Data publikacji: 13 Jun 2014 Zakres stron: 243 - 250
Abstrakt
Abstract
The gaseous part of cigarette smoke was brought into contact with the surfaces of different materials such as glass, stainless steel, silicone rubber, and condensed gas phase. Subsequent analysis by gaschromatography shows that the gas phase may be even less stable than is generally assumed. Inert as well as reactive components are reduced by a short surface contact, the former up to 50, the latter up to 300 %. Using a specially designed large syringe made of teflon and steel we observed the lowest loss of smoke constituents caused by trapping the gas phase at room temperature.
Data publikacji: 13 Jun 2014 Zakres stron: 251 - 262
Abstrakt
Abstract
The cold pentane traps of the precipitation procedure described in the preceding paper (cotton wool trap, water trap, pentane traps) favour the formation of N-nitroso components and, as a result, the emergence of artefacts. If, however, the smoke sojourns in the aerosol state for a period of 40 seconds (compared to 5 seconds) also that part of condensate of smoke from cigarette tobaccos rich in nitrates and bases which is trapped on cotton wool at normal temperature, contains N-nitroso-dimethylamine and N-nitroso-pyrrolidine in quantities corresponding to 0.004 µg N-NO per cigarette. The formation of N-nitroso components in the smoke of tobaccos of high nitrate and base contents accordingly occurs during a gas phase reaction which is dependent on time.
In conformity with the previously reported findings N-nitrosomethyl-n-butylamine was identified in the condensate gathered in pentane traps. Presumably, it has however to be regarded as an artefact produced by the precipitation system employed. Condensates collected in cold and acetone traps were found to contain more N-nitroso components than condensates precipitated simply by the gas phase reaction of the smoke. The quantity of N-nitroso components contained in condensates gathered in cold traps was found to increase during aging.
Model experiments with pure substances showed that the formation of N-nitroso components in the gas phase requires the presence of a mixture of NO and NO2.
The competitive reaction of dimethylamine and methanol with the gaseous mixture of nitrogen oxides displays the prevailing formation of N-nitroso-dimethylamine. The yield of N-nitroso-dimethylamine in NO-air-mixtures is probably only dependent on the rate of the oxidation NO undergoes to NO2.
Data publikacji: 13 Jun 2014 Zakres stron: 263 - 277
Abstrakt
Abstract
Three methods of quantitative determination of catechol in cigarette smoke condensate are presented. The procedures are based on:
a.Column chromatography of a smoke condensate solution in chloroform over polyamide powder, followed by elution with ethyl acetate and a spectrophotometric measure in methanol solution;
b.Liquid-liquid partitions of the smoke condensate, followed by a spectrophotometric measure based on a bathochromic shift of the absorption spectrum of catechol; and
c.Vapour-phase chromatography of the phenolic smoke components in the form of their methyl ethers. The procedure a. is best suited as a routine method, as it is easy to execute and gives fairly accurate and precise results. The procedures b. and c. both give less reproducible results, and c. shows insufficient analytical yields. Their advantages are the rapid execution of method b. and the high specificity of method c.
Contents between 200 and 500 µg of catechol per cigarette were found in the smoke of cigarettes.
Data publikacji: 13 Jun 2014 Zakres stron: 278 - 284
Abstrakt
Abstract
A gas-chromatographic procedure using the electron-capture detector is presented. By fractionation of cigarette smoke on silica gel, followed by gas-chromatographic analysis of the fractions, fifteen polycyclic aromatic hydrocarbons were identified. Application of this procedure to quantitative analysis was demonstrated in the case of benzo[a]pyrene. An analysis for benzo[a]pyrene in cigarette smoke which utilizes paper-chromatographic separation and fluorescence measurements is also presented. This procedure, which gives good precision with a 20-cigarette sample, represents a great simplification of existing methods.
Data publikacji: 13 Jun 2014 Zakres stron: 285 - 290
Abstrakt
Abstract
The determination of benzo[a]pyrene in cigarette smoke by a method based upon high-temperature gas-liquid chromatography is described. The extension of this method to the examination of other aromatic polycyclic hydrocarbons in smoke is briefly discussed.
Data publikacji: 13 Jun 2014 Zakres stron: 291 - 300
Abstrakt
Abstract
Construction and working principle of an automatic capillary press, a smoking machine for preparing instant smoke condensate of 15 cigarettes per smoking procedure, are presented. The smoking capacity is 500 cigarettes per day. Condensate production by means of total puffs smoking, in echelons as well as by means of individual puffs is possible. The reproducibility of smoke condensate and smoke nicotine yields is 2.5% R.S.D. Compared with electrostatic precipitation the smoke yield is 90%. The yields of condensate, nicotine, phenols, water, acids, and benzopyrene are reported. Changes of the results of total puffs yields and individual puff yields as a function of initial tobacco moisture as well as different precipitation procedures are indicated.
Data publikacji: 13 Jun 2014 Zakres stron: 301 - 305
Abstrakt
Abstract
The semi-automatic assembly presented here (photoelectric cells used to measure the static duration of combustion in cigarettes) resembles in principle the design published by Wiley and Holmes. Essentially it consists of an electrical start-stop device timed by 2 signals activated by the movement of the glowing zone through a thermo-transductor field. It differs from the earlier design in that, instead of a hot bi-metallic thermocoupling, it uses a photo-transistor very selective in IR (maximum response 1.55 mµ, with a 50 % drop for 0.8 and none for 2 mµ). The device also has a mechanical system for holding the cigarette and positioning the phototransistors, and an electrical cigarette lighting system. The apparatus is set up for simultaneous control of 5 cigarettes.
