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Dušica Mirković, 2019, doctoral dissertation

Abstract: The aim of this doctoral research was to develop and optimize parenteral nanoemulsions as well as the total parenteral nutrition (TPN) admixture containing a nanoemulsion obtained in the course of the optimization process (hereinafter referred to as optimal nanoemulsion), and to examine their physicochemical and biological quality as well. In addition, the quality of the prepared nanoemulsions was compared with the quality of the industrial nanoemulsion (Lipofundin® MCT/LCT 20%), and, in the end, the TPN admixture initially prepared was also compared with the admixture into which the industrial emulsion was incorporated. Parenteral nanoemulsions that were considered in this dissertation were prepared by the high-pressure homogenization method. This method is the most widely applied method for the production of nanoemulsions due to the shortest length of homogenization time, the best-obtained homogeneity of the product and the smallest droplet diameter. For the nanoemulsion formulation, preparation and optimization purposes, by using, firstly, the concept of the computer-generated fractional design, and, after that, the full experimental design, the assessment of both direct effects of different formulation and process parameters (the oil phase type, the emulsifier type and concentration, a number of homogenization cycles and the pressure under which homogenization was carried out) as well as the effects of their interactions on the characteristics of prepared nanoemulsions was performed. Monitoring the nanoemulsion physical and chemical stability parameters was carried out immediately after their preparation, and then after 10, 30 and 60 days. It included the visual inspection, the measurement of the droplet diameter (the mean and volume droplet diameter), the polydispersity index, the ζ-potential, the pH value, the electrical conductivity, and the peroxide number. After the preparation and after 60 days, the biological evaluation (the sterility test and the endotoxic test) of the prepared nanoemulsions was carried out. As far as the characterization of the TPN admixture is concerned, it included practically the same parameters. The dynamics of monitoring the characteristics of the TPN admixture was determined on the basis of practical needs of hospitalized patients (0h, 24h and 72h). The scope and comprehensiveness of this issue indicated the need to divide the doctoral dissertation into three basic stages. The first stage was preliminary. Using the 24-1 fractional factorial design, nanoemulsions for the parenteral nutrition were prepared. They contained either a combination of soybean and fish oil, or a combination of medium chain triglycerides and fish oil. In addition, the type and the amount of an emulsifier used, a number of high-pressure homogenization cycles, and the homogenization pressure, were also varied. The measurement of the above-mentioned parameters for the industrial nanoemulsion was parallely carried out (Lipofundin® MCT/LCT 20%). The objective of this part of the research was to identify critical numerical factors having the most significant effect on the characteristics that define the prepared parenteral nanoemulsions. Parameters that were singled out as the result of this stage of the research (the emulsifier concentration and a number of homogenization cycles) were used as independent variables in the second stage of the research.
Keywords: nanoemulsions, total parenteral nutrition admixtures, high pressure homogenization, design of experiments, optimization, analysis of variance, artificial neural networks
Published: 07.06.2019; Views: 10839; Downloads: 0
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The magnetic and colloidal properties of $CoFe_2O_4$ nanoparticles synthesized by co-precipitation
Sašo Gyergyek, Mihael Drofenik, Darko Makovec, 2014, original scientific article

Abstract: Magnetic $CoFe_2O_4$ nanoparticles were synthesized by co-precipitation at 80 °C. This co-precipitation was achieved by the rapid addition of a strong base to an aqueous solution of cations. The investigation of the samples that were quenched at different times after the addition of the base, using transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDXS) and X-ray powder diffractometry, revealed the formation of a Co-deficient amorphous phase and $Co(OH)_2$, which rapidly reacted to form small $CoFe_2O_4$ nanoparticles. The nanoparticles grew with the time of aging at elevated temperature. The colloidal suspensions of the nanoparticles were prepared in both an aqueous medium and in a non-polar organic medium, with the adsorption of citric acid and ricinoleic acid on the nanoparticles, respectively. The measurements of the room-temperature magnetization revealed the ferrimagnetic state of the $CoFe_2O_4$ nanoparticles, while their suspensions displayed superparamagnetic behaviour.
Keywords: cobalt ferrite, nanoparticles, co-precipitation, colloidal suspensions, magnetic properties
Published: 30.08.2017; Views: 1874; Downloads: 58
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Synthesis, crystal structure and magnetic properties of a new hydroxylammonium fluoroferrate
Brina Dojer, Matjaž Kristl, Zvonko Jagličić, Amalija Golobič, Marta Kasunič, Mihael Drofenik, 2012, original scientific article

