Structure of Soluble Silicates

1984 ◽  
Vol 32 ◽  
Author(s):  
Dale W. Schaefer ◽  
Keith D. Keefer
Keyword(s):  
Sol Gel ◽  
Branched Polymers ◽  
Glass Technology ◽  
Geometrical Structures ◽  
Chain Molecules ◽  
Chemical Systems ◽  
Organic Systems ◽  
X Ray Scattering ◽  
Saxs Curve

ABSTRACTSmall angle x-ray scattering (SAXS) is the technique of choice for the determination of structure on the 10–1000Å scale. We have used this technique to study the growth and topology of the macromolecules which precede gelation in several chemical systems used in sol-gel glass technology. The results show that branched polymers, as opposed to colloids, are formed. The alcoholic silica system is akin to organic systems where gelation occurs through growth and crosslinking of chain molecules. Data are reported from both the Porod and Guinier regions of the SAXS curve and these data are interpreted in terms of geometrical structures predicted by various disorderly growth processes. The results indicate that the degree of crosslinking can be controlled by catalytic conditions. The degree of crosslinking may, in turn, control phase separation and processability to a dense glass.

Determination of the molecular weight of proteins in solution from a single small-angle X-ray scattering measurement on a relative scale

2009 ◽  
Vol 43 (1) ◽  
pp. 101-109 ◽  
Author(s):  
H. Fischer ◽  
M. de Oliveira Neto ◽  
H. B. Napolitano ◽  
I. Polikarpov ◽  
A. F. Craievich
Keyword(s):  
Molecular Weight ◽  
Small Angle ◽  
Dilute Solution ◽  
X Ray ◽  
Molecular Weights ◽  
X Ray Scattering ◽  
Saxs Curve ◽  
Relative Scale ◽  
Ray Scattering

This paper describes a new and simple method to determine the molecular weight of proteins in dilute solution, with an error smaller than ∼10%, by using the experimental data of a single small-angle X-ray scattering (SAXS) curve measured on a relative scale. This procedure does not require the measurement of SAXS intensity on an absolute scale and does not involve a comparison with another SAXS curve determined from a known standard protein. The proposed procedure can be applied to monodisperse systems of proteins in dilute solution, either in monomeric or multimeric state, and it has been successfully tested on SAXS data experimentally determined for proteins with known molecular weights. It is shown here that the molecular weights determined by this procedure deviate from the known values by less than 10% in each case and the average error for the test set of 21 proteins was 5.3%. Importantly, this method allows for an unambiguous determination of the multimeric state of proteins with known molecular weights.

Optimization of sol-gel based fibre-optic cholinesterase biosensor for the determination of organophosphorus pesticides

2000 ◽  
Vol 42 (7-8) ◽  
pp. 283-290 ◽  
Author(s):  
H.-C. Tsai ◽  
R.-A. Doong
Keyword(s):  
Fiber Optic ◽  
Ph Value ◽  
Rapid Determination ◽  
Organophosphorus Pesticides ◽  
Sol Gel ◽  
Neutral Red ◽  
Fluorescent Indicators ◽  
Low Leakage ◽  
Fiber Optic System

A sol-gel based fiber-optic biosensor with acetylcholinesterase as the biorecognition element has been developed for the rapid determination of organophosphorus pesticides. Nine fluorescent indicators, acridine, acridine orange, neutral red, DAPI, rhodamine B, fluorescein, umbelliferone, FITC on celite and FITC-dextran, have been examined to optimize the fiber-optic system. Results showed that acridine and FITCs were sensitive to the change of pH value caused by the enzyme-substrate catalysis reaction. However, the sensitivity of acridine was 260 times lower than that of FITCs. Higher toxicity of acridine to acetylcholinesterase than FITC was also observed. Moreover, the high-molecular-weight FITC-dextran showed low leakage rate when immobilizing using sol-gel technology, showing that the FITC-dextran was a suitable pH sensitive fluorescent indicator for the OPPs biosensor. The response of the fiber-optic biosensor to the substrate, acetylcholine, was highly reproducible (RSD=3.5%). A good linearity of acetylcholine in the range from 0.5 to 20 mM was also obtained (R2=0.98). Furthermore, a 30% inhibition can be achieved in 30min when 152 ppb paraoxon was added into the system. The results show the possibility for real-time determination of organophosphorus pesticides by using the biosensor developed in this study.

