Deuterated hen egg-white lysozyme crystals: Optimization of the growth conditions and morphology

Deuterated and protonated tetragonal lysozyme crystals are grown using the hanging-drop vapor-diffusion method. The size of the lysozyme crystals grown is determined as a function of the concentration of sodium chloride used as a precipitant. It is found that crystallization leads to the formation of lysozyme crystals with three different habits. Morphological and X-ray diffraction analyses of the deuterated and protonated lysozyme crystals demonstrate that, despite the different habits, all the crystals grown belong to the tetragonal crystal system. The simple forms of lysozyme crystals are revealed. It is shown that the habits of the lysozyme crystals are determined by the specific combinations of simple forms. The mechanisms responsible for the formation of lysozyme crystals with different habits are discussed.     

Solubility of tetragonal and orthorhombic lysozyme crystals under high pressure

Two-beam interferometry was applied to measure lysozyme solubility under high pressure. This rapid method allowed determination of one data point within 3 h. The solubility of tetragonal lysozyme crystals was determined as a function of temperature at 0.1, 50, and 100 MPa, and that of orthorhombic crystals was measured at 0.1 and 100 MPa. The solubility of tetragonal crystals increased with pressure; however, that of orthorhombic crystals decreased. In both cases, the enthalpy and entropy of dissolution decreased with pressure.     

Growing of TGS and TGSe single crystals at various pH of solution

The influence of pH of solution on growth rates of the faces (001), (010), (100) and habit of TGS and TGSe single crystals was studied. The pH-values were determined when growth of TGS and TGSe crystals was ceased. At pH < 1 diglycine sulphate (DGS) and at pH < 2 diglycine selenate (DGSe) crystals are growing. The permittivity and resistivity of DGS and DGSe were measured. The resistivity of DGSe is an order of magnitude less than of TGSe for the same temperature. The possible mechanism of change of crystal morfology vs pH, supersaturation of solution and growth temperature is proposed.     

Gold distribution in pyrrhotite crystals grown under hydrothermal conditions

The distribution of gold between pyrrhotite and greenockite was studied by the method of hydrothermal thermal-gradient cocrystallization of the components at a temperature of 450°C, a pressure of 1 kbar, and different activities of sulfur in the presence of As and Se impurities. The structural component of Au impurity in these minerals was selected by studying statistical samplings of the analytical data for single crystals. Ferrous greenockite incorporates a maximum of 10 ± 2 ppm Au in solid solution. The incorporation limit of Au in stoichiometric pyrrhotite was estimated to be 25 ± 9 ppm; for nonstoichiometric pyrrhotites, it is lower. The As and Se impurities barely affect the concentration of structural gold in the minerals. It was shown that constitutional vacancies in pyrrhotite do not capture Au impurity. The observed phenomenon may be the growth effect related to the surface properties of nonstoichiometric pyrrhotite crystals grown under hydrothermal conditions. Differences in the surface structure of pyrrhotites of different composition and the products of their sorption of gold were revealed by X-ray photoelectron spectroscopy.     

Morphology of gallium orthophosphate crystals grown under hydrothermal conditions

Gallium orthophosphate crystals with sizes of 5 mm and more have been obtained by spontaneous nucleation from hydrothermal 5.6 – 15 M orthophosphoric acid solutions. Preferable concentrations of solvent were found in the range of 11 – 12 M, the temperature difference should not be over 6–10°C at the heating rate of 4 – 5 °C/day. Morphological investigations are carried out using optical and polarizing microscopies. GaPO₄ crystals, like quartz and berlinite, tends to grow with well developed {1 1}, {0 1}, {1 0}, {1 2}, and {0 2} faces, and they were divided into three habit types. Effect of orthophosphoric acid concentration on the crystal habit has been studied.     

Polarization distribution in DTGS crystals under nonequilibrium thermal conditions

The polarization distribution in crystals of deuterated triglycine sulphate in a constant temperature gradient is investigated on the basis of the dynamic method for studying the pyroelectric effect. It is shown that, under equilibrium thermal conditions, the polarization distribution is uniform except for the surface layer ～20-μm-thick. The nonuniform polarization distribution in this layer may indicate its multidomain state. In a steady-state temperature gradient, the layer thickens and its domains grow into the sample bulk.     

