Round-bottomed Flask Research Articles

Heteroleptic Cu-Based Sensitizers in Photoredox Catalysis.

Photochemistry is an important tool in organic synthesis that has largely been underdeveloped in comparison to thermal activation. Recent advances in technology have ushered in a new era in synthetic photochemistry. The emergence of photocatalysis, which exploits sensitizers for the absorption of visible light, has provided organic chemists with a new route to the generation of radical intermediates for synthesis. Of particular interest is the development of Cu-based complexes for photocatalysis, which possess variable photophysical properties and can display complementary reactivity with common photocatalysts based on heavier transition metals such as Ru or Ir. Heteroleptic Cu-based sensitizers incorporating the presence of both a bisphosphine and diamine ligand bound to the copper center are a promising class of photocatalysts. Their synthesis is a single step, often involving only precipitation for purification. In addition, it was shown that the sensitizers could be formed in situ in the reaction mixture, simplifying the experimental setup. The heteroleptic nature of the Cu-complexes also affords opportunities to fine-tune properties. For example, structurally rigidified bisphosphines reinforce geometries about the metal center to extend the excited state lifetime. Variation of the diamine ligand can influence the excited state oxidation/reduction potentials and optical absorbances. The heteroleptic complex Cu(XantPhos)(neo)BF4 has demonstrated utility in the synthesis of helical polyaromatic carbocycles. The synthesis of [5]helicene, a relatively simple member of the helicene family, was improved from the existing UV-light mediated method by eliminating the formation of unwanted byproducts. In addition, the Cu-based sensitizers also promoted the formation of novel pyrene/helicene hybrids for materials science applications. The synthetic methods that were developed were augmented when combined with continuous flow technology. The irradiation of reaction mixtures as they are pumped through small diameter tubing provides a more homogeneous and increased photon flux compared with irradiation in round-bottom flasks or other batch reactors. The value of continuous flow methods is also evident when examining UV-light photochemistry, where the simple and safe experimental set-ups allow for further exploration of high energy light for synthetic purposes. The synthesis of functionalized complex carbazoles was also studied using both a visible light method exploiting a heteroleptic copper-based sensitizer and a UV-light mediated method. It was demonstrated that both the photocatalysis methods and UV light photochemistries were rendered more user-friendly, safe, and reproducible when using continuous flow methods. Interestingly, the two photochemical methods often afford contrasting selectivities as a result of their inherently different mechanisms. It can be expected that the complementarity of the various photochemical methods will be an asset to synthetic chemists as the field continues to evolve.

Obtaining of Oxycellulose from Cotton Fibers by Action of Various Oxidants

Background. Development of production technologies of materials for various purposes of alternatives to crude oil and natural gas sources of raw material, in particular cellulose.Objective. To determine the optimal values of technological parameters of cotton fiber oxidation by action of various oxidants – hydrogen peroxide, Oxone, PINO – on quality of oxycellulose.Methods. Oxidation of mechanically chopped cotton fibers by solution of hydrogen peroxide, Oxone and PINO was performed with air bubbling by the compressor through solution of cellulose in round-bottomed flask immersed in a water bath of the required temperature. The methods of experiment planning and optimization were used to determine the optimum process parameters.Results. Studied oxidants for oxycellulose of cotton fibers to increase efficiency are in the following order: hydrogen peroxide – Oxone – PINO. The method of full factorial experiment was used to determine the adequate regression equations that describe the process of oxycellulose obtaining by action of Oxone and PINO, and the Gauss-Seidel method was used to determine the optimal values of technological parameters of oxycellulose obtaining. It is shown that oxidation of cotton fibers for optimal values of technological parameters allows getting oxycellulose with the content of carboxyl groups to 3 %.Conclusions. The obtained oxycellulose can be used in medicine as a component of non-toxic, hemostatic, antimicrobial materials.