Multi-walled Carbon Nanotubes Reinforced into Hollow Fiber by Chitosan Sol-gel for Solid/Liquid Phase Microextraction of NSAIDs from Urine Prior to HPLC-DAD Analysis

2019 ◽  
Vol 20 (5) ◽  
pp. 390-400 ◽  
Author(s):  
Nabil N. AL-Hashimi ◽  
Amjad H. El-Sheikh ◽  
Rania F. Qawariq ◽  
Majed H. Shtaiwi ◽  
Rowan AlEjielat
Keyword(s):  
Carbon Nanotubes ◽  
Liquid Phase ◽  
Hollow Fiber ◽  
Sol Gel ◽  
Liquid Phase Microextraction ◽  
Extraction Device ◽  
Multi Walled Carbon Nanotubes ◽  
Solid Liquid ◽  
Walled Carbon Nanotubes

Background: The efficient analytical method for the analysis of nonsteroidal antiinflammatory drugs (NSAIDs) in a biological fluid is important for determining the toxicological aspects of such long-term used therapies. Methods: In the present work, multi-walled carbon nanotubes reinforced into a hollow fiber by chitosan sol-gel assisted-solid/ liquid phase microextraction (MWCNTs-HF-CA-SPME) method followed by the high-performance liquid chromatography-diode array detection (HPLC–DAD) was developed for the determination of three NSAIDs, ketoprofen, diclofenac, and ibuprofen in human urine samples. MWCNTs with various dimensions were characterized by various analytical techniques. The extraction device was prepared by immobilizing the MWCNTs in the pores of 2.5 cm microtube via chitosan sol-gel assisted technology while the lumen of the microtube was filled with few microliters of 1-octanol with two ends sealed. The extraction device was operated by direct immersion in the sample solution. Results: The main factors influencing the extraction efficiency of the selected NSAIDs have been examined. The method showed good linearity R2 ≥ 0.997 with RSDs from 1.1 to 12.3%. The limits of detection (LODs) were 2.633, 2.035 and 2.386 µg L-1, for ketoprofen, diclofenac, and ibuprofen, respectively. The developed method demonstrated a satisfactory result for the determination of selected drugs in patient urine samples and comparable results against reference methods. Conclusion: The method is simple, sensitive and can be considered as an alternative for clinical laboratory analysis of selected drugs.

scholarly journals Selectivity of Tungsten Oxide Synthesized by Sol-Gel Method Towards Some Volatile Organic Compounds and Gaseous Materials in a Broad Range of Temperatures

Materials ◽  
2020 ◽  
Vol 13 (3) ◽  
pp. 523 ◽  
Author(s):  
Simonas Ramanavičius ◽  
Milda Petrulevičienė ◽  
Jurga Juodkazytė ◽  
Asta Grigucevičienė ◽  
Arūnas Ramanavičius
Keyword(s):  
Volatile Organic Compounds ◽  
Organic Compounds ◽  
Sol Gel ◽  
Temperature Dependent ◽  
Sensing Systems ◽  
Sensing Material ◽  
Operational Temperature ◽  
Volatile Organic ◽  
Different Gases

In this research, the investigation of sensing properties of non-stoichiometric WO3 (WO3−x) film towards some volatile organic compounds (VOC) (namely: Methanol, ethanol, isopropanol, acetone) and ammonia gas are reported. Sensors were tested at several temperatures within the interval ranging from a relatively low temperature of 60 up to 270 °C. Significant variation of selectivity, which depended on the operational temperature of sensor, was observed. Here, the reported WO3/WO3–x-based sensing material opens an avenue for the design of sensors with temperature-dependent sensitivity, which can be applied in the design of new gas- and/or VOC-sensing systems that are dedicated for the determination of particular gas- and/or VOC-based analyte concentration in the mixture of different gases and/or VOCs, using multivariate analysis of variance (MANOVA).

