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  • 1.
    Aguilar-Mamani, Wilson
    et al.
    Department of Chemistry, Faculty of Science and Technology, San Simon University, UMSS, Cochabamba.
    Akhtar, Farid
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Solution-mediated growth of NBA-ZSM-5 crystals retarded by gel entrapment2018In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 487, p. 57-64Article in journal (Refereed)
    Abstract [en]

    The synthesis of flat tablet-shaped ZSM-5 crystals from a gel using metakaolin as aluminosilicate source and n-butyl amine as structure directing agent was investigated. The evolution inside the solid phase was characterized by X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, thermogravimetry and mass spectrometry. A kinetic study indicated that the nucleation of the majority crystals occurred concurrently with the formation of the gel upon heating the starting liquid suspension. Microstructural evidences undeniably showed that the gel precipitated on ZSM-5 crystals and mineral impurities originating from kaolin. As a result, crystal growth was retarded by gel entrapment, as indicated by the configuration and morphology of the embedded crystals. The results presented herein are harmonized with a solution-mediated nucleation and growth mechanism. Our observations differ from the autocatalytic model that suggests that the nuclei rest inside the gel until released when the gel is consumed. Our results show instead that it is crystals that formed in an early stage before entrapment inside the gel that rest inside the gel until exposed at the gel surface. These results illustrate the limitation of the classical method used in the field to determine nucleation profiles when the crystals become trapped inside the gel.

  • 2.
    Cerreta, M.K.
    et al.
    Michigan State University.
    Berglund, Kris
    Contact nuclei formation in aqueous dextrose solutions1990In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 102, no 4, p. 869-876Article in journal (Refereed)
    Abstract [en]

    A laser Raman microprobe was used in situ to observe the growth of alpha dextrose monohydrate on alpha anhydrous dextrose crystals. The Raman spectra indicate growth of the monohydrate below 28.1°C, but the presence of only the anhydrous form above 40.5°C. Contact nucleation experiments with parent anhydrous crystals yielded only monohydrate nuclei below 28.1°C, while contacts in solutions between 34.5 and 41.0°C produced both crystalline forms, and contacts in solutions above 43.5°C produced only anhydrous nuclei. The inability of the monohydrate to grow on anhydrous crystals in the same solution that forms the two crystalline phases with a single contact precludes a simple attrition mechanism of nuclei formation. For the same reason, the hypothetical mechanism involving parent crystal stabilization of pre-crystalline clusters, allowing the clusters to grow into nuclei, is also contradicted. A third, mechanism, which may be a combination of the two, is believed to apply.

  • 3.
    Cerreta, M.K.
    et al.
    Michigan State University.
    Berglund, Kris
    The structure of aqueous solutions of some dihydrogen orthophosphates by laser Raman spectroscopy1987In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 84, no 4, p. 577-588Article in journal (Refereed)
    Abstract [en]

    Powdered crystals and pure, aqueous solutions of ammonium, sodium, and potassium dihydrogen orthophosphates in concentrations ranging from 0.01M to supersaturated were investigated at 30°C using laser Raman spectroscopy between 700 and 1350 cm-1. With increasing solute concentration, the peak position of the 875 cm-1 P-(OH)2 symmetric strech band increased. Extreme asymmetry in the 1075 cm-1 P=O2 symmetric stretch band developed to lower energy. The integrated intensity ratio of the 875 cm-1 band to the 1075 cm-1 band envelope remained constant. These observations are consistent with anion-anion association via hydrogen bonds. Deconvolution of the spectral bands showed only 40% and 20% of the phosphates exist as monomers in saturated potassium and ammonium solutions, respectively, and that anion association does not cease at the dimer. The spectra provided no evidence of quasi-crystalline entities in solution. The necessary breaking and reforming of hydrogen bonds during the growth process can explain rapid z-direction growth, growth activation energy, and the rate-limiting surface growth mechanism.