Abstract: This paper reports on the synthesis of a new hydroxylammonium fluoroferrate, with the formula $(NH_3OH)_3FeF_6$, obtained after dissolving iron powder in hydrofluoric acid and adding solid $NH_3OHF$. This new compound has been characterized by chemical and thermal analysis, single-crystal X-ray diffraction, and magnetic measurements. The title compound crystallizes trigonal, R3c, with cell parameters a = 11.4154(2) Å, c = 11.5720(2) Å, Z = 6. The structure consists of $NH_3OH^+$ cations and isolated $FeF_6^{3–}$ octahedra in which the central ion lies on a threefold axis. The oxygen and nitrogen atoms of the hydroxylammonium cations are donors of hydrogen bonds to fluoride anions, resulting in a network of hydrogen bonds between counterions. The effective magnetic moment $µ_{eff}$ = 5.8 BM was calculated and perfectly matches the expected value of high-spin Fe(III) ions. The thermal decomposition of the compound was studied by TG, DSC, and X-ray powder diffraction.
Keywords: inorganic chemistry, crystallography, coordination compounds, synthesis, crystal structure, characterization of compounds, determination of the structure of compounds, X-ray diffraction, magnetic measurements, thermal analysis, TG, DSC, hydrogen bond, metal complexes, hydroxylammonium fluoromethalatehydroxylammonium, fluoroferrate
Published: 25.08.2017; Views: 1100; Downloads: 50
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Synthesis and characterisation of hydroxylammonium fluorochromate
Matjaž Kristl, Mihael Drofenik, Ljubo Golič, Amalija Golobič, 2003, original scientific article

Abstract: Reactions in the system $Cr – NH_3OHF – HF – H_2O$ were investigated. Green crystals of a new compound with the formula $(NH_3OH)_3CrF_6$ have been isolated from the water solution and characterized by chemical analysis. The compound crystallizes as triclinic, P-1, with cell parameters: a = 6.5461(2) Å, b = 6.9347(2) Å, c = 9.4072(3) Å, α = 86.772(1)°, β = 83.804(1)°, γ = 70.283(1)°. The effective magnetic moment, $µ_{eff}$ = 3.82 BM, was calculated from magnetic susceptibility measurements in the temperature range 80-290 K. The thermal decomposition of the compound was studied by TG and DSC analysis. $(NH_3OH)_3CrF_6$ decomposes above 125 °C in three steps and the residue has been identified by X-ray powder diffraction as $α – Cr_2O_3$.
Keywords: inorganic chemistry, structural chemistry, crystalline structure, coordination compounds, synthesis, inorganic reactions, thermal decomposition, characterization of compounds, TG, DSC, X-ray diffraction, chromium complexes, hydroxylammonium fluoro chromates, crystals
Published: 25.08.2017; Views: 917; Downloads: 79
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Reactive sintering of $MnZn$ ferrites
Tomaž Kosmač, Mihael Drofenik, 2001, original scientific article

