Unraveling the evolving nature of gaseous and dissolved carbon dioxide in champagne wines: A state-of-the-art review,from the bottle to the tasting glass

In champagne and sparkling wine tasting, the concentration of dissolved CO₂ is indeed an analytical parameter of high importance since it directly impacts the four following sensory properties: (i) the frequency of bubble formation in the glass, (ii) the growth rate of rising bubbles, (iii) the mouth feel, and (iv) the nose of champagne, i.e., its so-called bouquet. In this state-of-the-art review, the evolving nature of the dissolved and gaseous CO₂ found in champagne wines is evidenced, from the bottle to the glass, through various analytical techniques. Results obtained concerning various steps where the CO₂ molecule plays a role (from its ingestion in the liquid phase during the fermentation process to its progressive release in the headspace above the tasting glass) are gathered and synthesized to propose a self-consistent and global overview of how gaseous and dissolved CO₂ impact champagne and sparkling wine science.     

Characterization by optical measurements of the effects of some stages of champagne technology on the adsorption layer formed at the gas/wine interface

This study analyzes the effects of some important factors of champagne technology on the ellipticity and Brewster angle microscopy (BAM) of the air/champagne interface in view of using the optical properties of the adsorption layer of base wine to forecast the stability of the champagne bubble collar. Using standard, ultrafiltered, and ultraconcentrated wines it was observed that champagne can lose amphiphilic macromolecules which adsorb on the inner glass wall of the bottle during storage, particles such as dead yeasts can adhere to the adsorption layer, a weak increase of the ethanol content during bottle fermentation can reduce significantly the ellipticity of the adsorption layer, and CO2 has no significant effect on the properties of that layer. Surprisingly, no visible differences of the adsorption layer were noticed between the experimental champagnes of the 2004 vintage of three vine varieties (Chardonnay, Pinot noir, and Pinot meunier). From analysis of all samples it is proposed that the mean value and standard deviation of the ellipticity measured during 30 min after pouring the wine in a Petri dish are physical quantities which satisfactorily characterize the adsorption layer of champagne. When needed, further characterization of the adsorption layer may be obtained by a detailed analysis of the kinetics of ellipticity during the same period and inspection of the BAM images of the interface.     

Recent advances in the science of champagne bubbles

The so-called effervescence process, which enlivens champagne and sparkling wines tasting, is the result of the fine interplay between CO(2)-dissolved gas molecules, tiny air pockets trapped within microscopic particles during the pouring process, and some liquid properties. This critical review summarizes recent advances obtained during the past decade concerning the physicochemical processes behind the nucleation, rise, and burst of bubbles found in glasses poured with champagne and sparkling wines. Those phenomena observed in close-up through high-speed photography are often visually appealing. Let's hope that your enjoyment of champagne will be enhanced after reading this fully illustrated review dedicated to the deep beauties of nature often hidden behind many everyday phenomena (51 references).     

Is the wall of a cellulose fiber saturated with liquid whether or not permeable with CO2 dissolved molecules? Application to bubble nucleation in champagne wines

In this paper, the transversal diffusion coefficient D perpendicular of CO2 dissolved molecules through the wall of a hydrated cellulose fiber was approached, from the liquid bulk diffusion coefficient of CO2 dissolved molecules modified by an obstruction factor. The porous network between the cellulose microfibrils of the fiber wall was assumed being saturated with liquid. We retrieved information from previous NMR experiments on the self-diffusion of water in cellulose fibers to reach an order of magnitude for the transversal diffusion coefficient of CO2 molecules through the fiber wall. A value of about D perpendicular approximately 0.2D0 was proposed, D0 being the diffusion coefficient of CO2 molecules in the liquid bulk. Because most of bubble nucleation sites in a glass poured with carbonated beverage are cellulose fibers cast off from paper or cloth which floated from the surrounding air, or remaining from the wiping process, this result directly applies to the kinetics of carbon dioxide bubble formation from champagne and sparkling wines. If the cellulose fiber wall was impermeable with regard to CO2 dissolved molecules, it was suggested that the kinetics of bubbling would be about three times less than it is.     

