Detection of Acetone Processing of Castor Bean Mash for Forensic Investigation of Ricin Preparation Methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kreuzer-Martin, Helen W.; Wahl, Jon H.; Metoyer, Candace N.

The toxic protein ricin is of concern as a potential biological threat agent (BTA) Recently, several samples of ricin have been seized in connection with biocriminal activity. Analytical methods are needed that enable federal investigators to determine how the samples were prepared, to match seized samples to potential source materials, and to identify samples that may have been prepared by the same method using the same source materials. One commonly described crude ricin preparation method is acetone extraction of crushed castor beans. Here we describe the use of solid-phase microextraction and headspace analysis of crude ricin preparation samples to determinemore » whether they were processed by acetone extraction. In all cases, acetone-extracted bean mash could be distinguished from un-extracted mash or mash extracted with other organic solvents. Statistical analysis showed that storage in closed containers for up to 109 days had no effect on acetone signal intensity. Signal intensity in acetone-extracted mash decreased during storage in open containers, but extracted mash could still be distinguished from un-extracted mash after 94 days.« less

Preparation and recrystallization behavior of spray-dried co-amorphous naproxen-indomethacin.

PubMed

Beyer, Andreas; Radi, Lydia; Grohganz, Holger; Löbmann, Korbinian; Rades, Thomas; Leopold, Claudia S

2016-07-01

To improve the dissolution properties and the physical stability of amorphous active pharmaceutical ingredients, small molecule stabilizing agents may be added to prepare co-amorphous systems. The objective of the study was to investigate if spray-drying allows the preparation of co-amorphous drug-drug systems such as naproxen-indomethacin and to examine the influence of the process conditions on the resulting initial sample crystallinity and the recrystallization behavior of the drug(s). For this purpose, the process parameters inlet temperature and pump feed rate were varied according to a 2(2) factorial design and the obtained samples were analyzed with X-ray powder diffractometry and Fourier-transformed infrared spectroscopy. Evaluation of the data revealed that the preparation of fully amorphous samples could be achieved depending on the process conditions. The resulting recrystallization behavior of the samples, such as the total recrystallization rate, the individual recrystallization rates of naproxen and indomethacin as well as the polymorphic form of indomethacin that was formed were influenced by these process conditions. For initially amorphous samples, it was found that naproxen and indomethacin recrystallized almost simultaneously, which supports the theory of formation of drug-drug heterodimers in the co-amorphous phase. Copyright © 2016 Elsevier B.V. All rights reserved.

Atmospheric vs. anaerobic processing of metabolome samples for the metabolite profiling of a strict anaerobic bacterium, Clostridium acetobutylicum.

PubMed

Lee, Sang-Hyun; Kim, Sooah; Kwon, Min-A; Jung, Young Hoon; Shin, Yong-An; Kim, Kyoung Heon

2014-12-01

Well-established metabolome sample preparation is a prerequisite for reliable metabolomic data. For metabolome sampling of a Gram-positive strict anaerobe, Clostridium acetobutylicum, fast filtration and metabolite extraction with acetonitrile/methanol/water (2:2:1, v/v) at -20°C under anaerobic conditions has been commonly used. This anaerobic metabolite processing method is laborious and time-consuming since it is conducted in an anaerobic chamber. Also, there have not been any systematic method evaluation and development of metabolome sample preparation for strict anaerobes and Gram-positive bacteria. In this study, metabolome sampling and extraction methods were rigorously evaluated and optimized for C. acetobutylicum by using gas chromatography/time-of-flight mass spectrometry-based metabolomics, in which a total of 116 metabolites were identified. When comparing the atmospheric (i.e., in air) and anaerobic (i.e., in an anaerobic chamber) processing of metabolome sample preparation, there was no significant difference in the quality and quantity of the metabolomic data. For metabolite extraction, pure methanol at -20°C was a better solvent than acetonitrile/methanol/water (2:2:1, v/v/v) at -20°C that is frequently used for C. acetobutylicum, and metabolite profiles were significantly different depending on extraction solvents. This is the first evaluation of metabolite sample preparation under aerobic processing conditions for an anaerobe. This method could be applied conveniently, efficiently, and reliably to metabolome analysis for strict anaerobes in air. © 2014 Wiley Periodicals, Inc.

Green Aspects of Techniques for the Determination of Currently Used Pesticides in Environmental Samples

PubMed Central

Stocka, Jolanta; Tankiewicz, Maciej; Biziuk, Marek; Namieśnik, Jacek

2011-01-01

Pesticides are among the most dangerous environmental pollutants because of their stability, mobility and long-term effects on living organisms. Their presence in the environment is a particular danger. It is therefore crucial to monitor pesticide residues using all available analytical methods. The analysis of environmental samples for the presence of pesticides is very difficult: the processes involved in sample preparation are labor-intensive and time-consuming. To date, it has been standard practice to use large quantities of organic solvents in the sample preparation process; but as these solvents are themselves hazardous, solvent-less and solvent-minimized techniques are becoming popular. The application of Green Chemistry principles to sample preparation is primarily leading to the miniaturization of procedures and the use of solvent-less techniques, and these are discussed in the paper. PMID:22174632

The NOSAMS sample preparation laboratory in the next millenium: Progress after the WOCE program

NASA Astrophysics Data System (ADS)

Gagnon, Alan R.; McNichol, Ann P.; Donoghue, Joanne C.; Stuart, Dana R.; von Reden, Karl; Nosams

2000-10-01

Since 1991, the primary charge of the National Ocean Sciences AMS (NOSAMS) facility at the Woods Hole Oceanographic Institution has been to supply high throughput, high precision AMS 14C analyses for seawater samples collected as part of the World Ocean Circulation Experiment (WOCE). Approximately 13,000 samples taken as part of WOCE should be fully analyzed by the end of Y2K. Additional sample sources and techniques must be identified and incorporated if NOSAMS is to continue in its present operation mode. A trend in AMS today is the ability to routinely process and analyze radiocarbon samples that contain tiny amounts (<100 μg) of carbon. The capability to mass-produce small samples for 14C analysis has been recognized as a major facility goal. The installation of a new 134-position MC-SNICS ion source, which utilizes a smaller graphite target cartridge than presently used, is one step towards realizing this goal. New preparation systems constructed in the sample preparation laboratory (SPL) include an automated bank of 10 small-volume graphite reactors, an automated system to process organic carbon samples, and a multi-dimensional preparative capillary gas chromatograph (PCGC).

A 96-well screen filter plate for high-throughput biological sample preparation and LC-MS/MS analysis.

PubMed

Peng, Sean X; Cousineau, Martin; Juzwin, Stephen J; Ritchie, David M

2006-01-01

A novel 96-well screen filter plate (patent pending) has been invented to eliminate a time-consuming and labor-intensive step in preparation of in vivo study samples--to remove blood or plasma clots. These clots plug the pipet tips during a manual or automated sample-transfer step causing inaccurate pipetting or total pipetting failure. Traditionally, these blood and plasma clots are removed by picking them out manually one by one from each sample tube before any sample transfer can be made. This has significantly slowed the sample preparation process and has become a bottleneck for automated high-throughput sample preparation using robotic liquid handlers. Our novel screen filter plate was developed to solve this problem. The 96-well screen filter plate consists of 96 stainless steel wire-mesh screen tubes connected to the 96 openings of a top plate so that the screen filter plate can be readily inserted into a 96-well sample storage plate. Upon insertion, the blood and plasma clots are excluded from entering the screen tube while clear sample solutions flow freely into it. In this way, sample transfer can be easily completed by either manual or automated pipetting methods. In this report, three structurally diverse compounds were selected to evaluate and validate the use of the screen filter plate. The plasma samples of these compounds were transferred and processed in the presence and absence of the screen filter plate and then analyzed by LC-MS/MS methods. Our results showed a good agreement between the samples prepared with and without the screen filter plate, demonstrating the utility and efficiency of this novel device for preparation of blood and plasma samples. The device is simple, easy to use, and reusable. It can be employed for sample preparation of other biological fluids that contain floating particulates or aggregates.

Microwave Crystallization of Lithium Aluminum Germanium Phosphate Solid-State Electrolyte.

PubMed

Mahmoud, Morsi M; Cui, Yuantao; Rohde, Magnus; Ziebert, Carlos; Link, Guido; Seifert, Hans Juergen

2016-06-23

Lithium aluminum germanium phosphate (LAGP) glass-ceramics are considered as promising solid-state electrolytes for Li-ion batteries. LAGP glass was prepared via the regular conventional melt-quenching method. Thermal, chemical analyses and X-ray diffraction (XRD) were performed to characterize the prepared glass. The crystallization of the prepared LAGP glass was done using conventional heating and high frequency microwave (MW) processing. Thirty GHz microwave (MW) processing setup were used to convert the prepared LAGP glass into glass-ceramics and compared with the conventionally crystallized LAGP glass-ceramics that were heat-treated in an electric conventional furnace. The ionic conductivities of the LAGP samples obtained from the two different routes were measured using impedance spectroscopy. These samples were also characterized using XRD and scanning electron microscopy (SEM). Microwave processing was successfully used to crystallize LAGP glass into glass-ceramic without the aid of susceptors. The MW treated sample showed higher total, grains and grain boundary ionic conductivities values, lower activation energy and relatively larger-grained microstructure with less porosity compared to the corresponding conventionally treated sample at the same optimized heat-treatment conditions. The enhanced total, grains and grain boundary ionic conductivities values along with the reduced activation energy that were observed in the MW treated sample was considered as an experimental evidence for the existence of the microwave effect in LAGP crystallization process. MW processing is a promising candidate technology for the production of solid-state electrolytes for Li-ion battery.

[Sample preparation and bioanalysis in mass spectrometry].

PubMed

Bourgogne, Emmanuel; Wagner, Michel

2015-01-01

The quantitative analysis of compounds of clinical interest of low molecular weight (<1000 Da) in biological fluids is currently in most cases performed by liquid chromatography-mass spectrometry (LC-MS). Analysis of these compounds in biological fluids (plasma, urine, saliva, hair...) is a difficult task requiring a sample preparation. Sample preparation is a crucial part of chemical/biological analysis and in a sense is considered the bottleneck of the whole analytical process. The main objectives of sample preparation are the removal of potential interferences, analyte preconcentration, and converting (if needed) the analyte into a more suitable form for detection or separation. Without chromatographic separation, endogenous compounds, co-eluted products may affect a quantitative method in mass spectrometry performance. This work focuses on three distinct parts. First, quantitative bioanalysis will be defined, different matrices and sample preparation techniques currently used in bioanalysis by mass spectrometry of/for small molecules of clinical interest in biological fluids. In a second step the goals of sample preparation will be described. Finally, in a third step, sample preparation strategies will be made either directly ("dilute and shoot") or after precipitation.

Handling Heavenly Jewels - 35 Years of Antarctic Meteorite Processing at Johnson Space Center

NASA Technical Reports Server (NTRS)

Satterwhite, C. E.; McBridge, K. M.; Harrington, R.; Schwarz, C. M.

2011-01-01

The ANSMET program began in 1976, and since that time more than 18,000 meteorites have been processed in the Meteorite Processing Lab at Johnson Space Center in Houston, TX[1]. The meteorites are collected and returned to JSC on a freezer truck and remain frozen until they are initially processed. Initial Processing of Meteorites: Initial processing involves drying the meteorites in a nitrogen glove box for 24 to 48 hours, photographing, measuring, weighing and writing a description of the interior and exterior. The meteorite is broken and a representative sample is sent to the Smithsonian Institution for classification. Newsletter & Requests: Once initial processing has been complete and the meteorites have been classified, the information is published in the Antarctic Meteorite Newsletter[2,3]. The newsletter is published twice yearly and is sent electronically to researchers around the world and is also available on line. Researchers are asked to fill out a request form and submit it to the Meteorite Working Group secretary. All sample requests will be reviewed by either the meteorite curator or the Meteorite Working Group de-pending on the type of meteorite and the research being conducted. Processing for Sample Requests: In the meteorite processing lab, meteorite samples are prepared several different ways. Most samples are prepared as chips obtained by use of stainless steel chisels in a chipping bowl or rock splitter. In special situations where a researcher needs a slab the meteorite samples can be bandsawed in a dry nitrogen glove box with a diamond blade, no liquids are ever introduced into the cabinet. The last type of sample preparation is thin/thick sections. The meteorite thin section lab at JSC can prepare standard 30-micron thin sections, thick sections of variable thickness (100 to 200 microns), or demountable sections using superglue. Information for researchers: It is important that re-searchers fill the sample request form completely, in order to make sure the meteorite is processed correctly[4]. Re-searchers should list any special requirements on the form, i.e. packaging of samples (poly vs. stainless), thick sections and thickness needed, superglue needed, interior chips, exterior chips, fusion crust, contamination issues, all concerns should be listed so processing can be done accurately and any concerns the researcher has can be addressed be-fore the meteorites are broken.

Simultaneous derivatization/preconcentration of volatile aldehydes with a miniaturized fiber-packed sample preparation device designed for gas chromatographic analysis.

PubMed

Saito, Yoshihiro; Ueta, Ikuo; Ogawa, Mitsuhiro; Jinno, Kiyokatsu

2006-10-01

A novel in-needle sample preparation device has been developed for the determination of volatile aldehydes in gaseous samples. The needle device is designed for the gas chromatographic (GC) analysis of aldehydes and ketones commonly found in typical in-house environments. In order to prepare the extraction device, a bundle of polymer-coated filaments was longitudinally packed into a specially designed needle. Derivatization reactions were prompted by 2,4-dinitrophenylhydrazine (NDPH) included in the needle, and so the aldehydes and ketones were derivatized to the corresponding hydrazones and extracted with the extraction needle. A reproducible extraction needle preparation process was established, along with a repeatable derivatization/extraction process that ensures the successful determination of aldehydes. The storage performance of the extraction needle was also evaluated at room temperature for three days. The results demonstrate the successful application of the fiber-packed extraction device to the preparation of a gaseous sample of aldehydes, and the future possibility of applying the extraction device to the analysis of in-house environments.

Method for preparing Pb-. beta. ''-alumina ceramic

DOEpatents

Hellstrom, E.E.