Screening of Ionic Liquids for Pretreatment of Taiwan Grass in Q-Tube Minireactors for Improving Bioethanol Production

In this study, a series of ionic liquids including conventional, protic and Bronsted acidic-type ionic liquids were evaluated as media for the pretreatment of Taiwan grass. The pretreatments were carried out in parallel format, for the first time, in a novel glass reactor known as Q-tube®. Based on the results, the Q-tube® was very efficient for the pretreatment of our lignocellulosic materials in comparison with the conventional equipment (round bottom flask). Pretreatments were completed in one hour with high yield of reducing and total sugars after enzymatic hydrolysis. Some protic and Bronsted acidic ionic liquids can depolymerize partially the cellulosic material in one step and after enzymatic hydrolysis the content of reducing sugars is up to 35 times higher in comparison with the material without pretreatment.

Conventional and modified hydrodistillation method for the extraction of glucosinolate hydrolytic products: a comparative account.

Eruca sativa is extensively used as raw and its oil is also used for cooking due to its exceptional flavour. The volatile nature of the hydrolytic products of glucosinolates makes the extraction difficult. The hydrodistillation method used previously yield very less amount of the extract as well as the absence of stirring in the round bottom flask causes burning of both the crushed seeds and the flask. To overcome these drawbacks, a method has been developed using magnetic stirrer and hot plate. The yield and composition of hydrolytic products in the extract with the modified method was increased along with an increase in the amount of major hydrolytic products as seen by GC–MS. This method thus has immense potential in pharmaceutical industries, due to the ease of extraction and isolation.

Ice-shell purification of ice-binding proteins

Ice-affinity purification is a simple and efficient method of purifying to homogeneity both natural and recombinant ice-binding proteins. The purification involves the incorporation of ice-binding proteins into slowly-growing ice and the exclusion of other proteins and solutes. In previous approaches, the ice was grown around a hollow brass finger through which coolant was circulated. We describe here an easily-constructed apparatus that employs ice affinity purification that not only shortens the time for purification from 1–2 days to 1–2 h, but also enhances yield and purity. In this apparatus, the surface area for the separation was increased by extracting the ice-binding proteins into an ice-shell formed inside a rotating round-bottom flask partially submerged in a sub-zero bath. In principle, any ice-binding compound can be recovered from liquid solution, and the method is readily scalable.

Autonomous Chemical Oscillator Circuit Based on Bidirectional Chemical‐Microfluidic Coupling

Autonomous Chemical Oscillator Circuit Based on Bidirectional Chemical‐Microfluidic Coupling

Cool Lab Tool Debuts

Rotary evaporators, which chemists fondly refer to as rotovaps, are used to swirl a sample in a round-bottom flask like a wine connoisseur swirls an expensive glass of Bordeaux. But instead of tryi...

Inhibition of Frying Oil Oxidation by Carbon Dioxide Blanketing.

The oxidation of oil starts, in general, from the penetration of atmospheric oxygen into oil. Inhibition of the vigorous oxidation of oil at deep-frying temperature under carbon dioxide flow, by disrupting the contact between oil and air, was first demonstrated using oil in a round bottom flask. Next, the minimum carbon dioxide flow rate necessary to blanket 4 L of frying oil in an electric fryer (surface area 690 cm(2)) installed with nonwoven fabric cover, was found to be 40 L/h. Then deep-frying of potato was done accordingly; immediately after deep-frying, an aluminum cover was placed on top of the nonwoven fabric cover to prevent the loss of carbon dioxide and the carbon dioxide flow was shut off. In conclusion, the oxidation of oil both at deep-frying temperature and during standing was remarkably inhibited by carbon dioxide blanketing at a practical flow rate and volume. Under the deep-frying conditions employed in this study, the increase in polar compound content was reduced to half of that of the control.