GasBench/isotope ratio mass spectrometry: a carbon isotope approach to detect exogenous CO(2) in sparkling drinks

A new procedure for the determination of carbon dioxide (CO(2)) (13)C/(12)C isotope ratios, using direct injection into a GasBench/isotope ratio mass spectrometry (GasBench/IRMS) system, has been developed to improve isotopic methods devoted to the study of the authenticity of sparkling drinks. Thirty-nine commercial sparkling drink samples from various origins were analyzed. Values of delta(13)C(cava) ranged from -20.30 per thousand to -23.63 per thousand, when C3 sugar addition was performed for a second alcoholic fermentation. Values of delta(13)C(water) ranged from -5.59 per thousand to -6.87 per thousand in the case of naturally carbonated water or water fortified with gas from the spring, and delta(13)C(water) ranged from -29.36 per thousand to -42.09 per thousand when industrial CO(2) was added. It has been demonstrated that the addition of C4 sugar to semi-sparkling wine (aguja) and industrial CO(2) addition to sparkling wine (cava) or water can be detected. The new procedure has advantages over existing methods in terms of analysis time and sample treatment. In addition, it is the first isotopic method developed that allows (13)C/(12)C determination directly from a liquid sample without previous CO(2) extraction. No significant isotopic fractionation was observed nor any influence by secondary compounds present in the liquid phase.     

Flow patterns of bubble nucleation sites (called fliers) freely floating in champagne glasses

Laser tomography techniques were used to capture the dynamics of bubbles released from particles (arbitrarily called fliers) freely floating in traditional flutes poured with champagne. By use of long exposure time photography, the trajectories of bubbles released by fliers were found to leave very elegant and characteristic "prints" as they crossed a section of champagne illuminated with a 1 mm thick laser sheet. This characteristic print was made with a succession of lighting filaments. Fine analysis of these prints left by fliers enabled us to deduce the bubbling frequency of each flier (which ranged from about 4 bubbles/s up to about 22 bubbles/s a few seconds after pouring), as well as its velocity through the liquid medium (which ranged from about 0.8 mm/s to about 7.6 mm/s). Finally, this flow visualization technique, very recently applied to the science of champagne and sparkling wines, also proved to be a useful technique to underscore fliers' bubbling instabilities along their rather erratic way through the liquid medium.     

Does the Temperature of the prise de mousse Affect the Effervescence and the Foam of Sparkling Wines?

The persistence of effervescence and foam collar during a Champagne or sparkling wine tasting constitute one, among others, specific consumer preference for these products. Many different factors related to the product or to the tasting conditions might influence their behavior in the glass. However, the underlying factor behind the fizziness of these wines involves a second in-bottle alcoholic fermentation, also well known as the prise de mousse. The aim of this study was to assess whether a low temperature (13 °C) or a high temperature (20 °C) during the in-bottle fermentation might have an impact on the effervescence and the foaming properties (i.e., collar height and bubble size) of three French sparkling wines (a Crémant de Loire and two Champagne wines), under standard tasting conditions. Our results showed that sparkling wines elaborated at 13 °C and served in standard tasting conditions (i.e., 100 mL, 18 °C) had better ability to keep the dissolved CO₂ (between 0.09 and 0.30 g/L) in the liquid phase than those elaborated at 20 °C (with P < 0.05). Most interestingly, we also observed, for the Crémant de Loire and for one Champagne wine, that the lower the temperature of the prise de mousse, the smaller (with P < 0.05) the bubbles in the foam collar throughout the wine tasting.     

