A gas chromatographic method was developed for the quantitative determination of a- and b-thiodan and thiodan sulphate on tobacco and in smoke condensate in concentrations as Iow as 0.01 parts per million. A survey was made of the thiodan and thiodan sulphate content of leaf tobacco and cigarettes. Thiodan and thiodan sulphate residues in leaf tobacco were found to amount to between 0.02 and 0.3 ppm and to between less than 0.02 and 0.05 ppm respectively. Cigarettes manufactured from Virginia tobacco were found to contain between 0.1 and 0.2 ppm of thiodan and less than 0.05 ppm of thiodan sulphate. The transfer rate of thiodan and thiodan sulphate from cigarette tobacco into the mainstream smoke ranged from 14.5 % to 16.3 %
Even to-day the theory of sorption phenomena does not provide for an exact analytical solution to the problem of the different types of binding existing between the liquid and gaseous phases and the material to be studied. Under these circumstances, the empirical relations between the equilibrium moisture content and the relative air humidity is of increasing significance. The validity of the mathematic principles of the Theory BET and of the Equation of Henderson is examined by comparison with experimental results obtained for tobacco. The limits set to determination reveal themselves even in the sphere of adsorption, if the calculation of the Theory BET is made on the basis of five molecular layers. Finally, the sorption theory which has recently been established by Kollmann and which is based on statistical investigations is presented. The author intends to apply Kollmann's theory to tobacco and will report the results at a later date
Maltol (2-hydroxy-3-methyl-4-pyrone) as a new tobacco smoke constituent was identified by thin layer chromatography and UV-spectrometry. After conversion into the methylether, by reaction with diazomethane, maltoI was identified by gas chromatography and mass spectrometry. The amount of maltol in the smoke of a cigarette, made from tobacco without any additives, was 5 to 10 µg/cigarette. As far as we know, the occurrence of γ-pyrone derivatives in tobacco smoke has not been reported until now. It might be possible that the newly found γ-pyrone derivative is only the first representative of a new class of chemical smoke constituents
A specific, sensitive method for the determination of formaldehyde in cigarette smoke is described employing the spectrophotometric detection of the product formed by reaction of formaldehyde with p-rosaniline and sulphur dioxide. The procedure is applicable to the analysis of smoke from cigarettes manufactured from flue-cured, Burley and fermented tobaccos. Smoking parameters and the use of Cambridge filters have been found to affect delivery markedly. The effect of several commercial filters on formaldehyde delivery has been examined.
A qualitative and quantitative procedure has been developed for the determination of humectants in manufactured tobacco by gas-chromatographic method with a flame ionization detector. It consists of extraction with methanol, concentration of the extract and treatment with Tri-Sil reagents. The operating gas-chromatographic conditions are set forth. Samples of tobacco containing glycerine, propylene glycol, diethylene glycol, triethylene glycol, 1-3 butylene glycol and sorbitol have been analysed with recoveries, for the first five ones, in the range of 95-104 %. In order to verify that each chromatographic peak corresponded to the relative glycol, with no interference by other silylated compounds, the mass spectra were obtained through the combination of gas-chromatography with mass spectrometry. The results achieved confirm, as far as tobacco is concerned, that the procedure is accurate and precise. The same method for the determination of humectants was extended to cigarette smoke. Even though this involves morecomplicated problems, as compared to tobacco, because of the presence of silylated compounds, it was found that, for certain glycols, the gas-chromatography of the trimethyl derivatives can be also used as a method of analysis. The mass spectra of some polyhydric alcohols are shown
By the use of gaschromatographic and mass spectrometric methods gas phase condensate from cigarette smoke, isolated on a preparative scale, has been compared with the native gas phase from the smoke of the same cigarettes and investigated for qualitative composition. With regard to composition, there is a satisfactory conformity between both mixtures of substances. It has been possible to identify or to characterize more than 60 constituents
An automatic dropping-applicator for fresh cigarette smoke condensate is described. The new applicator makes it possible to apply separately a solvent and the smoke condensate produced by a capillary press. 15 animals can be treated simultaneously