1984-08-30

A process is disclosed for preparing impermeable, polycrystalline samples of Pb-..beta..''-alumina ceramic from Na-..beta..''-alumina ceramic by ion exchange. The process comprises two steps. The first step is a high-temperature vapor phase exchange of Na by K, followed by substitution of Pb for K by immersing the sample in a molten Pb salt bath. The result is a polycrystalline Pb-..beta..''-alumina ceramic that is substantially crack-free.

Method for preparing Pb-.beta."-alumina ceramic

DOEpatents

Hellstrom, Eric E.

1986-01-01

A process is disclosed for preparing impermeable, polycrystalline samples of Pb-.beta."-alumina ceramic from Na-.beta."-alumina ceramic by ion exchange. The process comprises two steps. The first step is a high-temperature vapor phase exchange of Na by K, followed by substitution of Pb for K by immersing the sample in a molten Pb salt bath. The result is a polycrystalline Pb-.beta."-alumina ceramic that is substantially crack-free.

Characterization and phenol adsorption performance of activated carbon prepared from tea residue by NaOH activation.

PubMed

Tao, Jun; Huo, Peili; Fu, Zongheng; Zhang, Jin; Yang, Zhen; Zhang, Dengfeng

2017-10-05

The preparation of activated carbon (AC) using tea residue was addressed in this work. The preparation process incorporated two-step pyrolysis and activation using NaOH. The influence of activation temperature between 500°C and 700°C on the properties of the AC sample was investigated. The physicochemical properties of the AC sample were characterized. The results show that the optimum temperature for the activation process is 700°C, which generates the AC sample with higher specific surface area and total pore volume, respectively, of 819 m 2  g -1 and 0.443 cm 3  g -1 . The oxygen-containing functional groups evolve on the AC sample during the activation process. The phenol adsorption test was performed to evaluate the adsorption performance of the AC sample. The adsorption data confirm that phenol adsorption on the AC sample obtained at 700°C follows the pseudo-second-order kinetics model. Hereby, the electron donor-acceptor interaction mechanism can describe the adsorption process. The AC sample obtained at 700°C performs superior phenol adsorption performance. The maximum phenol adsorption capacity is 320 mg g -1 , which is higher than that of several AC samples reported previously. Thus, the tea residue acts as a good precursor for the AC with promising adsorption capacity by the NaOH chemical activation method.

Synchrotron/crystal sample preparation

NASA Technical Reports Server (NTRS)

Johnson, R. Barry

1993-01-01

The Center for Applied Optics (CAO) of the University of Alabama in Huntsville (UAH) prepared this final report entitled 'Synchrotron/Crystal Sample Preparation' in completion of contract NAS8-38609, Delivery Order No. 53. Hughes Danbury Optical Systems (HDOS) is manufacturing the Advanced X-ray Astrophysics Facility (AXAF) mirrors. These thin-walled, grazing incidence, Wolter Type-1 mirrors, varying in diameter from 1.2 to 0.68 meters, must be ground and polished using state-of-the-art techniques in order to prevent undue stress due to damage or the presence of crystals and inclusions. The effect of crystals on the polishing and grinding process must also be understood. This involves coating special samples of Zerodur and measuring the reflectivity of the coatings in a synchrotron system. In order to gain the understanding needed on the effect of the Zerodur crystals by the grinding and polishing process, UAH prepared glass samples by cutting, grinding, etching, and polishing as required to meet specifications for witness bars for synchrotron measurements and for investigations of crystals embedded in Zerodur. UAH then characterized these samples for subsurface damage and surface roughness and figure.

Preparation and evaluation of Apollo 14 composite experiments

NASA Technical Reports Server (NTRS)

Steurer, W. H.; Kaye, S.

1971-01-01

An account is given of the work aimed at flight experiments on Apollo 14, in relation to space manufacturing processes. Evaluation of suitable materials, definition of in-flight processing procedures, preparation of preprocessed materials and delivery, and evaluation of the space-processed samples after return from the Apollo 14 flight are presented.

SLUDGE BATCH 7B QUALIFICATION ACTIVITIES WITH SRS TANK FARM SLUDGE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pareizs, J.; Click, D.; Lambert, D.

2011-11-16

Waste Solidification Engineering (WSE) has requested that characterization and a radioactive demonstration of the next batch of sludge slurry - Sludge Batch 7b (SB7b) - be completed in the Shielded Cells Facility of the Savannah River National Laboratory (SRNL) via a Technical Task Request (TTR). This characterization and demonstration, or sludge batch qualification process, is required prior to transfer of the sludge from Tank 51 to the Defense Waste Processing Facility (DWPF) feed tank (Tank 40). The current WSE practice is to prepare sludge batches in Tank 51 by transferring sludge from other tanks. Discharges of nuclear materials from Hmore » Canyon are often added to Tank 51 during sludge batch preparation. The sludge is washed and transferred to Tank 40, the current DWPF feed tank. Prior to transfer of Tank 51 to Tank 40, SRNL typically simulates the Tank Farm and DWPF processes with a Tank 51 sample (referred to as the qualification sample). With the tight schedule constraints for SB7b and the potential need for caustic addition to allow for an acceptable glass processing window, the qualification for SB7b was approached differently than past batches. For SB7b, SRNL prepared a Tank 51 and a Tank 40 sample for qualification. SRNL did not receive the qualification sample from Tank 51 nor did it simulate all of the Tank Farm washing and decanting operations. Instead, SRNL prepared a Tank 51 SB7b sample from samples of Tank 7 and Tank 51, along with a wash solution to adjust the supernatant composition to the final SB7b Tank 51 Tank Farm projections. SRNL then prepared a sample to represent SB7b in Tank 40 by combining portions of the SRNL-prepared Tank 51 SB7b sample and a Tank 40 Sludge Batch 7a (SB7a) sample. The blended sample was 71% Tank 40 (SB7a) and 29% Tank 7/Tank 51 on an insoluble solids basis. This sample is referred to as the SB7b Qualification Sample. The blend represented the highest projected Tank 40 heel (as of May 25, 2011), and thus, the highest projected noble metals content for SB7b. Characterization was performed on the Tank 51 SB7b samples and SRNL performed DWPF simulations using the Tank 40 SB7b material. This report documents: (1) The preparation and characterization of the Tank 51 SB7b and Tank 40 SB7b samples. (2) The performance of a DWPF Chemical Process Cell (CPC) simulation using the SB7b Tank 40 sample. The simulation included a Sludge Receipt and Adjustment Tank (SRAT) cycle, where acid was added to the sludge to destroy nitrite and reduce mercury, and a Slurry Mix Evaporator (SME) cycle, where glass frit was added to the sludge in preparation for vitrification. The SME cycle also included replication of five canister decontamination additions and concentrations. Processing parameters were based on work with a nonradioactive simulant. (3) Vitrification of a portion of the SME product and characterization and durability testing (as measured by the Product Consistency Test (PCT)) of the resulting glass. (4) Rheology measurements of the SRAT receipt, SRAT product, and SME product. This program was controlled by a Task Technical and Quality Assurance Plan (TTQAP), and analyses were guided by an Analytical Study Plan. This work is Technical Baseline Research and Development (R&D) for the DWPF. It should be noted that much of the data in this document has been published in interoffice memoranda. The intent of this technical report is bring all of the SB7b related data together in a single permanent record and to discuss the overall aspects of SB7b processing.« less

The influence of surface roughness and high pressure torsion on the growth of anodic titania nanotubes on pure titanium

NASA Astrophysics Data System (ADS)

Hu, Nan; Gao, Nong; Starink, Marco J.

2016-11-01

Anodic titanium dioxide nanotube (TNT) arrays have wide applications in photocatalytic, catalysis, electronics, solar cells and biomedical implants. When TNT coatings are combined with severe plastic deformation (SPD), metal processing techniques which efficiently improve the strength of metals, a new generation of biomedical implant is made possible with both improved bulk and surface properties. This work investigated the effect of processing by high pressure torsion (HPT) and different mechanical preparations on the substrate and subsequently on the morphology of TNT layers. HPT processing was applied to refine the grain size of commercially pure titanium samples and substantially improved their strength and hardness. Subsequent anodization at 30 V in 0.25 wt.% NH4F for 2 h to form TNT layers on sample surfaces prepared with different mechanical preparation methods was carried out. It appeared that the local roughness of the titanium surface on a microscopic level affected the TNT morphology more than the macroscopic surface roughness. For HPT-processed sample, the substrate has to be pre-treated by a mechanical preparation finer than 4000 grit for HPT to have a significant influence on TNTs. During the formation of TNT layers the oxide dissolution rate was increased for the ultrafine-grained microstructure formed due to HPT processing.

Effects of preparation on nutrient and environmental contaminant levels in Arctic beluga whale (Delphinapterus leucas) traditional foods.

PubMed

Binnington, Matthew J; Lei, Ying D; Pokiak, Lucky; Pokiak, James; Ostertag, Sonja K; Loseto, Lisa L; Chan, Hing M; Yeung, Leo W Y; Huang, Haiyong; Wania, Frank

2017-08-16

For Canadian Arctic indigenous populations, marine mammal (MM) traditional foods (TFs) represent sources of both important nutrients and hazardous environmental contaminants. Food preparation is known to impact the nutrient and environmental contaminant content of processed items, yet the impacts of preparation on indigenous Arctic MM TFs remain poorly characterized. In order to determine how the various processes involved in preparing beluga blubber TFs affect their levels of nutrients and environmental contaminants, we collected blubber samples from 2 male beluga whales, aged 24 and 37 years, captured during the 2014 summer hunting season in Tuktoyaktuk, Northwest Territories, and processed them according to local TF preparation methods. We measured the levels of select nutrients [selenium (Se), polyunsaturated fatty acids (PUFAs)] and contaminants [organochlorine pesticides, perfluoroalkyl and polyfluoroalkyl substances (PFASs), polybrominated diphenyl ethers, polychlorinated biphenyls, polycyclic aromatic hydrocarbons (PAHs), mercury (Hg)] in raw and prepared (boiled, roasted, aged) beluga blubber TFs. The impacts of beluga blubber TF preparation methods on nutrient and environmental contaminant levels were inconsistent, as the majority of processes either did not appear to influence concentrations or affected the two belugas differently. However, roasting and ageing beluga blubber consistently impacted certain compounds: roasting blubber increased concentrations of hydrophilic substances (Se and certain PFASs) through solvent depletion and deposited PAHs from cookfire smoke. The solid-liquid phase separation involved in ageing blubber depleted hydrophilic elements (Se, Hg) and some ionogenic PFASs from the lipid-rich liquid oil phase, while PUFA levels appeared to increase, and hydrophobic persistent organic pollutants were retained. Ageing blubber adjacent to in-use smokehouses also resulted in considerable PAH deposition to processed samples. Our findings demonstrated that contaminant concentration differences were greater between the two sets of whale samples, based on age differences, than they were within each set of whale samples, due to variable preparation methods. When considering means to minimize human contaminant exposure while maximizing nutrient intake, consumption of aged liquid from younger male whales would be preferred, based on possible PUFA enhancement and selective depletion of hydrophilic environmental contaminants in this food item.

Fluidics platform and method for sample preparation and analysis

DOEpatents

Benner, W. Henry; Dzenitis, John M.; Bennet, William J.; Baker, Brian R.

2014-08-19

Herein provided are fluidics platform and method for sample preparation and analysis. The fluidics platform is capable of analyzing DNA from blood samples using amplification assays such as polymerase-chain-reaction assays and loop-mediated-isothermal-amplification assays. The fluidics platform can also be used for other types of assays and analyzes. In some embodiments, a sample in a sealed tube can be inserted directly. The following isolation, detection, and analyzes can be performed without a user's intervention. The disclosed platform may also comprises a sample preparation system with a magnetic actuator, a heater, and an air-drying mechanism, and fluid manipulation processes for extraction, washing, elution, assay assembly, assay detection, and cleaning after reactions and between samples.

The effect of reaction temperature on the room temperature ferromagnetic property of sol-gel derived tin oxide nanocrystal

NASA Astrophysics Data System (ADS)

Sakthiraj, K.; Hema, M.; Balachandra Kumar, K.

2018-06-01

In the present study, nanocrystalline tin oxide materials were prepared using sol-gel method with different reaction temperatures (25 °C, 50 °C, 75 °C & 90 °C) and the relation between the room temperature ferromagnetic property of the sample with processing temperature has been analysed. The X-ray diffraction pattern and infrared absorption spectra of the as-prepared samples confirm the purity of the samples. Transmission electron microscopy images visualize the particle size variation with respect to reaction temperature. The photoluminescence spectra of the samples demonstrate that luminescence process in materials is originated due to the electron transition mediated by defect centres. The room temperature ferromagnetic property is observed in all the samples with different amount, which was confirmed using vibrating sample magnetometer measurements. The saturation magnetization value of the as-prepared samples is increased with increasing the reaction temperature. From the photoluminescence & magnetic measurements we accomplished that, more amount of surface defects like oxygen vacancy and tin interstitial are created due to the increase in reaction temperature and it controls the ferromagnetic property of the samples.

Author Contribution to the Pu Handbook II: Chapter 37 LLNL Integrated Sample Preparation Glovebox (TEM) Section

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wall, Mark A.

The development of our Integrated Actinide Sample Preparation Laboratory (IASPL) commenced in 1998 driven by the need to perform transmission electron microscopy studies on naturally aged plutonium and its alloys looking for the microstructural effects of the radiological decay process (1). Remodeling and construction of a laboratory within the Chemistry and Materials Science Directorate facilities at LLNL was required to turn a standard radiological laboratory into a Radiological Materials Area (RMA) and Radiological Buffer Area (RBA) containing type I, II and III workplaces. Two inert atmosphere dry-train glove boxes with antechambers and entry/exit fumehoods (Figure 1), having a baseline atmospheremore » of 1 ppm oxygen and 1 ppm water vapor, a utility fumehood and a portable, and a third double-walled enclosure have been installed and commissioned. These capabilities, along with highly trained technical staff, facilitate the safe operation of sample preparation processes and instrumentation, and sample handling while minimizing oxidation or corrosion of the plutonium. In addition, we are currently developing the capability to safely transfer small metallographically prepared samples to a mini-SEM for microstructural imaging and chemical analysis. The gloveboxes continue to be the most crucial element of the laboratory allowing nearly oxide-free sample preparation for a wide variety of LLNL-based characterization experiments, which includes transmission electron microscopy, electron energy loss spectroscopy, optical microscopy, electrical resistivity, ion implantation, X-ray diffraction and absorption, magnetometry, metrological surface measurements, high-pressure diamond anvil cell equation-of-state, phonon dispersion measurements, X-ray absorption and emission spectroscopy, and differential scanning calorimetry. The sample preparation and materials processing capabilities in the IASPL have also facilitated experimentation at world-class facilities such as the Advanced Photon Source at Argonne National Laboratory, the European Synchrotron Radiation Facility in Grenoble, France, the Stanford Synchrotron Radiation Facility, the National Synchrotron Light Source at Brookhaven National Laboratory, the Advanced Light Source at Lawrence Berkeley National Laboratory, and the Triumph Accelerator in Canada.« less

New Methods of Sample Preparation for Atom Probe Specimens

NASA Technical Reports Server (NTRS)

Kuhlman, Kimberly, R.; Kowalczyk, Robert S.; Ward, Jennifer R.; Wishard, James L.; Martens, Richard L.; Kelly, Thomas F.

