sigma Chemical Co.) http://legacy.library.ucsf.edu/tid/iyl97h00/pdf
Coumarin standard solutions in dichloromethane (0.0015%i 0,0025%, 0,0050%, 0,0075%.) GC CONDITIONS Nitrogen flow : ^Omls/min. Column.temperature : 220 isothermal Attenuation : 50 x 1 Chart speed : 2,5 min,/cm, 9 PROCEDURE 1. Calibration of standard solutions 2ul of each of the standard solutions are injected into the gas ohromatograph. Attenuation is 50 x 1, A graph of peak height vs ug/ul of coumarin is plotted. This calibration graph is used to obtain the approximate concentration of coumarin in the sample. It is recommended that the calibration graphB are checked each day and that the standard solutions are kept in a refrigerator and renewed weekly* 2. Treatment of Sample '. (a) The Cambridge filter containing the smoke from 25 cigarettes is placed in a macerator flask, Celite (5g)» lead acetate (20ml, Q% solution) and hot water (200ml, approx. 50 C) are added and the mixture is macerated for 3 minutes. The macerator is then turned off and the residue is washed off the lid and Bides of the flask into the body of the solution with distilled water (approx, 10ml) Maceration is continued for a further 2 minutes. .The macerator is then switched off and the residue adhering to the lid and sides of the flask is washed into the solution with more distilled water (approx, 10ml), http://legacy.library.ucsf.edu/tid/iyl97h00/pdf (b) The mixture is filtered by suction through a Cambridge filter pad into a Buchner flask. The residue on the filter pad is washed with two 50ml portions of warm water. (o) The aqueous filtrate (plus washings) 1B cooled to room temperature by running cold water over the surface of the Buchner flask. The contents of thG.-JBuchner flask are then transferred to a 50ml separatory funnel |nd washed with four successive portions of solvent mixture A (1 x 150, 2 x 100, 1 x 50ml),, the upper organic layer being retained on each occasion. The organic extractions are combined and washed with sodium bicarbonate (40ml, 4% solution) in the same separatory funnel. The lower bicarbonate layer is drawn off into a 50ml beaker. The upper organic layer is then drawn off into a conical flask (11) containing anhydrous magnesium sulphate (approx, 30-40g). The bicarbonate layer is washed with an additional 40mle of solvent mixture A, The lower aqueous bicarbonate layer is discarded and the organic layer is added to the contents of the conical flask. The flask is stoppered and the solution is left to dry for a minimum of 45 minutes.
Page 1 and 2: COUMARIK IN TOBACCO gHK DETERMINATI
Page 3 and 4: IABLE II COTJMARIN IEVEL IN PARK DR
Page 5 and 6: TIT;...,'"("" ". ; *."•" jt 6± 1
Page 7: 7* SWMAKY o In view of the low coum
Page 11 and 12: 3* CALCULATION OF RESULT AMOUNT OP
Page 13: 1 http://legacy.library.ucsf.edu/ti

gHK DETERMINATION OP COUMARIN 301 TOBACCO AND ...

Create successful ePaper yourself

Delete template?

Save as template?