Spinning Band Column Research Articles

Citral enrichment in Lemongrass (Cymbopogon flexuosus) oil using spinning band equipped high vacuum distillation column and sensory evaluation of fractions

Citral is the major constituent of Lemongrass oil (LGO) and has various application in the food, cosmetic and pharmaceutical industry. The present study was focused on enhancement of citral content in LGO employing spinning band column equipped high vacuum fractional distillation setup. The collected fractions were investigated for volatile composition using gas chromatography-mass spectrometry (GC–MS), antioxidant activity using 1,1-diphenyl-2-picrylhydrazyl (DPPH) method and antibacterial activity against Gram-positive and Gram-negative bacteria. The total citral content varied from 1.90 to 88% in various fractions with highest in major fraction, residue experiment-B (RSD, Ex-B, 88%) with collection of 63 mL. RSD, Ex-B demonstrated the lowest IC50 value of 6.77±0.42µL/mL with 55.84 percent inhibition. Further, strong inhibition was demonstrated by RSD, Ex-B against all tested bacterial strains. The sensory analysis revealed that Lemongrass leaves were dominated with lemony, fresh and grassy; LGO with lemony and fresh; and RSD (Ex-B) with lemony, sweet and fresh notes. The distillation process changed the overall aroma profile of RSD (Ex-B) by eliminating grassy and off odors and makes it useful product for flavor and fragrance application. Citral rich fractions have high economic value as well as application in food industry as a flavor, preservative; in home care and self-hygiene products.

Spinning band distillation of biomass pyrolysis oil phenolics to produce pure phenol

Competitive pricing for biofuels will require the coproduction of biobased products and chemicals to improve the economic outlook of biorefineries. Phenolics have been eyed due to their natural abundance in bio-oils relative to petroleum, as well as their potential profit margins. In bio-oils, the wide product distribution (especially phenolics) prevents meaningful separation. We’ve shown previously that bio-oils with relatively low oxygen (<15 wt%) from advanced pyrolysis processes can be distilled and/or extracted, producing a fraction rich in phenol and cresols. To further improve separation, we utilized a spinning band column distillation system, designed to perform at 200 theoretical plates. Catalytic (HZSM-5) pyrolysis bio-oils from switchgrass biomass first underwent extraction directly, producing a phenolic fraction and a hydrocarbon fraction. Subsequently, the phenolic fraction underwent a preliminary flash distillation ahead of spinning band distillation, in order to remove residues. Spinning band distillation resulted in fractions with more than 80 wt% phenol (the balance o-cresol), which can be purified by recrystallization in pentane. Both GC/MS and NMR indicate phenol crystals were obtained at ∼92 wt% purity. To complete the biorefinery concept, the hydrocarbon fraction was distilled to obtain a fuel product and heavy polyaromatic residues. The residues were thermally treated to produce bio-pitch.

δ18O of Ethanol in Wine and Spirits for Authentication Purposes

Since 1986 the European Union has established official isotopic analysis methods for detecting the illegal addition of sugar and water to wine and to enable geographical traceability. In this paper we investigate the possibility of using analysis of the 18O/16O stable isotope ratio (expressed as δ 18O) of ethanol to improve detection of the watering of wine and to determine the origin of ethanol. Sixty-nine authentic wine samples from all over Italy, 59 spirits from fruit and cereals, 5 chemically synthesized ethanols, one concentrated and rectified must, one beet and one cane sugar, one fresh must, and 6 waters with increasing δ 18O values were considered. Ethanol was recovered by distillation, using a Cadiot spinning band column, following the official OIV methods. The residual water was trapped by storing the distillate for at least 24 h on a molecular sieve. The 18O/16O ratio was measured using a pyrolyser interfaced with an isotope ratio mass spectrometer. The δ (-18)O of ethanol is significantly related to the δ 18O of the fermentation water and can be considered as a reliable internal reference. The values ranged from +24‰ to +36‰ in wine (years 2008 to 2012), +10‰ to +26‰ in fruit and cereal distillates, and from -2‰ to +12‰ in synthetic ethanol. The method was shown to be effective in improving detection of the watering of wine and determining the origin of ethanol (from grapes, other fruit, or synthesis), but not in detecting the addition of cane or beet sugar to wine.

ChemInform Abstract: Trifluoromethanesulfonic Acid, Chlorobis(1,1‐Dimethylethyl)silyl Ester

AbstractReview: 9 refs.