2003-01-01

Magnetite is a common conductive mineral found on Earth and Mars. Disk-shaped precipitates approximately 40 nm in diameter have been shown to have manganese and aluminum concentrations. Atom-probe field-ion microscopy (APFIM) is the only technique that can potentially quantify the composition of these precipitates. APFIM will be used to characterize geological and planetary materials, analyze samples of interest for geomicrobiology; and, for the metrology of nanoscale instrumentation. Prior to APFIM sample preparation was conducted by electropolishing, the method of sharp shards (MSS), or Bosch process (deep reactive ion etching) with focused ion beam (FIB) milling as a final step. However, new methods are required for difficult samples. Many materials are not easily fabricated using electropolishing, MSS, or the Bosch process, FIB milling is slow and expensive, and wet chemistry and the reactive ion etching are typically limited to Si and other semiconductors. APFIM sample preparation using the dicing saw is commonly used to section semiconductor wafers into individual devices following manufacture. The dicing saw is a time-effective method for preparing high aspect ratio posts of poorly conducting materials. Femtosecond laser micromachining is also suitable for preparation of posts. FIB time required is reduced by about a factor of 10 and multi-tip specimens can easily be fabricated using the dicing saw.

14C sample preparation for AMS microdosing studies at Lund University using online combustion and septa-sealed vials

NASA Astrophysics Data System (ADS)

Sydoff, Marie; Stenström, Kristina

2010-04-01

The Department of Physics at Lund University is participating in a European Union project called EUMAPP (European Union Microdose AMS Partnership Programme), in which sample preparation and accelerator mass spectrometry (AMS) measurements of biological samples from microdosing studies have been made. This paper describes a simplified method of converting biological samples to solid graphite for 14C analysis with AMS. The method is based on online combustion of the samples, and reduction of CO 2 in septa-sealed vials. The septa-sealed vials and disposable materials are used to eliminate sample cross-contamination. Measurements of ANU and Ox I standards show deviations of 2% and 3%, respectively, relative to reference values. This level of accuracy is sufficient for biological samples from microdosing studies. Since the method has very few handling steps from sample to graphite, the risk of failure during the sample preparation process is minimized, making the method easy to use in routine preparation of samples.

A "three-in-one" sample preparation method for simultaneous determination of B-group water-soluble vitamins in infant formula using VitaFast(®) kits.

PubMed

Zhang, Heng; Lan, Fang; Shi, Yupeng; Wan, Zhi-Gang; Yue, Zhen-Feng; Fan, Fang; Lin, Yan-Kui; Tang, Mu-Jin; Lv, Jing-Zhang; Xiao, Tan; Yi, Changqing

2014-06-15

VitaFast(®) test kits designed for the microbiological assay in microtiter plate format can be applied to quantitative determination of B-group water-soluble vitamins such as vitamin B12, folic acid and biotin, et al. Compared to traditional microbiological methods, VitaFast(®) kits significantly reduce sample processing time and provide greater reliability, higher productivity and better accuracy. Recently, simultaneous determination of vitamin B12, folic acid and biotin in one sample is urgently required when evaluating the quality of infant formulae in our practical work. However, the present sample preparation protocols which are developed for individual test systems, are incompatible with simultaneous determination of several analytes. To solve this problem, a novel "three-in-one" sample preparation method is herein developed for simultaneous determination of B-group water-soluble vitamins using VitaFast(®) kits. The performance of this novel "three-in-one" sample preparation method was systematically evaluated through comparing with individual sample preparation protocols. The experimental results of the assays which employed "three-in-one" sample preparation method were in good agreement with those obtained from conventional VitaFast(®) extraction methods, indicating that the proposed "three-in-one" sample preparation method is applicable to the present three VitaFast(®) vitamin test systems, thus offering a promising alternative for the three independent sample preparation methods. The proposed new sample preparation method will significantly improve the efficiency of infant formulae inspection. Copyright © 2013 Elsevier Ltd. All rights reserved.

Optical properties of micro and nano LiNbO3 thin film prepared by spin coating

NASA Astrophysics Data System (ADS)

Fakhri, Makram A.; Salim, Evan T.; Abdulwahhab, Ahmed W.; Hashim, U.; Salim, Zaid T.

2018-07-01

This paper deals with preparing of Lithium-Niobate thin films based on Sol-Gel technique on a substrate made of quartz, samples have been deposited under three different stirrer times. At 3000 round per minute of spin coating strategy, the deposition processes have been accomplished. The results showed an enhancement in the crystalline structure of the prepared samples with increasing the duration of stirrer time. The AFM measurement has assured that the structure of the prepared samples is more regular distributed, homogeneous and crack-free in their structures. Further, measurements and calculations of lattice constant, energy band gap, refractive index, and optical dielectric constant are also considered and agreed with experimental data collected by the characterized samples.

M3FT-17OR0301070211 - Preparation of Hot Isostatically Pressed AgZ Waste Form Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jubin, Robert Thomas; Bruffey, Stephanie H.; Jordan, Jacob A.

The production of radioactive iodine-bearing waste forms that exhibit long-term stability and are suitable for permanent geologic disposal has been the subject of substantial research interest. One potential method of iodine waste form production is hot isostatic pressing (HIP). Recent studies at Oak Ridge National Laboratory (ORNL) have investigated the conversion of iodine-loaded silver mordenite (I-AgZ) directly to a waste form by HIP. ORNL has performed HIP with a variety of sample compositions and pressing conditions. The base mineral has varied among AgZ (in pure and engineered forms), silver-exchanged faujasite, and silverexchanged zeolite A. Two iodine loading methods, occlusion andmore » chemisorption, have been explored. Additionally, the effects of variations in temperature and pressure of the process have been examined, with temperature ranges of 525°C–1,100°C and pressure ranges of 100–300 MPa. All of these samples remain available to collaborators upon request. The sample preparation detailed in this document is an extension of that work. In addition to previously prepared samples, this report documents the preparation of additional samples to support stability testing. These samples include chemisorbed I-AgZ and pure AgI. Following sample preparation, each sample was processed by HIP by American Isostatic Presses Inc. and returned to ORNL for storage. ORNL will store the samples until they are requested by collaborators for durability testing. The sample set reported here will support waste form durability testing across the national laboratories and will provide insight into the effects of varied iodine content on iodine retention by the produced waste form and on potential improvements in waste form durability provided by the zeolite matrix.« less

Semiautomated Sample Preparation for Protein Stability and Formulation Screening via Buffer Exchange.

PubMed

Ying, William; Levons, Jaquan K; Carney, Andrea; Gandhi, Rajesh; Vydra, Vicky; Rubin, A Erik

2016-06-01

A novel semiautomated buffer exchange process workflow was developed to enable efficient early protein formulation screening. An antibody fragment protein, BMSdab, was used to demonstrate the workflow. The process afforded 60% to 80% cycle time and scientist time savings and significant material efficiencies. These efficiencies ultimately facilitated execution of this stability work earlier in the drug development process, allowing this tool to inform the developability of potential candidates for development from a formulation perspective. To overcome the key technical challenges, the protein solution was buffer-exchanged by centrifuge filtration into formulations for stability screening in a 96-well plate with an ultrafiltration membrane, leveraging automated liquid handling and acoustic volume measurements to allow several cycles of exchanges. The formulations were transferred into a vacuum manifold and sterile filtered into a rack holding 96 glass vials. The vials were sealed with a capmat of individual caps and placed in stability stations. Stability of the samples prepared by this process and by the standard process was demonstrated to be comparable. This process enabled screening a number of formulations of a protein at an early pharmaceutical development stage with a short sample preparation time. © 2015 Society for Laboratory Automation and Screening.

Follow-up of the fate of imazalil from post-harvest lemon surface treatment to a baking experiment.

PubMed

Vass, Andrea; Korpics, Evelin; Dernovics, Mihály

2015-01-01

Imazalil is one of the most widespread fungicides used for the post-harvest treatment of citrus species. The separate use of peel during food preparation and processing may hitherto concentrate most of the imazalil into food products, where specific maximum residue limits hardly exist for this fungicide. In order to monitor comprehensively the path of imazalil, our study covered the monitoring of the efficiency of several washing treatments, the comparison of operative and related sample preparation methods for the lemon samples, the validation of a sample preparation technique for a fatty cake matrix, the preparation of a model cake sample made separately either with imazalil containing lemon peel or with imazalil spiking, the monitoring of imazalil degradation into α-(2,4-dichlorophenyl)-1H-imidazole-1-ethanol because of the baking process, and finally the mass balance of imazalil throughout the washing experiments and the baking process. Quantification of imazalil was carried out with an LC-ESI-MS/MS set-up, while LC-QTOF was used for the monitoring of imazalil degradation. Concerning the washing, none of the addressed five washing protocols could remove more than 30% of imazalil from the surface of the lemon samples. The study revealed a significant difference between the extraction efficiency of imazalil by the EN 15662:2008 and AOAC 2007.1 methods, with the advantage of the former. The use of the model cake sample helped to validate a modified version of the EN 15662:2008 method that included a freeze-out step to efficiently recover imazalil (>90%) from the fatty cake matrix. The degradation of imazalil during the baking process was significantly higher when this analyte was spiked into the cake matrix than in the case of preparing the cake with imazalil-containing lemon peel (52% vs. 22%). This observation calls the attention to the careful evaluation of pesticide stability data that are based on solution spiking experiments.

Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation.

PubMed

Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

2016-06-01

A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa.

Sample and data processing considerations for the NIST quantitative infrared database

NASA Astrophysics Data System (ADS)

Chu, Pamela M.; Guenther, Franklin R.; Rhoderick, George C.; Lafferty, Walter J.; Phillips, William

1999-02-01

Fourier-transform infrared (FT-IR) spectrometry has become a useful real-time in situ analytical technique for quantitative gas phase measurements. In fact, the U.S. Environmental Protection Agency (EPA) has recently approved open-path FT-IR monitoring for the determination of hazardous air pollutants (HAP) identified in EPA's Clean Air Act of 1990. To support infrared based sensing technologies, the National Institute of Standards and Technology (NIST) is currently developing a standard quantitative spectral database of the HAPs based on gravimetrically prepared standard samples. The procedures developed to ensure the quantitative accuracy of the reference data are discussed, including sample preparation, residual sample contaminants, data processing considerations, and estimates of error.

Inverse supercritical fluid extraction as a sample preparation method for the analysis of the nanoparticle content in sunscreen agents.

PubMed

Müller, David; Cattaneo, Stefano; Meier, Florian; Welz, Roland; de Vries, Tjerk; Portugal-Cohen, Meital; Antonio, Diana C; Cascio, Claudia; Calzolai, Luigi; Gilliland, Douglas; de Mello, Andrew

2016-04-01

We demonstrate the use of inverse supercritical carbon dioxide (scCO2) extraction as a novel method of sample preparation for the analysis of complex nanoparticle-containing samples, in our case a model sunscreen agent with titanium dioxide nanoparticles. The sample was prepared for analysis in a simplified process using a lab scale supercritical fluid extraction system. The residual material was easily dispersed in an aqueous solution and analyzed by Asymmetrical Flow Field-Flow Fractionation (AF4) hyphenated with UV- and Multi-Angle Light Scattering detection. The obtained results allowed an unambiguous determination of the presence of nanoparticles within the sample, with almost no background from the matrix itself, and showed that the size distribution of the nanoparticles is essentially maintained. These results are especially relevant in view of recently introduced regulatory requirements concerning the labeling of nanoparticle-containing products. The novel sample preparation method is potentially applicable to commercial sunscreens or other emulsion-based cosmetic products and has important ecological advantages over currently used sample preparation techniques involving organic solvents. Copyright © 2016 Elsevier B.V. All rights reserved.

Atmospheric Processing Platform | Photovoltaic Research | NREL

Science.gov Websites

printing units to the left and sample preparation and rapid thermal processing units to the right. In variety of substrates and then further process into optoelectronic materials using rapid thermal , however, occur within a vacuum (i.e., thermal evaporation, sputtering). Samples can remain in ambient

A Combined Fabrication and Instrumentation Platform for Sample Preparation.

PubMed

Guckenberger, David J; Thomas, Peter C; Rothbauer, Jacob; LaVanway, Alex J; Anderson, Meghan; Gilson, Dan; Fawcett, Kevin; Berto, Tristan; Barrett, Kevin; Beebe, David J; Berry, Scott M

2014-06-01

While potentially powerful, access to molecular diagnostics is substantially limited in the developing world. Here we present an approach to reduced cost molecular diagnostic instrumentation that has the potential to empower developing world communities by reducing costs through streamlining the sample preparation process. In addition, this instrument is capable of producing its own consumable devices on demand, reducing reliance on assay suppliers. Furthermore, this instrument is designed with an "open" architecture, allowing users to visually observe the assay process and make modifications as necessary (as opposed to traditional "black box" systems). This open environment enables integration of microfluidic fabrication and viral RNA purification onto an easy-to-use modular system via the use of interchangeable trays. Here we employ this system to develop a protocol to fabricate microfluidic devices and then use these devices to isolate viral RNA from serum for the measurement of human immunodeficiency virus (HIV) viral load. Results obtained from this method show significantly reduced error compared with similar nonautomated sample preparation processes. © 2014 Society for Laboratory Automation and Screening.

