Crystallization relative humidity

The predicted solids based on thermodynamic measurements and models derived from them depend strongly on chemical composition. However, small aqueous aerosols remain meta-stable with decreasing RH until reaching a crystallization relative humidity(CRH). In contrast, solid aerosols t e up water at the thermodynamically favored deliquescence relative humidity(DRH). This hysteresis causes a dependence of aerosol phase on RH history. 

Calcium cyanide Ca(CN)2 Reacts with air moisture to release HCN. If finely ground and the relative humidity of the air is >35%, this can occur fairly rapidly Releases HCN slowly on contact with water or CO2, or rapidly with acids Do not handle with bare hands Nonflammable white powder or crystals... 

Unpigmented paint samples were brushed onto a potassium bromide crystal or polyethylene sheet (paint film thickness about 5 microns) and stored at controlled relative humidity using saturated salt solutions in closed vessels or a climate controlled room. 

Until 2004, no betalain standards were commercially available and current products lack the required purity. Preparative isolation from plant material is laborious and costly and the resulting standard substances vary in relative humidity, crystal water, and salts, resulting in over- or under-estimation of pigment contents... 

Figure 6.3 The effect of environmental conditions on the surface of a zinc phosphate cement (d) stable and undulating surface with no sign of crystallites observed under dry conditions, (b) crystal growth observed in an atmosphere of 100 % relative humidity, (c) extreme porosity observed in the bulk of the cement pores are 0-5 pm in diameter (Servais Cartz, 1971).

H.M. Wei, L.S. Wang, B.G. Zhang, C.J. Liu and J.X. Feng, An application of artificial neural networks. Simultaneous determination of the concentration of sulfur dioxide and relative humidity with a single coated piezoelectric crystal. Anal. Chem., 69 (1997) 699-702. 

Sensitivity was found to decrease with increasing temperature (20-50° C) for the gold-plated crystal. Water vapor at 50% relative humidity was not a serious interference. The smallest weight of diisopropyl methylphosphonate detected at 10 g L 1 was approximately 0.5 ng (Kristoff and Guilbault 1983). 

Polymorphs are different crystal forms of the same compound [55], They are usually prepared by crystallization of the drug from different solvents under diverse conditions. However, exposure to changes in temperature, pressure, relative humidity, and comminution which are encountered in processes such as drying, granulation, milling, and compression may also lead to polymorphic transformations. 

Accelerated aging and crystal transformation rates have also been traced to high residual moisture content. Ando et al. studied the effect of moisture content on the crystallization of anhydrous theophylline in tablets [9]. Their results also indicate that anhydrous materials convert to hydrates at high levels of relative humidity. In addition, if hygroscopic materials (e.g., polyethylene glycol 6000) are also contained in the formulation, needle-like crystals form at the tablet surface and significantly reduce the release rate of the theophylline. 

As indicated above, evaluation of the thermodynamics of a polymorphic or solva-tomorphic system provides valuable insight into the nature of the system, but is all too often overlooked in many studies. However, Sacchetti [6] used aqueous/organic slurries of the anhydrate and hydrate forms of GW2016 to determine the relative stability of crystal forms interrelated by solution-mediated transformation. It was reported that the use of slurries enabled experiments to be completed in a day that enabled an understanding of the relative stability of the forms as a function of relative humidity. 

The formation of niclosamide hydrates, and the effect of relative humidity on the solvatomorphs obtained from acetone and ethyl acetate has been studied [79], The acetone and ethyl acetate solvatomorphs could be desolvated, and exposure to elevated humidity resulted in the formation of two hydrate structures. Each hydrate could be dehydrated into a different anhydrate phase, but only the hydrate formed from the acetone desolvate could be rehydrated to form a hydrate phase. Dynamic vapor sorption has been used to develop a method for determining the onset relative humidity of a glass transition and associated crystallization process [80]. 

The effect of physical aging on the crystallization state and water vapor sorption behavior of amorphous non-solvated trehalose was studied [91]. It was found that annealing the amorphous substance at temperatures below the glass transition temperature caused nucleation in the sample that served to decrease the onset temperature of crystallization upon subsequent heating. Physical aging caused a decrease in the rate and extent of water vapor adsorption at low relative humidities, but water sorption could serve to remove the effects of physical aging due to a volume expansion that took place in conjunction with the adsorption process. 

The utilization of IR spectroscopy is very important in the characterization of pseudopolymorphic systems, especially hydrates. It has been used to study the pseudopolymorphic systems SQ-33600 [36], mefloquine hydrochloride [37], ranitidine HC1 [38], carbovir [39], and paroxetine hydrochloride [40]. In the case of SQ-33600 [36], humidity-dependent changes in the crystal properties of the disodium salt of this new HMG-CoA reductase inhibitor were characterized by a combination of physical analytical techniques. Three crystalline solid hydrates were identified, each having a definite stability over a range of humidity. Diffuse reflectance IR spectra were acquired on SQ-33600 material exposed to different relative humidity (RH) conditions. A sharp absorption band at 3640 cm-1 was indicative of the OH stretching mode associated with either strongly bound or crystalline water (Fig. 5A). The sharpness of the band is evidence of a bound species even at the lowest levels of moisture content. The bound nature of this water contained in low-moisture samples was confirmed by variable-temperature (VT) diffuse reflectance studies. As shown in Fig. 5B, the 3640 cm-1 peak progressively decreased in intensity upon thermal... 