Vapor−Liquid Equilibrium Data, Excess Enthalpy Data, and Azeotropic Data for the Binary System Dibutyl Ether + o-Xylene

For the binary system dibutyl ether + o-xylene, isothermal and isobaric vapor−liquid equilibrium (VLE) data were measured with the static synthetic and the dynamic method. Additionally, excess enthalpy (HE) data were determined by means of an isothermal flow calorimeter, and azeotropic data were investigated using a spinning band column. The experimental data from this work were correlated using linear temperature-dependent UNIQUAC interaction parameters.

Vapor−Liquid−Liquid Equilibria, Azeotropic, and Excess Enthalpy Data for the Binary System n-Undecane + Propionamide and Pure-Component Vapor Pressure and Density Data for Propionamide

Vapor−liquid−liquid equilibria (VLLE), azeotropic, and excess enthalpy (HE) data for the binary system n-undecane + propionamide were measured at temperatures from 359.25 to 416.65 K. Additionally, pure-component vapor pressure and density data for propionamide were determined experimentally. The LLE and VLLE measurements were performed in a stirred glass cell and in a static equilibrium cell with a capability to take small samples from the different phases by using pneumatic micro samplers. For the HE measurements, an isothermal flow calorimeter was used, and the azeotropic data were obtained from distillation experiments using a micro spinning band column. The pure-component vapor pressures and densities were measured with the help of the dynamic method (ebulliometer) and a vibrating tube densimeter, respectively. To the experimental mixture data from this work linear temperature-dependent interaction parameters for the NRTL model were fitted. They can be used to represent the phase equilibrium behavior and excess enthalpies of the investigated system.

Structural Characterization of Polysilicate Intermediates Formed During Sol-Gel Polymerization

ABSTRACTIdentification of polysilicate intermediates formed during sol-gel processing of silica gels and glasses is an important step toward understanding the nature of this process on a molecular level. Although capillary gas chromatography using mass spectrometric detection gives the molecular formulas for low molecular weight intermediates [1], this approach is only semi-quantitative and provides no structural information. An improved protocol has been developed that allows structural assignment and quantitative determination of the principal mono- through hexasilicate structural isamers formed by hydrolysis of methanolic tetramethylorthosilicate in the presence of HC1. This protocol combines quenching by diazomethane, fractionation using spinning band column distillation, identification by capillary gas chromatography, and structural characterization using 29Si{1H} NMR techniques (l-pulse, ID-INADEQUATE, and 2D-INADEQUATE) to provide structural assignments and response factors for the components separated by gas chromatography.

Pyrrolidine Carboxaldehyde Hydrohalide Catalyzed Halogenations of Aliphatic Aldehydes

Abstract Efficient methods for the direct chlorination or bromination of aliphatic aldehydes to their corresponding α,α-dihalo aldehydes in high yield and purity are unknown. Many approaches have suffered from one or more of the following, formation of byproducts, aldol condensations incomplete conversions and losses through tedious workup procedures. Early investigations have shown that the vapor phase chlorination of aliphatic ketones has produced good yields of 2-chloro ketones,(1) while the vapor phase chlorination of aliphatic aldehydes has resulted in the formation of acid chlorides.(2) One of the first successful acid catalyzed chlorinations of propionaldehyde was reported by Dick(3) who obtained 50–60% yields of 2,2-dichloropropionaldehyde accompanied by aldol condensations and polyhalogenated trioxanes. The reaction was carried out in standardized aqueous mineral acid solutions and the product was isolated by means of a laborious azeotropic distillation. The use of sulfuryl chloride in the presence of a catalytic amount of diphenyl sulfide for the chlorination of aldehydes was shown by Dalman(4) to give 60–70% yields of 2-chloro and 2,2-dichlorinated aldehydes. Clean separations i.e. products free of sulfuryl chloride could only be obtained by distillation with a spinning band column at high reflux ratios.

