Vacuum volatilization

A sample of the polymer prepared in toluene with BuLi at -78°C was heated to 350°C under vacuum. Volatile materials were obtained in 86% yield. More than 90% of the materials were the MMA monomer. 

Uranium tetrafluoride precipitated from aqueous solutions exists as UF4 5H20, and it is difficult to remove the waters of hydration so that the dry reaction above is preferred.) UF4 is frequently used to make accelerator targets of uranium by vacuum volatilization. 

Analysis of the vacuum volatile constituents of fresh tomatoes was carried out using capillary GLC-MS and packed column GLC separation with Infrared, NMR and CI-MS analysis. Evidence was obtained for the presence of the unusual components 3-damascenone, 1-nltro-2--phenylethane, 1-nltro-3-methylbutane, 3-cyclocltral and epoxy-3-1onone. A method for the quantitative analysis of the volatile aroma components In fresh tomato has been Improved and applied to fresh tomato samples. The quantitative data obtained have been combined with odor threshold data to calculate odor unit values (ratio of concentration / threshold) for 30 major tomato components. These calculations Indicate that the major contributors to fresh tomato aroma Include (Z)-3-hexenal, 3-lonone, hexanal, 3-damascenone, 1-penten-3-one, 3-methylbutanal, (E)-2-hexenal, 2-lso-butylthlazole, 1-nltrophenylethane and (E)-2-heptenal. 

Stevenson and Nettleton [71] studied the polycondensation of low-molecular-weight PET over the range 221—251°C in the presence of antimony trioxide catalyst (Table 5), essentially paralleling Challa s earlier research [68, 69, 70] on the uncatalysed reactions. The catalysed reactions were faster, but the rate coefficient for polycondensation was relatively low even though the reverse reaction had been taken into account. They considered that a vacuum-volatile constituent of the reaction mixture was responsible for deactivation of the catalyst, thus slowing the reaction. Antimony trioxide does not vigorously catalyse the polycondensation of the pure monomer, bis(2-hydroxyethyl)-terephthalate, and Stevenson and Nettleton concluded that the latter substance was responsible for the proposed deactivation of the catalyst. 

Since the difference in cost would be very large, there would be no difficulty in making a choice. However, just as defining boundaries between gases, liquids, and solids is a tenuous exercise in the face of considerations of vacuum, volatility, and thermal stability, so the choice of mass analyzer can become a difficult one. 

Since esterification is an equilibrium reaction, the treatment was performed using an excess of alcohol. The grafting of alcohols or diols was performed in an autoclave at 150°C. For PEG, special care was taken to avoid oxidation (outgassing of the silica/PEG mix and treatment under N2 in a sealed tube at 150°Q. In each case, the excess reagent was eliminated either by heat treatment under vacuum (volatile alcohols and diols), or by solvent extraction (THF) in a Soxhlet extractor. 

Vacuum Volatile products released from the reactant are lost most easily during reactions in vacuum. No corrections are required for sample buoyancy or atmosphere flow. However, the absence of convective heating reduces the rates of heat movement and may introduce uncertainties into measured reactant temperatures. The effect of product availability on rates of reversible reactions is reduced, but, at least in some of these reactions,... 

A review and some new results on the thermal degradation of poly-p-xylylene have been presented by Jellinek and Lipovac [303]. Little volatile material is formed but appreciable amounts of dimer, trimer, tetramer and pentamer were isolated. Typical vacuum volatilization curves are given in Fig. 73. It has been proposed that the mechanism consists of random chain scission at abnormal structures in the chain, followed by a depropagation reaction resulting in low molecular weight polymer but very little monomer. 

Samples of gases and volatile liquids can be introduced directly into the ionization chamber. Because the interior of a mass spectrometer is kept at a high vacuum, volatile liquids and even some solids are vaporized. For less volatile liquids and solids, the sample may be placed on the tip of a heated probe that is then inserted directly into the ionization chamber. Another extremely useful method for introducing a sample into the ionization chamber is to link a gas chromatograph (GC) or liquid chromatograph (LC) directly to the mass spectrometer. These machines can separate complex mixtures of molecules into pure firactions. Each firaction eluted firom the chromatograph enters directly into the ionization chamber of the mass spectrometer, enabling mass determination of the individual components. 

Preparation of films for sufficiently volatile molecules can also be perfonned by evaporating tire molecules in vacuum (gas-phase deposition) or by tire use of a desiccator which contains tire substrate and tire dilute solution in a vessel separately and which is evacuated to 0.1 mbar and kept under vacuum for several hours ( 24 h). This also results in a vapour-phase-like deposition of tire molecules onto tire substrates. 

D. Now the ether will be a deep reddish yellow. Distill off the ether...quack...and take the temp up to 170 C to drive off any other volatiles. Should recover 90%+ of the original weight of oil. Now add 500 ml of saturated bisulfite and stir for 1.5 hours...Quack Vacuum Filter, the duck fat crystals Wash with water and ether, yield dull fine ppt in the filter cake...stable bisulfite addition product...can be stored forever...QuackU Yield -50 to 80% depending on a ducks technique ... 