Second virial coefficient: variations with lysozyme crystallization conditions

Interparticle lysozyme interactions in solution have been studied by small angle X-ray scattering (SAXS) as a function of salt type (NaCl, NaNO₃, NaSCN and NaOAc), salt concentration, and as a function of temperature between 30°C and 10°C. The choice of conditions was made to cover variations from (undersaturated) solutions to (supersaturated) crystallization conditions. The second virial coefficients (A₂) were determined from the X-ray structure factors extrapolated to the origin, as a function of protein concentration. The A₂ values which correspond to lysozyme crystallization conditions were found to be in a range from about zero to −8.0×10⁻⁴ mol ml g⁻², in agreement with previous determinations by other groups. The variations of the second virial coefficient from positive (repulsive interactions) to negative (attractive interactions) were found to follow the efficiency of salts to induce crystallization. The choice of the second virial coefficient as a tool to predict crystallization conditions is discussed.     

Small-angle X-ray scattering study of conditions for the formation of growth units of protein crystals in lysozyme solutions

The structural composition of lysozyme solutions favorable for the formation of the tetragonal form of protein crystals was studied by synchrotron-based small-angle X-ray scattering depending on the protein concentration and the temperature. Along with lysozyme monomers, dimers and octamers are found in crystallization solutions; the octamer content increases with an increase in the protein concentration.     

Autodeformation bending of gypsum crystals grown under the conditions of counterdiffusion

The dynamics and kinetics of growth-induced bending of gypsum crystals grown from solution have been studied. Crystallization was performed by the method of chemical reaction under the conditions of component counterdiffusion. It is established that autodeformation bending occurs in the [001] direction at the growth front and is caused by cationic impurities. The crystal curvature depends on the anisotropy of growth rate and increases at lower supersaturations. The mechanism of growth-induced crystal bending is suggested which takes into account the heterometry stresses providing the appearance of a bending moment at the growth front.     

Physical and physicochemical processes accompanying powder synthesis, growth of PbMoO4 crystals, and their annealing in various media: VI. Anomalous biaxiality and thermoplastic stresses in PbMoO4 crystals in the relationship with the growth conditions

The optical anomalies are investigated and the internal stresses are calculated for lead molybdate crystals grown by the Czochralski method. An effect of the growth conditions on the distribution of stresses in the crystals is revealed.     

Effect of various precipitants on the nucleation rate of tetragonal hen egg-white lysozyme crystals in an AC external electric field

It was observed that the effect of an external electric field on the nucleation rate of tetragonal hen egg-white lysozyme crystals varied depending on the precipitant used (NaCl, NiCl₂ or YbCl₃) and that the electric double layer (EDL) played an important role in generating an external electric field of the necessary strength to control the nucleation rate. This phenomenon depended on the ionic strength of the precipitant used; that is, a precipitant of greater ionic strength resulted in a thinner EDL and increased the effect of the external electric field as the driving force for nucleation. The dependence of the nucleation rate on the precipitant was attributed to the magnitudes of the external electric fields generated in EDLs of varying thickness which were formed in the presence of different precipitants.     

Efficient conditions for the growth of MoO3 single crystals under oxygen atomsphere

Single crystals of MoO₃ have been grown under an oxygen atmosphere using a horizontal tubular furnace. The temperature and pressure necessary to grow satisfactory crystals in oxygen along [100] and [010] directions are determined.     

Critical size of crystals growing under diffusion conditions for loss of polyhedral stability

A new expression is proposed for calculating the critical size for which, when reached, the polyhedral stability of a crystal growing under diffusion controlled mass transfer disappears. The well-known relationships for critical size are obtained as special cases of the proposed expression, for infinitely dilute solutions. In addition, it is shown that when the solubility increases, the critical size of the crystal must also increase, all other parameters remaining identical. Similar is the dependence of the critical size on the concentration.     