Abstract: Reaction-formed $MnZn$ ferrite was prepared and the decrease in shrinkage after sintering due to the volume expansion accompanying iron oxidation was studied. Green compacts consisting of the milled raw oxides $Fe_2O_3$, $Mn_3O_4$, $ZnO$ and metallic iron powder were sintered at 1350 °C in air. During the first hold at 800 °C, $Fe$ was oxidized to $\alpha-Fe_2O_3$ and $Zn$ ferrite was formed. Above 1300 °C the reaction bonding was completed and $MnZn$ ferrite, exhibiting a relatively low shrinkage, was formed. The chemical reactions involved during reaction bonding were associated with a volume expansion and porosity formation, compensating for the shrinkage on sintering. Intensive milling decreases the porosity after sintering but induces the oxidation of iron, and partially removes the shrinkage compensation caused by the presence of metallic iron.
Keywords: reaction-forming, $MnZn$ ferrite, inorganic technology, ferrite ceramics, reaction bonded ceramics, sintering, iron oxides, iron
Published: 25.08.2017; Views: 520; Downloads: 70
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Ammoniumbis(hydroxylammonium) pentafluoridooxidovanadate(IV)
Brina Dojer, Matjaž Kristl, Zvonko Jagličić, Mihael Drofenik, Anton Meden, 2008, original scientific article

Abstract: Turquoise crystals of a new hydroxylammonium compound with the formula $NH_4(NH_3OH)_2[VOF_5]$ have been synthesized by the reaction of solid $NH_3OHF$ and the aqueous solution of vanadium in HF. The compound crystallizes monoclinic, $P2_1/n$, with cell parameters: a = 10.5658(2) Å, b = 6.6143(1) Å, c = 11.6618(2) Å, β = 96.282(1). Magnetic susceptibility was measured using a SQUID device over a temperature range 2–300 K at magnetic field $10^3 Oe$ giving the result $µ_{eff}$ = 1.65 BM. The thermal decomposition was studied by TG and DSC analysis. $NH_4(NH_3OH)_2[OF_5V]$ decomposes above 354 K in three steps, obtaining $NH_4VOF_3$ after the first step and $V_2O_5$ as the final residue.
Keywords: hydroxylammonium fluorovanadates, x-ray powder diffraction, x-ray structure determination, thermal analysis
Published: 17.08.2017; Views: 820; Downloads: 67
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Efekt PTKU v močno donorsko dopirani keramiki ▫$BaTiO_3$▫
Nina Ule, Darko Makovec, Mihael Drofenik, 2000, original scientific article

Abstract: Navadno izdelujejo upore s pozitivnim temperaturnim koeficientom upornosti (PTK-upore) s sintranjem nizko donorsko dopiranega ▫$BaTiO_3$▫ na zraku. Koncentracija donorja ne sme preseči kritične velikosti (-0,3 mol.% med sintranjem na zraku), ki povzroči zaustavitev pretirane rasti zrn med sintranjem. S sintranjem v redukcijski atmosferi lahko povišamo kritično koncentracijo donorja, in tako dobimo močno donorsko dopiran ▫$BaTiO_3$▫ z grobo zrnato mikrostrukturo. V grobo zrnatem ▫$BaTiO_3$▫ lahko s poznejšo reoksidacijo z žganjem na zraku uravnavamo PTKU-efekt. V tem delu so predstavljeni rezultati raziskave PTKU-efekta v keramikah ▫$BaTiO_3$▫, dopiranih s koncentracijami La od o do 20 ml.%. Vzorci so bili sintrani v redukcijski mešanici ▫$N_2$▫ z 1 % ▫$H_2$▫ in pozneje reoksidirani z žganjem na zraku.
Keywords: polprevodni ▫$BaTiO_3$▫, donorsko dopiranje, električne lastnosti, PTKU-efekt, mikrostruktura
Published: 27.07.2017; Views: 467; Downloads: 58
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Priprava Co-feritnih nanodelcev z ozko porazdelitvijo velikosti z metodo termičnega razpada oleatov
Sašo Gyergyek, Darko Makovec, Mihael Drofenik, 2008, original scientific article