Development and characterization of lecithin-based self-assembly mixed micellar drug delivery systems for curcumin

Event Abstract Back to Event Development and characterization of lecithin-based self-assembly mixed micellar drug delivery systems for curcumin Ling-Chun Chen1*, Yin-Chen Chen1, Chia-Yu Su1, Wan-Ping Wong1, Ming-Thau Sheu1* and Hsiu-O Ho1 1 Taipei Medical University, College of Pharmacy, Taiwan Curcumin is the active ingredient extracted from the root of Curcuma longa. However, the great therapeutic applications of curcumin are restricted because of its low aqueous solubility, rapid hydrolysis in alkaline media, light instability and hydrophobic character, resulting in poor bioavailability (BA) (only 1% in rats). Mixed polymeric micelle (MPM), which is able to increase the volume of the hydrophobic core by incorporating extra hydrophobic materials providing larger space for hydrophobic drugs to be solubilized, was developed to overcome major obstacles associated with curcumin delivery. Lecithin is a biocompatible surfactant which is an important component of cell membrane and makes drug easily absorbed, and an additional amphiphilic polymer (sodium dedoxycholate (NaDOC), d-alpha tocopheryl polyethylene glycol succinate (TPGS), Cremophor® and Pluronic® series) were added to form MPM. Curcumin-MPM was prepared by thin film method. Briefly, a predetermined ratio of curcumin, lecithin and another polymer (NaDOC, Pluronic® series of F87, F127, F68, L121, F108, and P123, TPGS, and Cremophor® RH40 and ELP) were added into 1 mL of mixed solvent (Methanol/dichloromethane=3/7, v/v) in the round bottom flask. The mixture was shaken and subsequently evaporated by rotary evaporation under reduced pressure to remove solvent and obtain a thin film. Self-assembly of the thin films resulting in micelle formation was formed by adding 1 mL of deionized water and shook the micelle solution gently until the thin film was completely dispersed. Self-assembling curcumin-MPM was evaluated to determine characteristics such as the average particle size and size distribution, encapsulation efficacy [EE] and drug loading [DL]. After formulation optimization, the formulations were curcumin/ lecithin/ NaDOC= 2/1/5 and curcumin/lecithin/Pluronic® P123=5/2/20, with particle size of less than 200 nm, EE of >80%, and DL of >10%. The formulated system efficiently improved the stability of curcumin in PBS at room temperature or 4 ℃, and in FBS or PBS at 37℃, and retarded in vitro curcumin release. In vivo PK studies shows for oral administration, the absolute BA was 3- and 5-fold increased for curcumin-loaded NaDOC and Pluronic® P123 MPM, respectively; for intravenous administration, the absolute BA was 2.32- and 5.73-fold improvement for curcumin-loaded NaDOC MPM and Pluronic® P123 MPM, respectively.Whereas, for native curcumin solution, the level was not detected beyond 24 h and 2 h with oral and intravenous administration. Our results suggested the slow release of curcumin from micelles, reduced degradation, and prolonged duration resulted in the increase of BA in rats regardless of oral or intravenous administration. In conclusion, lecithin-based MPM represented a useful curcumin delivery system, thereby improving the solubility, stability and BA of curcumin. The enhancement of curcumin BA via lecithin-based MPM can bring this natural molecule to the forefront of therapeutic agents which can treat dreadful cancer. Figure1. Plasma concentration-time curves of curcumin after intravenous administration of lecithin-based mixed micelles (NaDOC and Pluronic® P123) and free curcumin (5 mg/kg) to rats. Figure2. Plasma concentration-time curves of curcumin after oral administration of lecithin-based mixed micelles (NaDOC and Pluronic® P123) and free curcumin (100 mg/kg) to rats. NSC 102-2320-B-038 -022 -MY3

Preparation of 1,5-Dioxaspiro[5.5]undecan-3-one.