The main difference between field ionization (FI) and field desorption ionization (FD) lies in the manner in which the sample is examined. For FI, the substance under investigation is heated in a vacuum so as to volatilize it onto an ionization surface. In FD, the substance to be examined is placed directly onto the surface before ionization is implemented. FI is quite satisfactory for volatile, thermally stable compounds, but FD is needed for nonvolatile and/or thermally labile substances. Therefore, most FI sources are arranged to function also as FD sources, and the technique is known as FI/FD mass spectrometry. 

Liquids examined by FAB are introduced into the mass spectrometer on the end of a probe inserted through a vacuum lock in such a way that the liquid lies in the target area of the fast atom or ion beam. There is a high vacuum in this region, and there would be little point in attempting to examine a solution of a sample in one of the commoner volatile solvents such as water or dichloromethane because it would evaporate extremely quickly, probably as a burst of vapor when introduced into the vacuum. Therefore it is necessary to use a high-boiling solvent as the matrix material, such as one of those listed in Table 13.1. 

Of course, some substances are sufficiently volatile that a heated inlet line can be used to get them into a mass spectrometer. Even here, there are practical problems. Suppose a liquid or solid is sufficiently volatile, that heating it to 50°C is enough to get the vapor into the mass spectrometer through a heated inlet line. If the mass spectrometer analyzer is at 30°C, there is a significant possibility that some of the sample will condense onto the inner walls of the spectrometer and slowly vaporize from there. If the vacuum pumps cannot remove this vapor quickly, then the mass... 

DeodoriZation. Removal of volatile odorous material and residual fatty acids is the final step ki ok processkig prior to packagkig or filling for bulk shipment (28). The ok is heated to 230—260°C under vacuum. Steam is passed through the ok to assist ki carrying over the volatile material. 

Deodorization can be carried out ki batch, continuous, or semicontkiuous systems. Figure 4 shows a typical design for a semicontkiuous deodorizer. The heated ok is passed through a series of trays under vacuum. Steam is passed through the ok through a steam sparge ki the bottom of the tray. Volatiles are carried through the headspace and condensed. In addition to fatty acids and compounds responsible for odor, some tocopherols and sterols are also distilled kito the condensate. The amount of tocopherols distilled depends on deodorization temperature and vacuum. 

Continuous deaeration occurs when the viscose is warmed and pumped into thin films over cones in a large vacuum tank. The combination of the thinness of the Hquid film and the dismption caused by the boiling of volatile components allows the air to get out quickly. Loss of water and CS2 lower the gamma value and raise the cellulose concentration of the viscose slightly. Older systems use batch deaeration where the air bubbles have to rise through several feet of viscose before they are Hberated. 

Molybdenum hexafluoride [7783-77-9] MoF, is a volatile liquid at room temperature. It is very moisture sensitive, hydrolysing immediately upon contact with water to produce HF and molybdenum oxyfluorides. MoF should therefore be handled in a closed system or in a vacuum line located in a chemical hood. The crystals possess a body-centered cubic stmcture that changes to orthorhombic below —96° C (1,2). The known physical properties are Hsted in Table 1. 

Vacuum Outgassing and Permeability. Under vacuum, modified ethylene—tetrafluoroethylene copolymers give off Htde gas at elevated temperatures. The loss rate is about one-tenth of the acceptable maximum rates for spacecraft uses. Exposing 750-pm specimens for 24 h at 149°C to a high vacuum results ia a maximum weight loss of 0.12% volatile condensible material is less than 0.02%. 

Concentration and Aroma Recovery. Concentration of juice from deciduous fmit is best carried out using an evaporator that causes as httle thermal degradation as possible and that permits recovery of volatile materials important to the aroma of the fresh fmit, ie, essence. Evaporators that use a high temperature for a short time and operate under a vacuum, such as the APV Crepaco falling film plate evaporator or the Alfa Laval centrifugal... 

Use of ultrafiltration (UF) membranes is becoming increasingly popular for clarification of apple juice. AH particulate matter and cloud is removed, but enzymes pass through the membrane as part of the clarified juice. Thus pasteurization before UF treatment to inactivate enzymes prevents haze formation from enzymatic activity. Retention of flavor volatiles is lower than that using a rack-and-frame press, but higher than that using rotary vacuum precoat-filtration (21). 

Thermal Cracking. In addition to the gases obtained by distillation of cmde petroleum, further highly volatile products result from the subsequent processing of naphtha and middle distillate to produce gasoline, as well as from hydrodesulfurization processes involving treatment of naphthas, distillates, and residual fuels (5,61), and from the coking or similar thermal treatment of vacuum gas oils and residual fuel oils (5). 

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