Application of dosimetry tools for the assessment of e-cigarette aerosol and cigarette smoke generated on two different in vitro exposure systems

The diluted aerosols from a cigarette (3R4F) and an e-cigarette (Vype ePen) were compared in two commercially available in vitro exposure systems: the Borgwaldt RM20S and Vitrocell VC10. Dosimetry was assessed by measuring deposited aerosol mass in the exposure chambers via quartz crystal microbalances, followed by quantification of deposited nicotine on their surface. The two exposure systems were shown to generate the same aerosols (pre-dilution) within analytically quantified nicotine concentration levels (p = 0.105). The dosimetry methods employed enabled assessment of the diluted aerosol at the exposure interface. At a common dilution, the per puff e-cigarette aerosol deposited mass was greater than cigarette smoke. At four dilutions, the RM20S produced deposited mass ranging 0.1–0.5 µg/cm²/puff for cigarette and 0.1–0.9 µg/cm²/puff for e-cigarette; the VC10 ranged 0.4–2.1 µg/cm²/puff for cigarette and 0.3–3.3 µg/cm²/puff for e-cigarette. In contrast nicotine delivery was much greater from the cigarette than from the e-cigarette at a common dilution, but consistent with the differing nicotine percentages in the respective aerosols. On the RM20S, nicotine ranged 2.5–16.8 ng/cm²/puff for the cigarette and 1.2–5.6 ng/cm²/puff for the e-cigarette. On the VC10, nicotine concentration ranged 10.0–93.9 ng/cm²/puff for the cigarette and 4.0–12.3 ng/cm²/puff for the e-cigarette. The deposited aerosol from a conventional cigarette and an e-cigarette in vitro are compositionally different; this emphasises the importance of understanding and characterising different product aerosols using dosimetry tools. This will enable easier extrapolation and comparison of pre-clinical data and consumer use studies, to help further explore the reduced risk potential of next generation nicotine products.

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Graphical abstract A cigarette and an e-cigarette (top left) were assessed on two different in vitro exposure systems, the Borgwaldt RM20S (top right) and the VC 10 (bottom right). Compositionally the product aerosols were different, but there was no difference between the same product on different machines (bottom left).

     

Organosilica materials with 1,5-bis-(2’-ethyl)-2,4-dimethyl benzene bridging groups

Using 1,5-bis-(2-trichlorosilylethyl)-2,4-dimethyl benzene, we have obtained porous organosilica materials containing 1.5 to 100 mole % 1,5-bis-(2-ethyl)-2,4-dimethyl benzene bridging groups. We have used X-ray phase analysis, adsorption, Fourier transform IR (FTIR) spectroscopy, thermogravimetry, and temperature-programmed desorption mass spectrometry methods to study their structure and composition. We have shown that the materials obtained generally are characterized by a biporous structure and aerosol properties: large pore volume (up to 4 cm³/g) and low density (~70 mg/cm³).Translated from Teoreticheskaya i Éksperimentalnaya Khimiya, Vol. 40, No. 6, pp. 373–379, November–December, 2004.     

Sample preparation of archaeological materials for PIXE analysis

A method to prepare thin samples of archeological materials such as potteries and bones for PIXE analysis is presented. In this method fine powder of the matter under analysis is suspended and deposited on polycarbonate filters. The process takes place in a chamber where clean air and the powder are mixed and forced to pass through the filter. Thin samples with typical mass density of about 50 g cm^–2 are obtained. The uniformity of the mass deposit has been optically tested with a He–Ne laser showing fluctuations of the order of one percent. Samples of clay standards from NIST were prepared with this method and analyzed by PIXE. The agreement between our results and NIST values is very good, with linear correlation factors close to unity. The method was applied to study the elemental composition of clay from different fragments of a Chilean pre-Hispanic pottery piece. These results are very consistent showing that the analysis of samples from a small fragment can represent the whole piece.Work supported in part by FONDECYT Grant 1052-92.     

Uses of PGAA at the Dalat reactor

A facility for neutron capture prompt -ray spectroscopy for activation analysis has been intstalled at the tangential beam tube of the 500 kW Dalat reactor. Using a single crystal of silicon for filtering the thermal neutron beam and the 73 cm³ HP-G detector shielded by common materials with flexible configurations suitable to various samples, LOD of nearly 30 elements were estimated. Applications of PGAA in the determination of elemental concentrations in biological, environmental, geological and industrial product samples are presented.     