A. 3-Amino-3-(hydroxymethyl)-1,5-dioxaspiro[5.5]undecane. A 1-L single-necked, round-bottomed flask is equipped with an egg-shaped, Teflon®-coated magnetic stirring bar (3.5 cm x 1.5 cm), capped with a rubber septum, flame-dried under vacuum, and cooled under an argon atmosphere (Note 1). After cooling to ambient temperature (21-23 °C), to the flask is added anhydrous N,N-dimethylformamide (DMF, 365 mL, 0.78 M) via cannula. Subsequently, tris(hydroxymethyl)aminomethane hydrochloride (45.0 g, 286 mmol, 1.00 equiv) (Note 2 and 3) is added in a single portion as white crystalline solid. The reaction vessel is immediately resealed with a rubber septum under inert atmosphere and stirring is commenced (Figure 1). To this white suspension is added 1,1-dimethoxycyclohexane (50.0 mL, 47.4 g, 329 mmol, 1.15 equiv) via syringe in one portion (Note 4). Lastly, to the off-white slurry is added para-toluenesulfonic acid monohydrate (p-TsOH•H2O, 1.63 g, 8.57 mmol, 0.03 equiv) as a solid in one portion quickly, immediately replacing the rubber septum to maintain an inert atmosphere.

Potassium tert-Butoxide-Catalyzed Dehydrogenative Cross-Coupling of Heteroarenes with Hydrosilanes

A. 1-Methyl-2-(triethylsilyl)-1H-indole (2). An oven-dried 100-mL round-bottom Schlenk flask is equipped with a Teflon-coated magnetic stir bar (25 x 8 mm) and capped with a rubber septum (Note 1). The side arm of the flask is connected to Schlenk line and the flask is cooled to room temperature under vacuum and back-filled with nitrogen. Potassium tert-butoxide (1.34 g, 12.0 mmol, 0.2 equiv) is added to the flask under positive nitrogen flow (Notes 2 and 3), and then the flask is evacuated and back-filled with nitrogen three times. N-Methylindole (7.48 mL, 7.86 g, 60.0 mmol, 1.0 equiv) and triethylsilane (28.6 mL, 20.82 g, 179.5 mmol, 3.0 equiv) are added sequentially via syringe through the septum, resulting in a yellow heterogeneous mixture (Figure 1). After the septum is replaced with a glass stopper (Note 4), the reaction mixture is degassed (Note 5) and stirred at 45 oC for 76 h (Note 6), resulting in a dark purple solution. The heating bath is removed and the reaction mixture is allowed to cool to ambient temperature (~25 oC), then anhydrous diethyl ether (30 mL) is added slowly while stirring (Note 7).

Preparation, characterization, and blood compatibility of polyurethanes derived from aliphatic diisocyanates and polycarbonate urethane