Characterisation by drop tensiometry and by ellipsometry of the adsorption layer formed at the air/champagne wine interface

A foam ring composed of small bubbles on the surface of a champagne glass is one of its hallmarks. The equilibrium state of that ring is linked with the rate of formation and of disappearance of bubbles. The stability of bubbles is usually ascribed to the occurrence and to the properties of an adsorption layer formed at the gas/liquid interface. Our goal is to characterise such an adsorption layer at the gas/wine interface in order to understand its role in bubble stability. Alcohol in wine lowers the surface tension to 49 mN/m. The adsorption of other molecules may cause a further decrease of 2 mN/m. Such a situation makes the study of adsorption by surface tension measurement inaccurate. To overcome this problem, we have diluted the wine four times with water before its surface tension measurement by pendant drop shape analysis. In these conditions, ethanol lowers the surface tension to 64 mN/m and the adsorption of other molecules of the wine can be monitored over 6-8 mN/m. The usual behaviour of such a diluted wine is a lowering of the surface tension during at least 20 min after drop formation. Since the role of macromolecules on the foaming properties of wine had been previously observed, we have chosen to evaluate the effect of this fraction of the wine molecules on its surface properties. Thus, wines were ultrafiltrated on a membrane with a 10000 molecular mass cut-off. The ultrafiltrate (UF) does not show any decrease of its surface tension over a 20-min period while the ultraconcentrate (UC) has a kinetics similar to that of unfiltered wine. Mixtures of UF and UC have behaviours intermediate between those of these products. A technological treatment of the wine with bentonite, believed to lower the content of macromolecules, yields a wine similar to UF. The effect of ultrafiltration was also analysed by spectroscopic ellipsometry. UF has a spectrum similar to that of a water/alcohol mixture with the same ethanol content and its ellipticity is stable during at least 20 min. On the contrary, wine or UC show spectra with the features of an adsorption layer and those characteristics increase during more than 20 min. Two varieties of vine were compared: 'Chardonnay' and 'Pinot noir'. The former is known to have better foaming properties than the latter. Its surface properties measured in this study are also more pronounced than those of Pinot noir. However, the representation of the dilational modulus against the surface pressure (which, in some instances, may be a mathematical transformation of the state equation) puts all the samples (wines, UF and UC of each) on the same master curve, a fact in favour of a common nature for all the adsorption layers. It can be concluded that surface properties of champagne wines are mostly determined by ethanol and by macromolecules with a molecular mass larger than 10000. Moreover, the adsorption layers seem to have the same nature, irrespective of the vine variety and of the concentration ratio of the wine.     

Quantification approach for assessment of sparkling wine volatiles from different soils, ripening stages, and varieties by stir bar sorptive extraction with liquid desorption

Stir bar sorptive extraction with liquid desorption followed by large volume injection coupled to gas chromatography-quadrupole mass spectrometry (SBSE-LD/LVI-GC-qMS) was applied for the quantification of varietal and fermentative volatiles in sparkling wines. The analytical data were performed by using suitable standards of monoterpene hydrocarbons (α-pinene), monoterpenols (linalool), sesquiterpenoids (E,E-farnesol, Z-nerolidol, and guaiazulene), C₁₃ norisoprenoids (β-ionone), aliphatic and aromatic alcohols (hexanol and 2-phenylethanol), and esters (hexyl acetate and ethyl decanoate) as model compounds. The wine volatiles were quantified using the structurally related standards. The methodology showed good linearity over the concentration range tested, with correlation coefficients ranging from 0.950 to 0.997, and a reproducibility of 9-18%. The SBSE-LD/LVI-GC-qMS methodology allowed, in a single run, the quantification of 71 wine volatiles that can be quantified accurately at levels lower than their respective olfactory thresholds. This methodology was used for assessment of sparkling wine volatiles from different soils, ripening stages, and varieties. The variety and soil influenced significantly the volatile composition of sparkling wines; lower effect was observed for the ripening stage of grapes picked up one week before or after the maturity state.     