Determination of suspended particulates matter of major significance to human health using nuclear techniques in kenya

Energy dispersive X-ray fluorescence (EDXRF) analysis of aerosol samples in Nairobi is presented. Results show that elemental concentrations are of the order of 10^–4 to 10^–6 g/m³ for most elements analyzed. The total suspended particulate (TSP) matter was between 30–80 g/m³ for the entire sampling period between December 1993 to October 1994. Levels of lead (Pb) are below WHO guidelines. However, the obtained bromine (Br) to Pb ratio: 0.3–0.51, shows the origin of Pb to be from vehicular emissions. This ratio was particularly high during the months of April to July 1994 which were also found to be very active in terms of weather parameters.     

Fast determination of trace elements on aerosol-loaded filters by X-ray fluorescence analysis considering the inhomogeneous elemental distribution

X-ray fluorescence (XRF) analysis was successfully applied for the determination of Ca, Cu, Fe, Mn, Ni, Pb, V and Zn on aerosol filters with a diameter of 150 mm. Ambient aerosol was collected on quartz-fibre filters by Digitel high-volume samplers. For XRF analysis three small filter pieces with a diameter of 32 mm were cut out of each filter, considering the radial dependence of elemental distribution on the filter. Elemental concentration decreases by 8-10% from the centre to the outer circle for coarse mode elements. Distribution of fine mode elements display only small radial dependence (2-4%). Results of quantitative analysis by XRF were compared with atomic spectrometric methods (GF-AAS, ICP-OES). The good agreement between the methods confirmed the application of XRF spectrometry for routine analysis of filter samples loaded with ambient aerosol.     

Zur Bestimmung der Lanthanoiden durch R?ntgenfluorescenzanalyse

Zusammenfassung Zur Bestimmung aller Lanthanoiden (außer Pm) nebeneinander mit Sr als innerem Standard wurde eine RFA-Dünnschichtmethode entwickelt, bei der die Proben aus Lösungen auf Filterpapier hergestellt werden. Für geeignete L-Strahlungen sind die Eichkurven bis zu gesättigten Lösungen linear. Matrixeffekte werden eliminiert, Reflexüberlagerungen lassen sich wirksam korrigieren. Die statistischen Nachweisgrenzen betragen zwischen 0,2 und 0,6 g/cm², d. h. bezogen auf die Lösung zwischen 20 und 60 ppm.

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A contribution to X-ray fluorescence analysis of the lanthanoides

Summary A thin-layer method of X-ray fluorescence analysis has been developed for determining the lanthanoides (except Pm) in the presence of each other with Sr as internal standard. Samples are prepared from solutions on filter paper. With suitable L-radiations, linear calibration curves are obtained up to saturated solutions. Matrix effects are eliminated, reflection overlap is corrected efficiently. Statistical detection limits are between 0.2 and 0.6 g/cm², i.e. between 20 and 60 ppm in solution.

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Wir danken dem Fonds der Chemischen Industrie für die Förderung dieser Untersuchung.     

Fast determination of trace elements on aerosol-loaded filters by X-ray fluorescence analysis considering the inhomogeneous elemental distribution

X-ray fluorescence (XRF) analysis was successfully applied for the determination of Ca, Cu, Fe, Mn, Ni, Pb, V and Zn on aerosol filters with a diameter of 150 mm. Ambient aerosol was collected on quartz-fibre filters by Digitel high-volume samplers. For XRF analysis three small filter pieces with a diameter of 32 mm were cut out of each filter, considering the radial dependence of elemental distribution on the filter. Elemental concentration decreases by 8–10% from the centre to the outer circle for coarse mode elements. Distribution of fine mode elements display only small radial dependence (2–4%). Results of quantitative analysis by XRF were compared with atomic spectrometric methods (GF-AAS, ICP-OES). The good agreement between the methods confirmed the application of XRF spectrometry for routine analysis of filter samples loaded with ambient aerosol.     