Determination of the Growth Rate of Hydrothermally Synthesised ZnO2 Crystallites

2017 ◽  
Vol 50 ◽  
pp. 41-47 ◽  
Author(s):  
Martin Egblewogbe ◽  
Garu Gebreyesus ◽  
Samuel A. Atarah
Keyword(s):  
Growth Rate ◽  
Zinc Acetate Dihydrate ◽  
Hydrothermal Process ◽  
Growth Rate Constant ◽  
Acetate Dihydrate ◽  
X Ray ◽  
X Ray Scattering ◽  
Transmission Electron ◽  
Zinc Peroxide

Powders consisting of nanoparticles of zinc peroxide were prepared via a simple hydrothermal process using zinc acetate dihydrate and hydrogen peroxide precursors. The size of the crystallites was determined using x-ray powder diffraction. Over a period of 5 hours the crystallite radius increased from 4 nm – 9 nm at a temperature of 68 °C ± 5 °C, with growth rate constant of 0.23 nm3 min−1 calculated using the Lifshitz, Slyozov, and Wagner model. The powders were further characterised with High Resolution Transmission Electron Microscopy, Energy Dispersive X-ray analysis, and Small Angle X-ray Scattering, showing well-crystallised ZnO2 nanoparticles.

Structural refinement by restrained molecular-dynamics algorithm with small-angle X-ray scattering constraints for a biomolecule

2004 ◽  
Vol 37 (1) ◽  
pp. 103-109 ◽  
Author(s):  
Masaki Kojima ◽  
Alexander A. Timchenko ◽  
Junichi Higo ◽  
Kazuki Ito ◽  
Hiroshi Kihara ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Molecular Dynamics ◽  
Small Angle ◽  
Protein Structures ◽  
Saxs Data ◽  
X Ray ◽  
X Ray Scattering ◽  
Saxs Curve ◽  
Restrained Molecular Dynamics ◽  
Ray Scattering

A new algorithm to refine protein structures in solution from small-angle X-ray scattering (SAXS) data was developed based on restrained molecular dynamics (MD). In the method, the sum of squared differences between calculated and observed SAXS intensities was used as a constraint energy function, and the calculation was started from given atomic coordinates, such as those of the crystal. In order to reduce the contribution of the hydration effect to the deviation from the experimental (objective) curve during the dynamics, and purely as an estimate of the efficiency of the algorithm, the calculation was first performed assuming the SAXS curve corresponding to the crystal structure as the objective curve. Next, the calculation was carried out with `real' experimental data, which yielded a structure that satisfied the experimental SAXS curve well. The SAXS data for ribonuclease T1, a single-chain globular protein, were used for the calculation, along with its crystal structure. The results showed that the present algorithm was very effective in the refinement and adjustment of the initial structure so that it could satisfy the objective SAXS data.

scholarly journals Flow injection analysis of water. Part 1: Automatic preconcentration determination of sulphate, ammonia and iron(II)/iron(III)

1993 ◽  
Vol 15 (4) ◽  
pp. 141-146 ◽  
Author(s):  
J. S. Cosano ◽  
M. D. Luque de Castro ◽  
M. Valcárcel
Keyword(s):  
Flow Injection ◽  
Good Reproducibility ◽  
Chemical Systems ◽  
Sequential Determination ◽  
On Line ◽  
Exchange Material ◽  
Iron Complexation ◽  
Simple Flow ◽  
Ammonia Formation

This paper describes a simple flow-injection (FI) manifold for the determination of a variety of species in industrial water. The chemical systems involved in the determination of ammonia (formation of Indophenol Blue), sulfate (precipitation with Ba(II)), and iron (complexation with 1,10-phenanthroline with the help of a prior redox reaction for speciation) were selected so that a common manifold could be used for the sequential determination of batches of each analyte. A microcolumn of a suitable ion exchange material was used for on-line preconcentration of each analyte prior to injection; linear ranges for the determination of the analytes at the ng/ml levels were obtained with good reproducibility. The manifold and methods are ready for full automation.

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