Volume of solvent

Dinitrophenylhydra2ones usually separate in well-formed crystals. These can be filtered at the pump, washed with a diluted sample of the acid in the reagent used, then with water, and then (when the solubility allows) with a small quantity of ethanol the dried specimen is then usually pure. It should, however, be recrystallised from a suitable solvent, a process which can usually be carried out with the dinitrophenylhydrazones of the simpler aldehydes and ketones. Many other hydrazones have a very low solubility in most solvents, and a recrystallisation which involves prolonged boiling with a large volume of solvent may be accompanied by partial decomposition, and with the ultimate deposition of a sample less pure than the above washed, dried and unrecrystal-lised sample. 

If a small Beckmann thermometer, similar to that used in the Sucharda-Bobranski method (p. 442) is available, the above method can be readily modified by replacing the tube T (Fig. 79) by an ordinary small boiling-tube without the side-arm A. The thermometer B and the stirrer S are fitted as in Fig. 79. The volume of solvent (usually ca 5 ml.) must of course cover the bulb of the thermometer. 

Hence one extraction with 100 ml. of benzene removes 3 0 g. (or 75 per cent.) of the n-butyric acid, whilst three extractions remove 3 5 g. (or 87-5 per cent.) of the total acid. This clearly shows the greater efficiency of extraction obtainable with several extractions when the total volume of solvent is the same. Moreover, the smaller the distribution coefficient between the organic solvent and the water, the larger the number of extractions that will be necessary. 

Synthesis by high-dilution techniques requires slow admixture of reagents ( 8-24 hrs) or very large volumes of solvents 100 1/mmol). Fast reactions can also be carried out in suitable flow cells (J.L. Dye, 1973). High dilution conditions have been used in the dilactam formation from l,8-diamino-3,6-dioxaoctane and 3,6-dioxaoctanedioyl dichloride in benzene. The amide groups were reduced with lithium aluminum hydride, and a second cyclization with the same dichloride was then carried out. The new bicyclic compound was reduced with diborane. This ligand envelops metal ions completely and is therefore called a cryptand (B. Dietrich, 1969). 

Temp., °C Unit Volume of Solvent Temp., °C Unit Volume of Solvent ... 

Many continuous extractions involving solid samples are carried out with a Soxhiet extractor (Figure 7.18). The extracting solvent is placed in the lower reservoir and heated to its boiling point. Solvent in the vapor phase moves upward through the tube on the left side of the apparatus to the condenser where it condenses back to the liquid state. The solvent then passes through the sample, which is held in a porous cellulose filter thimble, collecting in the upper reservoir. When the volume of solvent in the upper reservoir reaches the upper bend of the return tube, the solvent and any extracted components are siphoned back to the lower reservoir. Over time, the concentration of the extracted component in the lower reservoir increases. 

The experiment we have just described is not very satisfactory from a practical point of view, since it is very difficult to deposit a thin layer of solution between two bulk portions of solvent without some mixing. An experimentally more convenient method consists of layering equal volumes of solvent and solution so that a sharp boundary exists between them at x = 0, with c = Cq for... 

To use GPC for molecular weight determination, we must measure the volume of solvent that passes through the column before a polymer of particular molecular weight is eluted. This quantity is called the retention volume Vj. Figure 9.14 shows schematically the relationship between M and Vj it is an... 

The specifications set the maximum vol % of solvent that may be added to the cylinder shell (measured by its water capacity). The volume of solvent also varies with the capacity of the cylinder. Cylinders in the 90—92% porosity range with a capacity above 9.1 kg of water may contain a maximum acetone charge of 43.4%, whereas those with 9.1 kg or less water capacity may contain up to 41.8 vol %. The first category of cylinders are normally referred to as welding cylinders and the latter as small tanks (those with 0.28 and 1.12 m acetylene capacity). 

The use of fixed bed catalysts is described in several patents (33—37). Methods of operation include upflow, trickle bed, and even vapor phase. Typically, a large volume of solvent is used to moderate the temperature rise associated with the high heat of reaction for nitro group reduction. 

Liquid sulfur dioxide expands by ca 10% when warmed from 20 to 60°C under pressure. Pure liquid sulfur dioxide is a poor conductor of electricity, but high conductivity solutions of some salts in sulfur dioxide can be made (216). Liquid sulfur dioxide is only slightly miscible with water. The gas is soluble to the extent of 36 volumes pet volume of water at 20°C, but it is very soluble (several hundred volumes per volume of solvent) in a number of organic solvents, eg, acetone, other ketones, and formic acid. Sulfur dioxide is less soluble in nonpolar solvents (215,217,218). The use of sulfur dioxide as a solvent and reaction medium has been reviewed (216,219). 

The performance of the dmg dehvery system needs to be characterized. The rate of dmg release and the total amount of dmg loaded into a dmg dehvery system can be deterrnined in a dissolution apparatus or in a diffusion ceU. Typically, the dmg is released from the dmg dehvery system into a large volume of solvent, such as water or a buffer solution, that is maintained at constant temperature. The receiver solution is weU stirred to provide sink conditions. Samples from the dissolution bath are assayed periodically. The cumulative amount released is then plotted vs time. The release rate is the slope of this curve. The total dmg released is the value of the cumulative amount released that no longer changes with time. 

If the sample is relatively insoluble in the mobile phase, then it can be dissolved, as a dilute solution, in a relatively large volume of solvent. A large volume of the solution can then be placed on the column, a procedure that results in volume overload. 