Studies on mutagenic constituents of apple brandy and various alcoholic beverages collected in western France, a high incidence area for oesophageal cancer

Apple brandies, alcoholic spirits produced in the west of France, as well as other types of alcoholic beverage (rums, whiskies, armagnacs, cognacs) were tested for mutagenicity on Salmonella typhimurium TA98 and TA100 in the plate-incorporation assay in the presence or the absence of rat-liver S9. The mutagenic activity of acrolein, γ-butyrolactone, furfural and glycidol, chemicals usually found in these spirits, was assayed by the same procedure. Glycidol was mutagenic in TA1535 and TA100 without metabolic activation. We found higher and more frequently positive responses in home-made apple brandies than in the other beverages; therefore, further fractionation for isolation of the mutagenic compound(s) was performed by using spinning band column distillation, HPLC and gas chromatography. The fractions contained various types of mutagen, i.e., frameshift and/or base-pair substitution mutagens; some required metabolic activation and others did not in either the alcoholic, aqueous or non-volatile fractions. The results indicate that the high incidence of oesophageal cancer correlated with the alcoholic consumption in these areas might be at least partially attributable to the presence of mutagens in apple brandies.

The stereoisomeric composition of the 4-methyl-3-heptanol produced by Scolytus scolytus and the preparation and biological activity of the four synthetic stereoisomers

Racemic threo and erythro 4-methyl-3-heptanol, obtained from the commercial alcohol by fractional distillation using a spinning band column, were resolved by high-pressure liquid chromatographic separation of their (−)-MTPA diastereoesters. The biological activity of the four stereoisomers towards Scolytus scolytus was examined in a laboratory bioassay and by coupled gas chromatography-electroantennography. Antennae of both male and female S. scolytus responded to all the stereoisomers but stronger responses were given by both sexes to the (−)-threo and (−)-erythro stereoisomers than to the (+)-threo and (+)-erytho stereoisomers. Both male and female beetles responded to all the stereoisomers in the laboratory bioassay, there being no statistically significant differences in the degree of response to each isomer. These results are discussed in relation to the field response of S. scolytus to the stereoisomers. A method is also described for the determination of the stereoisomeric composition of natural 4-methyl-3-heptanol, starting with 0.5–5 μg of the alcohol. Male S. scolytus beetles from two distinct laboratory cultures were found to produce trace (−)-threo and (−)-erythro steroisomers of 4-methyl-3-heptanol, while females from one of the cultures produced trace quantities of the (−)-erythro stereoisomer only.

Application of high vacuum fractional distillation to complex mixtures of methyl esters of polyunsaturated fatty acids

AbstractA technique for the high vacuum fractional distillation, with a spinning band column, of methyl esters of polyunsaturated fatty acids employing a carrier of long chain acetates is described. The carrier is used to facilitate the fractionation of minor components and minimize artifact formation in mixtures of methyl esters containing up to six double bonds. The technique is demonstrated on a standard mixture of methyl esters and applied to a concentrate of unsaturated methyl esters containing a large number of minor components as well as methyl docosahexaenoate.

Preparation of Fluorocyclopropanes by Reductive Dechlorination of Chlorofluorocyclopropanes

Angewandte Chemie International Edition in EnglishVolume 6, Issue 7 p. 629-629 Communication Preparation of Fluorocyclopropanes by Reductive Dechlorination of Chlorofluorocyclopropanes† Priv.-Doz. Dr. M. Schlosser, Priv.-Doz. Dr. M. Schlosser Organisch-Chemisches Institut der Universität, Tiergartenstr., 69 Heidelberg (Germany)Search for more papers by this authorDipl.-Chem. G. Heinz, Corresponding Author Dipl.-Chem. G. Heinz Organisch-Chemisches Institut der Universität, Tiergartenstr., 69 Heidelberg (Germany)Organisch-Chemisches Institut der Universität, Tiergartenstr., 69 Heidelberg (Germany)Search for more papers by this author Priv.-Doz. Dr. M. Schlosser, Priv.-Doz. Dr. M. Schlosser Organisch-Chemisches Institut der Universität, Tiergartenstr., 69 Heidelberg (Germany)Search for more papers by this authorDipl.-Chem. G. Heinz, Corresponding Author Dipl.-Chem. G. Heinz Organisch-Chemisches Institut der Universität, Tiergartenstr., 69 Heidelberg (Germany)Organisch-Chemisches Institut der Universität, Tiergartenstr., 69 Heidelberg (Germany)Search for more papers by this author First published: July 1967 https://doi.org/10.1002/anie.196706291Citations: 6 † Dedicated to Professor G. Wittig on his 70th birthday AboutPDF ToolsRequest permissionExport citationAdd to favoritesTrack citation ShareShare Give accessShare full text accessShare full-text accessPlease review our Terms and Conditions of Use and check box below to share full-text version of article.I have read and accept the Wiley Online Library Terms and Conditions of UseShareable LinkUse the link below to share a full-text version of this article with your friends and colleagues. Learn more.Copy URL Share a linkShare onFacebookTwitterLinkedInRedditWechat No abstract is available for this article.Citing Literature Volume6, Issue7July 1967Pages 629-629 RelatedInformation

