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Abstract

Advances in science and technology are now at the heart of the global economy, but the number of students earning degrees in the sciences, technology, engineering, and math (STEM) fields has stalled. According to the National Association for Colleges and Employers (NACE), programs have been initiated nationwide to nurture interest in the sciences, including research competitions, co-ops and internships, and K-12 STEM education. Senior thermal analysis scientists are not only researchers, they are role models, mentors and teachers intimately involved in the recruitment and training of young scientists. The authors present guidelines for thermal analysis research project planning for high school students, undergraduate students and master’s and doctoral candidates. Project planning includes developmentally appropriate techniques, methods, instruments, scope and significance. Case studies illustrate examples of short-term, concrete materials analysis projects tailored to younger student researchers, as well as master’s level projects making significant contributions to the state of the science and innovative doctoral research. In addition to designing projects for students at all levels, senior thermal analysis scientists can use specific teaching and training techniques to help young scientists develop their abilities in the lab and at the podium.

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Journal of Thermal Analysis and Calorimetry
Authors: Cheila G. Mothé, Michelle G. Mothé, Alan T. Riga, and Kenneth S. Alexander

Abstract

Thermal properties of some shedded snake skins in comparison with human skins are represented by thermogravimetry (TG), derivative thermogravimetry (DTG), and differential thermal analysis (DTA) to predict process condition as dermal pathway for administration of drugs or it be used as model membranes for permeation studies. Thermal behavior by TG/DTG and DTA curves for four kinds of shedded snake skins as Boelens Python (BP), Eastern Indigo Snake (EIS), Emerald Tree Boa (ETB), and Cascavel (CBR) were similar in relation to their decomposition temperatures at 100 °C and 230–400 °C of its constituents, however, their properties were different in the residue content (inorganic or carbonaceous substances). Similar thermal properties were also exhibited by human skins’ samples, however, they presented different residue and constituents’ content.

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Abstract

Cytokines are small regulatory proteins secreted mostly by cells of the immune system. Cytokines participate in anti-inflammatory and pro-inflammatory processes in the body and in responses to host exposure to pathogens. In this study, the thermal behavior of human recombinant cytokines and soluble cytokine receptors; IFNγ, TNFα, IL-1 receptor antagonist, soluble TNF-receptor types 1 and 2, and sIL-2 receptor α were analyzed by dielectric thermal analysis at 37 °C and by thermogravimetry. Measurements were performed at a frequency range of 0.1–300,000 Hz. Permittivity and loss factor measurements were used to calculate mobility of charges (tan δ values) in the proteins from Debye plots. Peak frequencies and polarization times were used to determine dielectric signatures for each cytokine and receptor. Peak frequencies and polarization times were obtained for each cytokine and receptor analyzed. Detection of unique dielectric signatures of the proteins will aid development of sensitive dielectric sensors capable of detecting cytokines and soluble cytokine receptors in various human samples for malaria diagnosis.

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Journal of Thermal Analysis and Calorimetry
Authors: Libby Yoerg, M. Ellen Matthews, Lakshmi Kaza, Naullage Indika Perera, David W. Ball, John Moran, and Alan T. Riga

Abstract

Three aldohexose monosaccharides, d-glucose, d-mannose, and d-galactose, were examined by scanning temperature dielectric analysis (DEA) from ambient temperatures through their melts. Phase transitions, including glass transition (T g) and melting temperature (T m), were evaluated by differential scanning calorimetry (DSC). The monosaccharides were found to exhibit thermally-induced dielectric loss spectra in their amorphous-solid phase before melting. Activation energies for electrical charging of each of the monosaccharides were calculated from an Arrhenius plot of the tan delta (e″/e′, dielectric loss factor/relative permittivity) peak frequency versus reciprocal temperature in Kelvin. The DEA profiles were also correlated with the DSC phase diagrams, showing the changes in electrical behavior associated with solid–solid and solid–liquid transitions.

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Journal of Thermal Analysis and Calorimetry
Authors: Lakshmi Kaza, Hany F. Sobhi, Jeffrey A. Fruscella, Chris Kaul, Shravan Thakur, Naullage I. Perera, Kenneth Alexander, and Alan T. Riga

Abstract

A standard protocol was developed to determine the water content by thermal analysis of milk of magnesia (MoM). Differential scanning calorimetry (DSC) and thermogravimetry (TG) were used in a novel manner for examining the physical characteristics of the commercial pharmaceutical suspensions. Moisture analyzer and oven-dry methods validate the proposed protocol. MoM consists primarily of water and magnesium hydroxide [Mg(OH)2]. Experimental design of the thermal analysis parameters were considered including sample size, flowing atmosphere, sample pan, and heating rate for both DSC and TG. The results established the optimum conditions for minimizing heat and mass transfer effect. Sample sizes used were: (5–15 mg) for DSC and (30–50 mg) for TG. DSC analysis used crimped crucibles with a pinhole, which allowed maximum resolution and gave well-defined mass (water) loss. TG analysis used a heating rate of 10 °C/min−1 in an atmosphere of nitrogen. The heat of crystallization, heat of fusion, and heat of vaporization of unbound water are 334, 334, and 2,257 Jg−1, respectively (Mitra et al. Proc NATAS Annu Conf Therm Anal Appl 30:203–208, ). The DSC average water content of (MoM) was 80 wt% for name brand and 89.5 wt% for generic brand, based on the relative crystallization, melting and vaporization heats/Jg−1 of distilled water in the recently purchased (2011) MoM samples. The TG showed a two-step process, losing water at 80–135 °C for unbound water and bound water (MgO·H2O) at 376–404 °C, yielding a total average water loss of 91.9 % for name brand and 90.7 % for generic brand by mass. The difference between the high-temperature TG and the lower-temperature DSC can be attributed for the decomposition of magnesium hydroxide or MgO·H2O. Therefore in performing this new approach to water analysis by heating to a high temperature decomposed the magnesium hydroxide residue. It was determined that the TG method was the most accurate for determining bound and unbound water.

