Volatile materials

Carius tube A thick-walled glass lube originally used in the Carius method but used in any reaction involving volatile materials. 

It is possible to modify the quality of the coke by calcination at high temperatures (1200-1400°C) this has the effect of reducing the volatile material and to increase the density. 

Sand. Buckets of dry sand for fire-extinguishing should be available in the laboratory and should be strictly reserved for this purpose, and not encumbered with sand-baths, waste-paper, etc. Most fires on the bench may be quickly smothered by the ample use of sand. Sand once used for this purpose should always be thrown away afterwards, and not returned to the buckets, as it may contain appreciable quantities of inflammable, non-volatile materials e.g., nitrobenzene), and be dangerous if used a second time. 

A set-up for distillation under reduced pressure is shown in Fig. 11,60,3 it is generally more convenient to use a Kon receiver or a Perkin triangle (Fig. 11, 56, 31). The vessel at the side, connected to the assembly by rubber pressure tubing, may be immersed in a Dry Ice-acetone bath and serves as a trap for volatile materials. 

Sample Preservation Without preservation, many solid samples are subject to changes in chemical composition due to the loss of volatile material, biodegradation, and chemical reactivity (particularly redox reactions). Samples stored at reduced temperatures are less prone to biodegradation and the loss of volatile material, but fracturing and phase separations may present problems. The loss of volatile material is minimized by ensuring that the sample completely fills its container without leaving a headspace where gases can collect. Samples collected from materials that have not been exposed to O2 are particularly susceptible to oxidation reactions. For example, the contact of air with anaerobic sediments must be prevented. 

In volatilization gravimetry, thermal or chemical energy is used to decompose the sample containing the analyte. The mass of residue remaining after decomposition, the mass of volatile products collected with a suitable trap, or a change in mass due to the loss of volatile material are all gravimetric measurements. 

There are ill-defined limits on EI/CI usage, based mostly on these issues of volatility and thermal stability. Sometimes these limits can be extended by preparation of a suitable chemical derivative. For example, polar carboxylic acids generally give either no or only a poor yield of molecular ions, but their conversion into methyl esters affords less polar, more volatile materials that can be examined easily by EL In the absence of an alternative method of ionization, EI/CI can still be used with clever manipulation of chemical derivatization techniques. 

These effects of differential vapor pressures on isotope ratios are important for gases and liquids at near-ambient temperatures. As temperature rises, the differences for volatile materials become less and less. However, diffusion processes are also important, and these increase in importance as temperature rises, particularly in rocks and similar natural materials. Minerals can exchange oxygen with the atmosphere, or rocks can affect each other by diffusion of ions from one type into another and vice versa. Such changes can be used to interpret the temperatures to which rocks have been subjected during or after their formation. 

Gases and volatile materials can be swept into the center of an argon plasma flame, where they are fragmented into ions of their constituent elements. The m/z values of ions give important information for identification of the elemental composition of a sample, and precise measurement of ion abundances is used to provide accurate isotope ratios. 

Compounds having low vapor pressures at room temperature are treated in water-cooled or air-cooled condensers, but more volatile materials often requite two-stage condensation, usually water cooling followed by refrigeration. Minimising noncondensable gases reduces the need to cool to extremely low dew points. Partial condensation may suffice if the carrier gas can be recycled to the process. Condensation can be especially helpful for primary recovery before another method such as adsorption or gas incineration. Both surface condensers, often of the finned coil type, and direct-contact condensers are used. Direct-contact condensers usually atomize a cooled, recirculated, low vapor pressure Hquid such as water into the gas. The recycle hquid is often cooled in an external exchanger. 

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. 

Essential Oil The volatile material, derived by a physical process, usually distillation, from odorous plant material of a single botairical form and spices with which it agrees in name and odor. 

Fluorocarbons are made commercially also by the electrolysis of hydrocarbons in anhydrous hydrogen fluoride (Simons process) (14). Nickel anodes and nickel or steel cathodes are used. Special porous anodes improve the yields. This method is limited to starting materials that are appreciably soluble in hydrogen fluoride, and is most useflil for manufacturing perfluoroalkyl carboxyflc and sulfonic acids, and tertiary amines. For volatile materials with tittle solubility in hydrofluoric acid, a complementary method that uses porous carbon anodes and HF 2KF electrolyte (Phillips process) is useflil (14). 

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... 

Open-Arc Furnaces. Most of the open-arc furnaces are used in melting and refining operations for steel and iron (Fig. 1). Although most furnaces have three electrodes and operate utilizing three-phase a-c power to be compatible with power transmission systems, d-c furnaces are becoming more common. Open-arc furnaces are also used in melting operations for nonferrous metals (particularly copper), slag, refractories, and other less volatile materials. 