Three new oilseeds rich incis‐11‐eicosenoic acid

AbstractMarshallia cacspitosa Nutt. seed oil (family Compositae) contains 44%cis‐11‐eicosenoic acid, and is the first oil from the Compositae found to contain a high proportion of C20‐monoenoic acid. Seed oils ofAlyssum maritimum (L.) Lam. and ofSelenia grandis Martin (family Cruciferae) contain 42 and 58% of the same acid, respectively.The C20 acids from all three oils were obtained in nearly pure form by fractional distillation of the mixed methyl esters by means of a spinning band column. Permanganate‐periodate oxidation of the purified methyl esters yielded predominantly nonanoic and undecanedioic acids.

Head and Fraction Cutter for Small-Scale Spinning Band Column

Head and Fraction Cutter for Small-Scale Spinning Band Column

Vacuum distillation II: Performance of a Vigreux column and a spinning band column over a wide range of pressures

Performance figures referring to a 11 mm diameter Vigreux column and a 6 mm diameter spinning band column over a pressure range of about 0·13 kN/m 2–101·5 kN/m 2 (about 1–760 mm Hg) are presented. In order to gain an insight into the mechanisms of material transfer involved, analyses of separate vapour and liquid phase resistances were made. In the case of the Vigreux column it was found that liquid phase resistance was about half the total resistance at atmospheric pressure. A reduction in pressure causes the liquid phase resistance to be increased by increasing liquid viscosity on the one hand and to be decreased by the higher vapour rates on the other hand. These two compensating factors cause a total efficiency loss of the Vigreux column of about 25% when the pressure is reduced from atmospheric value to about 0·13 kN/m 2 (1 mm Hg). at this top pressure the maximum pressure drop along the Vigreux section is about 0·3 kN/m 2 (3–4 mm Hg) per metre. In a spinning band column the main resistance to material transfer is offered by the vapour phase. This resistance is reduced by creating turbulence through rotation of the spinning band. The present study disclosed the existance of two limiting values of rotational speed: a lower limit below which rotation does not yet cause turbulence, and a higher limit above which back mixing in the liquid phase causes the separating power to be independent of—or to decrease with—speed of rotation. Due to the fact that the extent to which turbulence can be effected in the vapour phase proves to depend on rotational speed and vapour density to the same degree, the sensitiveness to pressure variations of the spinning band column is rather great. Reduction of the pressure from atmospheric value to about 1·3 kN/m 2 (10 mm Hg) causes an efficiency loss of about 70%; in fact at this pressure the separating power of the spinning band column was not better than that of a wetted wall column of the same dimensions.

A spinning-band column for vacuum fractionation of fatty-acid esters

A spinning-band column which is specially adapted for the vacuum fractionation of fatty-acid esters is described. Plate-efficiency tests carried out at 760 mm. and in the range 3.0-0.5 mm. show that the lowest value for the H.E.T.P. is 2.64 cm. at atmospheric pressure, this value increasing at the lower pressures. Distillation curves for ester mixtures show that the column is very suitable for analytical ester fractionation at pressures of the order of 1 mm.

Studies of waxes. III. The alcohols of carnauba wax

SummaryA study has been made of the composition of the non‐saponifiable portion of carnauba wax by acetylation followed by fractionation in a spinning band column, using both simple fractional and amplified distillation. The straight chain alcohols of even carbon number, C24 to C34, were estimated to be present in the following percentages, below C24 : 1%, C24 (+C26 ?) : 4%, C28 : 5%, C30 : 14%, C32 : 51%, C34 : 22%. In addition, three high melting alcohols, totalling 2% of the wax alcohols, have been isolated and appear to be closely related glycols. The hydrocarbon fraction (M.P. 63.0–63.5°C.) forms less than 1% of the non‐saponifiable fraction and is considered to be a mixture.

Spinning band column for high vacuum fractionation

AbstractA fractionating column is described together with its ancillary equipment for operation at high vacuum (0·01–2·5 mm. of mercury). At atmospheric pressure the column is equivalent to 16‐6 theoretical plates, and under vacuum conditions at a boil‐up rate of it operates with a total pressure drop of only 0·04 mm.