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Journal of Thermal Analysis and Calorimetry
Authors: Susan Moreno-Molek, Salaam Saleh, Druthiman Reddy Mantheni, Manik Pavan Kumar Maheswaram, Tobili Sam-Yellowe, and Alan T. Riga

Abstract

Cytokines and soluble cytokine receptors serve as important protein biomarkers for chronic and infectious disease diagnosis. The development of biosensors capable of detecting cytokines or their soluble receptors in patient bodily fluids is a growing area of research. In an ongoing series of studies to understand the thermal analytical behavior of cytokines and their soluble receptors, dielectric thermal analysis (DETA) and thermogravimetry (TG) were used in investigations to determine if differentiations based on dielectric properties (e.g., conductivity) of the proteins could be identified. Permittivity (∊′) and dielectric loss factor (∊″) measurements were performed over a frequency range of 0.1–300,000 Hz. Up to 20 min, water associated with the samples was conductive, interacting with the proteins and affecting the temperature-dependent relaxation spectra of proteins. A trend analysis revealed differences between surface charge at 0.1 Hz and bulk charge at 300,000 Hz. In addition, the greatest change detected among proteins was due to the conductivity (dielectric loss factor). Beyond a 20 min drying time, the observed conductivity was due to intrinsic properties of the proteins with limited dependence on frequency. A 100% water loss was obtained for samples within 20–30 min by TG. Sample drying by TG could serve as a preparatory step in drying protein samples for further DETA and DSC analysis.

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Solid-state mechanical properties of crystalline drugs and excipients

New data substantiate discovered dielectric viscoelastic characteristics

Journal of Thermal Analysis and Calorimetry
Authors: Shravan Singh Thakur, Manik Pavan Kumar Maheswaram, Dhruthiman Reddy Mantheni, Lakshmi Kaza, Indika Perara, David W. Ball, John Moran, and Alan T. Riga

Abstract

Thermal mechanical analysis (TMA) of crystalline drugs and excipients in their pre-melt temperature range performed in this study corroborate their newly found linear dielectric conductivity properties with temperature. TMA of crystalline active pharmacy ingredients (APIs) or excipients shows softening at 30–100 °C below the calorimetric melting phase transition, which is also observed by dielectric analysis (DEA). Acetophenetidin melts at 135 °C as measured calorimetrically by DSC, but softens under a low mechanical stress at 95 °C. At this pre-melting temperature, the crystals collapse under the applied load, and the TMA probe shows rapid displacement. The mechanical properties yield a softening structure and cause a dimensionally slow disintegration resulting in a sharp dimensional change at the melting point. In order to incorporate these findings into a structure–property relationship, several United States Pharmacopeia (USP) melting-point standard drugs were evaluated by TMA, DSC, and DEA, and compared to the USP standard melt temperatures. The USP standard melt temperature for vanillin (80 °C) [], acetophenetidin (135 °C) [], and caffeine (235 °C) [] are easily verified calorimetrically via DSC. The combined thermal analysis techniques allow for a wide variety of the newly discovered physical properties of drugs and excipients.

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Journal of Thermal Analysis and Calorimetry
Authors: Dhruthiman R. Mantheni, M. P. K. Maheswaram, Hany F. Sobhi, Naullage Indika Perera, Alan T. Riga, M. Ellen Matthews, and K. Alexander

Abstract

Novel dielectric behavior of a linear increase in ionic conductivity prior to melt temperature was observed for active pharmaceutical ingredients (APIs), organic chemicals, amino acids, and carbohydrates. Though, there are solids like polyolefins and long chain organic compounds (tetracosane, pentacosane) which do not exhibit this premelt behavior (i.e., the temperature where the onset of increase in ionic conductivity to melt temperature). We have discovered novel electrical conductivity properties and other physical analytical variations which can lead to unique synthetic routes of certain chemical entities. The above-mentioned unique variations are not related to solid–solid transitions which are quite often observed in pharmaceutical crystalline solids. These new properties are related to amorphous crystalline behavior of a solid. We have also studied the effect of various experimental variables: such as amount of mass tested, applied frequency at a given electric field and heating rate, which results in varying the onset temperature of the increase in ionic conductivity. Melting of the solids was correlated using differential scanning calorimetry (DSC). Activation energies for all the solids were measured in the premelt region using an Arrhenius plot at a specific frequency since we observed changes in the conductivity with frequency. This study focused on frequencies 0.1 to 10 Hz, since the conductivity at these frequencies related to surface analysis. This new physical properties are leading to new electro synthetic procedures to modify or prepare chemicals.

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