Analytical Chemistry Commons^™

Tio2 Crystallization At Room Temperature And Preparation Of Transparent Carbon Counter Electrode For Low-Cost Dye-Sensitized Solar Cells, Muhammad Iqbal Syauqi, Afiten Rahmin Sanjaya, Mohammad Jihad Madiabu, Munawar Khalil, Jarnuzi Gunlazuardi

Makara Journal of Science

We developed a low-cost dye-sensitized solar cell (DSSC) using TiO₂ fabricated via rapid breakdown anodization (RBA) and ultrafast room-temperature crystallization (URTC). The prepared TiO₂ was deposited on a self-made fluorine-doped tin oxide (FTO) conductive glass, and the FTO/TiO₂ system was sensitized using curcumin dye. The DSSC was constructed by sandwiching the FTO/TiO₂/curcumin electrode with an I⁻/I₂ electrolyte and a transparent carbon counter electrode prepared using a liquid–liquid interface system. The characterization results showed that the TiO₂ freshly prepared via URTC was transformed into an anatase crystalline phase, which exhibited a 3.10 …

Physicochemical Changes And Role Of Analytical Chemistry In Black Garlic (Allium Sativum L.) Processing, Surjani Wonorahardjo, Dian Puspita Sari, Arini Salsabila, Estiyawati Estiyawati, Dewi Yuliani, Anugrah Ricky Wijaya, Suharti Suharti, Irma Kartika Kusumaningrum, Chariztya Anggita Maharani, Thjiong Angelina Noviyanti

Makara Journal of Science

Black garlic is a traditional spice having potential of herbal medicine; however, continuous heating darkens its color and changes its taste due to chemical processes and new equilibrium in the system. In this study, fresh garlic was processed into black garlic at 60 °C for 24 days. Changes in physical and chemical parameters, such as browning and protein content, reducing sugar content, and antioxidative components were recorded. Protein content was measured by Kjeldahl method, brown color development was analyzed using a color reader, reducing sugar was examined using a dinitro salicylic DNS reagent, and antioxidative activities were studied with a …

Applications In Opioid Analysis With Faims Through Control Of Vapor Phase Solvent Modifiers, Nathan Grimes

USF Tampa Graduate Theses and Dissertations

Field Asymmetric Ion Mobility Spectrometry (FAIMS), often coupled with mass spectrometry (MS), offers rapid analytical ion filtration, useful in reducing matrix interference and differentiating isomeric compounds. This study focuses on augmenting FAIMS-MS analyses through the incorporation of gas phase solvents, or "modifiers," inducing dynamic microsolvation, a particularly potent method of analysis enhancement.

Initially, the research utilized a bubbler-based system, incorporating a humidity sensor, improving modifier concentration control when using water. Our application in opioid detection and differentiation revealed considerable advancements. Notably, an increased peak capacity in an opioid mixture and successful separation of the isobaric opioid pair, alfentanil and ortho-isopropyl …

Long-Term Degradation Mechanisms In Application-Implemented Radical Thin Films, Ewa Malgorzata Nowik-Boltyk, Tobias Junghoefer, Mathias Glaser, Erika Giangrisostomi, Ruslan Ovsyannikov, Shuyang Zhang, Chan Shu, Andrzej Rajca, Arrigo Calzolari, M. Benedetta Casu

Department of Chemistry: Faculty Publications

Blatter radical derivatives are very attractive due to their potential applications, ranging from batteries to quantum technologies. In this work, we focus on the latest insights regarding the fundamental mechanisms of radical thin film (long-term) degradation, by comparing two Blatter radical derivatives. We find that the interaction with different contaminants (such as atomic H, Ar, N, and O and molecular H₂, N₂, O₂, H₂O, and NH₂) affects the chemical and magnetic properties of the thin films upon air exposure. Also, the radical-specific site, where the contaminant interaction takes place, plays …

Stepwise Assembly Of Quinary Multivariate Metal−Organic Frameworks Via Diversified Linker Exchange And Installation, Yuchen Hu, Xin Zhang, Rebecca Shu Hui Khoo, Christian Fiankor, Xu Zhang, Jian Zhang