The gaseous part of cigarette smoke was brought into contact with the surfaces of different materials such as glass, stainless steel, silicone rubber, and condensed gas phase. Subsequent analysis by gaschromatography shows that the gas phase may be even less stable than is generally assumed. Inert as well as reactive components are reduced by a short surface contact, the former up to 50, the latter up to 300 %. Using a specially designed large syringe made of teflon and steel we observed the lowest loss of smoke constituents caused by trapping the gas phase at room temperature.
The cold pentane traps of the precipitation procedure described in the preceding paper (cotton wool trap, water trap, pentane traps) favour the formation of N-nitroso components and, as a result, the emergence of artefacts. If, however, the smoke sojourns in the aerosol state for a period of 40 seconds (compared to 5 seconds) also that part of condensate of smoke from cigarette tobaccos rich in nitrates and bases which is trapped on cotton wool at normal temperature, contains N-nitroso-dimethylamine and N-nitroso-pyrrolidine in quantities corresponding to 0.004 µg N-NO per cigarette. The formation of N-nitroso components in the smoke of tobaccos of high nitrate and base contents accordingly occurs during a gas phase reaction which is dependent on time.
In conformity with the previously reported findings N-nitrosomethyl-n-butylamine was identified in the condensate gathered in pentane traps. Presumably, it has however to be regarded as an artefact produced by the precipitation system employed. Condensates collected in cold and acetone traps were found to contain more N-nitroso components than condensates precipitated simply by the gas phase reaction of the smoke. The quantity of N-nitroso components contained in condensates gathered in cold traps was found to increase during aging.
Model experiments with pure substances showed that the formation of N-nitroso components in the gas phase requires the presence of a mixture of NO and NO2.
The competitive reaction of dimethylamine and methanol with the gaseous mixture of nitrogen oxides displays the prevailing formation of N-nitroso-dimethylamine. The yield of N-nitroso-dimethylamine in NO-air-mixtures is probably only dependent on the rate of the oxidation NO undergoes to NO2.
Three methods of quantitative determination of catechol in cigarette smoke condensate are presented. The procedures are based on:
a.Column chromatography of a smoke condensate solution in chloroform over polyamide powder, followed by elution with ethyl acetate and a spectrophotometric measure in methanol solution;
b.Liquid-liquid partitions of the smoke condensate, followed by a spectrophotometric measure based on a bathochromic shift of the absorption spectrum of catechol; and
c.Vapour-phase chromatography of the phenolic smoke components in the form of their methyl ethers. The procedure a. is best suited as a routine method, as it is easy to execute and gives fairly accurate and precise results. The procedures b. and c. both give less reproducible results, and c. shows insufficient analytical yields. Their advantages are the rapid execution of method b. and the high specificity of method c.
Contents between 200 and 500 µg of catechol per cigarette were found in the smoke of cigarettes.
A gas-chromatographic procedure using the electron-capture detector is presented. By fractionation of cigarette smoke on silica gel, followed by gas-chromatographic analysis of the fractions, fifteen polycyclic aromatic hydrocarbons were identified. Application of this procedure to quantitative analysis was demonstrated in the case of benzo[a]pyrene. An analysis for benzo[a]pyrene in cigarette smoke which utilizes paper-chromatographic separation and fluorescence measurements is also presented. This procedure, which gives good precision with a 20-cigarette sample, represents a great simplification of existing methods.
The determination of benzo[a]pyrene in cigarette smoke by a method based upon high-temperature gas-liquid chromatography is described. The extension of this method to the examination of other aromatic polycyclic hydrocarbons in smoke is briefly discussed.
Construction and working principle of an automatic capillary press, a smoking machine for preparing instant smoke condensate of 15 cigarettes per smoking procedure, are presented. The smoking capacity is 500 cigarettes per day. Condensate production by means of total puffs smoking, in echelons as well as by means of individual puffs is possible. The reproducibility of smoke condensate and smoke nicotine yields is 2.5% R.S.D. Compared with electrostatic precipitation the smoke yield is 90%. The yields of condensate, nicotine, phenols, water, acids, and benzopyrene are reported. Changes of the results of total puffs yields and individual puff yields as a function of initial tobacco moisture as well as different precipitation procedures are indicated.
The semi-automatic assembly presented here (photoelectric cells used to measure the static duration of combustion in cigarettes) resembles in principle the design published by Wiley and Holmes. Essentially it consists of an electrical start-stop device timed by 2 signals activated by the movement of the glowing zone through a thermo-transductor field. It differs from the earlier design in that, instead of a hot bi-metallic thermocoupling, it uses a photo-transistor very selective in IR (maximum response 1.55 mµ, with a 50 % drop for 0.8 and none for 2 mµ). The device also has a mechanical system for holding the cigarette and positioning the phototransistors, and an electrical cigarette lighting system. The apparatus is set up for simultaneous control of 5 cigarettes.