The high lead slag from the smelting furnace is tapped continuously and transferred down a heated launder directly into the reduction furnace through a port in the side of the vessel. Lump coal for reduction is fed continuously to the furnace by conveyor and dropped direcdy into the bath. Heating for the endothermic reduction reactions is provided by oil injected down the lance. The combustion air stoichiometry is set at 95% of that required for complete oil combustion. Air is injected into the top of the furnace to afterbum the volatile materials from the coal and provide additional heat to the top of the furnace. Reduction temperatures range from 1170 to 1200°C to maintain slag duidity. 

Solvent extraction followed by gas chromatographic analysis is used to determine paraffin wax antioxidants (qv), ie, butylated hydroxyanisole and butylated hydroxytoluene and other volatile materials. Trace amounts of chlorinated organic compounds, eg, polychlorinated biphenyls, can be deterrnined by using a gas chromatograph with an electron-capture detector (22). 

Concretes and absolutes, both obtained by total extraction of the plant material and not subject to any form of distillation other than solvent removal, are complex mixtures containing many chemical types over wide molecular weight ranges. In some cases, gas chromatographic analysis shows httle volatile material. Yet these products have powerful odors and contribute in important ways to the perfumes in which they are used. 

A residuum, often shortened to resid, is the residue obtained from petroleum after nondestmctive distillation has removed all the volatile materials. The temperature of the distillation is usually below 345°C because the rate of thermal decomposition of petroleum constituents is substantial above 350°C. Temperatures as high as 425°C can be employed in vacuum distillation. When such temperatures are employed and thermal decomposition occurs, the residuum is usually referred to as pitch. By inference, the name is used in the same manner as when it refers to the nonvolatile residue from the thermal decomposition of coal tar (3). 

Distillation. This is the point at which refining begins and was the first method by which petroleum was refined. Originally, distillation (qv) involved a batch operation in which the stiU was a cast-iron vessel mounted on brickwork over a fire and the volatile materials were passed through a pipe or gooseneck which led from the top of the stiU to a condenser. The latter was a coil of pipe, or a "worm" (hence the expression worm end products), immersed in a tank of miming water. 

Chemicals responsible for odor in some PUR foams were synthesised by polymerisation of PO in CH2CI2 with Bp2(C2H )20 catalyst (114). The yield was 25% volatile material and 75% polymeric material. The 25% fraction consisted of dimethyldioxane isomers, dioxolane isomers, DPG, TPG, crown ethers, tetramers, pentamers, etc, and 2-ethy1-4,7-dimethyl-1,3,6-trioxacane (acetal of DPG and propionaldehyde). The latter compound is mainly responsible for the musty odor found in some PUR foams. This material is not formed under basic conditions but probably arises during the workup when acidic clays are used for catalyst removal. 

Moderately Volatile Ma.teria.ls, For moderately volatile materials, such as the amines commonly used in feedwater and boiler water chemical treatment, the distribution ratios vary from 0.1 to 30 for gases, the ratios are much higher. The distribution ratios of amines and organic acids are generally temperature-dependent. The distribution ratios for ammonia [7664-41-7] morpholine [110-91-8] and acetic acid [64-19-7] are shown in Figure 16 as examples. 

Asphalts develop an internal stmcture with age, steric hardening (3), in which viscosity can increase upon aging without any loss of volatile material (73,83). Those with a particularly high degree of gel stmcture exhibit thixotropy. 

Redistillation does not gready reduce the impurity level of volatile materials such as magnesium. Volatile alkaH metals can be separated from calcium by passing the vapors over refractory oxides such as or Cr202 to form the nonvolatile Na20 and K O (14). Purification techniques include... 

The simplest analytical procedure is to oxidize a sample in air below the fusion point of the ash. The loss on ignition is reported as graphitic carbon. Refinements are deterrninations of the presence of amorphous carbon by gravity separation with ethylene bromide, or preferably by x-ray diffraction, and carbonates by loss of weight on treating with nitric acid. Corrections for amorphous carbon and carbonates are appHed to the ignition data, but loss of volatile materials and oxidation may introduce errors. 

Graphite is frequently, although incorrectly, analyzed by the proximate method used for coal in which the volatile material is deterrnined by strongly beating the sample in a covered or luted cmcible. Some oxidation of the graphite always occurs so that the value obtained for volatile matter is high and thus the "fixed carbon" is too low. The method lacks both accuracy and precision. 

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