CESIUM REMOVAL FROM TANKS 241-AN-103 & 241-SX-105 & 241-AZ-101/102 COMPOSITE FOR TESTING IN BENCH SCALE STEAM REFORMER

DOE Office of Scientific and Technical Information (OSTI.GOV)

DUNCAN JB; HUBER HJ

2011-06-08

This report documents the preparation of three actual Hanford tank waste samples for shipment to the Savannah River National Laboratory (SRNL). Two of the samples were dissolved saltcakes from tank 241-AN-103 (hereafter AN-103) and tank 241-SX-105 (hereafter SX-105); one sample was a supernate composite from tanks 241-AZ-101 and 241-AZ-102 (hereafter AZ-101/102). The preparation of the samples was executed following the test plans LAB-PLAN-10-00006, Test Plan for the Preparation of Samples from Hanford Tanks 241-SX-105, 241-AN-103, 241-AN-107, and LAB-PLN-10-00014, Test Plan for the Preparation of a Composite Sample from Hanford Tanks 241-AZ-101 and 241-AZ-102 for Steam Reformer Testing at the Savannahmore » River National Laboratory. All procedural steps were recorded in laboratory notebook HNF-N-274 3. Sample breakdown diagrams for AN-103 and SX-105 are presented in Appendix A. The tank samples were prepared in support of a series of treatability studies of the Fluidized Bed Steam Reforming (FBSR) process using a Bench-Scale Reformer (BSR) at SRNL. Tests with simulants have shown that the FBSR mineralized waste form is comparable to low-activity waste glass with respect to environmental durability (WSRC-STI-2008-00268, Mineralization of Radioactive Wastes by Fluidized Bed Steam Reforming (FBSR): Comparisons to Vitreous Waste Forms and Pertinent Durability Testing). However, a rigorous assessment requires long-term performance data from FB SR product formed from actual Hanford tank waste. Washington River Protection Solutions, LLC (WRPS) has initiated a Waste Form Qualification Program (WP-S.2.1-20 1 0-00 1, Fluidized Bed Steam Reformer Low-level Waste Form Qualification) to gather the data required to demonstrate that an adequate FBSR mineralized waste form can be produced. The documentation of the selection process of the three tank samples has been separately reported in RPP-48824, 'Sample Selection Process for Bench-Scale Steam Reforming Treatability Studies Using Hanford Waste Samples.'« less

CESIUM REMOVAL FROM TANKS 241-AN-103 & 241-SX-105 & 241-AZ-101 & 241AZ-102 COMPOSITE FOR TESTING IN BENCH SCALE STEAM REFORMER

DOE Office of Scientific and Technical Information (OSTI.GOV)

DUNCAN JB; HUBER HJ

2011-04-21

This report documents the preparation of three actual Hanford tank waste samples for shipment to the Savannah River National Laboratory (SRNL). Two of the samples were dissolved saltcakes from tank 241-AN-103 (hereafter AN-103) and tank 241-SX-105 (hereafter SX-105); one sample was a supernate composite from tanks 241-AZ-101 and 241-AZ-102 (hereafter AZ-101/102). The preparation of the samples was executed following the test plans LAB-PLAN-10-00006, Test Plan for the Preparation of Samples from Hanford Tanks 241-SX-105, 241-AN-103, 241-AN-107, and LAB-PLN-l0-00014, Test Plan for the Preparation of a Composite Sample from Hanford Tanks 241-AZ-101 and 241-AZ-102 for Steam Reformer Testing at the Savannahmore » River National Laboratory. All procedural steps were recorded in laboratory notebook HNF-N-274 3. Sample breakdown diagrams for AN-103 and SX-105 are presented in Appendix A. The tank samples were prepared in support of a series of treatability studies of the Fluidized Bed Steam Reforming (FBSR) process using a Bench-Scale Reformer (BSR) at SRNL. Tests with simulants have shown that the FBSR mineralized waste form is comparable to low-activity waste glass with respect to environmental durability (WSRC-STI-2008-00268, Mineralization of Radioactive Wastes by Fluidized Bed Steam Reforming (FBSR): Comparisons to Vitreous Waste Forms and Pertinent Durability Testing). However, a rigorous assessment requires long-term performance data from FBSR product formed from actual Hanford tank waste. Washington River Protection Solutions, LLC (WRPS) has initiated a Waste Form Qualification Program (WP-5.2.1-2010-001, Fluidized Bed Steam Reformer Low-level Waste Form Qualification) to gather the data required to demonstrate that an adequate FBSR mineralized waste form can be produced. The documentation of the selection process of the three tank samples has been separately reported in RPP-48824, Sample Selection Process for Bench-Scale Steam Reforming Treatability Studies Using Hanford Waste Samples.« less

Manipulation of surface morphology of flower-like Ag/ZnO nanorods to enhance photocatalytic performance

NASA Astrophysics Data System (ADS)

U-thaipan, Kasira; Tedsree, Karaked

2018-06-01

The surface morphology of flower-like Ag/ZnO nanorod can be manipulated by adopting different synthetic routes and also loading different levels of Ag in order to alter their surface structures to achieve the maximum photocatalytic efficiency. In a single-step preparation method Ag/ZnO was prepared by heating directly a mixture of Zn2+ and Ag+ precursors in an aqueous NaOH-ethylene glycol solution, while in the two-step preparation method an intermediate of flower-shaped ZnO nanorod was obtained by a hydrothermal process before depositing Ag particles on the ZnO surfaces by chemical reduction. The structure, morphology and optical properties of the synthesized samples were characterized using TEM, SEM, XRD, DRS and PL techniques. The sample prepared by single-step method are characterized with agglomeration of Ag atoms as clusters on the surface of ZnO, whereas in the sample prepared by two-step method Ag atoms are found uniformly dispersed and deposited as discrete Ag nanoparticles on the surface of ZnO. A significant enhancement in the adsorption of visible light was evident for Ag/ZnO samples prepared by two-step method especially with low Ag content (0.5 mol%). The flower-like Ag/ZnO nanorod prepared with 0.5 mol% Ag by two-step process was found to be the most efficient photocatalyst for the degradation of phenol, which can decompose 90% of phenol within 120 min.

Utility of Cytospin and Cell block Technology in Evaluation of Body Fluids and Urine Samples: A Comparative Study.

PubMed

Qamar, Irmeen; Rehman, Suhailur; Mehdi, Ghazala; Maheshwari, Veena; Ansari, Hena A; Chauhan, Sunanda

2018-01-01

Cytologic examination of body fluids commonly involves the use of direct or sediment smears, cytocentrifuge preparations, membrane filter preparations, or cell block sections. Cytospin and cell block techniques are extremely useful in improving cell yield of thin serous effusions and urine samples, and ensure high diagnostic efficacy. We studied cytospin preparations and cell block sections prepared from 180 samples of body fluids and urine samples to compare the relative efficiency of cell retrieval, preservation of cell morphology, ease of application of special stains, and diagnostic efficacy. Samples were collected and processed to prepare cytospin smears and cell block sections. We observed that overall, cell yield and preservation of individual cell morphology were better in cytospin preparations as compared to cell blocks, while preservation of architectural pattern was better in cell block sections. The number of suspicious cases also decreased on cell block sections, with increased detection of malignancy. It was difficult to prepare cell blocks from urine samples due to low cellularity. Cytospin technology is a quick, efficient, and cost-effective method of increasing cell yield in hypocellular samples, with better preservation of cell morphology. Cell blocks are better prepared from high cellularity fluids; however, tissue architecture is better studied, with improved rate of diagnosis and decrease in ambiguous results. Numerous sections can be prepared from a small amount of material. Special stains and immunochemical stains can be easily applied to cell blocks. It also provides a source of archival material.

Growth of carbon nanofibers using resol-type phenolic resin and cobalt(II) catalyst.

PubMed

Kim, Taeyun; Mees, Karina; Park, Ho-Seon; Willert-Porada, Monika; Lee, Chang-Seop

2013-11-01

This study investigated carbon nanofibers (CNFs) grown on reticulated vitreous carbon (RVC) foam through catalytic deposition of ethylene. Before growing the CNFs, Co(II) on the RVC foam was expected to act as a catalyst by deposition. The preparation of the CNFs was a two-step process. The first step was preparing the RVC from polyurethane (PU) foam. Changes in weight over time were evaluated using two kinds of resol. The change in the mass and state of the sample with the change in temperature was studied during the carbonization process. The second step was to prepare the CNFs. An OH group was attached by the oxidation of the RVC foam. A change in the shape and mass of the sample was observed due to a change in nitric acid concentration and oxidation time. Then, cobalt was deposited to grow CNFs on the RVC foam. Hydrolysis helped to deposit the Co(ll) on the RVC foam. The appropriate time and temperature were investigated for the reduction process. In the last step, CNFs were prepared by the introducing ethylene gas. The resulting samples were analyzed using scanning electron microscopy, energy dispersive spectroscopy, N2-sorption, and X-ray photoelectron spectroscopy.

Basic tree-ring sample preparation techniques for aging aspen

Treesearch

Lance A. Asherin; Stephen A. Mata

2001-01-01

Aspen is notoriously difficult to age because of its light-colored wood and faint annual growth rings. Careful preparation and processing of aspen ring samples can overcome these problems, yield accurate age and growth estimates, and concisely date disturbance events present in the tree-ring record. Proper collection of aspen wood is essential in obtaining usable ring...

Electrodeposition as an alternate method for preparation of environmental samples for iodide by AMS

DOE PAGES

Adamic, M. L.; Lister, T. E.; Dufek, E. J.; ...

2015-03-25

This paper presents an evaluation of an alternate method for preparing environmental samples for 129I analysis by accelerator mass spectrometry (AMS) at Idaho National Laboratory. The optimal sample preparation method is characterized by ease of preparation, capability of processing very small quantities of iodide, and ease of loading into a cathode. Electrodeposition of iodide on a silver wire was evaluated using these criteria. This study indicates that the electrochemically-formed silver iodide deposits produce ion currents similar to those from precipitated silver iodide for the same sample mass. Furthermore, precipitated silver iodide samples are usually mixed with niobium or silver powdermore » prior to loading in a cathode. Using electrodeposition, the silver is already mixed with the sample and can simply be picked up with tweezers, placed in the sample die, and pressed into a cathode. The major advantage of this method is that the silver wire/electrodeposited silver iodide is much easier to load into a cathode.« less

Method and apparatus for automated processing and aliquoting of whole blood samples for analysis in a centrifugal fast analyzer

DOEpatents

Burtis, C.A.; Johnson, W.F.; Walker, W.A.

1985-08-05

A rotor and disc assembly for use in a centrifugal fast analyzer. The assembly is designed to process multiple samples of whole blood followed by aliquoting of the resultant serum into precisely measured samples for subsequent chemical analysis. The assembly requires minimal operator involvement with no mechanical pipetting. The system comprises: (1) a whole blood sample disc; (2) a serum sample disc; (3) a sample preparation rotor; and (4) an analytical rotor. The blood sample disc and serum sample disc are designed with a plurality of precision bore capillary tubes arranged in a spoked array. Samples of blood are loaded into the blood sample disc by capillary action and centrifugally discharged into cavities of the sample preparation rotor where separation of serum and solids is accomplished. The serum is loaded into the capillaries of the serum sample disc by capillary action and subsequently centrifugally expelled into cuvettes of the analyticaly rotor for conventional methods. 5 figs.

Method and apparatus for automated processing and aliquoting of whole blood samples for analysis in a centrifugal fast analyzer

DOEpatents

Burtis, Carl A.; Johnson, Wayne F.; Walker, William A.

1988-01-01

A rotor and disc assembly for use in a centrifugal fast analyzer. The assembly is designed to process multiple samples of whole blood followed by aliquoting of the resultant serum into precisely measured samples for subsequent chemical analysis. The assembly requires minimal operator involvement with no mechanical pipetting. The system comprises (1) a whole blood sample disc, (2) a serum sample disc, (3) a sample preparation rotor, and (4) an analytical rotor. The blood sample disc and serum sample disc are designed with a plurality of precision bore capillary tubes arranged in a spoked array. Samples of blood are loaded into the blood sample disc in capillary tubes filled by capillary action and centrifugally discharged into cavities of the sample preparation rotor where separation of serum and solids is accomplished. The serum is loaded into the capillaries of the serum sample disc by capillary action and subsequently centrifugally expelled into cuvettes of the analytical rotor for analysis by conventional methods.

Rocket Research at Georgia Tech.

DTIC Science & Technology

1981-11-01

samples were prepared by dry pressing 30% Valley Met H- 30 aluminum, 7% carnauba wax , and 63% 100 P AP. One sample was prepared using as received H-30, a...Al, and Carnauba wax powders. Sandwiches with aluminum in the binder lamina. Both pre-oxidation and pre-stretching treatments of aluminum particles...two different processes. 1. Dry-pressing powder mixtures in which polymeric binder is replaced by carnauba wax powder. 2. Hand mixing small samples of

Visualizing BPA by molecularly imprinted ratiometric fluorescence sensor based on dual emission nanoparticles.

PubMed

Lu, Hongzhi; Xu, Shoufang

2017-06-15

Construction of ratiometric fluorescent probe often involved in tedious multistep preparation or complicated coupling or chemical modification process. The emergence of dual emission fluorescent nanoparticles would simplify the construction process and avoids the tedious chemical coupling. Herein, we reported a facile strategy to prepare ratiometric fluorescence molecularly imprinted sensor based on dual emission nanoparticles (d-NPs) which comprised of carbon dots and gold nanoclusters for detection of Bisphenol A (BPA). D-NPs emission at 460nm and 580nm were first prepared by seed growth co-microwave method using gold nanoparticles as seeds and glucose as precursor for carbon dots. When they were applied to propose ratiometric fluorescence molecularly imprinted sensor, the preparation process was simplified, and the sensitivity of sensor was improved with detection limit of 29nM, and visualizing BPA was feasible based on the distinguish fluorescence color change. The feasibility of the developed method in real samples was successfully evaluated through the analysis of BPA in water samples with satisfactory recoveries of 95.9-98.9% and recoveries ranging from 92.6% to 98.6% in canned food samples. When detection BPA in positive feeding bottles, the results agree well with those obtained by accredited method. The developed method proposed in this work to prepare ratiometric fluorescence molecularly imprinted sensor based on dual emission nanoparticles proved to be a convenient, reliable and practical way to prepared high sensitive and selective fluorescence sensors. Copyright © 2017 Elsevier B.V. All rights reserved.