Department of Chemistry: Faculty Publications

Multivariate MOFs (MTV-MOFs) constructed from multiple components with atomistic precision hold the promise for many fascinating developments in both fundamental sciences and applications. Sequential linker installation can be an effective method to introduce different functional linkers into an MOF that contains coordinatively unsaturated metal sites. However, in many cases, these linkers must be installed according to a specific sequence and the complete synthetic flexibility and freedom is yet to be realized. Here, we rationally decreased the size of the primary ligand used in NPF-300, a Zr-MOF with scu topology (NPF = Nebraska Porous Framework), and synthesized its isostructure, NPF-320. NPF-320 …

Synthesis And Study Of High-Spin Stable Organic Radicals For Electrical Conductors And Mannosamine Nitroxide For Mri Contrast Agents, Shuyang Zhang

Department of Chemistry: Dissertations, Theses, and Student Research

In the first project, we describe the synthesis of an ambient stable high spin organic diradical 4 based on the Blatter moiety. The high-spin (S = 1) organic diradical 4, which consists of two Blatter radical moieties in a conjugated structure, exhibits a nearly exclusive population (88%) on triplet ground state at room temperature as a consequence of a large single-triplet energy gap (ΔEST = 0.5 kcal/mol). The target diradical molecule is synthesized over five steps with structural confirmation by single-crystal X-ray diffraction. The thermogravimetric analysis (TGA) shows the onset of decomposition at ~264 oC, indicating the diradical molecule has …

Identification Of Different Hair Dyes In Dyed Hair Using Attenuated Total Reflectance (Atr Ft-Ir), Surface Enhancing Raman Spectroscopy (Sers) Techniques, Nicholas Lovera

Student Theses

This investigation compares the ability of Attenuated Total Reflection Fourier Transfer Infrared Spectroscopy (ATR FT-IR) and Surface Enhance Raman Spectroscopy (SERS) to identify and differentiate different hair dye brands on dyed hair samples. Hair is a common type of trace evidence found at crime scenes and can provide numerous information through forensic hair analysis. Cosmetic hair treatment such as dying the hair different colors has grown and became popular, thus it can be a very common type of trace evidence. This study can provide a forensic scientist an additional method for analyzing dyed hair samples. The goal was to compare …

Sers For The Detection Of Trace Materials, Omari Kirkland

Dissertations, Theses, and Capstone Projects

In this dissertation are presented three projects that contribute to the body of research on SERS in the forensic, heritage, and semiconductor fields. The first project, Charge-Transfer mapping on GaN/Ag, a silver-decorated nanopillar semiconductor substrate fabricated from the GaN is used with the Raman probe Rhodamine 6 G (R6G) to map the effect of the nanofeatures on the CT resonance. The second project, in collaboration with Marco Leona from the Metropolitan Museum of Art, explores the use of AgNIFs to identify colorants used on textile fiber samples from four 19th century works of Japanese art. The final project analyzes the …

The Effect Of The Carbon Nanotubes’ Surface Area On The Morphology And Performance Of Cellulose Acetate Nanocomposite Membranes In Nanofiltration Applications, Nouran Elbadawi

Theses and Dissertations

Population increase and climate change have significantly affected the availability of fresh water for consumption. Studies by UNESCO showed that more than 28% of the world population didn’t have access to clean safe drinking water in 2020. This situation is expected to get more serious over the coming 30 years with the limited availability of natural fresh water sources. The need to find solutions from alternative non-freshwater resources for drinking or irrigation is becoming a necessity. Within the context of desalination technologies, thousands of investigations are conducted to find the cheapest most efficient way of water treatment aiming at expanding …

The Kappa Opioid Receptor Agonist 16-Bromo Salvinorin A Has Anti-Cocaine Effects Without Significant Effects On Locomotion, Food Reward, Learning And Memory, Or Anxiety And Depressive-Like Behaviors, Ross Van De Wetering, Amy Ewald, Susan Welsh, Lindsay Kornberger, Samuel E. Williamson, Bryan D. Mcelroy, Eduardo R. Butelman, Thomas E. Prisinzano, Bronwyn M. Kivell