Event Abstract Back to Event Preparation, characterization, and blood compatibility of polyurethanes derived from aliphatic diisocyanates and polycarbonate urethane Xinyu Wang1, 2, Rong Zhu1, 2, Zongrui Zhang1, 2, Daiwei Ma1, 2 and Mingbei Zhu1, 2* 1 Wuhan University of Technology, State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, China 2 Wuhan University ofTechnology, Biomedical Materials and Engineering Research Center of Hubei Province, China Introduction: In this study, to obtain biomedical polyurethane elastomers with good mechanical properties and biocompatibily [1],a series of polycarbonate urethanes were synthesized via a two-step solution of polymerization method using the poly(1,6-hexanediol)carbonate diols (PCDL) as the soft segment, 4,4’-methylenebis(cyclohexyl isocyanate) (H12MDI), 1,6-hexamethylene diisocyanate (HDI) and 1,4-butanediol (BDO) as the hard segment with dibutyltin dilaurate as the catalyst. In this article, we illustrated the physical behaviors were obviously influenced by synthetic routes. And their chemical and physical structures were investigated by GPC,DSC,FT-IR and mechanical properties tests [2]. The surface wettability were studied by contact angle measurement (CA). A comparative analysis was made between the commercial medical polyurethane materials and the synthesized materials, showing the poly(carbonate-urethane) elastomers were better in mechanical properties [3]. Finally, the results of the hemolysis and platelet adhesive tests were recorded by spectrophotometer and SEM, indicating the materials were in accordance with the standard for biomaterials. Materials and Methods: The polyurethane films can be easily synthesized via a two-step reaction using PCDL and diisocyanate coupled with a chain extender BDO.And all the reagents added to the reacting round-bottomed flask were dissolved in DMAc or DMF. After that, the mixture was cast into a beaker for precipitation, with ether-water solution in it. And then the polymer was placed in Soxhlet extrator using deionized water as extracing agent for removing small molecules for at least 24h. And then, after being dissolved in THF (7.5 wt%) with stirring at 800 r/min for 2 h, the polyurethane solution was placed in a vacuum oven at 45℃. Finally, in order to keep the surface of the polyurethane flat, the prepared polymer solution was put in homemade molds carefully for drying at room temperature. The tests on mechanical properties could be carried out after drying in the vacuum oven at 40 ℃ for at least 5 days. Results and Discussion: The polycarbonate polyurethane films have been successfully synthesized and the results of CA measurement indicated H12MDI-PUs were better in hydrophobic property. As for mechanical properties showed in, the series of polyurethane films were better than Pellethane 2363-80A did, especially for H12MDI 1.5-PU. It displayed tensile strength of less than 10 MPa and showed the best properties in elongation getting about 850% at break. The results of the hemolytic tests indicated the materials were in accordance with the standard for biomaterials and the SEM pictures of platelet adhesion experiment in showed there were little platelet adhering to the polyurethane films. In order to get more advantages as a kind of short-term biomaterial, we’ll concentrated on doing some researches to enhance the hydrophobicity and improve the biocompatibility without reducing the mechanical properties. Conclusion: In this article, the physical properties of our prepared polymers were even better in flexibility and elongation at break after the comparison with a commercial biomedical polyurethane. Our ongoing work have demonstrated that H12MDI 1.5-PU has great potential in biomedical field. In order to get better applications as a candidate for elastic biomedical material, some modifications are still should be made to improve their biocompatibility. The HongKong, Macao and Taiwan Science & Technology Cooperation Program of China (No.2015DFH30180); the Key Grant Project of Chinese Ministry of Education (No.313041); the Key Technology Research Plan of Wuhan Municipality (No.2014060202010120); the Fundamental Research Funds for the Central Universities (WUT:2014-Ⅶ-028)

Utilización del colorante índigo en el laboratorio docente de Química Orgánica

Indigo is one of the first examples of vat dyeing, being the reduction of the dye to its soluble form (leuco-indigo) the critical step of that process. A new method to address such reduction reaction has been tested which improves the overall results for the staining with this dye, at a didactic level in an Organic Chemistry laboratory practice. The innovation introduced consists of using a small sized round-bottom flask along with a balloon and a needle to release the inner overpressure. Compared to the traditional process, the new method allows for the reduction at lower temperatures (30°C vs. 66°C) and a more homogeneous fabric dyeing.

Composition of the essential oil of two Salvia taxa (Salvia sclarea and Salvia verticillata subsp. verticillata) from Turkey

Objective: The essential oil composition of two Salvia taxa (Salvia sclarea and Salvia verticillata subsp. verticillata) analysed and yield of compositions were analysed Material and Methods: The essential oil was extracted by hydro distillation using a modified Clevenger apparatus coupled to a 2 L round-bottom flask. A total of 100 g of fresh plant material (aerial parts) and 1 L of water were used for the extraction. Gas chromatography / Mass spectrometry (GC-MS) analysis were applied to extracts. Results: The essential oil yields of Salvia sclarea and Salvia verticillata L. subsp. verticillata were found as 0.4 and 0.3 %v/w, respectively. Overall, thirty seven compounds which accounted for 97.9% in Salvia sclarea and seventy four constituents, which accounted for 98.6% of the total compositions of each oil are determined in Salvia verticillata L. subsp. verticillata. The spathulenol (19%), caryophyllene oxide (15.5%), linolyl acetate (11.3%) and linalool L (8.5%) were the major compounds of Salvia sclarea and the germacrene D (13.8%), spathulenol (10%) and limonene (4.5%), 1.8- cineole (4.5%) were the main compounds of the Salvia verticillata L. subsp. Verticillata Conclusion: spathulenol was found as major compound for both Salvia sclarea and Salvia verticillata subsp. verticillata while, the other main components were not showed similarity