  • 4.
    Chakraborty, Reena
    et al.
    Michigan State University.
    Berglund, Kris
    Steady state fluorescence spectroscopy of pyranine as a trace extrinsic probe to study structure in aqueous sugar solutions1992In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 125, no 1-2, p. 81-96Article in journal (Refereed)
    Abstract [en]

    The steady state fluorescence behavior of pyranine has been monitored in aqueous solutions of sucrose, glucose, fructose, and lactose. In each case it is possible to use the ratio of peak intensities at 440 and 511 nm (the PIR) as an indicator of the degree of supersaturation of the sugar solutions. We observed both bulk water and water of solvation in all solutions examined, regardless of degree of sapersaturation. In each case the amounts of bulk water and water of solvation per molecule of sugar appear to be nearly equal at saturation. We did not observe any evidence of solvent exclusive clusters in any of the systems we studied

  • 5.
    Dunuwila, D.D.
    et al.
    Michigan State University.
    Berglund, Kris
    ATR FTIR spectroscopy for in situ measurement of supersaturation1997In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 179, no 1-2, p. 185-193Article in journal (Refereed)
    Abstract [en]

    The current contribution establishes the technical feasibility of Attenuated Total Reflection (ATR) Fourier transform infrared (FTIR) spectroscopy for the in situ measurement of supersaturation in crystallization processes. The approach was inspired by recent advancements in ATR spectroscopy by way of various light transfer systems for remote sensing and by the increasing availability of ATR configurations well suited for remote, in situ measurements. The feasibility of the technique was investigated using a DIPPER-210® immersion probe manufactured by Axiom Analytical, Inc. Initial experiments conducted using aqueous maleic acid proved that ATR FTIR spectroscopy can be successfully employed to measure supersaturation, solubility and the metastable limit, in situ, with sufficient accuracy and precision.

  • 6.
    Dunuwila, Dilum D.
    et al.
    Michigan State University.
    Carroll, Leslie B.
    Michigan State University.
    Berglund, Kris
    An investigation of the applicability of attenuated total reflection infrared spectroscopy for measurement of solubility and supersaturation of aqueous citric acid solutions1994In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 137, no 3-4, p. 561-568Article in journal (Refereed)
    Abstract [en]

    Currently applied methods for measurement of solubility and supersaturation based on viscometry, refractometry, interferometry and density require the separation of phases prior to measurement. ATR (attenuated total reflection) infrared spectroscopy provides a unique configuration in which the infrared spectrum of a liquid phase can be obtained in a slurry without phase separation. The applicability of the technique was investigated using a micro Circle® open boat cell equipped with a ZnSe (zinc selenide) ATR rod. Experiments conducted with aqueous citric acid proved that ATR infrared spectroscopy can be successfully employed to determine solubility and supersaturation.

  • 7.
    Garcia, Gustavo
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Solid State and Theoretical Chemistry, Chemistry Research Institute, San Andres Mayor University.
    Cabrera, Saúl
    Solid State and Theoretical Chemistry, Chemistry Research Institute, San Andres Mayor University, University Campus.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Selective synthesis of FAU-type zeolites2018In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 489, p. 36-41Article in journal (Refereed)
    Abstract [en]

    In the present work, parameters influencing the selectivity of the synthesis of FAU-zeolites from diatomite were studied. The final products after varying synthesis time were characterized by scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction and gas adsorption. It was found that high concentrations of NaCl could completely inhibit the formation of zeolite P, which otherwise usually forms as soon as maximum FAU crystallinity is reached. In the presence of NaCl, the FAU crystals were stable for extended time after completed crystallization of FAU before formation of sodalite. It was also found that addition of NaCl barely changed the crystallization kinetics of FAU zeolite and only reduced the final FAU particle size and SiO2/Al2O3 ratio slightly. Other salts containing either Na or Cl were also investigated. Our results suggest that there is a synergistic effect between Na+ and Cl-. This is attributed to the formation of (Na4Cl)3+ clusters that stabilize the sodalite cages. This new finding may be used to increase the selectivity of syntheses leading to FAU-zeolites and avoid the formation of undesirable by-products, especially if impure natural sources of aluminosilica are used.

  • 8.
    Guo, S.J.
    et al.
    Luleå tekniska universitet.
    Easterling, K.E.
    Luleå tekniska universitet.
    Dou, S.X.
    School of Materials Science and Engineering, University of New South Wales.
    Liu, H.K.
    School of Materials Science and Engineering, University of New South Wales.
    Improved single crystal growth in the Bi-Sr-Ca-Cu-O system using a sealed cavity technique1990In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 100, no 1-2, p. 303-308Article in journal (Refereed)
    Abstract [en]

