Thermal decompositions of Y,La and light lanthanide thiodiglycolates

The conditions of thermal decomposition of the thiodiglycolates of Y, La and light lanthanides from Ce to Gd have been studied. On heating, these complexes decompose in various ways. Hydrated thiodiglycolates of La,Ce(III), Pr(III) and Gd lose crystallization water in one step, while those of Y, Nd, Sm and Eu(III) do so in two steps. The anhydrous complexes subsequently decompose in several steps to the oxysulfates Ln₂O_3–x((SO₄)_x.

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Zusammenfassung Bedingungen der thermischen Zersetzung der Thiodiglycolate von Y, La und den leichten Lanthaniden von Ce bis Gd wurden untersucht. Beim Erhitzen zersetzen sich diese Komplexe auf verschiedene Weise. Hydratisierte Thiodiglycolate von La, Ce(III), Pr(III) und Gd verlieren das Kristallwasser in einem Schritt, die von Y, Nd, Sm, und Eu(III) dagegen in zwei Schritten. Die wasserfreien Komplexe zersetzen sich in mehreren Schritten zu den Oxysulfaten Ln₂O_3–x(SO₄)_x.

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. . . , , , , , . Ln₂O_3–x(SO₄)_x.

     

Ultrathin functional films of titanium(IV) oxide

Chemistry and physics of thin semiconducting layers of various types are subjects of intense research. Especially when nanotechnology methods such as self-assembly are involved, amazing structural and/or functional properties may appear. Also modern physical methods using variously organized plasma arrangements are able to produce uniform structures with distinctive functionality. In this review, based virtually on our own work, discussions on the preparation, structure, morphology, and function of titanium(IV) oxide nanoscopic thin films are presented. It was shown that structurally and functionally similar titanium(IV) oxide films can be prepared via completely different preparation techniques. Function tests were arranged as “primary”, covering the assessment of the light induced charge separation efficiency, and “secondary”, based on photocatalytic surface oxidations.     

The DSC approach to study non-freezing water contents of hydrated hydroxypropylcellulose (HPC)

Journal of Thermal Analysis and Calorimetry - The research consisted of investigation of non-freezable bound water (NFW) contents of raw hydroxypropylcellulose (HPC) Klucel® Pharm HF, MF, and...     

Professor Jan Krzek (1946–2015)

JPC – Journal of Planar Chromatography – Modern TLC -     

Reversed-phase high-performance liquid chromatography determination of selected phenolic acids in propolis concentrates in terms of standardization for drug manufacturing purposes

A reversed-phase high-performance liquid chromatography method with gradient elution was developed for the determination of the caffeic, p-coumaric, and ferulic acids in propolis concentrates. Solid-phase extraction on an RP18 column was applied for preliminary purification, and chromatographic separation was performed on 100 RP18e Lichrospher column of particle size 5 microm. The mobile phase was obtained by mixing in appropriate ratios 0.03 mM NaH2PO4, acidified with H3PO4 up to pH = 3.0, with acetonitrile to obtain a gradient in the elution process. Spectrophotometric detection was conducted at 320 nm. Under the established conditions, the method featured high sensitivity, good precision, and comparability of results, as proven by method validation and statistical analysis of the obtained results. The limits of detection were 0.315, 0.325, and 0.695 microg/mL for caffeic, p-coumaric, and ferulic acids, respectively. The corresponding recovery values were 98.14, 101.05, and 99.42% and the linearity ranges from 1.31 to 99.18 microg/mL, 1.52 to 119.16 microg/mL, and 2.42 to 184.14 microg/mL. The precision of the method was expresed by relative standard deviation values that did not exceed 3%. It was also shown that the propolis concentrates under examination had similar antibacterial activity against Staphylococcus aureus ranging from 119.8 to 124.3 microg/mL, contrary to model mixtures that showed no antibacterial activity.     

