Pure compounds melting point

Nitroisobutylglycerine for nitrating purposes should have a melting point not lower than 150°C (the pure compound melts at 164-165°C). 

A solution of 3-acetamino-adamantane-l-carboxylic acid (3.0 g) in 4 N sodium hydroxide (40 ml) was refluxed for 5 h. After cooling, the pH of the solution was adjusted to 7 with acetic acid. The crystalline precipitate was filtered off, washed with ethanol and dried to yield 2.20 g of the desired compound, melting point over 330°C. In order to purify the compound, 2.0 g of it was suspended in water (10 ml), 4 N NaOH (2 ml) was added, and the resulting solution filtered through a filter aid known under the registered trademark Dicalite. The filtrate was adjusted to a pH of 6.5 with acetic acid. The resulting crystalline precipitate was filtered off, washed with a little water followed by alcohol, and dried to yield 1.55 g of pure 3-amino-adamantane-l-carboxylic acid. 

Either lithium carbonate (or other lithium compounds) or lithium mineral concentrates may be used as the lithium source in many types of glass, with several of the pure ore melting points being spodumene 1423°C, eucryptite 1397°C and... 

Pure hydrazine is a colourless liquid, melting point 275 K, and boiling point 387 K. It is surprisingly stable for an endothermic compound = -i- 50.6 kJ mol ). Each nitrogen atom has a lone pair of electrons and either one or both nitrogen atoms are able to accept protons to give and the less stable... 

Checking the Purification. The purity of the dry re-crystallised material must now be determined, as it is possible that repeated recrystallisation may be necessary to obtain the pure material. The purity is therefore checked by a melting-point determination, and the recrystallisation must be repeated until a sharp melting-point is obtained. Should the compound have no well-defined melting-point e.g.y the salt of an organic acid or base), it must be analysed for one suitable component element, until its analysis agrees closely with that theoretically required. 

Decolorisation by Animal Charcoal. It sometimes hap pens (particularly with aromatic and heterocyclic compounds) that a crude product may contain a coloured impurity, which on recrystallisation dissolves in the boiling solvent, but is then partly occluded by crystals as they form and grow in the cooling solution. Sometimes a very tenacious occlusion may thus occur, and repeated and very wasteful recrystallisation may be necessary to eliminate the impurity. Moreover, the amount of the impurity present may be so small that the melting-point and analytical values of the compound are not sensibly affected, yet the appearance of the sample is ruined. Such impurities can usually be readily removed by boiling the substance in solution with a small quantity of finely powdered animal charcoal for a short time, and then filtering the solution while hot. The animal charcoal adsorbs the coloured impurity, and the filtrate is usually almost free from extraneous colour and deposits therefore pure crystals. This decolorisation by animal charcoal occurs most readily in aqueous solution, but can be performed in almost any organic solvent. Care should be taken not to use an excessive quantity... 

The general case of two compounds forming a continuous series of solid solutions may now be considered. The components are completely miscible in the sohd state and also in the hquid state. Three different types of curves are known. The most important is that in which the freezing points (or melting points) of all mixtures lie between the freezing points (or melting points) of the pure components. The equilibrium diagram is shown in Fig. 7, 76, 1. The hquidus curve portrays the composition of the hquid phase in equihbrium with sohd, the composition of... 

The student should read Sections 1,10 to 1,16 carefully before commencing any experimental work. A supply of melting point capillaries is prepared as described in Section 11,10 (compare Fig. 77, R , I). The apparatus illustrated in Fig. 77. 10, 2, a is assembled with concentrated sulphuric acid as the bath liquid the thermometer selected should have a small bulb. The melting points of pure samples of the following compounds are determined in the manner detailed in Section 11,10 —... 

Determine the melting point of pure cinnamic acid (133°) and pure urea (133°). Intimately mix approximately equal weights (ca. 01 g.) of the two finely-powdered compounds and determine the melting point a considerable depression of melting point will be observed. Obtain an unknown substance from the demonstrator and, by means of a mixed melting point determination, discover whether it is identical with urea or cinnamic acid. 

Determination of the physical constants and the establishment of the purity of the compound. For a solid, the melting point is of great importance if recrystalhsation does not alter it, the compound may be regarded as pure. For a hquid, the boiling point is first determined if most of it distils over a narrow range (say, 1-2°), it is reasonably pure. (Constant boUing point mixtures, compare Section 1,4, are, however known.) The refractive index and the density, from which the molecular refractivity may be calculated, are also valuable constants for liquids. 

Optically Inactive Chiral Compounds. Although chirality is a necessary prerequisite for optical activity, chiral compounds are not necessarily optically active. With an equal mixture of two enantiomers, no net optical rotation is observed. Such a mixture of enantiomers is said to be racemic and is designated as ( ) and not as dl. Racemic mixtures usually have melting points higher than the melting point of either pure enantiomer. 

The modification shows that the transition temperature may vary significantly from those stated above and in general shift to higher temperatures as the gas pressure in the synthesis process increases. The transition from one zone to the next is not abmpt, but smooth. Hence, the transition temperatures should not be considered as absolute but as guidelines. Furthermore, not all zones are found in all types of deposit. For example. Zone T (see Fig. 7) is not prominent in pure metals, but becomes more pronounced in complex alloys, compounds, or in deposits produced at higher gas pressures. Zone 3 is not often seen in materials with high melting points. 

Properties and Reactions. Amine boranes are usually colodess, crystalline compounds, which exhibit sharp melting points and thermal stability when pure. Primary and secondary amine boranes are generally soHds at ambient temperatures. With the exception of trimetbylamine borane, the ahphatic /-amine boranes are Hquids. The nature of the bonding in amine boranes has been the subject of theoretical investigations (21—23). 

Basic pure component constants required to characterize components or mixtures for calculation of other properties include the melting point, normal boiling point, critical temperature, critical pressure, critical volume, critical compressibihty factor, acentric factor, and several other characterization properties. This section details for each propeidy the method of calculation for an accurate technique of prediction for each category of compound, and it references other accurate techniques for which space is not available for inclusion. 

The viscous magnesium compound formed is cautiously decomposed with dilute acetic acid (75 cc. in 300 cc. of water), the flask being cooled under the tap. Two clear layers are formed, and after separation, the aqueous layer is extracted with 100 cc. of ether, the combined ethereal solution is washed with water and dried with sodium sulfate, and the ether is distilled on the steam bath. The residue is distilled vmder reduced pressure. After a small fore-run the temperature rapidly rises to 130 at 10 mm. when the pure tricarbethoxymethane begins to distil. The yield of material collected over a five-degree interval is 204-215 g. (88-93 per cent of the theoretical amount). The product solidifies at 25°. The melting point of the pure substance is 28-29°. 

The melting point of this compound is ill-defined by reason of considerable darkening and shrinking that start at 175. The product thus obtained is sufficiently pure for use in further reactions. ... 

Vanillin forms fine white" needles melting at 81° to 82°, or when. absolutely pure at 82° to 84°, and possessing an intense vanilla odour. Some of the cheaper commercial samples are heavily adulterated with the quite odourless compound, acetanilide. The effect of this body is to lower the melting-point even if present in large quantity, but it is very easily detected, as by boiling with solution of potash, aniline is formed. 

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