THE COMBINATION OF DIFFERENT MODELING TECHNIQUES TO ARCHAEOLOGICAL VESSELS, DATA TRASOLOGICAL EXPERIMENTAL AND ETHNOGRAPHIC

The study of technological methods of manufacturing ceramic materials is considered by the example of the Maikop culture in the North Caucasus and the data of ethnography. As an example the experimental simulation of round-the Maikop culture vessels, made by several methods. Trasological study of the structure of the test pieces of ceramics in the fracture showed that it is possible to determine the area of joints tapes. External and internal ceramic surface smoothed, but you can define a manual molding of thin lines multidirectional polishing. Manual molding can also be defined and some fragments of ceramics on its inner surface, to maintain the following bands modeling and smoothing the surface of joints by hand. Some fragments have a very dense homogeneous structure, which is formed as a result of receiving use knockout, using a wooden spatula or forging of vessel walls using stone tools on both sides. Some techniques for making vascular managed modeled by experiments. Research data on the manufacturing technique of ethnography round bottom flask showed that the modeling techniques such vessels much more. The paper presents the archaeological, ethnographic and experimental data on manufacturing as the flat-bottomed and round bottom flask using a technique manual molding, punch and forging (forging the walls of stone tools from both sides). Recently, using the technique of punch it was carried out a series of experiments on modeling the round bottom flask. Trasological study technology of round bottomed flask with two knockout techniques, not previously considered.

Distillation Assisted by Microwave for Extracting Essential Oil from Java Cananga Flowers

Cananga oil is one type of essential oil that called etheric oil or light oil. To increase the production of canangaoil, it is need to improve distillation methods and operating conditions, so that extraction process can producecananga oil more efficient. The aims of this research are to study several factors that influence the distillationmethods assisted by microwave, i.e.: flowers conditions, extraction time, mass of material, and microwave power.The experiment was conducted in a round bottom flask distiller that was placed inside a microwave oven andequipped with a Liebig condenser. The operating variables are: flowers conditions (fresh, wilted, chopped). Thecontent of distiller (100, 150, 200 gr). The results of this research shows that the yield of fresh flowers (0.6251 -1.1965%) were higher than wilted flowers (0.5391 - 1.0755%). The mass ratio of material by volume ofdistillation flask influences on yield obtained. The denser of material, the less of oil yield be obtained. The oilyield increase with time extraction, microwave power and temperature. The distillation assisted by microwave ismore efficient than conventional distillation, because we can increase the oil yield with shorter extraction time.The quality of cananga oil obtained by distillation assisted by microwave is conforming to quality standard ofIndonesian (SNI) and Essential Oil Association (EOA).

The influence of different agitation techniques on the adsorption kinetics of 4-chlorophenol on granular activated carbon