Native ethylene glycol in wine: Application of a dead volume free,very fast “deans heart-cut” system on-line with multi-chromatography

Data about the existence of native HO? CH₂? CH₂? OH (MEG) in natural wines and champagne has led to delicate questions because of legal decisions already made to declare wine or champagne illegal for sale if the MEG concentrations found are above 10 mg/liter. Action has been taken because of the DEG (diethylene glycol) disaster in European wines of 1985…86. An incorrect legal decision was made due to the belief that MEG cannot be produced biochemically by grape vines. A further reason may be lack of correct data on native MEG trace concentrations, as a result of the special behavior of this diol. As first member of a homologous series whose higher members (C₄) are normally found in all wines at quite high concentration levels, MEG shows extremely adsorptive behavior. The solution of the chromatographic problems is summarized in this paper. MEG concentrations in Riesling as example are in the range of 2 to 6 mg/liter and can easily be increased by biotechnological steps to a level of around 10 to 60 mg/liter. This is again due to the specific adsorptive behavior of MEG, which can be enriched on filter surfaces and displaced when the wine acidity changes with changing types. In order to control and guarantee the qualitative and quantitative results of MEG analyses we used a combination of Deans heart cutting on-line with Multi-Chromatography. It was easy to produce false data by many otherwise useful single column or two-dimensional separation processes, etc.     

Changes in the Volatile Profile of Wheat Sourdough Produced with the Addition of Cava Lees

The volatile fraction is of great importance for the organoleptic quality and consumer acceptance of bread. The use of sourdough improves the sensory profile of bread, as well as the addition of new ingredients to the fermentation. Cava lees are a sparkling wine by-product formed of dead microorganisms, tartaric acid, and other inorganic compounds, rich in antioxidant compounds as well as β-glucans and mannoproteins. The aim of this study was to evaluate the effect of different concentrations of Cava lees (0–2% w/w) on sourdough volatile compounds to re-valorize this by-product of the wine industry. Headspace solid-phase microextraction (HS-SPME) was optimized to study the volatile fractions of sourdoughs. The parameters selected were 60 °C, 15 min of equilibrium, and 30 min of extraction. It was found that the addition of Cava lees resulted in higher concentrations of volatile compounds (alcohols, acids, aldehydes, ketones and esters), with the highest values being reached with the 2% Cava lees. Moreover, Cava lees contributed to aroma due to the compounds usually found in sparkling wine, such as 1-butanol, octanoic acid, benzaldehyde and ethyl hexanoate.     

Quantification of chloroanisoles in cork using headspace solid-phase microextraction and gas chromatography with electron capture detection

Chloroanisoles can migrate from the cork stopper in wine bottles to the wine and give it a musty taint so it is important to find a method by which they can be determined. The aim of this paper is to develop a method for quantifying 2,4-dichloroanisole, 2,6-dichloroanisole, 2,4,6-trichloroanisole, 2,3,4,6-tetrachloroanisole and 2,3,4,5,6-pentachloroanisole in cork using headspace solid-phase microextraction and gas chromatography with electron capture detection. After we had prepared the cork standards that were so essential to the work we optimised the parameters that most influence headspace solid-phase microextraction: fibre coating, vial volume, cork, kind and volume of solvent to help the extraction, extraction temperature and time, ionic strength and stirring. The method quantifies the total amount of chloroanisoles in cork stoppers (natural, agglomerated, agglomerated with disks and sparkling wine stoppers), at suitable concentrations so that the capacity of these compounds to give wine a musty taint can be evaluated. The quantification limits are: 2,6-dichloroanisole (8.6 ng/g), 2,4,6-trichloroanisole (0.8 ng/g), 2,4-dichloroanisole (3.5 ng/g), 2,3,4,6-tetrachloroanisole (0.6 ng/g), 2,3,4,5,6-pentachloroanisole (0.8 ng/g). The other quality parameters are: recoveries (90.3-105.8%), repeatability (4-13% (RSD expressed)) and intermediate precision (5-14% (RSD expressed)).     

Characterization of low-molecular weight peptides in champagne wine by liquid chromatography/tandem mass spectrometry

This paper reports the use of an on-line LC–ESI–MS/MS method for the identification and quantification of di- and tripeptides in champagne wine without laborious sample pretreatment. The identification of these compounds, in their underivatised form, is based on identical retention times and ESI–MS spectra to those of reference standards. The presence of nine dipeptides (Arg–Ile, Ile–Arg, Ile–Val, Lys–Phe, Lys–Tyr, Phe–Lys, Tyr–Gln, Tyr–Lys, Val–Ile) and the absence of two tripeptides (Phe–Arg–Arg and Lys–Met–Asn) have been evidenced in the matrix. Calibration curves for each analyte were established using Phe–Arg as internal standard. The calibration curves were linear in the concentration range 0.1–10 mg L⁻¹ with a determination coefficient, r², better than 0.992. The accuracy for the calibration standard was estimated at between 92 and 102%. This method allows high recovery and satisfies the necessary requirements with respect to accuracy, repeatability and sensitivity. The first application of this analytical method to the measurement of di- and tri-peptides in different vintages of champagne wine is reported. Compositional changes in the peptides occurred depending on the vintage.     

