Hoeil Chung

Simultaneous Measurements of Glucose, Glutamine, Ammonia, Lactate, and Glutamate in Aqueous Solutions by Near-Infrared Spectroscopy

Calibration models are generated and evaluated for the measurement of five different components in synthetic mixtures prepared in aqueous solutions. Mixtures of glucose, glutamine, ammonia, lactate, and glutamate were prepared to simulate concentration levels expected during routine bioreactor fermentation processes. Near-IR spectra were collected from these solutions over the spectral range from 5000 to 4000 cm−1. This spectral information was used to build individual multivariate calibration models for each analyte. Models were constructed on the basis of partial least-squares regression of raw and Fourier filtered absorbance spectra. Each analyte could be detected selectively with mean percent errors of prediction ranging from 4 to 8%.

Discrimination of herbal medicines according to geographical origin with near infrared reflectance spectroscopy and pattern recognition techniques.

Herbal medicines have an important role in clinical therapy in Asian countries such as Korea, Japan, and China. The objective of this study is to develop a nondestructive and accurate analytical method to discriminate herbal medicines according to geographical origin. Even though they are the same species, their qualities are different by growing conditions such as climate and soil. Near infrared (NIR) reflectance spectroscopy and a pattern recognition technique were applied for discrimination of herbal medicines according to geographical origin (Korea and China). Astragali Radix (AR), Ganoderma, and Smilacis Rhizoma (SR) were examined. It is shown that the representative NIR reflectance spectra in each group are different according to geographical origin after second derivatization to enhance spectral features. Also, the NIR reflectance spectra of Chinese and Korean samples were differentiated using principal component (PC) score plots. To establish the discrimination rule, Mahalanobis distance and discriminant analysis with PLS2 were utilized.

A three-dimensional gold nanodendrite network porous structure and its application for an electrochemical sensing.

A three dimensional (3D) gold (Au) nanodendrite network porous structure constructed by a simple electrochemical synthetic method has been presented, and its utility for sensitive electrochemical measurement was demonstrated in this study. The 3D nanodendrite network porous structure was constructed on a platinum surface through electrodeposition of Au under the presence of hydrogen bubbles generated from the same surface. Iodide, used as a co-reagent, played an important role in the construction of the nanodendrite network by preventing continual growth of Au into larger agglomerates as well as inhibiting coalescence of neighboring nanodendrites. An electrochemical sensor incorporating the structure was built and used to detect As(III) in ultra low concentration range. For the purpose of comparison, bare gold and gold nanoparticle-incorporated electrodes were also prepared. With the use of 3D nanodendrite network porous structure, a much more sensitive detection of As(III) was possible due to its large surface area.

Comparison of near-infrared and mid-infrared spectroscopy for the determination of distillation property of kerosene

Abstract Near-infrared (NIR) and mid-infrared (MIR) spectroscopy have been compared and evaluated for the determination of the distillation property of kerosene with the use of partial least squares (PLS) regression. Since kerosene is a complex mixture of similar hydrocarbons, both spectroscopic methods will be best evaluated with this complex sample matrix. PLS calibration models for each percent recovery temperature have been developed by using both NIR and MIR spectra without spectral pretreatment. Both methods have shown good correlation with the corresponding reference method, however NIR provided better calibration performance over MIR. To rationalize the improved calibration performance of NIR, spectra of the same kerosene sample were continuously collected and the corresponding spectral reproducibility was evaluated. The greater spectral reproducibility including signal-to-noise ratio of NIR led to the improved calibration performance, even though MIR spectroscopy provided more qualitative spectral information. The reproducibility of measurement, signal-to-noise ratio, and richness of qualitative information should be simultaneously considered for proper selection of a spectroscopic method for quantitative analysis.

Enhancement of quaternary nitrogen doping of graphene oxide via chemical reduction prior to thermal annealing and an investigation of its electrochemical properties

A simple and efficient method to enhance the quaternary nitrogen doping (N-doping) of graphene has been demonstrated. Recent studies have shown that quaternary N in the graphene network provides more efficient electrocatalytic activity. Therefore, a novel strategy to enhance the quaternary N-doping is currently in high demand. The strategy employed in this work was to modify graphene oxide (GO) prior to thermal annealing so as to provide a more efficient structure for quaternary N doping. GO was first chemically reduced with hydrazine to substantially increase the formation of CC bonds and simultaneously decrease the atomic oxygen concentration. The reduced graphene oxide (RGO) was then annealed in the presence of NH3. Although N-doping via the replacement of oxygen is preferred, the probability of carbon being substituted with N dopants in the graphitic structure of RGO could increase due to the relatively higher content of CC when compared to the atomic oxygen concentration. In addition, due to the decreased atomic oxygen concentration, the electro-conductivity was enhanced. Cyclic voltammograms (CVs) of 5 mM K3Fe(CN)6 and 2 mM H2O2 were used to examine the electrochemical response of the quaternary N-maximized RGO. An improvement in electrocatalytic reduction and a higher electro-conductivity were confirmed based on an analysis of the obtained CVs.