    Bi-Sr-Ca-Cu-O single crystals obtained thus far commonly have a very small thickness in the c-axis because of the weak bonding between two adjacent BiO layers and the high vapour pressure of Bi2O3 at high temperature. To overcome these difficulties a presintered SrCaCu4O6 was used to seal the Bi-Sr-Ca-Cu-O melt from which the single crystals grew during slow cooling. In the SrCaCu4O6 sealed cavity the Bi loss through vaporization was prevented and Sr and Ca were enriched in the superconducting crystals. The resulting single crystals have a dimension of up to 3.0×1.5×0.7 mm3, which is two orders of magnitude thicker than those grown from alkali chloride flux. The composition of the crystals is Bi2.2Sr1.8Ca0.75Cu1.8Ox and they possess a zero resistance at temperature above liquid nitrogen

  • 9.
    Kugler, Veronika M.
    et al.
    Department of Physics, Linköping University.
    Söderlind, Fredrik
    Department of Physics, Linköping University.
    Music, Denis
    Department of Physics, Linköping University.
    Helmersson, Ulf
    Department of Physics, Linköping University.
    Andreasson, Johanna
    Lindbäck, Ture
    Low temperature growth and characterization of (Na,K)NbOx thin films2003In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 254, no 3-4, p. 400-404Article in journal (Refereed)
    Abstract [en]

    Thin (Na,K)NbOx perovskite films (NKN) have been deposited on SiO2/Si(0 0 1) substrates at low temperatures, from 350°C to 550°C, by RF magnetron sputtering. The effects of substrate temperature on microstructure, electrical-, and mechanical properties of the NKN films have been studied. X-ray diffraction analysis revealed that films deposited at temperatures in the range of 450-550°C were crystalline, growing as a single phase, with a preferred orientation of (0 0 1). Films deposited at 350°C, were shown to be amorphous. The growth temperature had a strong influence on the electrical properties of the NKN films and the relative dielectric constants of the obtained films were in between 38 and 78. Variations of the mechanical properties of the NKN films were observed for different substrate temperatures: The elastic moduli and the hardness values ranged from 205±26 to 93±29 GPa, and from 12±2 to around 2 GPa, for films deposited at 550°C and 450°C, respectively.

  • 10.
    Kugler, Veronika M
    et al.
    Linköping universitet.
    Söderlind, Fredrik
    Linköping universitet.
    Music, Denis
    Linköping universitet.
    Helmersson, Ulf
    Linköping universitet.
    Andreasson, Johanna
    Luleå tekniska universitet.
    Lindbäck, Ture
    Microstructure/dielectric property relationship of low temperature synthesised (Na,K)NbOx thin films2004In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 262, no 1-4, p. 322-326Article in journal (Refereed)
    Abstract [en]

    Thin films of (Na,K)NbOx (NKN) were grown by reactive RF magnetron sputtering on polycrystalline Pt80Ir20 substrates, at relatively low growth temperatures between 300°C and 450°C. The results show that the electrical performance and the microstructure of the films are a strong function of the substrate temperature. X-ray diffraction of films grown up to 400°C revealed the formation of only one crystalline NKN-phase with a preferred (002)-orientation. However, a mixed orientation together with a secondary, paraelectric potassium niobate phase, were observed for NKN films deposited at 450°C. The differences in the microstructure explains the variations in the dielectric constants and losses: The single phase NKN films displayed a dielectric constant and a dielectric loss of 506 and 0.011, respectively, while the films with mixed phases exhibited values of 475 and 0.022, respectively. The possibility of fabricating NKN films with relatively high dielectric properties at low growth temperatures, as demonstrated here, is of high technological importance

  • 11.
    LeCaptain, D.J.
    et al.
    Michigan State University.
    Berglund, Kris
    Applicability of second harmonic generation for in situ measurement of induction time of selected crystallization systems1999In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 203, no 4, p. 564-569Article in journal (Refereed)
    Abstract [en]

    The nonlinear optical technique of second harmonic generation (SHG) is introduced as a novel technique for monitoring particle formation in batch crystallizations. SHG is more sensitive and is less prone to interference than turbidometric methods. The studies presented show the applicability of SHG as a method for in situ measuring the induction time of a number of noncentrosymmetric crystal systems.