Modeling the kinetics of bubble nucleation in champagne and carbonated beverages

In champagne and carbonated beverages, bubble nucleation was mostly found to take place from tiny Taylor-like bubbles trapped inside immersed cellulose fibers stuck on the glass wall. The present paper complements a previous paper about the thorough examination of the bubble nucleation process in a flute poured with champagne (Liger-Belair et al. J. Phys. Chem. B 2005, 109, 14573). In this previous paper, a model was built that accurately reproduces the dynamics of these tiny Taylor-like bubbles that grow inside the fiber's lumen by diffusion of CO(2)-dissolved molecules. In the present paper, by use of the model recently developed, the frequency of bubble formation from cellulose fibers is accessed and linked with various liquid and fiber parameters, namely, the concentration c(L) of CO(2)-dissolved molecules, the liquid temperature theta, its viscosity eta, the ambient pressure P, the course of the gas pocket growing trapped inside the fiber's lumen before releasing a bubble, and the radius r of the fiber's lumen. The relative influence of the latter parameters on the bubbling frequency is discussed and supported with recent experimental observations and data.     

Modeling nonclassical heterogeneous bubble nucleation from cellulose fibers: application to bubbling in carbonated beverages

In this paper, the kinetics of CO(2) bubble nucleation from tiny gas pockets trapped inside cellulose fibers immersed in a glass of champagne were investigated, in situ, from high-speed video recordings. Taking into account the diffusion of CO(2)-dissolved molecules from the liquid bulk to the gas pocket, a model was derived which enabled us to connect the kinetics of bubble nucleation with both fiber and liquid parameters. Convection was found to play a major role in this process. The boundary layer around the gas pocket where a gradient of CO(2)-dissolved molecules exists was also indirectly approached and found to be in the order of 10-20 mum. Because most of the particles adsorbed on the wall of a container or vessel free from any particular treatment are also believed to be cellulose fibers coming from the surrounding air, the results of this paper could be indeed extended to the more general field of nonclassical heterogeneous bubble nucleation from supersaturated liquids.     

Monitoring of an industrial process by multivariate control charts based on principal component analysis

The control and monitoring of an industrial process is performed in this paper by the multivariate control charts. The process analysed consists of the bottling of the entire production of 1999 of the sparkling wine "Asti Spumante". This process is characterised by a great number of variables that can be treated with multivariate techniques. The monitoring of the process performed with classical Shewhart charts is very dangerous because they do not take into account the presence of functional relationships between the variables. The industrial process was firstly analysed by multivariate control charts based on Principal Component Analysis. This approach allowed the identification of problems in the process and of their causes. Successively, the SMART Charts (Simultaneous Scores Monitoring And Residual Tracking) were built in order to study the process in its whole. In spite of the successful identification of the presence of problems in the monitored process, the Smart chart did not allow an easy identification of the special causes of variation which casued the problems themselves.     

Identification of sources and production processes of bottled waters by stable hydrogen and oxygen isotope ratios