Abstract: V prispevku opisujemo sintezo nanodelcev kobaltovega ferita z ozko porazdelitvijo velikosti z metodo termičnega razpada organskega kompleksa. Sinteza nanodelcev je potekala v dveh stopnjah. V prvi smo sintetizirali železov in kobaltov oleat z reakcijo kobaltovega (II) in železovega (III) klorida z natrijevim oleatom v mešanici topil. V drugi stopnji smo raztopino oleatov, ki smo ji dodali različne količine oleinske kisline, segreli do vrelišča topila (heksadeken 282 °C ali oktadeken 316 °C). Na povišani temperaturi oleati razpadejo in tvorijo oksidne nanodelce. Na nanodelce je vezan monomolekulski sloj oleinske kisline, ki omogoča dispergiranje nanodelcev v nepolarnih topilih. Povprečna velikost nanodelcev kobaltovega ferita je odvisna od temperature, časa siteze in količine dodane oleinske kisline. Sintetizirani nanodelci v območju velikosti med 9 nm in 20 nm izkazujejo ferimagnetno vedenje ter magnetne lastnosti, ki se spreminjajo s povprečno velikostjo nanodelcev. Predpostavili smo mehanizem nastanka nanodelcev kobaltovega ferita, ki vključuje koalescenco manjših nanodelcev in njihovo rekristalizacijo.
Keywords: kobaltov ferit, nanodelci, magnetni nanodelci
Published: 27.07.2017; Views: 493; Downloads: 79
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Monolithic magneto-optical nanocomposites of barium hexaferrite platelets in PMMA
Gregor Ferk, Peter Krajnc, Anton Hamler, Alenka Mertelj, Federico Cebollada, Mihael Drofenik, Darja Lisjak, 2015, original scientific article

Abstract: The incorporation of magnetic barium hexaferrite nanoparticles in a transparent polymer matrix of poly(methyl methacrylate) (PMMA) is reported for the first time. The barium hexaferrite nanoplatelets doped with Sc3+, i.e., BaSc0.5Fe11.5O12 (BaHF), having diameters in the range 20 to 130 nm and thicknesses of approximately 5 nm, are synthesized hydrothermally and stabilized in 1-butanol with dodecylbenzenesulfonic acid. This method enables the preparation of monolithic nanocomposites by admixing the BaHF suspension into a liquid monomer, followed by in-situ, bulk free-radical polymerization. The PMMA retains its transparency for loadings of BaHF nanoparticles up to 0.27 wt.%, meaning that magnetically and optically anisotropic, monolithic nanocomposites can be synthesized when the polymerization is carried out in a magnetic field. The excellent dispersion of the magnetic nanoparticles, coupled with a reasonable control over the magnetic properties achieved in this investigation, is encouraging for the magneto-optical applications of these materials.
Keywords: polymer composites, nanoparticles, polymethyl methacrylate, PMMA
Published: 23.06.2017; Views: 666; Downloads: 364
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Priprava feritov MnZn s hidrotermalno obdelavo oksidov
Darko Makovec, Andrej Žnidaršič, Mihael Drofenik, 2004, original scientific article

Abstract: V članku poročamo o rezultatih raziskovalnega dela v okviru sodelovanja med Institutom "Jožef Stefan" in tovarno ISKRA Feriti, d.o.o., v katerem smo razvili nov postopek za masovno pripravo MnZn-feritov, ki temelji na pripravi feritnih prahov s hidrotermalno obdelavo izhodnih oksidov. Z omenjeno metodo smo dobili feritne prahove, ki so po fazni sestavo podobni tistim, pripravljenim po klasičnem keramičnem postopku. Priprava prahov po hidrotermalni metodi je zahtevala prilagoditev celotnega tehnološkega procesa priprave feritov. Prednost hidrotermalne metode pred klasičnim keramičnim postopkom je predvsem v manjši porabi energije, saj poteka termična obdelava oksidne mešanice pri relativno nizkih temperaturah (260 [kompozitum]C - 320 [kompozitum]C) ter bistveno krajših časih, hkrati pa se je izkazalo, da imajo hidrotermalni prahovi velik potencial pri pripravi feritov MnZn z izboljšanimi lastnostmi.
Keywords: priprava prahov, hidrotermalna sinteza, magnetni materiali, feriti MnZn
Published: 27.03.2017; Views: 467; Downloads: 61
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