Markey Cancer Center Faculty Publications

Kappa opioid receptor (KOR) agonists have preclinical antipsychostimulant effects; however, adverse side effects have limited their therapeutic development. In this preclinical study, conducted in Sprague Dawley rats, B6-SJL mice, and non-human primates (NHPs), we evaluated the G-protein-biased analogue of salvinorin A (SalA), 16-bromo salvinorin A (16-BrSalA), for its anticocaine effects, side effects, and activation of cellular signaling pathways. 16-BrSalA dose-dependently decreased the cocaine-primed reinstatement of drug-seeking behavior in a KOR-dependent manner. It also decreased cocaine-induced hyperactivity, but had no effect on responding for cocaine on a progressive ratio schedule. Compared to SalA, 16-BrSalA had an improved side effect profile, with …

Enhanced Methods In Forensic Mass Spectrometry For Targeted And Untargeted Drug Analysis, Dina M. Swanson

USF Tampa Graduate Theses and Dissertations

Forensic science has long used mass spectrometry for the analysis of drugsand metabolites. Traditionally, screening methods consisted of color tests or immunoassay and confirmation methods used gas chromatography with mass spectrometry, which was considered the gold standard for identification. In the last several decades, advances in liquid chromatography with mass spectrometry (LCMS) have brought this technology to the forefront of forensic drug identification. Drug identification in forensic drug chemistry and forensic toxicology has become increasingly challenging due to the rapid increase in illicit drug analogs including novel opioids such as fentanyl analogs. Traditional screening methodologies are often unable to identify …

Design, Synthesis, Biological And Computational Studies Of Flavonoid Acetamide Derivatives, Daniel Kasungi Isika

Dissertations

Flavonoid compounds (FC) have extensive biological applications through potent antimicrobial, anti-inflammatory, anticancer, antidiabetic, and antioxidant properties. These applications are nevertheless limited by low bioavailability, poor aqueous solubility, enzymatic degradation, rapid metabolism, and fast body clearance. FC show unique structure-activity relationships (SARs) essential in assessing and mitigating the prevalent challenges impeding their applications. These challenges can be addressed by structural modification of the FC through functionalization of the phenolic rings, modification of the ketone group, and modification of the phenolic hydroxyl groups with bioisosteres.

The objectives of this work are to (i) design and synthesize novel flavonoid acetamide derivatives (FADs) and …

Biopolymer-Coated Magnetite Nanoparticles For The Removal Of Emerging Contaminants From Aqueous Solutions, Hebatullah Farghal

Theses and Dissertations

Abstract

Biopolymers are gaining interest as promising materials for water purification due to their functionality, biodegradability, abundance, and safe use. In this work, three biopolymer-based systems were developed as adsorbents for removing emerging contaminants from water. The first system of biopolymeric nanocomposites was synthesized by coating chitosan/xylan biopolymeric nanocomposites on magnetite nanoparticles (CsXM) to facilitate their separation from water via a magnetic field. The prepared mesoporous CsXM nanocomposite was thermally stable and possessed a particle size of 11 nm and a neutral to slightly negative charge over the studied pH range of about 3 to 10. The nanocomposite efficiently removed …

Advances In Structure Elucidation Of Small Molecules And Peptides By Nuclear Magnetic Resonance Spectroscopy And Mass Spectrometry, Ryan D. Cohen

Seton Hall University Dissertations and Theses (ETDs)

This dissertation reports on improvements in nuclear magnetic resonance (NMR) and mass spectrometry (MS) structure determination methods of organic compounds, with particular focus on challenging cyclic peptides. A recent and important innovation in NMR spectroscopy is the combination of theoretical property predictions, such as chemical shifts, using density functional theory (DFT) to aid in challenging NMR structure assignments, such as determination of regio- and stereo-configurations. In the first part of this thesis, a comprehensive benchmark study of DFT chemical shift prediction methods was performed using experimental NMR data collected from 50 well curated compounds, which was referred to as the …

Developing A Sample-Efficient Analytical Pathway For A Qualitative Chemical Investigation Of Ancestral Chilkat Dyeing And Weaving Practices, Dario Gerlando Durastanti