Inhibited THF is problematic for semipreparative separations. Because small quantities of polymer are being collected along with larger volumes of solvent, more inhibitor, usually butylated hydroxytoluene (BHT), than sample is often collected in each fraction. Thus, one must carefully consider if the BHT will cause a problem in the subsequent analysis of the isolated fractions. If it does, uninhibited THF or other alternate solvents should be used. It must be remember that if uninhibited THF is used, the analyst must pay careful attention to the inevitable peroxide formation in the solvent/fractions. 

Together with this solvent effect, another effect, called phase soaking, occurs in the retention gap technique if a large volume of solvent vapour has saturated the carrier gas, the properties of the stationary phase can be altered by swelling (thicker apparent film), a change in the viscosity or changed polarity. The consequence is that the column shows an increased retention power, which can be used to better retain the most volatile components. 

The removal of a large volume of solvent prior to distillation or crystallization is frequently necessary. If the solvent and product have similar boiling points (within 75"), careful fractional distillation of the entire solution is required. In other cases, the solvent may be removed by boiling on a steam bath, by rapid distillation at atmospheric pressure, or on a rotary evaporator. The rotary evaporator, used under aspirator pressure in conjunction with a heated water bath, allows rapid removal of most solvents boiling up to about 12071 atm (Fig. A3.12a). The presence of a thin film of liquid on the... 

Sodium methylete is mede by dropping 11.7 g of sodium strips into 199 ml of absolute methanol in a 1-liter three-necked flask. 93.9 g of o-benzylphenol ere dissolved in 200 ml of dry toluene end added to the sodium methylete solution. The solution is distilled until the boiling point of toluene is reached. At the end of the distillation, enough toluene is added to restore the original volume of solvent. 

Since the alcohol has a relatively high solubility in petroleum ether, the yield from the crystallization depends on the volume of solvent used. However, by concentrating the mother liquor the overall yield from the first and second crops of crystals varies from 74% to 94%. 

For reagent solutions as defined above (i.e. 1) it is usually sufficient to weigh out approximately the amount of material required, using a watchglass or a plastic weighing container, and then to add this to the required volume of solvent which has been measured with a measuring cylinder. 

Polar organic solvents readily precipitate exopolysaccharides from solution. The solvents commonly used are acetone, methanol, ethanol and propan-2-ol. Cation concentration of the fermentation liquor influences the amount of solvent required for efficient product recovery. In the case of propan-2-ol, increasing the cation concentration can lead to a four-fold reduction in die volume of solvent required to precipitate xanthan gum. Salts such as calcium nitrate and potassium chloride are added to fermentation broths for this purpose. 

Further reduction in the volume of solvent required can be achieved by heat treatment of the exopolysaccharide at 100-130°C for 1-15 minutes before solvent precipitation. 

The main disadvantage of precipitation with a polar (water-soluble) solvent is the need for a costly distillation stage to recover the relatively laige volumes of solvent used. Another disadvantage is the precipitation of proteins, salts and, in some cases, pigments which reduces the purity and leads to discoloration of the product. To overcome these problems, precipitation using less polar solvents, such as methylethylketone, has been proposed. Only 23% (w/v) methylethylketone is sufficient to saturate the aqueous phase and precipitate exopolysaccharides quantitatively. 

We now press in the piston 1 so that a mol of solute goes out of the Yi space into the V2 space across the plane of contact, at the same time allowing the piston 2 to move out so that the requisite volume of solvent enters and the concentrations are unaltered. The work done is... 

A solution prepared from Mo202L4 (concentration 2C, where L = Et2NCSe2) in 1,2-dichloroethane was mixed with the same volume of solvent. The absorbance of the solution decreased exponentially. Use the following linear equation of k2 against C to calculate the rate constants ... 

The product can also be recrystallized from ethanol, but a substantially larger volume of solvent is required. 

The crude solid is readily dissolved in a smaller amount of solvent, but employing the indicated volumes is recommended in order to achieve better yields of recrystallization. With this volume of solvent, heating at 74°C is sufficient to have complete solubilization of the solid. 

Because molarity is defined in terms of the volume of the solution, not the volume of solvent used to prepare the solution, the volume must be measured after the solutes have been added. The usual way to prepare an aqueous solution of a solid substance of given molarity is to transfer a known mass of the solid into a volumetric flask, dissolve it in a little water, fill the flask up to the mark with water, and then mix the solution thoroughly by tipping the flask end over end (Fig. G.8I. 

It is seen that, although the dimensions and particle sizes may not be precisely matched, all three columns are of a size closely similar to those commercially available with, perhaps, the exception of the long high efficiency column. The small 3 cm column is excellent for the preliminary assessment of a sample. As a result of its size it does not use large volumes of solvent and can be quickly reconditioned after a separation in readiness for the next run. It is very convenient for choosing the best phase system in method development. The other columns would be chosen on a basis of the efficiency required to separate the critical pair in the reduced chromatogram of the sample for analysis. 

Reference standards can be used in two ways a weighed amount of the standard can be added directly to the sample and the area of the peaks of interest compared with that of the standard alternatively, a weighed amount of the standard can be made up in a known volume of solvent, a sample placed on the column and chromatographed under exactly the same conditions as the original sample. The peak area... 

To remove any metallic Au, the reaction mixture is evaporated to dryness and subsequently passed over a commercial terra infusorii column in a minimal volume of solvent. Crystallization may be performed by slow diffusion of a two-layer system. Yields are low (10-60%). The metal evaporation technique (see 8.2.1.2) gives higher yields than the sodium borohydride method. 

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