The influence of different agitation techniques on the adsorption of organic compounds, represented by 4-chlorophenol, onto granular activated carbon was investigated. The effect of the flask type and the type of agitator, including a laboratory shaker, mechanical agitator, magnetic stirrer as well as mixing with gas bubbles, was studied. The results of adsorption kinetics demonstrate that the adsorption process of 4-chlorophenol on the activated carbon follows a pseudo-second order kinetic model closely. The adsorption equilibrium was reached faster in the Erlenmeyer flask than in the round-bottomed flask. At the same agitation speed (200 rpm), the better adsorption rate and adsorption efficiency were observed using the mechanical and magnetic stirrers than the laboratory shaker. At the gas flow rate of 1.5 dm3 min−1, the mixing with the air or nitrogen bubbles was comparable with the agitation when using mechanical and magnetic stirrers at 200 rpm. The effect of the agitation speed on the adsorption of the 4-chlorophenol by the activated carbon was also tested. The kinetic experiments were carried out at 100, 200, 300 and 500 rpm and it was found that the adsorption rate increases with the increase in the agitation speed. As the stirring rate increased from 100 to 500 rpm, the adsorption rate constants increased from 0.577 to 1.264 g mmol−1 h−1 (mechanical agitator) and from 0.560 to 1.231 g mmol−1 h−1 (magnetic stirrer), respectively. The experimental results demonstrate that the agitation affects the adsorption kinetics significantly as well as the adsorption equilibrium of the organic compounds on the activated carbon, and should be taken into account in such studies.

Low-Cost Nickel Hexacyanoferrate Nanoparticle As Cathode Material of Lithium-Ion Batteries for Large-Scale Applications

1. Introduction Rechargeable lithium ion batteries become a solution to the world’s ever-increasing demand for energy storage and created excellent opportunities for communication via portable electric devices. However, LIBs are limited to the portable electronic devices and are still too expensive to be used in large-scale applications such as renewable energies. Transition metal hexacyanoferrates (MHCFs) are promising cathode materials because of easy production, low cost and promising electrochemical performance. MHCF were investigated as hosts for alkali ions in 1999 [1]. In 2012, Prof. J. Goodenough’s group showed promising Na ion battery using MHCF as a cathode [2]. In this work, NiHCF is synthesized via a simple co-precipitation method. This cathode showed very promising performance in LIBs with stable cycle life and flat charge/discharge plateaus. 2. Experiments NiHCF was synthesized via a simple co-precipitation method. Typically, 0.01 mol Ni(NO3)2 and 0.005 mol K3Fe2(CN)6were dissolved in 250 mL DI water, respectively. These two solutions were added dropwise into DI water in a round bottom flask under magnetic stirring at 70 °C [3]. The yellow precipitates were filtered, washed and dried in a vacuum oven at 35 °C for 72 h. The NiHCF was characterized by XRD (X’Pert PRO, PANalytical) and TEM (Libra 120, Carl Zeiss). NiHCF was homogeneously mixed with Acetylene Black (MTI Co.), polyvinylidene difluoride (Kynar) in 8:1:1 ratio and coated on a carbon current collector (Alfa Aesar), and dried in 35 °C for 24 h. The mass loading of NiHCF was around 4-5 mg/cm2. CR2032 coin cells were assembled to investigate NiHCF electrochemical behavior. Lithium chips was used as reference/counter electrode, Celgard 2400 was used as a separator and 1 M LiPF6 in EC:DEC:DMC (1:1:1 vol.) was used as electrolyte. The electrochemical investigations were carried out using galvanostat/potentiostat tester (VMP3, Biologic). 3. Results and discussion The pure NiHCF phase was confirmed from the XRD result, and sharp characteristic peaks indicated good crystallinity of NiHCF as presented in Fig. 1a. Transmission electron microscopy (Fig. 1b)showed that NiHCF consisted of agglomerated nanoparticles around 20–50 nm in size. Fig. 2 is the cyclic voltammetry of NiHCF at 0.1 mV s-1 between 2 - 4.2 V vs. Li/Li+. NiHCF has a well distinguished pair of symmetric peak around 3.3 V, which corresponds to the lithiation/delithiation of NiHCF during discharge and charge process. The charge/discharge profiles are shown in Fig. 3. The excellent flat plateaus around 3.3 V are well-matched with the CV results in Fig. 2. NiHCF showed a capacity of 52 mAh g-1at a current density of 0.2 C, which is about 87% of its theoretical capacity. Further information and results on this research will be presented at the Meeting. Acknowledgments This research was supported by the Institute of Batteries LLC, a research grant from the Ministry of Education and Science of Kazakhstan, and a Research Project from Nazarbayev University.