Dissertations and Theses

The project goal is to identify the dyestuffs used in hand-woven Chilkat blankets from the collection of the Alaska State Museum and the Sheldon Jackson Museum. Chilkat weaving is practiced by Northwest coastal clans, particularly in Southeast Alaska since at least the early 19th century. Through this collaboration, 117 wool fibers from 23 Chilkat textiles, and 193 reference samples consisting of dyed fibers using both natural and synthetic dye sources, raw dye material, and dye bath aliquots were provided to the lab for reference characterization and identification. In these analyses, dyes were classified as being either natural or synthetic, subdivided …

Synthesis And Characterization Of Porphyrin-Encapsulated Nanoparticles: Investigations With Scanning Probe Microscopy, Olajumoke Helen Olubowale

LSU Doctoral Dissertations

Scanning probe microscopy (SPM) encompasses a family of surface measurements that use a sharp probe to “feel” a surface. The tip is scanned point-by-point to build a map of the sample topography, which can be correlated with local measurements of surface properties. This dissertation outlines the history of SPM and describes techniques, operational modes, and applications. A review of force volume mapping (FVM), a 3D characterization mode of SPM used to map material properties detailed. Force volume mapping can be achieved by measuring multiple force measurements point-by-point in a grid pattern. Local properties such as chemical forces, dielectric properties, nanomechanical …

Investigating Reactivity Of Artificial Copper Peptides With Small Molecules, Allyson Bryant

Honors Theses

The design of artificial enzymes has been a topic of significant interest in the field of biochemistry, as they can provide new opportunities for catalytic processes and drug development. De novo protein design has emerged as a promising approach to create such enzymes, and the study of metalloproteins, particularly copper-binding peptides, has become a focus of this research. This thesis investigates the reactivity of a mutated copper-binding peptide, I5A-3SCC, with oxygen and its implications in the development of artificial enzymes.

The parent peptide, 3SCC, was mutated by replacing Isoleucine residues with smaller Alanine side chains, which was hypothesized to enhance …

Ramie (Boehmeria Nivea): An Underutilized Plant For A Multipurpose Industrial Application; A Perennial Plant With Protein Identification Using Maldi-Ms, A Biosorbent For Hg (Ii) Removal From Water And As A Bast Fiber Production Via Enzymatic Degumming, Abdul Rashid Issifu

Master's Theses

Identifying plant species that can offer life support to humans and animals without damaging the environment is quite challenging. Ramie, one of the oldest fiber crops was studied due to its nutritional value as fodder and other multipurpose applications in, e.g., medicinal, environmental, and textile industrial fields.

With a brief discussion of background in Chapter I, Chapter II focused on using a proteomic method to investigate unknown proteins in the leaves of ramie and to study their benefits to the biological system. PPiase and RuBisCO with molecular weight 15 and 52 KDa were identified as the proteins after peptide mass …

Low-Cost Microstereolithography 3d Printing With Microfluidic Microsampling Applications, Lauren Twombly

Chemistry & Biochemistry Undergraduate Honors Theses

The growing field of stereolithography 3D printing has welcomed a new age ofmicrofluidic device fabrication techniques. When compared to previous planar fabrication techniques such as soft-lithography, stereolithography 3D printing offers highly automated procedures, reduced fabrication times, and greater complexity of device features. To date, the greatest tradeoff for 3D printing in microfluidic device fabrication is poorer resolution when compared to soft-lithography which can produce feature sizes on the nanometer scale. The poorer resolution of 3D printing limits the feasible size of features. While highly sophisticated 3D printers are capable of achieving sub 10 μm resolution, these instruments are incredibly expensive …

Detection Of Nitrogen Dioxide Via Graphene-Enhanced Raman Scattering, Spencer Hazeslip

Chemistry & Biochemistry Undergraduate Honors Theses

This paper presents the development of a nitrogen dioxide (NO₂) sensor that utilizes the phenomenon of graphene-enhanced Raman scattering (GERS). The sensor consists of monolayer graphene on a silicon wafer, functionalized noncovalently with Copper(II) 2,9,16,23-tetra-tert-butyl-29H,31H-phthalocyanine (CuTTPc) via the solution soaking method. A custom sensing chamber was constructed to enable Raman spectra to be collected during NO₂ exposure. The response of the sensor was found to be linear between 10 and 100 ppm NO₂, indicating that it could be used for both detection and quantification. Furthermore, the sensor was shown to be reusable after …