Synthesis and characterization of manganese diselenide nanoparticles (MnSeNPs): Determination of capsaicin by using MnSeNP-modified glassy carbon electrode

A new type of manganese diselenide nanoparticles (MnSeNPs) was synthesized by using a hydrothermal method. Their surface morphology, crystallinity and elemental distribution were characterized by using transmission electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy which scrutinize the formation of the NPs. The NPs were coated on a glassy carbon electrode (GCE), and electrochemical impedance spectroscopy, cyclic voltammetry and differential pulse voltammetry were applied to study the electroanalytical properties towards the oxidation of the food additive capsaicin. The modified GCE displays lower charge transfer resistance (R _ct ?=?29.52 Ω), a larger active surface area (0.089 cm²/g, and more efficient electrochemical oxidation of capsaicin compared to a MnS₂/GCE and a bare GCE. The oxidation peak potential is 0.43 V (vs. Ag/AgCl) which is lower than that of previously reported GCEs. The sensor has a detection limit as low as 0.05 μM and an electrochemical sensitivity of 2.41 μA μM^?1 cm^?2. The method was applied to the determination of capsaicin in pepper samples.

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Graphical abstract Electrochemical determination of capsaicin in pepper extract by using MnSeNPs modified electrode.

     

Quantitative Bestimmung leichter Elemente mit Hilfe der R?ntgenfluorescenzanalyse: Kalium

Zusammenfassung Es wird ein Verfahren für die quantitative Bestimmung von Kalium mit Hilfe der energiedispersiven Röntgenfluorescenzanalyse beschrieben, das für die Anwendung auf Wasserproben ausgearbeitet wurde. Das Kalium wird als Tetraphenylborat gefällt und gemessen. Zur Anregung der Fluorescenzstrahlung dient eine Röntgenröhre mit Wolframanode und Titan als Sekundärtarget, zur Messung der Röntgenspektren wird ein Si(Li)-Detektor verwendet. Unter den beschriebenen Versuchsbedingungen können 0,1–1000 g (0,04–400 g/cm²) Kalium bestimmt werden.

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Quantitative determination of ligth elements by X-ray fluorescence analysis: Potassium

Summary A procedure is described for the quantitative determination of potassium in water samples, using energy dispersive X-ray fluorescence analysis. Potassium is precipitated and measured as tetraphenyloborate. The fluorescence radiation is excited employing a tungsten X-ray tube and titanium as secondary target. A Si(Li)-detector is used for measuring the X-ray spectra. With the conditions described, 0.1–1000 g (0.04–400 g/cm²) of potassium can be determined.

     

Determination of carbon in high-purity iron by a modified combustion method

Summary A newly developed apparatus was used for the determination of carbon in pure and high-purity iron samples. It enables the differentiation between the carbon content of the surface and the bulk by temperature-controlled heating in an oxygen flow. The carbon dioxide formed was measured by an IR-gas analyzer, type BINOS. At sample weights of about 0.1 g with surface areas of about 0.5 cm², carbon concentrations of 0.04 g/cm² of the surface and of 0.2 g/g of the bulk can be determined. By means of the results on 6 certified reference materials with low carbon concentrations and on 7 high-purity iron samples, the influence of sample form, treatment and storage on surface and bulk carbon is demonstrated. The findings confirm the already formerly stated tendency to too high values in the certificates of reference samples with carbon concentrations in the lower g/g range.

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Bestimmung von Kohlenstoff in Reinsteisen nach einem modifizierten Verbrennungsverfahren

     

Analysis of heavy metal aerosols on filters by laser-induced plasma spectroscopy

Particulate heavy metals can lead to severe toxic and carcinogenic effects in humans when inhaled in higher concentrations. For the development of a quasi-continuous emission monitor based on automatic filter sampling on a filter band, laser-induced plasma spectroscopy (LIPS) was studied for analysis of heavy metal aerosols on quartz fiber filters. The system consists of a 19-inch laser and detector module connected to a miniaturized sensor head through fiber optics, allowing maximum flexibility of the set-up. Parameters for optimum time-resolved analysis, i.e. detection wavelength, timing and filter material, were established. The LIPS investigations were accompanied by a rigorous reference analysis based on total reflection X-ray fluorescence (TXRF) analysis. The detection limits for heavy metals (Cd, Ni, As, Co, Mn, Sb, Cr, Tl, Sn, V, Cu and Pb) on filters varied between 0.01 and approximately 0.91 μg cm⁻², corresponding to volume detection limits of 0.02–2.73 μg m⁻³. Analysis of filter samples from waste incineration demonstrated the potential of the LIPS approach. In combination with an echelle spectrometer, ambient samples from environmental monitoring could be characterized in much better detail, due to the improved detection limits and the superior spectral resolution, and spectral range of the echelle.     