用大孔凝胶阴离子交换剂从含亚氨二醛酸试液中分离镧、镨化合物

在采用阴离子交换剂从含氨基多羧酸试液中分离稀土的研究中 ,发现在醋酸和亚氨二醋酸试液中 ,稀土元素与亚氨二醋酸的亲合力顺序是 :Dy3 >Ho3 >Gd3 >Eu3 >Er3 >Y3 >Sm3 >Tm3 >Nd3 >Pr3 >>La3 。根据镧亲合力最小的特点 ,有可能将镧与其他稀土分离 (例如Pr)。在本研究中 ,采用了强碱性凝胶阴离子交换剂Dowex 1× 8(1型 )和Dowex 2× 8(2型 )以及强碱性大孔阴离子交换剂DowexMSA 1。研究表明 ,大孔离子交换剂其海棉状基质 ,孔径大于其分子直径 ,故大离子的交换速度快。另外 ,大孔凝胶阴离子交换剂可在亚氨二醋酸试液中将La ,Pr分离而提纯出镧化合物。     

Quantification of Saponins in Different Plant Parts of Lysimachia L. Species by validated HPTLC—Densitometric Method

JPC – Journal of Planar Chromatography – Modern TLC - Quantitative high-performance thin-layer chromatography (HPTLC) analysis of triterpene saponins in different parts of eight...     

Growth and properties of Ti-Cu films with respect to plasma parameters in dual-magnetron sputtering discharges

Properties of different methods of magnetron sputtering (dc-MS, dual-MS and dual-HiPIMS) are studied and compared with respect to intermetallic Ti-Cu film formation. The quality and features of thin films are strongly influenced by the energy of incoming particles. The ion velocity distribution functions (IVDFs) were measured by time-resolved retarding field analyzer (RFA) in the substrate position. Thin films were characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffractometry (XRD) and X-ray reflectometry (XR). Properties and crystallography of Ti-Cu films are discussed as a function of ion energy which is affected by the mode of sputtering. It was found that IVDFs measured in pulsed discharges exhibit double-peak distribution. The IVDFs reach the maximum at ion energies about  ~8 eV. The ion saturated current is highest in dual-HiPIMS discharge (~5 μA/cm²) and is mostly represented by Cu⁺ and Ar⁺ ions. The mode of sputtering influences chemical composition and film formation. The copper forms polycrystalline fcc-phase while much smaller Ti particles enwraps the copper crystallites or are part of a solid solution.     

Thin-layer chromatography-densitometric measurements for determination of N-(hydroxymethyl)nicotinamide in tablets and stability evaluation in solutions

A thin-layer chromatography (TLC)-densitometric method was developed to determine N-(hydroxymethyl)nicotinamide in tablets and basic solutions along with nicotinic acid. Analysis was performed on silica gel F254 plates using chloroform-ethanol (2 + 3, v/v) mobile phase. The densitometric observations were made at 260 nm. The results showed good precision and accuracy; relative standard deviation was 2.37%, and recovery ranged from 97.60 to 100.82%. The limit of detection was 0.1 microg/spot, while the linearity range was from 0.2 to 1.75 microg/spot. Applicability of the newly developed method was tested for determination of N-(hydroxymethyl)nicotinamide in the preparation Cholamid. Densitometric measurements were used to evaluate stability of N-(hydroxymethyl)nicotinamide in basic solutions. It was found that decomposition corresponded to first-order reaction kinetics. The computed kinetic and thermodynamic parameters at 30 degrees C were as follows: k = 0.00675/min, t0,5 = 1.71 h, t0,1 = 0.26 h, and Ea = 44.75 kJ/mol.     

Photodegradation assessment of amisulpride,doxepin, haloperidol,risperidone, venlafaxine,and zopiclone in bulk drug and in the presence of excipients

Monatshefte für Chemie - Chemical Monthly - Photostability of amisulpride, doxepin, haloperidol, risperidone, venlafaxine, and zopiclone in APIs and powdered tablets during exposure to UVA...