Amino Acids from Lichens of the Genera Cladina and Cladonia

The protein content in samples of the studied species were determined by the Lowry method [4], which is based on formation of a colored complex from the reaction of the protein with an alkaline solution of copper sulfate and sodium tungstate and molybdate. The protein content in C. stellaris was 0.48%; C. mitis, 0.65; and C. uncialis, 0.62. Amino acids in the aqueous extract that was passed beforehand over a column of Al 2 O 3 (h = 4 cm, d = 2 cm) in order to remove phenolic compounds were detected using TLC. The eluate was chromatographed in ascending mode on Silufol plates using PrOH–H 2 O (70:30, 1), BuOH–HOAc–H 2 O (8:2:2, 2), and EtOH (96%)–NH 4 OH (conc.) (16:4.5, 3). Plates were preheated at 110°C for 30 min. Extract (0.005 mL) was placed at the origin of the chromatography plate using a micropipette. The plate with sample was dried in air for 15 min and placed into a previously saturated chamber. When the solvent front reached the end of the plate, the plate was removed, dried in air to remove completely the solvent, treated with alcoholic ninhydrin (0.5%), and heated in a drying cabinet at 60°C for 10 min [5, 6]. Spots of amino acids were separated best using solvent system 1. Lichen C. stellaris showed five spots with R f1 0.024 (violet) and R f2 0.36, R f3 0.41, R f4 0.51, and R f5 0.63 (orange); C. mitis, two spots with R f1 0.65 (violet) and R f2 0.72 (pink); C. uncialis, two spots with R f1 0.64 and R f2 0.73 (pink). The color intensities of the spots were different. Thus, lichen C. stellaris contained at least five free amino acids; C. mitis and C. uncialis, at least two. The amino-acid composition was studied further using an AAA 339 amino-acid analyzer (Czech Rep.). Total amino acids were extracted from ground lichens (~10.0 g, accurate weight) using refluxing EtOH (80%, 150 mL) in a 250-mL roundbottomed flask on a boiling-water bath for 1 h. Pulp was separated by centrifugation and rinsed with EtOH (80%, 20 mL). The combined extracts were purified of phenolic substances by passage over a column of Al 2 O 3 . The resulting extract was evaporated to a small volume (10 mL), and treated with EtOH (50 mL) to precipitate polymeric compounds. The precipitate was separated by centrifugation. The filtrate was evaporated to a dry solid that was dissolved in citrate buffer (5 mL), a part (100 L) of which was passed over the column (0.6 22 cm, DF-6 ion-exchange resin, 50–65°C, flow rate 25 mL/h) of the amino-acid analyzer. The eluent was sodium citrate buffer of sequential pH values 5.2, 4.0, and 2.0. The qualitative composition of the amino acids in the samples was determined from retention times. The internal standard was a standard mixture of 17 amino acids. The quantitative contents of the detected amino acids were calculated in mg% of the absolute dry raw material. Peak areas were used as the quantitative parameter. The amino-acid analyzer was calibrated using nanomolar standard amino-acid samples. Table 1 presents the analytical results.

Pharmaceutical process chemistry: evolution of a contemporary data-rich laboratory environment.

Over the past 20 years, the industrial laboratory environment has gone through a major transformation in the industrial process chemistry setting. In order to discover and develop robust and efficient syntheses and processes for a pharmaceutical portfolio with growing synthetic complexity and increased regulatory expectations, the round-bottom flask and other conventional equipment familiar to a traditional organic chemistry laboratory are being replaced. The new process chemistry laboratory fosters multidisciplinary collaborations by providing a suite of tools capable of delivering deeper process understanding through mechanistic insights and detailed kinetics translating to greater predictability at scale. This transformation is essential to the field of organic synthesis in order to promote excellence in quality, safety, speed, and cost efficiency in synthesis.