A gas chromatographic method was developed for the quantitative determination of a- and b-thiodan and thiodan sulphate on tobacco and in smoke condensate in concentrations as Iow as 0.01 parts per million. A survey was made of the thiodan and thiodan sulphate content of leaf tobacco and cigarettes. Thiodan and thiodan sulphate residues in leaf tobacco were found to amount to between 0.02 and 0.3 ppm and to between less than 0.02 and 0.05 ppm respectively. Cigarettes manufactured from Virginia tobacco were found to contain between 0.1 and 0.2 ppm of thiodan and less than 0.05 ppm of thiodan sulphate. The transfer rate of thiodan and thiodan sulphate from cigarette tobacco into the mainstream smoke ranged from 14.5 % to 16.3 %
Even to-day the theory of sorption phenomena does not provide for an exact analytical solution to the problem of the different types of binding existing between the liquid and gaseous phases and the material to be studied. Under these circumstances, the empirical relations between the equilibrium moisture content and the relative air humidity is of increasing significance. The validity of the mathematic principles of the Theory BET and of the Equation of Henderson is examined by comparison with experimental results obtained for tobacco. The limits set to determination reveal themselves even in the sphere of adsorption, if the calculation of the Theory BET is made on the basis of five molecular layers. Finally, the sorption theory which has recently been established by Kollmann and which is based on statistical investigations is presented. The author intends to apply Kollmann's theory to tobacco and will report the results at a later date
Maltol (2-hydroxy-3-methyl-4-pyrone) as a new tobacco smoke constituent was identified by thin layer chromatography and UV-spectrometry. After conversion into the methylether, by reaction with diazomethane, maltoI was identified by gas chromatography and mass spectrometry. The amount of maltol in the smoke of a cigarette, made from tobacco without any additives, was 5 to 10 µg/cigarette. As far as we know, the occurrence of γ-pyrone derivatives in tobacco smoke has not been reported until now. It might be possible that the newly found γ-pyrone derivative is only the first representative of a new class of chemical smoke constituents
A specific, sensitive method for the determination of formaldehyde in cigarette smoke is described employing the spectrophotometric detection of the product formed by reaction of formaldehyde with p-rosaniline and sulphur dioxide. The procedure is applicable to the analysis of smoke from cigarettes manufactured from flue-cured, Burley and fermented tobaccos. Smoking parameters and the use of Cambridge filters have been found to affect delivery markedly. The effect of several commercial filters on formaldehyde delivery has been examined.
A qualitative and quantitative procedure has been developed for the determination of humectants in manufactured tobacco by gas-chromatographic method with a flame ionization detector. It consists of extraction with methanol, concentration of the extract and treatment with Tri-Sil reagents. The operating gas-chromatographic conditions are set forth. Samples of tobacco containing glycerine, propylene glycol, diethylene glycol, triethylene glycol, 1-3 butylene glycol and sorbitol have been analysed with recoveries, for the first five ones, in the range of 95-104 %. In order to verify that each chromatographic peak corresponded to the relative glycol, with no interference by other silylated compounds, the mass spectra were obtained through the combination of gas-chromatography with mass spectrometry. The results achieved confirm, as far as tobacco is concerned, that the procedure is accurate and precise. The same method for the determination of humectants was extended to cigarette smoke. Even though this involves morecomplicated problems, as compared to tobacco, because of the presence of silylated compounds, it was found that, for certain glycols, the gas-chromatography of the trimethyl derivatives can be also used as a method of analysis. The mass spectra of some polyhydric alcohols are shown
By the use of gaschromatographic and mass spectrometric methods gas phase condensate from cigarette smoke, isolated on a preparative scale, has been compared with the native gas phase from the smoke of the same cigarettes and investigated for qualitative composition. With regard to composition, there is a satisfactory conformity between both mixtures of substances. It has been possible to identify or to characterize more than 60 constituents
An automatic dropping-applicator for fresh cigarette smoke condensate is described. The new applicator makes it possible to apply separately a solvent and the smoke condensate produced by a capillary press. 15 animals can be treated simultaneously