Tuning the reactivity of Al/Fe{sub 2}O{sub 3} nanoenergetic materials via an approach combining soft template self-assembly with sol–gel process process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Tianfu; Wang, Zhen; Li, Guoping

2015-10-15

A bottom-up approach combining soft template self-assembly with sol–gel process, was adopted to prepare the assembled Al/Fe{sub 2}O{sub 3} nanoenergetic materials, assembly-Al/Fe{sub 2}O{sub 3} sample. The other two unassembled Al/Fe{sub 2}O{sub 3}a nanoenergetic materials, sol–gel–Al/Fe{sub 2}O{sub 3} sample and mixing-Al/Fe{sub 2}O{sub 3} sample, were prepared by sol–gel method and physical mixing method respectively. The assembly process within the preparation of the assembly-Al/Fe{sub 2}O{sub 3} sample was analyzed through the changes in the average hydrodynamic diameters of the particles and the micelles in solution. SEM, EDS and TEM tests were performed to demonstrate a significant improvement regarding to dispersity and arrangementsmore » of the Al and Fe{sub 2}O{sub 3} particles in the assembled samples, compared to that of the unassembled Al/Fe{sub 2}O{sub 3} samples. DSC test was employed to characterize the reactivity of the samples. The heat release of the assembled Al/Fe{sub 2}O{sub 3} sample was 2088 J/g, about 400 and 990 J/g more than that of the sol–gel–Al/Fe{sub 2}O{sub 3} sample and mixing-Al/Fe{sub 2}O{sub 3} sample, respectively. - Graphical abstract: Modified aluminum (Al) nanoparticles with hydrophobic surface assembled into the Brij S10 micelle in Fe(III) sol, then the well dispersed system was transformed into Al/Fe{sub 2}O{sub 3} nanoenergetic materials with high reactivity. - Highlights: • An approach combining soft template self-assembly with sol–gel process was adopted. • The aggregation of Al nanoparticles in the final product was reduced significantly. • The reactivity of Al/Fe{sub 2}O{sub 3} nanoenergetic materials was improved to a large extent.« less

Optimization of Sample Preparation processes of Bone Material for Raman Spectroscopy.

PubMed

Chikhani, Madelen; Wuhrer, Richard; Green, Hayley

2018-03-30

Raman spectroscopy has recently been investigated for use in the calculation of postmortem interval from skeletal material. The fluorescence generated by samples, which affects the interpretation of Raman data, is a major limitation. This study compares the effectiveness of two sample preparation techniques, chemical bleaching and scraping, in the reduction of fluorescence from bone samples during testing with Raman spectroscopy. Visual assessment of Raman spectra obtained at 1064 nm excitation following the preparation protocols indicates an overall reduction in fluorescence. Results demonstrate that scraping is more effective at resolving fluorescence than chemical bleaching. The scraping of skeletonized remains prior to Raman analysis is a less destructive method and allows for the preservation of a bone sample in a state closest to its original form, which is beneficial in forensic investigations. It is recommended that bone scraping supersedes chemical bleaching as the preferred method for sample preparation prior to Raman spectroscopy. © 2018 American Academy of Forensic Sciences.

Magnetic separation techniques in sample preparation for biological analysis: a review.

PubMed

He, Jincan; Huang, Meiying; Wang, Dongmei; Zhang, Zhuomin; Li, Gongke

2014-12-01

Sample preparation is a fundamental and essential step in almost all the analytical procedures, especially for the analysis of complex samples like biological and environmental samples. In past decades, with advantages of superparamagnetic property, good biocompatibility and high binding capacity, functionalized magnetic materials have been widely applied in various processes of sample preparation for biological analysis. In this paper, the recent advancements of magnetic separation techniques based on magnetic materials in the field of sample preparation for biological analysis were reviewed. The strategy of magnetic separation techniques was summarized. The synthesis, stabilization and bio-functionalization of magnetic nanoparticles were reviewed in detail. Characterization of magnetic materials was also summarized. Moreover, the applications of magnetic separation techniques for the enrichment of protein, nucleic acid, cell, bioactive compound and immobilization of enzyme were described. Finally, the existed problems and possible trends of magnetic separation techniques for biological analysis in the future were proposed. Copyright © 2014 Elsevier B.V. All rights reserved.

Utility of Cytospin and Cell block Technology in Evaluation of Body Fluids and Urine Samples: A Comparative Study

PubMed Central

Qamar, Irmeen; Rehman, Suhailur; Mehdi, Ghazala; Maheshwari, Veena; Ansari, Hena A.; Chauhan, Sunanda

2018-01-01

Background: Cytologic examination of body fluids commonly involves the use of direct or sediment smears, cytocentrifuge preparations, membrane filter preparations, or cell block sections. Cytospin and cell block techniques are extremely useful in improving cell yield of thin serous effusions and urine samples, and ensure high diagnostic efficacy. Materials and Methods: We studied cytospin preparations and cell block sections prepared from 180 samples of body fluids and urine samples to compare the relative efficiency of cell retrieval, preservation of cell morphology, ease of application of special stains, and diagnostic efficacy. Samples were collected and processed to prepare cytospin smears and cell block sections. Results: We observed that overall, cell yield and preservation of individual cell morphology were better in cytospin preparations as compared to cell blocks, while preservation of architectural pattern was better in cell block sections. The number of suspicious cases also decreased on cell block sections, with increased detection of malignancy. It was difficult to prepare cell blocks from urine samples due to low cellularity. Conclusions: Cytospin technology is a quick, efficient, and cost-effective method of increasing cell yield in hypocellular samples, with better preservation of cell morphology. Cell blocks are better prepared from high cellularity fluids; however, tissue architecture is better studied, with improved rate of diagnosis and decrease in ambiguous results. Numerous sections can be prepared from a small amount of material. Special stains and immunochemical stains can be easily applied to cell blocks. It also provides a source of archival material. PMID:29643653

Miniaturized sample preparation needle: a versatile design for the rapid analysis of smoking-related compounds in hair and air samples.

PubMed

Saito, Yoshihiro; Ueta, Ikuo; Ogawa, Mitsuhiro; Hayashida, Makiko; Jinno, Kiyokatsu

2007-05-09

Miniaturized needle extraction device has been developed as a versatile sample preparation device designed for the rapid and simple analysis of smoking-related compounds in smokers' hair samples and environmental tobacco smoke. Packed with polymeric particle, the resulting particle-packed needle was employed as a miniaturized sample preparation device for the analysis of typical volatile organic compounds in tobacco smoke. Introducing a bundle of polymer-coated filaments as the extraction medium, the needle was further applied as a novel sample preparation device containing simultaneous derivatization/extraction process of volatile aldehydes. Formaldehyde (FA) and acetaldehyde (AA) in smoker's breath during the smoking were successfully derivatized with two derivatization reagents in the polymer-coated fiber-packed needle device followed by the separation and determination in gas chromatography (GC). Smokers' hair samples were also packed into the needle, allowing the direct extraction of nicotine from the hair sample in a conventional GC injector. Optimizing the main experimental parameters for each technique, successful determination of several smoking-related compounds with these needle extraction methods has been demonstrated.

A comparison of sample preparation strategies for biological tissues and subsequent trace element analysis using LA-ICP-MS.

PubMed

Bonta, Maximilian; Török, Szilvia; Hegedus, Balazs; Döme, Balazs; Limbeck, Andreas

2017-03-01

Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is one of the most commonly applied methods for lateral trace element distribution analysis in medical studies. Many improvements of the technique regarding quantification and achievable lateral resolution have been achieved in the last years. Nevertheless, sample preparation is also of major importance and the optimal sample preparation strategy still has not been defined. While conventional histology knows a number of sample pre-treatment strategies, little is known about the effect of these approaches on the lateral distributions of elements and/or their quantities in tissues. The technique of formalin fixation and paraffin embedding (FFPE) has emerged as the gold standard in tissue preparation. However, the potential use for elemental distribution studies is questionable due to a large number of sample preparation steps. In this work, LA-ICP-MS was used to examine the applicability of the FFPE sample preparation approach for elemental distribution studies. Qualitative elemental distributions as well as quantitative concentrations in cryo-cut tissues as well as FFPE samples were compared. Results showed that some metals (especially Na and K) are severely affected by the FFPE process, whereas others (e.g., Mn, Ni) are less influenced. Based on these results, a general recommendation can be given: FFPE samples are completely unsuitable for the analysis of alkaline metals. When analyzing transition metals, FFPE samples can give comparable results to snap-frozen tissues. Graphical abstract Sample preparation strategies for biological tissues are compared with regard to the elemental distributions and average trace element concentrations.

Improved thermoelectric properties of Bi2Te3-xSex alloys by melt spinning and resistance pressing sintering

NASA Astrophysics Data System (ADS)

Cai, Xinzhi; Fan, Xi'an; Rong, Zhenzhou; Yang, Fan; Gan, Zhanghua; Li, Guangqiang

2014-03-01

Starting from bismuth, tellurium and selenium chunks, n-type Bi2Te3-xSex (x ⩽ 0.3) alloys were obtained by melt spinning (MS) combined with a resistance pressing sintering (RPS) process. The phases, microstructures and compositions of the samples were evaluated by x-ray diffraction, field emission scanning electron microscopy, and energy dispersive x-ray spectroscopy during each step in the preparation process, respectively. The influences of Se doping, MS and RPS processes on the thermoelectric (TE) properties of Bi2Te3-xSex alloys were investigated in detail. The Bi2Te3-xSex powders could be well compacted by the RPS process and the relative densities of the bulks prepared by RPS were all higher than 96%. The partially oriented lamellar structure could be observed at some regions of the samples prepared by RPS, and the monolayer thickness of the lamellar structure in the MS-RPS samples was smaller than that in the smelting-RPS sample. The MS process was confirmed as an excellent method to obtain fine microstructures and low lattice thermal conductivity for the TE materials. All evidence about electrical and thermal transport properties suggested that suitably increasing the Se content could effectively improve the ZT value. The maximum ZT value of 0.84 was obtained for the Bi2Te2.7Se0.3 prepared by MS-RPS at 423 K. As opposed to the conventional hot pressing and spark plasma sintering, the RPS method introduced here is more suitable for practical industrial application due to its cost saving and high efficiency.

The preparation of Ag-BiVO4 metal composite oxides and its application in efficient photocatalytic oxidative thiophene

NASA Astrophysics Data System (ADS)

Gao, Xiao-Ming; Fu, Feng; Zhang, Li-Ping; Li, Wen-Hong

2013-06-01

A series of Ag-BiVO4 photocatalysts was synthesized by the hydrothemal synthesis method for different pH values. A strong correlation was found among the prepared processing, structure and property of the samples. With increasing pH value from 5 to 9, the crystallinity increases and the as-prepared Ag-BiVO4 sample gradually disappeared from the nanostructures. The light absorption became higher in the UV and visible range, accompanied by a bathochromic shift of the absorption edge. The competitive relations between crystallinity and surface area affecting photocatalytic activity were also discussed. Photocatalytic desulfurization on the as-prepared Ag-BiVO4 samples using thiophene dissolved in n-octane as a model organosulfur compound was performed. It showed that the photocatalytic desulfurization on the as-prepared Ag-BiVO4 sample at pH=7 can be up to 95%, which existed as various size particles and had significant high surface area of 13.768 m2 g-1.

Sample treatments prior to capillary electrophoresis-mass spectrometry.

PubMed

Hernández-Borges, Javier; Borges-Miquel, Teresa M; Rodríguez-Delgado, Miguel Angel; Cifuentes, Alejandro

2007-06-15

Sample preparation is a crucial part of chemical analysis and in most cases can become the bottleneck of the whole analytical process. Its adequacy is a key factor in determining the success of the analysis and, therefore, careful selection and optimization of the parameters controlling sample treatment should be carried out. This work revises the different strategies that have been developed for sample preparation prior to capillary electrophoresis-mass spectrometry (CE-MS). Namely the present work presents an exhaustive and critical revision of the different samples treatments used together with on-line CE-MS including works published from January 2000 to July 2006.

Preparation, certification and interlaboratory analysis of workplace air filters spiked with high-fired beryllium oxide.

PubMed

Oatts, Thomas J; Hicks, Cheryl E; Adams, Amy R; Brisson, Michael J; Youmans-McDonald, Linda D; Hoover, Mark D; Ashley, Kevin

2012-02-01

Occupational sampling and analysis for multiple elements is generally approached using various approved methods from authoritative government sources such as the National Institute for Occupational Safety and Health (NIOSH), the Occupational Safety and Health Administration (OSHA) and the Environmental Protection Agency (EPA), as well as consensus standards bodies such as ASTM International. The constituents of a sample can exist as unidentified compounds requiring sample preparation to be chosen appropriately, as in the case of beryllium in the form of beryllium oxide (BeO). An interlaboratory study was performed to collect analytical data from volunteer laboratories to examine the effectiveness of methods currently in use for preparation and analysis of samples containing calcined BeO powder. NIST SRM(®) 1877 high-fired BeO powder (1100 to 1200 °C calcining temperature; count median primary particle diameter 0.12 μm) was used to spike air filter media as a representative form of beryllium particulate matter present in workplace sampling that is known to be resistant to dissolution. The BeO powder standard reference material was gravimetrically prepared in a suspension and deposited onto 37 mm mixed cellulose ester air filters at five different levels between 0.5 μg and 25 μg of Be (as BeO). Sample sets consisting of five BeO-spiked filters (in duplicate) and two blank filters, for a total of twelve unique air filter samples per set, were submitted as blind samples to each of 27 participating laboratories. Participants were instructed to follow their current process for sample preparation and utilize their normal analytical methods for processing samples containing substances of this nature. Laboratories using more than one sample preparation and analysis method were provided with more than one sample set. Results from 34 data sets ultimately received from the 27 volunteer laboratories were subjected to applicable statistical analyses. The observed performance data show that sample preparations using nitric acid alone, or combinations of nitric and hydrochloric acids, are not effective for complete extraction of Be from the SRM 1877 refractory BeO particulate matter spiked on air filters; but that effective recovery can be achieved by using sample preparation procedures utilizing either sulfuric or hydrofluoric acid, or by using methodologies involving ammonium bifluoride with heating. Laboratories responsible for quantitative determination of Be in workplace samples that may contain high-fired BeO should use quality assurance schemes that include BeO-spiked sampling media, rather than solely media spiked with soluble Be compounds, and should ensure that methods capable of quantitative digestion of Be from the actual material present are used.