Bottled water is a food product that considerably depends on the environment from which it originates, not only at the place where it is produced, but predominantly on the conditions in the recharge area of the wells captured for bottling. According to their source and the bottling process, bottled waters can be divided into natural and artificially sparkling waters, still and flavoured waters. These waters originate from various parts of the hydrological cycle and their natural origin is reflected in their hydrogen and oxygen stable isotopic compositions (delta(2)H and delta(18)O). A total of 58 domestic and foreign brands and 16 replicates of bottled waters, randomly collected on the Slovene market in September 2004, were analysed for delta(2)H and delta(18)O. The isotopic composition varied between -83 per thousand and -46 per thousand with an average of -66 per thousand for hydrogen, and between -11.9 per thousand and -7.5 per thousand with an average of -9.6 per thousand for oxygen. This investigation helped (1) to determine and test the classification of bottled waters, (2) to determine the natural origin of bottled water, and (3) to indicate differences between the natural and production processes. The production process may influence the isotopic composition of flavoured waters and artificially sparkling waters. No such modification was observed for still and natural sparkling waters. The methods applied, together with hydrological knowledge, can be used for the authentication of bottled waters for regulatory and consumer control applications.     

A novel silica aerogel microspheres loaded with ammonium persulfate gel breaker for mid-deep reservoirs

Sol–gel based transparent functional coatings such as easy-to-clean coatings, anti-glare coatings, anti-reflective coatings, and anti-fingerprint coatings have been developed and commercialized for display applications. These coatings can be applied by a spray process on the glass substrates followed by a low temperature curing at 100° to 150?°C. Hydrophobic easy-to-clean coatings exhibit high water contact angles at ≥115°, with an excellent wear durability by passing 10,000 cycles using #0000 steel wool under 1?kg load. In addition, easy-to-clean coatings show a silky touch feel with a coefficient of friction of less than 0.03. Anti-glare coatings without particles have a gloss value between 50 to 100 gloss units, an adhesion of 5B, a pencil hardness ≥8?H, and no sparkling issues on touch screen displays. A combination of easy-to-clean coatings on top of anti-glare coatings significantly increases the stylus pen durability. Single-layer anti-reflective coatings show a transmittance increase of 1.5% to 2.0% by spray coating on a single side of the glass substrate, or a transmittance increase of more than 4.0% by dip-coating on a polycarbonate substrate. Anti-fingerprint coatings show less obvious fingerprints on the coated glass surface compared to those on uncoated glass surface. These coating solutions have been scaled up to 1000?kg batch in PPG’s Tianjin plant, China.

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Anti-glare coatings with irregular surface microstructures formed during a spray process have a gloss value between 50 to 100 gloss units, a pencil hardness ≥8H, and no sparkling issues on touch screen displays. Optical profiler image (with ×50.3 magnification) of the anti-glare coating surface (70 gloss units) shows irregular microstructure patterns which are random locally but uniform in large area. The light scattering on the anti-glare coating surface is caused by these irregular surface microstructures. Thus the specular reflection is significantly reduced, causing glare reduction, gloss decrease, and haze increase.

     

Simultaneous determination of preservatives in beverages,vinegar, aqueous sauces,and quasi-drug drinks by stir-bar sorptive extraction (SBSE) and thermal desorption GC-MS

A method for the simultaneous determination of seven preservatives - sorbic acid, benzoic acid, and p-hydroxybenzoic acid ethyl, isopropyl, propyl, isobutyl, and butyl esters - in beverages, vinegar, aqueous sauces, and quasi-drug drinks has been developed using the stir-bar sorptive extraction technique then thermal desorption GC-MS analysis. The extraction conditions - pH, sample volume, extraction temperature, salt addition, and extraction time - were examined. d5-Benzoic acid and p-hydroxybenzoic acid sec-butyl ester were added as surrogate internal standards to compensate for the effect of sample matrix and coexisting analytes on the sorptive extraction. The linearity of the method was good over the concentration range from 1 to 1000 microg mL(-1) for sorbic acid, 10-1000 microg mL(-1) for benzoic acid, and 0.1-100 microg mL(-1) for p-hydroxybenzoic acid ethyl, isopropyl, propyl, isobutyl, and butyl esters, and the correlation coefficients were higher than 0.9984. The limit of detection ranged from 0.015 to 3.3 microg mL(-1). The recoveries (95-105%) and precision (RSD: 0.86-6.0%) of the method were examined by analyzing a sparkling soft drink, white wine, red wine, balsamic vinegar, soy sauce, and quasi-drug drink samples fortified at the 5 to 50 microg mL(-1) level.