Elemental composition studies of fugitive and ambient air dust particulates from a thermal power station by instrumental neutron activation analysis

In order to assess the source of pollutants and the atmosphere quality in and around a thermal power plant, fugitive dust particulates from seven different locations and ambient air dust from six locations have been analyzed for 32 elements (As, Au, Ba, Br, Ce, Cl, Co, Cr, Cs, Cu, Eu, Fe, Ga, Hg, Hf, K, La, Lu, Mg, Mn, Na, P, Rb, Sb, Sc, Se, Ta, Tb, Te, Th, W and Yb) by employing instrumental neutron activation analysis (INAA). The method involves the irradiation of samples and comparator standards in a thermal neutron flux range of 10¹²–10¹³ n·cm^–2·s^–1 in a nuclear reactor for 10 min and 1 day followed by high resolution -spectrometry. Wide differences have been observed in the mean elemental concentrations of Fe, Co, Br, Mn, As, P. Ba and Cu in fugitive and ambient dust particulates coliected from these different locations. Further, a comparison of the elemental contents of the dust particulates from the plant with environmental standards (Urban Particulate Matter, Coal Fly Ash, Vehicle Exhaust and Coal) show significantly lower or comparable amounts of toxic and pollutant elements in the environmental samples.     

Concept and validation of a novel approach for producing large batches of reference material of ambient aerosols on filters

A novel method for preparing reference material of aerosol particulate matter (PM) on filters was developed by using the concept of very high volume, multiport sampling, and this was subsequently applied to produce more than 300 well-characterised units. The dedicated sampler built for this purpose features a 0.94-m-diameter, vacuum-tight main chamber with a total of 349 monitor ports, each holding a 37-mm-diameter, cellulose acetate–nitrate ester (CA) membrane filter with a nominal pore size of 0.8 m. At a pressure difference of about 130 hPa across the filter cassettes, the total initial air flow rate was 350 m³ h^–1 (1.0 m³ h^–1 per filter). Investigations into the variability of filter parameters showed that the flow resistance of CA filters is mostly determined by and proportional to their blank mass, with a mean uncertainty of about 5%. Total suspended particulate matter (TSP) was sampled for a total of 50 h using 349 selected filters with a relatively narrow spread in blank mass. The mean TSP mass per filter thus produced was 3.35 mg. Corrected for small differences in blank mass of the filters, the normalised aerosol masses per filter of 96% of the samples exhibited normal distributions with standard deviations of only 2.1 and 3.4%, depending on details of the normalisation procedure. Within the limits of the technique, a variation of aerosol mass with radial distance from the centre of the sampler is not clearly evident. The results provide evidence that the multiport approach allows large batches of particulate matter on filters to be produced in a reliable manner.     

3-Hydroxy-2-(2-thienyl)-4H-chromen-4-one as a new reagent for the extraction and trace determination of molybdenum(VI)

A simple, sensitive and selective method for the extraction and trace determination of molybdenum(VI) has been developed; it is based on its reaction with 3-hydroxy-2-(2-thienyl)-4H-chromen-4-one (HTC) in sulphuric acid medium. The 1:2 Mo (VI)-HTC yellow complex is quantitatively extractable into chloroform (_max 420 nm) and is stable for more than 4 h. The procedure eliminates the interference of a large number of metal ions and complexing agents. Beer's law is obeyed in the range of 0–2.85 g Mo/mL with a molar absorptivity, Sandell's sensitivity and standard deviation of 5.28×10⁴ L mol^–1 cm^–1, 0.0018 g Mo/cm² and ±0.0054, respectively. The method has successfully been used for the spectrophotometric determination of molybdenum in steel samples.     