Microextraction by packed sorbent: an emerging, selective and high-throughput extraction technique in bioanalysis.

PubMed

Pereira, Jorge; Câmara, José S; Colmsjö, Anders; Abdel-Rehim, Mohamed

2014-06-01

Sample preparation is an important analytical step regarding the isolation and concentration of desired components from complex matrices and greatly influences their reliable and accurate analysis and data quality. It is the most labor-intensive and error-prone process in analytical methodology and, therefore, may influence the analytical performance of the target analytes quantification. Many conventional sample preparation methods are relatively complicated, involving time-consuming procedures and requiring large volumes of organic solvents. Recent trends in sample preparation include miniaturization, automation, high-throughput performance, on-line coupling with analytical instruments and low-cost operation through extremely low volume or no solvent consumption. Micro-extraction techniques, such as micro-extraction by packed sorbent (MEPS), have these advantages over the traditional techniques. This paper gives an overview of MEPS technique, including the role of sample preparation in bioanalysis, the MEPS description namely MEPS formats (on- and off-line), sorbents, experimental and protocols, factors that affect the MEPS performance, and the major advantages and limitations of MEPS compared with other sample preparation techniques. We also summarize MEPS recent applications in bioanalysis. Copyright © 2014 John Wiley & Sons, Ltd.

Advanced Curation Activities at NASA: Preparing to Receive, Process, and Distribute Samples Returned from Future Missions

NASA Technical Reports Server (NTRS)

McCubbin, Francis M.; Zeigler, Ryan A.

2017-01-01

The Astromaterials Acquisition and Curation Office (henceforth referred to herein as NASA Curation Office) at NASA Johnson Space Center (JSC) is responsible for curating all of NASA's extraterrestrial samples. Under the governing document, NASA Policy Directive (NPD) 7100.10F JSC is charged with curation of all extraterrestrial material under NASA control, including future NASA missions. The Directive goes on to define Curation as including documentation, preservation, preparation, and distribution of samples for research, education, and public outreach. Here we briefly describe NASA's astromaterials collections and our ongoing efforts related to enhancing the utility of our current collections as well as our efforts to prepare for future sample return missions. We collectively refer to these efforts as advanced curation.

Rapid quantitation of atorvastatin in process pharmaceutical powder sample using Raman spectroscopy and evaluation of parameters related to accuracy of analysis.

PubMed

Lim, Young-Il; Han, Janghee; Woo, Young-Ah; Kim, Jaejin; Kang, Myung Joo

2018-07-05

The purpose of this study was to determine the atorvastatin (ATV) content in process pharmaceutical powder sample using Raman spectroscopy. To establish the analysis method, the influence of the type of Raman measurements (back-scattering or transmission mode), preparation of calibration sample (simple admixing or granulation), sample pre-treatment (pelletization), and spectral pretreatment on the Raman spectra was investigated. The characteristic peak of the active compound was more distinctively detected in transmission Raman mode with a laser spot size of 4mm than in the back-scattering method. Preparation of calibration samples by wet granulation, identical to the actual manufacturing process, provided unchanged spectral patterns for the in process sample, with no changes and/or shifts in the spectrum. Pelletization before Raman analysis remarkably improved spectral reproducibility by decreasing the difference in density between the samples. Probabilistic quotient normalization led to accurate and consistent quantification of the ATV content in the calibration samples (standard error of cross validation: 1.21%). Moreover, the drug content in the granules obtained from five commercial batches were reliably quantified, with no statistical difference (p=0.09) with that obtained by HPLC assay. From these findings, we suggest that transmission Raman analysis may be a fast and non-invasive method for the quantification of ATV in actual manufacturing processes. Copyright © 2018 Elsevier B.V. All rights reserved.

Rapid quantitation of atorvastatin in process pharmaceutical powder sample using Raman spectroscopy and evaluation of parameters related to accuracy of analysis

NASA Astrophysics Data System (ADS)

Lim, Young-Il; Han, Janghee; Woo, Young-Ah; Kim, Jaejin; Kang, Myung Joo

2018-07-01

The purpose of this study was to determine the atorvastatin (ATV) content in process pharmaceutical powder sample using Raman spectroscopy. To establish the analysis method, the influence of the type of Raman measurements (back-scattering or transmission mode), preparation of calibration sample (simple admixing or granulation), sample pre-treatment (pelletization), and spectral pretreatment on the Raman spectra was investigated. The characteristic peak of the active compound was more distinctively detected in transmission Raman mode with a laser spot size of 4 mm than in the back-scattering method. Preparation of calibration samples by wet granulation, identical to the actual manufacturing process, provided unchanged spectral patterns for the in process sample, with no changes and/or shifts in the spectrum. Pelletization before Raman analysis remarkably improved spectral reproducibility by decreasing the difference in density between the samples. Probabilistic quotient normalization led to accurate and consistent quantification of the ATV content in the calibration samples (standard error of cross validation: 1.21%). Moreover, the drug content in the granules obtained from five commercial batches were reliably quantified, with no statistical difference (p = 0.09) with that obtained by HPLC assay. From these findings, we suggest that transmission Raman analysis may be a fast and non-invasive method for the quantification of ATV in actual manufacturing processes.

Single molecule targeted sequencing for cancer gene mutation detection.

PubMed

Gao, Yan; Deng, Liwei; Yan, Qin; Gao, Yongqian; Wu, Zengding; Cai, Jinsen; Ji, Daorui; Li, Gailing; Wu, Ping; Jin, Huan; Zhao, Luyang; Liu, Song; Ge, Liangjin; Deem, Michael W; He, Jiankui

2016-05-19

With the rapid decline in cost of sequencing, it is now affordable to examine multiple genes in a single disease-targeted clinical test using next generation sequencing. Current targeted sequencing methods require a separate step of targeted capture enrichment during sample preparation before sequencing. Although there are fast sample preparation methods available in market, the library preparation process is still relatively complicated for physicians to use routinely. Here, we introduced an amplification-free Single Molecule Targeted Sequencing (SMTS) technology, which combined targeted capture and sequencing in one step. We demonstrated that this technology can detect low-frequency mutations using artificially synthesized DNA sample. SMTS has several potential advantages, including simple sample preparation thus no biases and errors are introduced by PCR reaction. SMTS has the potential to be an easy and quick sequencing technology for clinical diagnosis such as cancer gene mutation detection, infectious disease detection, inherited condition screening and noninvasive prenatal diagnosis.

Process test plan, phase II: waste retrieval sluicing system emissions collection

DOE Office of Scientific and Technical Information (OSTI.GOV)

POWERS, R.L.

1999-06-01

This Process Test Plan is prepared to continue from HNF-3733 which was Phase I of the test. Supplemental operational controls and sampling requirements are defined to safely obtain gas samples from the 296-C-006 ventilation system stack during active operation of the sluicing equipment.

Desired Student Preparation in the Job Application Process as Perceived by the Business Community.

ERIC Educational Resources Information Center

Allen, Thomas R., Jr., Comp.

The major purpose of this study was to determine from the business community what competencies in the job application process are needed by students preparing to enter the job market for their first full-time position. Data were collected from 100 human resource administrators (out of a sample of 400). The general feeling of the administrators was…

Single-cell transcriptome conservation in cryopreserved cells and tissues.

PubMed

Guillaumet-Adkins, Amy; Rodríguez-Esteban, Gustavo; Mereu, Elisabetta; Mendez-Lago, Maria; Jaitin, Diego A; Villanueva, Alberto; Vidal, August; Martinez-Marti, Alex; Felip, Enriqueta; Vivancos, Ana; Keren-Shaul, Hadas; Heath, Simon; Gut, Marta; Amit, Ido; Gut, Ivo; Heyn, Holger

2017-03-01

A variety of single-cell RNA preparation procedures have been described. So far, protocols require fresh material, which hinders complex study designs. We describe a sample preservation method that maintains transcripts in viable single cells, allowing one to disconnect time and place of sampling from subsequent processing steps. We sequence single-cell transcriptomes from >1000 fresh and cryopreserved cells using 3'-end and full-length RNA preparation methods. Our results confirm that the conservation process did not alter transcriptional profiles. This substantially broadens the scope of applications in single-cell transcriptomics and could lead to a paradigm shift in future study designs.

Processing-property relations in YBa2Cu3O(6+x) superconductors

NASA Astrophysics Data System (ADS)

Safari, A.; Wachtman, J. B., Jr.; Parkhe, V.; Caracciolo, R.; Jeter, D.

Processing of YBa2Cu3O(6+x) superconducting samples by employing different precursor powder preparation techniques such as ball milling, attrition milling, and narrow particle size distribution powder preparation through coprecipitation by spraying will be discussed. CuO coated with oxalates shows the lowest resistance above Tc up to room temperature. The extent of corrosion by water has been studied by employing magnetic susceptibility, XPS, and X-ray diffraction. Superconducting samples are affected to a considerable extent when treated in water at 60 C and the severity of the attack increases with time.

Effect of processing temperature on the properties of Fe-Hydroxyapatite

NASA Astrophysics Data System (ADS)

Kathriarachchi, Vindu; Leventouri, Theodora; Rondinone, Adam; Sorge, Korey

2015-03-01

Multi-substituted Hydroxyapatite (HAp), Ca5(PO4)3OH, is the main mineral phase in physiological apatite. Fe is a minor substitution element in bone and enamel substituting Ca in the HAp structure. Crystal structure, magnetic and microstructure properties of Ca5-xFex(PO4)3OH depend on processing parameters. We present results from our research on the Ca5-xFex(PO4)3OH system (x = 0.0, 0.05, 0.1, 0.2 and 0.3) prepared at 37° C, and 80° C. Hydroxyapatite single-phase was detected for x <0.1 in both sets of samples, while hematite and/or maghemite develops starting at x = 0.1. Rietveld refinements of XRD and NPD patterns show that the a and c lattice constants decrease with increasing Fe concentration for both sets of samples. Pure HAp is diamagnetic but as x increases, Fe-HAp transitions from paramagnetic to weak ferromagnetic behavior. TEM images show spherical particles in samples prepared at 37° C, and elongated particles in samples prepared at 80° C. XRF studies confirm the iron substitution and show that the Ca/P stoichiometric ratio of 1.67 decreases with increasing the Fe concentration. Further, the Fe/Ca +Fe atomic ratios of samples prepared at 37° C are greater than those prepared at 80° C. TEM and XRF data were collected at the Center for Nanophase Materials Sciences which is a DOE Office of Science User Facility. NPD data were collected at the SNS of the ORNL.

Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

PubMed Central

Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma

2014-01-01

In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from one side, toward automatization and online coupling of sample preparation units. The primary objective of this review is to present the recent developments in microextraction sample preparation methods for analysis of drugs in biological fluids. Microextraction techniques allow for less consumption of solvent, reagents, and packing materials, and small sample volumes can be used. In this review the use of solid phase microextraction (SPME), microextraction in packed sorbent (MEPS), and stir-bar sorbtive extraction (SBSE) in drug analysis will be discussed. In addition, the use of new sorbents such as monoliths and molecularly imprinted polymers will be presented. PMID:24688797

Microwave Processing for Sample Preparation to Evaluate Mitochondrial Ultrastructural Damage in Hemorrhagic Shock

NASA Astrophysics Data System (ADS)

Josephsen, Gary D.; Josephsen, Kelly A.; Beilman, Greg J.; Taylor, Jodie H.; Muiler, Kristine E.

2005-12-01

This is a report of the adaptation of microwave processing in the preparation of liver biopsies for transmission electron microscopy (TEM) to examine ultrastructural damage of mitochondria in the setting of metabolic stress. Hemorrhagic shock was induced in pigs via 35% total blood volume bleed and a 90-min period of shock followed by resuscitation. Hepatic biopsies were collected before shock and after resuscitation. Following collection, biopsies were processed for TEM by a rapid method involving microwave irradiation (Giberson, 2001). Samples pre- and postshock of each of two animals were viewed and scored using the mitochondrial ultrastructure scoring system (Crouser et al., 2002), a system used to quantify the severity of ultrastructural damage during shock. Results showed evidence of increased ultrastructural damage in the postshock samples, which scored 4.00 and 3.42, versus their preshock controls, which scored 1.18 and 1.27. The results of this analysis were similar to those obtained in another model of shock (Crouser et al., 2002). However, the amount of time used to process the samples was significantly shortened with methods involving microwave irradiation.

Temperature-Driven Structural and Morphological Evolution of Zinc Oxide Nano-Coalesced Microstructures and Its Defect-Related Photoluminescence Properties

PubMed Central

Lim, Karkeng; Abdul Hamid, Muhammad Azmi; Shamsudin, Roslinda; Al-Hardan, N.H.; Mansor, Ishak; Chiu, Weesiong

2016-01-01

In this paper, we address the synthesis of nano-coalesced microstructured zinc oxide thin films via a simple thermal evaporation process. The role of synthesis temperature on the structural, morphological, and optical properties of the prepared zinc oxide samples was deeply investigated. The obtained photoluminescence and X-ray photoelectron spectroscopy outcomes will be used to discuss the surface structure defects of the prepared samples. The results indicated that the prepared samples are polycrystalline in nature, and the sample prepared at 700 °C revealed a tremendously c-axis oriented zinc oxide. The temperature-driven morphological evolution of the zinc oxide nano-coalesced microstructures was perceived, resulting in transformation of quasi-mountain chain-like to pyramidal textured zinc oxide with increasing the synthesis temperature. The results also impart that the sample prepared at 500 °C shows a higher percentage of the zinc interstitial and oxygen vacancies. Furthermore, the intensity of the photoluminescence emission in the ultraviolet region was enhanced as the heating temperature increased from 500 °C to 700 °C. Lastly, the growth mechanism of the zinc oxide nano-coalesced microstructures is discussed according to the reaction conditions. PMID:28773425

Lead Free Electric Primer

DTIC Science & Technology

2011-10-06

composites were prepared with varying metal to oxidizer (M/O) ratios ranging from 0.782 to 3.165 (see Table 7). The performance was measured by the...and the Army was expecting to begin their processing efforts in the near future. The Army purchased primer metal parts and was prepared to perform...43 Table 19 – Samples Prepared Using Different Mix Times and Amplitudes

Evidence of a miscibility gap in the FeTe1-xSex polycrystalline samples prepared with a melting process

NASA Astrophysics Data System (ADS)

Sala, A.; Palenzona, A.; Bernini, C.; Caglieris, F.; Cimberle, M. R.; Ferdeghini, C.; Lamura, G.; Martinelli, A.; Pani, M.; Hecher, J.; Eisterer, M.; Putti, M.

