Laboratory manual crystal growth


















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Photostability chambers provide high intensity lighting for pharmaceutical stability studies conducted under ICH guidelines. Each shelf has a light array that combines black and cool white fluorescent bulbs to satisfy the ICH definition for Option 2 lighting. Sometimes, forgetting something is just as important as remembering it.

Unimportant memories take up space that could be better utilized to collect newer, more useful information. The details of memory formation are not well understood, although it is expected that An adult human brain contains approximately 86 billion neurons, along with about 85 billion non-neuronal cells.

All those cells work together to manage motor control, sensory perception, heart rate, breathing, and more.

While the human brain is extremely complex, with The average global life expectancy was This value has soared in recent decades; for example, the average worldwide life expectancy in was only 48 years.

Most of this increase is credited to vast improvements in public health. Crystallization is the process of forming solid material from a liquid solution or melt, where the solid material formed has crystalline as opposed to amorphous structure.

A crystallization process generally has the following characteristics:. The feed material is either in solution or is a liquid above the melting point of the solid phase. If in solution, there may be more than one solvent present.

There may be dissolved or solid impurities present. Some impurities may have very similar properties to the solute especially for side-products from organic reactions. During crystallization, impurities may remain in solution, crystallize separately, or incorporate in some way into the product crystals. The waste stream from the process is liquid, containing both residual dissolved product and impurities. Operates at a lower temperature and with lower energy requirements than corresponding distillation separations.

Process kinetics are more complex and less well-understood than some alternatives; obtaining detailed kinetic parameters involves complex experimental procedures. Crystallization is used industrially in a wide variety of processes. Typical applications include bulk chemicals, such as salt, sugar and fertilizers; high value-added products such as specialty chemicals and pharmaceuticals; and difficult separations such as ortho- and para-xylene.

Crystallization processes relating to a single crystal and to multiple crystals in vessels are discussed below while typical equipment used for crystallization are dealt with in a separate article on Crystallizers. A crystal is a solid regular lattice of atoms, ions or molecules, formed by replicating a unit cell.

These lattices can be categorized by symmetry into a number of crystal systems: regular, tetragonal, orthorhombic, monoclinic, trigonal, triclinic and hexagonal. The shape or habit of a crystal is defined by the faces of the crystal, which can align in different ways with the crystal lattice.

The overall shape of a crystal is defined by the rate at which the various faces grow; the fastest growing faces disappear, leaving the slowest growing faces to dominate. Lattices can also have a range of defects. These can form sites for rapid crystal growth and, in some cases, are the dominant means for crystal growth. The driving force for both the formation of new crystals and the growth of existing ones is supersaturation.

This arises from the concentration of solute exceeding the equilibrium saturation solubility concentration. Now that you have finished the solubility tests, how do you decide which solvent to use for your recrystallization? The ideal solvent is one in which your compound is insoluble at room temperature but soluble at the boiling point. Remember, at room temperature, naphthalene was soluble in both toluene and acetone, so neither of these will work. After heating, naphthalene remained insoluble in water, even at the boiling point.

This means that ethanol is the solvent of choice. It dissolves the sample at its boiling point but not at room temperature. Now that we have decided on a solvent, it is time to dissolve the sample in some hot ethanol. Get ready by heating some ethanol in the water bath. Remember to add some boiling stones and clamp the flask securely so that it doesn't tip over.

Place the sample in an Erlenmeyer flask. But before adding solvent, it is a good idea to set aside a small crystal. It may come in handy later if you have trouble getting crystals to form. When dissolving your sample, use a minimal amount of hot solvent. This will ensure a good recovery of crystals in the end.

Add hot solvent in small amounts, swirling and heating in between each addition until the sample just dissolves. If it won't dissolve, it's probably an impurity. Take a close look at the solution. Is it the right color? For example, if you're expecting white crystals and your solution is yellow, then there is a soluble impurity.

One easy way to remove small amounts of colored impurities is with activated charcoal. Before adding any charcoal, cool your solution to slightly below the boiling point. Adding charcoal to a boiling solution will cause it to boil over. Do not add too much or the charcoal will also absorb your compound.

Swirl the flask. Boil it in the water bath for 2 to 3 minutes. Charcoal is very fine and can be hard to remove by filtration. Add only a small amount, swirl the flask, and heat it once again for 2 to 3 minutes before performing a hot filtration. If the solution is colorless, the decoloration step is unnecessary, but you still need to look carefully for any undissolved solid in the flask. If you find any, it can be removed by performing a hot gravity filtration with fluted filter paper.

Vacuum filtrations cool the solution too much and crystals are lost on the filter paper and funnel. Before filtering your solution, add some excess solvents and heat it to the boiling point to ensure that the compound stays dissolved during the filtration. Wet the filter paper with some hot solvent and filter the solution. Rinse the flask two or three times with hot solvent, filtering each rinse. Finally, rinse the filter paper with hot solvent to minimize product loss.

Crystals frequently form in the filtrate during the filtration, but they easily dissolve with heating. Your compound is no longer dissolved in a minimum amount of solvent. Remember to add a few boiling stones to the solution and boil until solid begins to form.



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