Growth rate of single acetaminophen crystals in supersaturated aqueous solution under different operating conditions

Single crystal growth experiments were conducted to investigate the growth rate of acetaminophen (paracetamol) crystals under carefully controlled conditions of temperature, supersaturation and pH value. The relative growth rate of the different faces was studied. Growth Rate Dispersion (GRD) was observed by studying the effect of supersaturation and temperature on the growth rate. The growth rate in all directions was found to be temperature dependant. Elongation of the crystals was measured due to the faster growth in the Y‐ direction and Xa direction compared to in the Xb direction. Dissolution of the crystals was observed at pH values greater than 8.5, and a growth rate retardation was observed when increasing the pH from 5.6, which is the normal value without additions, to higher values in both acidic and basic mediums up to 8.5. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The growth of single crystals of Ni-W alloy under conditions of high temperature gradient

The structure of single crystals of the NV-4 nickel alloy containing 32–36 wt % W is investigated. The temperature gradient at the crystallization front and the velocity of the crystallization front are the variable parameters of directional crystallization. The degrees of structural perfection of the single crystals grown under different conditions are compared. The crystallization parameters providing growth of single crystals that have high structural perfection and can be successfully used as seeds for the growth of single-crystal blades are determined. Typical defects formed upon directional crystallization of single crystals of the Ni-W (35 wt %) alloy are examined. The studied defects are classified, and the factors responsible for the disturbance of the single-crystal structure are analyzed.     

Bulk GaN single crystals: growth conditions by flux method

Hexagonal GaN platelet crystals with a size of 1–4 mm have been grown by a Li-based flux method. The influence of growth conditions such as the molar ratio of starting materials, temperature, pressure, the position of Li₃N in the crucible on the growth of GaN single crystals was studied. The quality of GaN single crystal was checked by optical microscope and X-ray rocking curve.     

Physical and physicochemical processes accompanying powder synthesis, growth of PbMoO4 crystals, and their annealing in various media: V. Morphological twisting of PbMoO4 and PbWO4 crystals during Czochralski growth

Twisting of PbMoO₄ and PbWO₄ crystals around the longitudinal axis during their growth in the [100] direction has been revealed. It is shown that this twisting is a purely morphological effect accompanying the development of facets on the growth front.     

Growth conditions and electrical properties of KDP crystals: II. Dielectric permittivity measurements

The dielectric properties of potassium dihydrophosphate single crystals, which were grown from crystallization solutions at different pH, have been studied. The dielectric response of the single crystals is shown to vary substantially depending on the growth conditions and can be significantly different for samples from different growth sectors of the same single crystals and even within one sector. The results of this study are useful for optimizing the growth conditions of these single crystals.     

Photoluminescence of annealed LLGG:Cr3+ crystals under high pressure

High pressure photoluminescence has been used for analysis of lattice disorder in La_2.7Lu_2.29Cr_0.01Ga₃O₁₂ and La_2.32Lu_2.59Cr_0.02Ga_3.07O₁₂ crystals. Photoluminescence of samples before annealing and those annealed for 5 h in oxygen and hydrogen atmosphere at 923 K has been measured. The pressure dependence of Cr³⁺ luminescence has been used to obtain the crystal field distribution (lattice disorder) and its dependence on the thermal treatment. The distribution energy of the ⁴T₂ state has been considered as a measure of disorder. Annealing in oxygen has been found to reduce the energies of ⁴T₂ states for all sites, and annealing in hydrogen – to increase these energies.     

Structural and spectral studies on gypsum crystals under simulated conditions of phosphoric acid production with and without organic and inorganic additives

In the dihydrate process to produce phosphoric acid, phosphate ore [Ca₁₀F₂(PO₄)₆] is leached with sulfuric and weak phosphoric acids to produce phosphoric acid and gypsum as a by‐product. Crystallization of gypsum occurs as the leaching is taking place. The effect of organic and inorganic additives on the structure and spectrum of gypsum crystals under simulated conditions of phosphoric acid production is studied using x‐ray diffraction and infrared spectroscopy. Structure and spectrum of formed gypsum crystals in the absence of additives are slightly different from the standard gypsum crystals (card No. 6‐0046), which reflect the effect of preparation medium on the crystal structure of gypsum crystals. Presence of additives such as cetyl trimethyl ammonium bromide and 1,2‐dihydroxybenzene‐3,5‐disulfonic acid, Al³⁺ and Mg²⁺ increase the crystallinity of gypsum, while presence of additives such as citric acid and sodium dodecyl sulfate decrease the crystallinity of gypsum. Presence of Al³⁺ and Mg²⁺ as additives lead to the formation of calcium sulfate hemihydrate beside calcium sulfate dihydrate. Presence of sodium dodecyl sulfate as an additive inhibits the crystallization of gypsum and leads to the formation of anhydrite and calcium sulfate hemihydrate.