2014-05-01

The study of overdoped FeTe1-xSex (0.5 < x < 1) polycrystalline superconductor samples is reported. The samples were prepared using a melting technique previously developed by our group. Increasing the Se content a phase separation related to the formation of FeSe inside the Fe(Se,Te) phase happens, as demonstrated by structural analysis and magnetic characterization. The proposed phase separation picture is likely the fingerprint of a miscibility gap in the Fe(Se,Te) system.

Semi-automated 96-well liquid-liquid extraction for quantitation of drugs in biological fluids.

PubMed

Zhang, N; Hoffman, K L; Li, W; Rossi, D T

2000-02-01

A semi-automated liquid-liquid extraction (LLE) technique for biological fluid sample preparation was introduced for the quantitation of four drugs in rat plasma. All liquid transferring during the sample preparation was automated using a Tomtec Quadra 96 Model 320 liquid handling robot, which processed up to 96 samples in parallel. The samples were either in 96-deep-well plate or tube-rack format. One plate of samples can be prepared in approximately 1.5 h, and the 96-well plate is directly compatible with the autosampler of an LC/MS system. Selection of organic solvents and recoveries are discussed. Also, precision, relative error, linearity and quantitation of the semi automated LLE method are estimated for four example drugs using LC/MS/MS with a multiple reaction monitoring (MRM) approach. The applicability of this method and future directions are evaluated.

Commander prepares glass columns for electrophoresis experiment

NASA Technical Reports Server (NTRS)

1982-01-01

Commander Jack Lousma prepares on of the glass columns for the electrophoresis test in the middeck area of the Columbia. The experiment, deployed in an L-shaped mode in upper right corner, consists of the processing unit with glass columns in which the separation takes place; a camera (partially obscurred by Lousma's face) to document the process; and a cryogenic freezer to freeze and store the samples after separation.

Rapid microscale in-gel processing and digestion of proteins using surface acoustic waves.

PubMed

Kulkarni, Ketav P; Ramarathinam, Sri H; Friend, James; Yeo, Leslie; Purcell, Anthony W; Perlmutter, Patrick

2010-06-21

A new method for in-gel sample processing and tryptic digestion of proteins is described. Sample preparation, rehydration, in situ digestion and peptide extraction from gel slices are dramatically accelerated by treating the gel slice with surface acoustic waves (SAWs). Only 30 minutes total workflow time is required for this new method to produce base peak chromatograms (BPCs) of similar coverage and intensity to those observed for traditional processing and overnight digestion. Simple set up, good reproducibility, excellent peptide recoveries, rapid turnover of samples and high confidence protein identifications put this technology at the fore-front of the next generation of proteomics sample processing tools.

Optimization of Machining Parameters of Milling Operation by Application of Semi-synthetic oil based Nano cutting Fluids

NASA Astrophysics Data System (ADS)

Giri Prasad, M. J.; Abhishek Raaj, A. S.; Rishi Kumar, R.; Gladson, Frank; M, Gautham

2016-09-01

The present study is concerned with resolving the problems pertaining to the conventional cutting fluids. Two samples of nano cutting fluids were prepared by dispersing 0.01 vol% of MWCNTs and a mixture of 0.01 vol% of MWCNTs and 0.01 vol% of nano ZnO in the soluble oil. The thermophysical properties such as the kinematic viscosity, density, flash point and the tribological properties of the prepared nano cutting fluid samples were experimentally investigated and were compared with those of plain soluble oil. In addition to this, a milling process was carried by varying the process parameters and by application of different samples of cutting fluids and an attempt was made to determine optimal cutting condition using the Taguchi optimization technique.

Salmonellae Associated with Further-processed Turkey Products1

PubMed Central

Bryan, Frank L.; Ayres, John C.; Kraft, Allen A.

1968-01-01

“Further-processed” turkey products, prepared from chilled, eviscerated, and thawed carcasses at two commercial turkey-processing plants, were evaluated, for the presence of salmonellae. These organisms were isolated from swab samples from 12% of chilled, eviscerated turkey carcasses, 27% of finished products, and 24% of processing equipment. The same serotypes as those found throughout a plant on any one visit were recovered from 31% of rinse-samples taken from hands and gloves of processing personnel. Salmonellae were found in samples taken on 37 of 48 visits; a greater number of recoveries were made on days when freshly killed turkeys were processed (87%) than when frozen-defrosted carcasses were processed (59%). The predominant serotype isolated from meat and environment usually changed from visit to visit. Salmonella sandiego and Salmonella anatum were the most frequent among 23 serotypes recovered. Most of the isolated serotypes are commonly associated with turkeys and have been incriminated as causative agents of human salmonellosis. The implication is that further-processed turkey products, if inadequately cooked by the consumer and if improperly refrigerated between the time of manufacture and consumption, could directly transmit salmonellae. These same products might also contaminate other foods by introducing salmonellae into food-preparation areas. PMID:5688832

Improvements to sample processing and measurement to enable more widespread environmental application of tritium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Moran, James; Alexander, Thomas; Aalseth, Craig

2017-08-01

Previous measurements have demonstrated the wealth of information that tritium (T) can provide on environmentally relevant processes. We present modifications to sample preparation approaches that enable T measurement by proportional counting on small sample sizes equivalent to 120 mg of water and demonstrate the accuracy of these methods on a suite of standardized water samples. This enhanced method should provide the analytical flexibility needed to address persistent knowledge gaps in our understanding of T behavior in the environment.

Blood Sampling and Preparation Procedures for Proteomic Biomarker Studies of Psychiatric Disorders.

PubMed

Guest, Paul C; Rahmoune, Hassan

2017-01-01

A major challenge in proteomic biomarker discovery and validation for psychiatric diseases is the inherent biological complexity underlying these conditions. There are also many technical issues which hinder this process such as the lack of standardization in sampling, processing and storage of bio-samples in preclinical and clinical settings. This chapter describes a reproducible procedure for sampling blood serum and plasma that is specifically designed for maximizing data quality output in two-dimensional gel electrophoresis, multiplex immunoassay and mass spectrometry profiling studies.

PCL foamed scaffolds loaded with 5-fluorouracil anti-cancer drug prepared by an eco-friendly route.

PubMed

Salerno, Aurelio; Domingo, Concepción; Saurina, Javier

2017-06-01

This study describes a new preparation method, which combines freeze drying and supercritical CO 2 foaming approaches, for the preparation of drug delivery scaffolds of polycaprolactone loaded with 5-fluorouracil, an anti-cancer drug, with low solubility in scCO 2 . It is a principal objective of this work to design a scCO 2 strategy to reduce 5-Fu solubility limitations in its homogeneous distribution into a PCL scaffold through the design of an innovative processing method. The design of this process is considered valuable for the development of clean technology in pharmacy and medicine, since most of the active agents have a null solubility in scCO 2 ·Supercritical CO 2 is used as a blowing agent to induce polymer foaming by means of the low temperature pressure quench process. The resulting samples have been prepared under different operational conditions focused on enhancing the performance of the release process. In this case, design of experiments (DOE) was considered for a more comprehensive and systematic optimization of the product. In particular, drug amount, equals to 4.8 or 9.1wt%, process temperature, of 45 or 50°C and depressurization rate, equals to 0.1MPas -1 or 2MPas -1 were selected as the factors to be investigated by a three-factor at two-level full factorial design. Samples were characterized to establish porosity data, drug loading percentage and, especially, release profile chromatographically monitored. Results from DOE have concluded which are the best samples providing a sustained drug release for several days, which may be of great interest to develop materials for tissue engineering and sustained release applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation, Characterization, and UV Irradiation of Mars Soil Analogues Under Simulated Martian Conditions to Support Detection of Molecular Biomarkers

NASA Astrophysics Data System (ADS)

Fornaro, T.; Brucato, J. R.; ten Kate, I. L.; Siljeström, S.; Steele, A.; Cody, G. D.; Hazen, R. M.

2018-04-01

We present laboratory activities of preparation, characterization, and UV irradiation processing of Mars soil analogues, which are key to support both in situ exploration and sample return missions devoted to detection of molecular biomarkers on Mars.

Curation of Frozen Samples

NASA Technical Reports Server (NTRS)

Fletcher, L. A.; Allen, C. C.; Bastien, R.

2008-01-01

NASA's Johnson Space Center (JSC) and the Astromaterials Curator are charged by NPD 7100.10D with the curation of all of NASA s extraterrestrial samples, including those from future missions. This responsibility includes the development of new sample handling and preparation techniques; therefore, the Astromaterials Curator must begin developing procedures to preserve, prepare and ship samples at sub-freezing temperatures in order to enable future sample return missions. Such missions might include the return of future frozen samples from permanently-shadowed lunar craters, the nuclei of comets, the surface of Mars, etc. We are demonstrating the ability to curate samples under cold conditions by designing, installing and testing a cold curation glovebox. This glovebox will allow us to store, document, manipulate and subdivide frozen samples while quantifying and minimizing contamination throughout the curation process.

Alternate method of source preparation for alpha spectrometry: No electrodeposition, no hydrofluoric acid

DOE PAGES

Kurosaki, Hiromu; Mueller, Rebecca J.; Lambert, Susan B.; ...

2016-07-15

An alternate method of preparing actinide alpha counting sources was developed in place of electrodeposition or lanthanide fluoride micro-precipitation. The method uses lanthanide hydroxide micro-precipitation to avoid the use of hazardous hydrofluoric acid. Lastly, it provides a quicker, simpler, and safer way of preparing actinide alpha counting sources in routine, production-type laboratories that process many samples daily.

Dual-view plane illumination microscopy for rapid and spatially isotropic imaging

PubMed Central

Kumar, Abhishek; Wu, Yicong; Christensen, Ryan; Chandris, Panagiotis; Gandler, William; McCreedy, Evan; Bokinsky, Alexandra; Colón-Ramos, Daniel A; Bao, Zhirong; McAuliffe, Matthew; Rondeau, Gary; Shroff, Hari

2015-01-01

We describe the construction and use of a compact dual-view inverted selective plane illumination microscope (diSPIM) for time-lapse volumetric (4D) imaging of living samples at subcellular resolution. Our protocol enables a biologist with some prior microscopy experience to assemble a diSPIM from commercially available parts, to align optics and test system performance, to prepare samples, and to control hardware and data processing with our software. Unlike existing light sheet microscopy protocols, our method does not require the sample to be embedded in agarose; instead, samples are prepared conventionally on glass coverslips. Tissue culture cells and Caenorhabditis elegans embryos are used as examples in this protocol; successful implementation of the protocol results in isotropic resolution and acquisition speeds up to several volumes per s on these samples. Assembling and verifying diSPIM performance takes ~6 d, sample preparation and data acquisition take up to 5 d and postprocessing takes 3–8 h, depending on the size of the data. PMID:25299154

Rapid fusion method for the determination of Pu, Np, and Am in large soil samples

DOE PAGES

Maxwell, Sherrod L.; Culligan, Brian; Hutchison, Jay B.; ...

2015-02-14

A new rapid sodium hydroxide fusion method for the preparation of 10-20 g soil samples has been developed by the Savannah River National Laboratory (SRNL). The method enables lower detection limits for plutonium, neptunium, and americium in environmental soil samples. The method also significantly reduces sample processing time and acid fume generation compared to traditional soil digestion techniques using hydrofluoric acid. Ten gram soil aliquots can be ashed and fused using the new method in 1-2 hours, completely dissolving samples, including refractory particles. Pu, Np and Am are separated using stacked 2mL cartridges of TEVA and DGA Resin and measuredmore » using alpha spectrometry. The method can be adapted for measurement by inductively-coupled plasma mass spectrometry (ICP-MS). Two 10 g soil aliquots of fused soil may be combined prior to chromatographic separations to further improve detection limits. Total sample preparation time, including chromatographic separations and alpha spectrometry source preparation, is less than 8 hours.« less

Anti-icing property of bio-inspired micro-structure superhydrophobic surfaces and heat transfer model

NASA Astrophysics Data System (ADS)

Liu, Yan; Li, Xinlin; Jin, Jingfu; Liu, Jiaan; Yan, Yuying; Han, Zhiwu; Ren, Luquan

2017-04-01

Ice accumulation is a thorny problem which may inflict serious damage even disasters in many areas, such as aircraft, power line maintenance, offshore oil platform and locators of ships. Recent researches have shed light on some promising bio-inspired anti-icing strategies to solve this problem. Inspired by typical plant surfaces with super-hydrophobic character such as lotus leaves and rose petals, structured superhydrophobic surface are prepared to discuss the anti-icing property. 7075 Al alloy, an extensively used materials in aircrafts and marine vessels, is employed as the substrates. As-prepared surfaces are acquired by laser processing after being modified by stearic acid for 1 h at room temperature. The surface morphology, chemical composition and wettability are characterized by means of SEM, XPS, Fourier transform infrared (FTIR) spectroscopy and contact angle measurements. The morphologies of structured as-prepared samples include round hump, square protuberance and mountain-range-like structure, and that the as-prepared structured surfaces shows an excellent superhydrophobic property with a WCA as high as 166 ± 2°. Furthermore, the anti-icing property of as-prepared surfaces was tested by a self-established apparatus, and the crystallization process of a cooling water on the sample was recorded. More importantly, we introduced a model to analyze heat transfer process between the droplet and the structured surfaces. This study offers an insight into understanding the heat transfer process of the superhydrophobic surface, so as to further research about its unique property against ice accumulation.

Rapid Radiochemical Methods for Asphalt Paving Material ...