Comparison of Near-Infrared, Infrared, and Raman Spectroscopy for the Analysis of Heavy Petroleum Products

Near-infrared (NIR) spectroscopy has been successfully applied to the determination of API (American Petroleum Institute) gravity of atmospheric residue (AR), which is the heaviest fraction in crude oil. This fraction is completely dark and very viscous. Preliminary studies involving Raman and infrared (IR) spectroscopies were also evaluated along with NIR spectroscopy. The Raman spectrum of AR was completely dominated by strong fluorescence from polycyclic aromatic hydrocarbons, called asphaltenes. IR spectroscopy provided reasonable spectral features; however, its spectral reproducibility was poorer and noisier than that of NIR. Although absorption bands in the NIR region were broad and less characterized, NIR provided better spectral reproducibility with higher signal-to-noise ratio (which is one of the most important parameters in quantitative calibration in comparison to Raman and IR spectroscopies). Partial least-squares (PLS) regression was utilized to develop calibration models. NIR spectra of AR samples were broad, and baselines were varying due to the strong absorption in the visible range. However, the necessary information was successfully extracted and correlated to the reference API gravity with the use of PLS regression. API gravities in the prediction set were accurately predicted with an SEP (standard error of prediction) of 0.22. Additionally NIR showed approximately three times better repeatability compared to the ASTM reference method, which directly influences the process control performance.

Simultaneous measurement of glucose and glutamine in aqueous solutions by near infrared spectroscopy.

A method is described for measuring the concentrations of both glucose and glutamine in binary mixtures from near infrared (NIR) absorption spectra. Spectra are collected over the range from 5000–4000/cm (2.0–2.5μm) with a 1-mm optical path length. Glucose absorbance features at 4710, 4400, and 4300/cm and glutamine features at 4700, 4580, and 4390/cm provide the analytical information required for the measurement. Multivariate calibration models are generated by using partial least squares (PLS) regression alone and PLS regression combined with a preprocessing digital Fourier filtering step. The ideal number of PLS factors and spectral range are identified separately for each analyte. In addition, the optimum Fourier filter parameters are established for both compounds. The best overall analytical performance is obtained by combining Fourier filtering and PLS regression. Glucose measurements are established over the concentration range from 1.66–59.91 mM, with a standard error of prediction (SEP) of 0.32 mM and a mean percent error of 1.84%. Glutamine can be measured over the concentration range from 1.10–30.65 mM with a SEP of 0.75 mM and a mean percent error of 6.67%. These results demonstrate the analytical utility of NIR spectroscopy for monitoring glucose and glutamine levels in mammalian and insect cell cultures.

Inkjet-compatible single-component polydiacetylene precursors for thermochromic paper sensors.

Inkjet-printable diacetylene (DA) supramolecules, which can be dispersed in water without using additional surfactants, have been developed. The supramolecules are generated from DA monomers that contain bisurea groups, which are capable of forming hydrogen-bonding networks, and hydrophilic oligoethylene oxide moieties. Because of suitable size distribution and stability characteristics, the single DA component ink can be readily transferred to paper substrates by utilizing a common office inkjet printer. UV irradiation of the DA-printed paper results in generation of blue-colored polydiacetylene (PDA) images, which show reversible thermochromic transitions in specific temperature ranges. Inkjet-printed PDAs, in the format of a two-dimensional (2D) quick response (QR) code on a real parking ticket, serve as a dual anticounterfeiting system that combines easy decoding of the QR code and colorimetric PDA reversibility for validating the authenticity of the tickets. This single-component ink system has great potential for use in paper-based devices, temperature sensors, and anticounterfeiting barcodes.

Phantoms for noninvasive blood glucose sensing with near infrared transmission spectroscopy

In vivo spectra from human subjects can be simulated with a phantom composed of different layers of water, fat and muscle tissue. All three components are necessary to simulate in vivo spectra collected over the combination spectral region (5000–4000 cm−1). Muscle tissue is not required, however, to accurately simulate overtone spectra (6600–5400 cm−1). The near‐IR spectral characteristics of fat and muscle tissue from several animal sources are essentially identical to those found for human tissue, hence, the animal source for these phantom components is not critical. Thickness of each tissue layer can be determined by a regression analysis where the in vivo spectrum of interest is regressed against standard absorbance spectra of the necessary model components (water, fat and muscle). In general, in vivo overtone spectra collected across human webbing tissue with a thickness of 6.7 mm can be simulated with water layer thicknesses ranging from 5.0 to 6.4 mm combined with fat layer thicknesses from 1.4 to 4.2 mm.

Dielectric studies of a nano-crystalline CaCu2.90Zn0.10Ti4O12 electro-ceramic by one pot glycine assisted synthesis from inexpensive TiO2 for energy storage capacitors

A facile way for the synthesis of nano-crystalline CaCu2.90Zn0.10Ti4O12 (CCZTO) using a solution combustion technique based on the glycine–nitrate process with inexpensive solid TiO2 powder as the raw material is introduced in this manuscript, for the first time. The precursor powder was calcined between 200 °C and 850 °C for 3 h in air. Phase formation, crystalline nature, morphology and chemical purity of the fabricated CCZTO were investigated with TG/DTA, FT-IR, FT-Raman, XRD, SAED patterns, SEM, TEM, EDX and XPS analyses, respectively. The XRD results indicated that all sintered samples had a major CaCu3Ti4O12 structure with some amount of CaTiO3 and CuO. The bright-field TEM micrographs revealed that the particle size was in the range of 15–50 nm, which was in good agreement with the average crystallite size obtained from XRD. SEM micrographs of the sintered CCZTO ceramics showed the average grain sizes were in the range of 800 nm–7 μm. EDX and XPS studies confirmed the stoichiometry and purity of the ceramics. The nature of the relaxation behavior of the ceramics was rationalized using impedance and modulus spectroscopy. The activation energies calculated from the grain-boundary relaxation time constant were found to be in the range of 0.79–0.52 eV, which confirmed the Maxwell–Wagner type of relaxation present in the ceramic. Our inexpensive novel solution chemistry based method for CCZTO_16h gives a high dielectric constant (799) and low dielectric loss (0.091) at 100 Hz at room temperature, which has potential significance for cost-effective technological applications in microelectronic devices.