  • 12.
    Pan, Borlan
    et al.
    Michigan State University.
    Berglund, Kris
    Time-resolved fluorescence and anisotropy of covalently coupled 1-pyrenebutyric acid for monitoring the crystallization conditions of lysozyme1997In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 171, no 1-2, p. 226-235Article in journal (Refereed)
    Abstract [en]

    Time-resolved fluorescence and anisotropy measurements of trace amounts of 1-pyrenebutyric acid labeled hen egg-white lysozyme (PBA-HEL) were used to characterize hen egg-white lysozyme (HEL) crystallization conditions. The effects of sodium chloride and protein concentrations on the fluorescence lifetimes and rotational correlation times of the labeled protein were examined. These results were compared with the effects of the salts ammonium acetate and ammonium sulfate. Addition of protein precipitants caused increases in the rotational correlation times which were attributed to a combination of steric, hydrodynamic, general electrostatic and specific ionic interactions. This decrease in the rotational mobility of HEL appears to be a necessary but not sufficient condition to allow the formation of specific interactions leading to crystallization. The results demonstrated that fluorescence measurements are effective in characterizing and monitoring protein crystallization processes prior to the appearance of macroscopic crystals.

  • 13.
    Pan, Borlan
    et al.
    Michigan State University.
    Chakraborty, Reena
    Michigan State University.
    Berglund, Kris
    Time resolved fluorescence and anisotropy of 1-pyrene butyric acid and pyranine as probes of solvent organization in sucrose solutions1993In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 130, no 3-4, p. 587-599Article in journal (Refereed)
    Abstract [en]

    The microenvironment of solute-solvent interactions in aqueous sucrose solutions, ranging from 0 to 80 wt% in concentration, was investigated using time resolved fluorescence techniques. The fluorescence lifetimes and rotational correlation times of the trace fluorescent probes, PBA (1-pyrene butyric acid) and pyranine (trisodium 8-hydroxy-1,3,6-pyrenetrisulfonate), were measured in sucrose solutions. The behavior of the fluorescence lifetimes and the increase in the rotational correlation times with increasing sucrose concentration provided no evidence for the formation of water exclusive solute clusters in the metastable solutions. Instead, the results indicated the formation of a network of hydrogen bonding interactions between dispersed sucrose molecules.

  • 14. Pankov, V.
    et al.
    Bartholdson, Å.
    Luleå tekniska universitet.
    Stukalov, O.
    Academy of Science Belarus.
    Smolenchuk, S.
    University of Technology of Belarus.
    Babushkin, O.
    Luleå tekniska universitet.
    Gremenok, V.
    Academy of Science Belarus.
    Growth of BaFe12O19 thin films formed by reactive diffusion2003In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 252, no 1-3, p. 382-390Article in journal (Refereed)
    Abstract [en]

    Thin films of BaFe12O19 have been grown on (00 l) oriented α-Fe2O3 single crystal substrates. The initial stages of the reaction between BaFe2O4 thin films and hematite single crystals have been investigated using AFM and SEM. The microstructure studies showed that (00 l) oriented BaFe12O19 microcrystallites formed during annealing at 900-1100°C. It was concluded that the surface diffusion had a dominating role in formation of thin BaFe12O19 films. Crystal growth was performed by stacking of layers with the thickness 2.3 nm, correlated with the c-parameter of the BaFe12O19 unit cell.

  • 15.
    Roqué Rosell, Josep
    et al.
    Departament de Mineralogia, Petrologia i Geologia Aplicada, Universitat de Barcelona, Marti i Franquès s/n, Barcelona, Catalunya 08028, Spain.
    Portillo Serra, Joaquim
    Centres Científics i Tecnològics, Universitat de Barcelona, Lluís Solé i Sabaris, 1-3, Barcelona; NanoMEGAS, Boulevard Edmond Machtens 79, Brussels B-1080, Belgium .
    Aiglsperger, Thomas
    Departament de Mineralogia, Petrologia i Geologia Aplicada, Universitat de Barcelona, Marti i Franquès s/n, Barcelona, Catalunya 08028, Spain.
    Plana-Ruiz, Sergi
    Centres Científics i Tecnològics, Universitat de Barcelona, Lluís Solé i Sabaris, 1-3, Barcelona, Catalunya 08028, Spain.
    Trifonov, Trifon
    Centre de Recerca de Nanoenginyeria, Universitat Politècnica de Catalunya, Pascual i Vila, 15 Edifici C Planta-1, Barcelona, Catalunya 08028, Spain.
    Proenza, Joaquín A.
    Departament de Mineralogia, Petrologia i Geologia Aplicada, Universitat de Barcelona, Marti i Franquès s/n, Barcelona, Catalunya 08028, Spain.
    Au crystal growth on natural occurring Au-Ag aggregate elucidated by means of precession electron diffraction (PED)2018In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 483, p. 228-235Article in journal (Refereed)
    Abstract [en]