Spectrophotometric determination of molybdenum(V) by extraction of its 2-(2′-furyl)-3-hydroxychromone complex

A simple method is described for the rapid spectrophotometric determination of molybedenum in synthetic and industrial samples containing 0.1-5% Mo. Molybdenum is reduced with ascorbic acid at room temperature in 1 mol dm^–3 H₂SO₄ and extracted with chloroform after adding 2-(2-furyl)-3-hydroxychromone (FHC). The yellow colour of the 1 2 Mo-FHC complex is measured at 414 nm against a reagent blank. Beer's law is obeyed over the range 0-2.7 g Mo cm^–3 of solvent phase. The molar absorptivity and Sandell's sensitivity are 5.18 × 10⁴ dm³ mol^–1 cm^–1 and 0.0018 g Mo cm^–2, respectively. Relative standard deviations are 0.2% for solutions and 0.5–1.5% for solid samples. Interference from tungsten and tin is removed by adding citrate and EDTA, respectively, while niobium and tantalum are masked by fluoride. Many elements such as V, Fe, Ti, U, Mn, Cr, Co, Ni, Re, Ru, Pt, Rh, Se, Au, Bi, Zr, Th, Ce, As and Al do not interfere even in large amounts, but antimony always interferes. Among the anions and complexing agents, only thiocyanate interferes seriously.     

Vibrational spectroscopy of acid treated vermiculites

The natural vermiculites from different localities (Bulgaria, Brazil, and South Africa) after acid treatment were used for this study. Differently acidified vermiculite samples were prepared from the natural vermiculite sample using different concentrations of hydrochloric acid (0.5 M and 1 M) and different reaction time (2 h and 4 h) at 80 °C. Natural vermiculites and acid treated vermiculites were analyzed by elemental analysis, X-ray diffraction (XRD) analysis and studied using Fourier transform infrared (FTIR) spectroscopy and dispersive Raman spectroscopy. According to the XRD analysis vermiculites are interstratified structures created in the different two-one-zero sheet hydrated phases. Ratio of intensities of spectrally deconvoluted bands at 1075 cm⁻¹ and 1000 cm⁻¹ (stretching vibration of SiO bonds of vermiculites and stretching vibration of SiO bonds of amorphous silica, respectively) was used to determine the content of amorphous silica in acid treated vermiculite samples. Study of the infrared and Raman spectra of the acidified vermiculites enable a comparison of these two spectroscopic data that have not yet been performed.     

Characterisation of chlorinated hydrocarbons in a third generation candidate fish reference material (Limanda limanda) prepared under cryogenic conditions

Summary This paper describes the cryogenic preparation of 50 individual specimens of dab (Limanda limanda) from the Baltic Sea to produce a homogeneous fish material. 950 subsamples (8 g each) are stored in the gaseous phase over liquid nitrogen. Five series of analyses were randomly selected out of store. The results show that the obtained precision of 8 to 9% could be used as an indication unit for the deviation of the mean values of CHC concentrations from true values. If the analytical variability is 5%, the maximum inhomogeneity in the subsamples is 3–4%. It may be concluded that the subsamples of the candidate fish reference material (RM) are homogeneous enough for analytical purposes. Thus ESB (German Environmental Specimen Bank) material prepared in accordance with the standard operating procedure (SOP) [1] are valuable and appropriate reference materials. The prepared fish RM is suitable for the analysis of chlorinated hydrocarbons in fat containing marine samples.     

Silicon determination in plant materials by instrumental epithermal neutron activation analysis

The Si determination with epithermal neutrons using the reaction²⁸Si (n,p)²⁸Al is described. Thermal neutrons are eliminated from the irradiation position with a BN-shield. Two first order interfering reactions with P and with Al necessitate appropriate corrections. The interfering reaction on Al is shown to depend heavily on the hydrogen (H) content of the sample, which therefore must be taken into account. The lower application range in plant samles is estimated to be 500 g g^–1. Reproducibility is <5% in suitable cases, but not as good if the necessary corrections are large. The capacity is 25 samples per 8 h. The method is applied to 3 plant standards (rice, hay and pine needles) and to 47 samples of spruce needles. The applicability to different plant materials is mainly limited by their relative Al, P and Si concentrations. Literature values are use to find plant categories in which Si can be reasonably determined by instrumental epithermal neutron activation analysis (IENA).