When stored under increasing relative humidities (RH), cromolyn sodium absorbed water, resulting in a continuous series of interstitial solid solutions [11]. The amount of water absorbed was proportional to the relative humidity of the environment and could be up to about nine molecules of water per molecule of drug. Such an unusual system was characterized by combining XPD with single-crystal x-ray studies. The unit cell parameters of cromolyn sodium were obtained from single-crystal x-ray studies, and this permitted the authors to index the powder pattern. The b axis spacing was found to increase dramatically as a function of the relative humidity up to 20% RH (Table 2). Above 40% RH, the unit cell dimensions were nearly constant. 

Lot to lot variations of several drugs and excipients are shown in Table 9. Specially crystallized lots of ibuprofen, for example, show substantial changes in Brittle Fracture and Bonding Indices. Phenacetin shows a significant increase in brittleness at higher relative humidity. It was observed by Hiestand and Smith [31] that compacts of dried phenacetin did not fracture, while the lot equilibrated at 40% relative humidity did, consistent with the Brittle Fracture Index change. 

Solids that form specific crystal hydrates sorb small amounts of water to their external surface below a characteristic relative humidity, when initially dried to an anhydrous state. Below this characteristic relative humidity, these materials behave similarly to nonhydrates. Once the characteristic relative humidity is attained, addition of more water to the system will not result in a further increase in relative humidity. Rather, this water will be sorbed so that the anhydrate crystal will be converted to the hydrate. The strength of the water-solid interaction depends on the level of hydrogen bonding possible within the lattice [21,38]. In some hydrates (e.g., caffeine and theophylline) where hydrogen bonding is relatively weak, water molecules can aid in hydrate stabilization primarily due to their space-filling role [21,38]. 

Since water molecules occupy regular positions within the lattice of a hydrate with a specific stoichiometry (e.g., 1 1 monohydrate, 2 1 dihydrate, 5 1 pentahydrate) to the solid, relatively large quantities of water are sorbed. Figure 3 shows a moisture uptake isotherm for ipratropium bromide [39]. This substance undergoes an apparent hydration of the crystal between 63% and 75% relative humidity. Above 75% relative humidity, approximately 4.6% water is sorbed (theoretical monohydrate is 4.4 g/g). Interestingly, as anhydrous ipratropium bromide is equilibrated for extended time periods (e.g., 2 months and 5 months respectively, as shown in Fig. (3), hydration of the crystal appears to occur at... 

When this compound is precipitated from solution, it crystallizes with many waters of hydration, as many as 29,2 Many of these waters are easily lost at moderate temperature. The last 6 waters are held more tightly, however, so that the "hexahydrate" is a material easily obtained by heating at 40 C and 20% relative humidity.1... 

The molecular structure of arsphenamin is a typical representative of a thermotropic mesogen. With its symmetrical arrangement of the atoms the same holds for disodium cromoglycate, DNCG [20], which forms both thermotropic liquid crystals and lyotropic mesophases in the presence of water. Micronized DNCG powder applied to the mucosa of the nose or the bronchi absorbs water from the high relative humidity of the respiration tract and is first transformed into a lyotropic mesophase and then into a solution depending on the amount of water available. 

Phosphate adsorption and desorption by goethites differing in crystal morphology. Soil Sd. Soc. Am. J. 54 1007-1012 Torrent, J. Guzman, R. Parra, M.A. (1982) Influence of relative humidity on the crystallization of Fe(III) oxides from ferrihydrite. Clays Clay Min. 30 337-340 Torrent, J. Schwertmann, U. Barron,V. 

White crystal, powder or flake highly hygroscopic the compound and its solutions absorb moisture from the air at various rates depending on calcium chloride concentrations, relative humidity and vapor pressure of water in the air, temperature, surface area of exposed material, and the rate of air circulation at 40% and 95% relative humidity and 25°C, one gram anhydrous calcium chloride may absorb about 1.4 g and 17 g water, respectively. (Shearer, W. L. 1978. In Kirk-Othmer Encyclopedia of Chemical Technology, 3rd ed., vol. 4, pp. 432-6. New York Wiley Interscience) density 2.15, 2.24, 1.85, 1.83 and 1.71 g/cm for the anhydrous salt and its mono-, di-, tetra- and hexahy-drates, respectively anhydrous salts melts at 772°C, while the mono-, di-, tetra- and hexahydrates decompose at 260°, 175°, 45.5° and 30°C, respectively the anhydrous salt vaporizes at 1,935°C highly soluble in water, moderate to high solubility in alcohol. 

Since the crystals of Csi 75 [Pt(CN)4] 2H20 lose water easily, they must be stored over a saturated solution of NH4C1 and KN03 that has a relative humidity of 72% at 23°.8 Recrystallization of Cs175[Pt(CN)4] have not been... 

Chowhan [9] defined different pathways of physical instability of tablet formulations. These physical paths may involve one or more complex physical processes, e.g. change in polymorphism, crystallization, vaporization and adsorption. These pathways and thus the physical tablet parameters, are influenced by different types of variables formulation variables (e.g. solubility and hygroscopicity), in-process variables (e.g. moisture content) and aging variables (e.g. temperature and relative humidity). 

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