    In the present work, a lamella from an Au—Ag aggregate found in Ni-laterites has been examined using Transmission Electron Microscope to produce a series of Precision Electron Diffraction (PED) patterns. The analysis of the structural data obtained, coupled with Energy Dispersive X-ray microanalysis, made it possible to determine the orientation of twinned native gold growing on the Au—Ag aggregate. The native Au crystal domains are found to have grown at the outermost part of the aggregate whereas the inner core of the aggregate is an Au—Ag alloy (∼4 wt% Ag). The submicron structural study of the natural occurring Au aggregate points to the mobilization and precipitation of gold in laterites and provides insights on Au aggregates development at supergene conditions. This manuscript demonstrates the great potential of electron crystallographic analysis, and in particular, PED to study submicron structural features of micron sized mineral aggregates by using the example of a gold grain found in a Ni-laterite deposits.

  • 16.
    Schwartz, Albert M.
    et al.
    University of Michigan.
    Berglund, Kris
    In situ monitoring and control of lysozyme concentration during crystallization in a hanging drop2000In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 210, no 4, p. 753-760Article in journal (Refereed)
    Abstract [en]

    Fiber optic Raman spectroscopy combined with a partial least-squares regression model was demonstrated as a monitor of lysozyme concentration during crystallization in a hanging drop experiment in real time. Raman spectral features of the buffer and protein were employed to build the regression model. The use of fiber optic technology coupled with Raman spectroscopy, which is ideal for use with aqueous solutions, results in a powerful noninvasive probe of the changing environment within the solution. Lysozyme concentrations were monitored in experiments at a constant reservoir ionic strength. Data from these uncontrolled experiments were used to determine rates of supersaturation, induction times, and the number and size of the resultant lysozyme crystals. Control experiments were performed by introducing step changes in the reservoir ionic strength. The step changes were initiated by comparing in situ rates of supersaturation with the rates of supersaturation calculated from the uncontrolled data. Monitoring the concentration changes of the lysozyme within the hanging drop permits a measurement of the level of supersaturation of the system and enhances the possibility of dynamic control of the crystallization process.

  • 17.
    Schwartz, A.M.
    et al.
    Michigan State University.
    Berglund, Kris
    Use of Raman spectroscopy for in situ monitoring of lysozyme concentration during crystallization in a hanging drop1999In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 203, no 4, p. 599-603Article in journal (Refereed)
    Abstract [en]

    Fiber optic Raman spectroscopy combined with a partial least-squares regression model was investigated as a means to monitor lysozyme concentration during crystallization in a hanging drop experiment in real time. Raman spectral features of the buffer and protein were employed to build the regression model. This model was used to calculate the compositional changes within the hanging drop. The use of fibre optic technology coupled with Raman spectroscopy, which is ideal for use with aqueous media, results in a powerful noninvasive probe of the changing environment within the solution. These preliminary findings indicate that solubility as well as supersaturation measurements can be made.

  • 18.
    Uusi-Penttilä, Marketta S
    et al.
    Michigan State University.
    Berglund, Kris
    Spectroscopic monitoring of environmentally benign anti-solvent crystallization1996In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 166, no 1-4, p. 967-970Article in journal (Refereed)
    Abstract [en]

    There are very few studies dealing with the fundamentals of anti-solvent crystallization, even though this crystallization method is widely used in the pharmaceutical industry. Anti-solvent crystallization is accomplished by adding a miscible anti-solvent into a mixture of solute and solvent, effectively reducing the solubility of the solute in the solvent, and thus, causing the crystallization of the solute. Unfortunately, many of the anti-solvents used today are chlorinated hydrocarbons suspected of environmental damage. The current research demonstrates the use of environmentally benign solvents for anti-solvent crystallization and new approaches for monitoring of the solvent behavior during an anti-solvent crystallization. Results are presented confirming the efficacy of various water and ester systems for anti-solvent crystallization. Furthermore, the application of fluorescence spectroscopy for monitoring these crystallizations is demonstrated.

1 - 18 of 18
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