EPA Pesticide Factsheets

Technical Brief Validated rapid radiochemical methods for alpha and beta emitters in solid matrices that are commonly encountered in urban environments were previously unavailable for public use by responding laboratories. A lack of tested rapid methods would delay the quick determination of contamination levels and the assessment of acceptable site-specific exposure levels. Of special concern are matrices with rough and porous surfaces, which allow the movement of radioactive material deep into the building material making it difficult to detect. This research focuses on methods that address preparation, radiochemical separation, and analysis of asphalt paving materials and asphalt roofing shingles. These matrices, common to outdoor environments, challenge the capability and capacity of very experienced radiochemistry laboratories. Generally, routine sample preparation and dissolution techniques produce liquid samples (representative of the original sample material) that can be processed using available radiochemical methods. The asphalt materials are especially difficult because they do not readily lend themselves to these routine sample preparation and dissolution techniques. The HSRP and ORIA coordinate radiological reference laboratory priorities and activities in conjunction with HSRP’s Partner Process. As part of the collaboration, the HSRP worked with ORIA to publish rapid radioanalytical methods for selected radionuclides in building material matrice

Crystallization characteristics of iron-rich glass ceramics prepared from nickel slag and blast furnace slag

NASA Astrophysics Data System (ADS)

Wang, Zhong-Jie; Ni, Wen; Li, Ke-Qing; Huang, Xiao-Yan; Zhu, Li-Ping

2011-08-01

The crystallization process of iron-rich glass-ceramics prepared from the mixture of nickel slag (NS) and blast furnace slag (BFS) with a small amount of quartz sand was investigated. A modified melting method which was more energy-saving than the traditional methods was used to control the crystallization process. The results show that the iron-rich system has much lower melting temperature, glass transition temperature ( T g), and glass crystallization temperature ( T c), which can result in a further energy-saving process. The results also show that the system has a quick but controllable crystallization process with its peak crystallization temperature at 918°C. The crystallization of augite crystals begins from the edge of the sample and invades into the whole sample. The crystallization process can be completed in a few minutes. A distinct boundary between the crystallized part and the non-crystallized part exists during the process. In the non-crystallized part showing a black colour, some sphere-shaped augite crystals already exist in the glass matrix before samples are heated to T c. In the crystallized part showing a khaki colour, a compact structure is formed by augite crystals.

Oligosaccharide formation during commercial pear juice processing.

PubMed

Willems, Jamie L; Low, Nicholas H

2016-08-01

The effect of enzyme treatment and processing on the oligosaccharide profile of commercial pear juice samples was examined by high performance anion exchange chromatography with pulsed amperometric detection and capillary gas chromatography with flame ionization detection. Industrial samples representing the major stages of processing produced with various commercial enzyme preparations were studied. Through the use of commercially available standards and laboratory scale enzymatic hydrolysis of pectin, starch and xyloglucan; galacturonic acid oligomers, glucose oligomers (e.g., maltose and cellotriose) and isoprimeverose were identified as being formed during pear juice production. It was found that the majority of polysaccharide hydrolysis and oligosaccharide formation occurred during enzymatic treatment at the pear mashing stage and that the remaining processing steps had minimal impact on the carbohydrate-based chromatographic profile of pear juice. Also, all commercial enzyme preparations and conditions (time and temperature) studied produced similar carbohydrate-based chromatographic profiles. Copyright © 2016 Elsevier Ltd. All rights reserved.

Tandem High-pressure Freezing and Quick Freeze Substitution of Plant Tissues for Transmission Electron Microscopy

PubMed Central

Bobik, Krzysztof; Dunlap, John R.; Burch-Smith, Tessa M.

2014-01-01

Since the 1940s transmission electron microscopy (TEM) has been providing biologists with ultra-high resolution images of biological materials. Yet, because of laborious and time-consuming protocols that also demand experience in preparation of artifact-free samples, TEM is not considered a user-friendly technique. Traditional sample preparation for TEM used chemical fixatives to preserve cellular structures. High-pressure freezing is the cryofixation of biological samples under high pressures to produce very fast cooling rates, thereby restricting ice formation, which is detrimental to the integrity of cellular ultrastructure. High-pressure freezing and freeze substitution are currently the methods of choice for producing the highest quality morphology in resin sections for TEM. These methods minimize the artifacts normally associated with conventional processing for TEM of thin sections. After cryofixation the frozen water in the sample is replaced with liquid organic solvent at low temperatures, a process called freeze substitution. Freeze substitution is typically carried out over several days in dedicated, costly equipment. A recent innovation allows the process to be completed in three hours, instead of the usual two days. This is typically followed by several more days of sample preparation that includes infiltration and embedding in epoxy resins before sectioning. Here we present a protocol combining high-pressure freezing and quick freeze substitution that enables plant sample fixation to be accomplished within hours. The protocol can readily be adapted for working with other tissues or organisms. Plant tissues are of special concern because of the presence of aerated spaces and water-filled vacuoles that impede ice-free freezing of water. In addition, the process of chemical fixation is especially long in plants due to cell walls impeding the penetration of the chemicals to deep within the tissues. Plant tissues are therefore particularly challenging, but this protocol is reliable and produces samples of the highest quality. PMID:25350384

New definitions for cotton fiber maturity ratio

USDA-ARS?s Scientific Manuscript database

Cotton fiber maturity affects fiber physical, mechanical, and chemical properties, as well as the processability and qualities of yarn and fabrics. New definitions of cotton fiber maturity ratio are introduced. The influences of sampling, sample preparation, measurement method, and correlations am...

Demonstration of Physical Separation/Leaching Methods for the Remediation of Heavy Metals Contaminated Soils at Small Arms Ranges.

DTIC Science & Technology

1997-09-01

8.8 WIND SOCK 8.9 SILT TRAP 8.10 BATTELLE SAMPLE PREPARATION AREA 8.11 RANGE 5 EXCAVATION PLAN 8.12 COMPONENTS THAT NEEDED MAINTENANCE, REPAIR...Pad Details 47 18 Soil Storage Bins 48 19 Power Distribution Station 49 20 Water Supply System 50 21 Wind Sock 50 22 Sample Preparation...washwater). Better process control, especially soil dewatering, would have reduced this occasional nuisance. The odor threshold for this acid is

Polymeric ionic liquid-based portable tip microextraction device for on-site sample preparation of water samples.

PubMed

Chen, Lei; Pei, Junxian; Huang, Xiaojia; Lu, Min

2018-06-05

On-site sample preparation is highly desired because it avoids the transportation of large-volume samples and ensures the accuracy of the analytical results. In this work, a portable prototype of tip microextraction device (TMD) was designed and developed for on-site sample pretreatment. The assembly procedure of TMD is quite simple. Firstly, polymeric ionic liquid (PIL)-based adsorbent was in-situ prepared in a pipette tip. After that, the tip was connected with a syringe which was driven by a bidirectional motor. The flow rates in adsorption and desorption steps were controlled accurately by the motor. To evaluate the practicability of the developed device, the TMD was used to on-site sample preparation of waters and combined with high-performance liquid chromatography with diode array detection to measure trace estrogens in water samples. Under the most favorable conditions, the limits of detection (LODs, S/N = 3) for the target analytes were in the range of 4.9-22 ng/L, with good coefficients of determination. Confirmatory study well evidences that the extraction performance of TMD is comparable to that of the traditional laboratory solid-phase extraction process, but the proposed TMD is more simple and convenient. At the same time, the TMD avoids complicated sampling and transferring steps of large-volume water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Methods of biological fluids sample preparation - biogenic amines, methylxanthines, water-soluble vitamins.

PubMed

Płonka, Joanna

2015-01-01

In recent years demands on the amount of information that can be obtained from the analysis of a single sample have increased. For time and economic reasons it is necessary to examine at the same time larger number of compounds, and compounds from different groups. This can best be seen in such areas as clinical analysis. In many diseases, the best results for patients are obtained when treatment fits the individual characteristics of the patient. Dosage monitoring is important at the beginning of therapy and in the full process of treatment. In the treatment of many diseases biogenic amines (dopamine, serotonin) and methylxanthines (theophylline, theobromine, caffeine) play an important role. They are used as drugs separately or in combination with others to support and strengthen the action of other drugs - for example, the combination of caffeine and paracetamol. Vitamin supplementation may be also an integral part of the treatment process. Specification of complete sample preparation parameters for extraction of the above compounds from biological matrices has been reviewed. Particular attention was given to the preparation stage and extraction methods. This review provides universal guidance on establishing a common procedures across laboratories to facilitate the preparation and analysis of all discussed compounds. Copyright © 2014 John Wiley & Sons, Ltd.

Mixed-mode ion exchange-based integrated proteomics technology for fast and deep plasma proteome profiling.

PubMed

Xue, Lu; Lin, Lin; Zhou, Wenbin; Chen, Wendong; Tang, Jun; Sun, Xiujie; Huang, Peiwu; Tian, Ruijun

2018-06-09

Plasma proteome profiling by LC-MS based proteomics has drawn great attention recently for biomarker discovery from blood liquid biopsy. Due to standard multi-step sample preparation could potentially cause plasma protein degradation and analysis variation, integrated proteomics sample preparation technologies became promising solution towards this end. Here, we developed a fully integrated proteomics sample preparation technology for both fast and deep plasma proteome profiling under its native pH. All the sample preparation steps, including protein digestion and two-dimensional fractionation by both mixed-mode ion exchange and high-pH reversed phase mechanism were integrated into one spintip device for the first time. The mixed-mode ion exchange beads design achieved the sample loading at neutral pH and protein digestion within 30 min. Potential sample loss and protein degradation by pH changing could be voided. 1 μL of plasma sample with depletion of high abundant proteins was processed by the developed technology with 12 equally distributed fractions and analyzed with 12 h of LC-MS gradient time, resulting in the identification of 862 proteins. The combination of the Mixed-mode-SISPROT and data-independent MS method achieved fast plasma proteome profiling in 2 h with high identification overlap and quantification precision for a proof-of-concept study of plasma samples from 5 healthy donors. We expect that the Mixed-mode-SISPROT become a generally applicable sample preparation technology for clinical oriented plasma proteome profiling. Copyright © 2018 Elsevier B.V. All rights reserved.

Lead and cadmium in mangrove root crab (Goniopsis cruentata), in natura and at food processing stages.

PubMed

Costa, Renata G; Bah, Homegnon A F; Bandeira, Matheus J; Oliveira, Sérgio S P; Menezes-Filho, José A

2017-09-01

Lead (Pb) and cadmium (Cd) were determined in mangrove root crab (Goniopsis cruentata) tissues (in natura) and in two culinary preparations by graphite furnace atomic absorption spectrometry. Mangrove root crab samples from three sampling sites along the Jaguaripe River, Bahia, Brazil, where lead-glazed ceramics are produced, and from two commercial preparations were collected or purchased in March and April 2016. Cd levels in raw and processed samples were below the methods' limits of detection (0.016 mg kg -1 ), while Pb levels in the raw tissues were determined only in the gills (0.67 mg kg -1 ) and in the hepatopancreas (0.14 mg kg -1 ). However, Pb levels increased from 0.05 to 2.84 mg kg -1 in boiled/sorted muscle and in the traditional stew (with a 57-fold increase), respectively. Pb levels augmented significantly in the processed food due to migration of Pb used in the glazing of cooking ceramic utensils, surpassing the Brazilian and international safety limits.

Luminescence studies and infrared emission of erbium-doped calcium zirconate phosphor.

PubMed

Tiwari, Neha; Dubey, Vikas

2016-05-01

The near-infrared-to-visible upconversion luminescence behaviour of Er(3+)-doped CaZrO3 phosphor is discussed in this manuscript. The phosphor was prepared by a combustion synthesis technique that is suitable for less-time-taking techniques for nanophosphors. The starting materials used for sample preparation were Ca(NO3)2.4H2O, Zr(NO3)4 and Er(NO3)2, and urea was used as a fuel. The prepared sample was characterized by X-ray diffraction (XRD). The surface morphology of prepared phosphor was determined by field emission gun scanning electron microscopy (FEGSEM). The functional group analysis was determined by Fourier transform infrared (FTIR) spectroscopy. All prepared phosphors with variable Er(3+) concentrations (0.5-2.5 mol%) were studied by photoluminescence analysis. It was found that the excitation spectra of the prepared phosphor showed a sharp excitation peak centred at 980 nm. The emission spectra with variable Er(3+) concentrations showed strong peaks in the 555 nm and 567 nm range, with a dominant peak at 555 nm due to the ((2)H(11/2),(4)S(3/2)) transition and a weaker transition at 567 nm associated with 527 nm. Spectrophotometric determination of the peak was evaluated by the Commission Internationale de I'Eclairage (CIE) method These upconverted emissions were attributed to a two-photon process. The excitation wavelength dependence of the upconverted luminescence, together with its time evolution after infrared pulsed excitation, suggested that energy transfer upconversion processes were responsible for the upconversion luminescence. The upconversion mechanisms were studied in detail through laser power dependence. Excited state absorption and energy transfer processes were discussed as possible upconversion mechanisms. The cross-relaxation process in Er(3+) was also investigated. Copyright © 2015 John Wiley & Sons, Ltd.

Room temperature ferromagnetism of tin oxide nanocrystal based on synthesis methods

NASA Astrophysics Data System (ADS)

Sakthiraj, K.; Hema, M.; Balachandrakumar, K.

2016-04-01

The experimental conditions used in the preparation of nanocrystalline oxide materials play an important role in the room temperature ferromagnetism of the product. In the present work, a comparison was made between sol-gel, microwave assisted sol-gel and hydrothermal methods for preparing tin oxide nanocrystal. X-ray diffraction analysis indicates the formation of tetragonal rutile phase structure for all the samples. The crystallite size was estimated from the HRTEM images and it is around 6-12 nm. Using optical absorbance measurement, the band gap energy value of the samples has been calculated. It reveals the existence of quantum confinement effect in all the prepared samples. Photoluminescence (PL) spectra confirms that the luminescence process originates from the structural defects such as oxygen vacancies present in the samples. Room temperature hysteresis loop was clearly observed in M-H curve of all the samples. But the sol-gel derived sample shows the higher values of saturation magnetization (Ms) and remanence (Mr) than other two samples. This study reveals that the sol-gel method is superior to the other two methods for producing room temperature ferromagnetism in tin oxide nanocrystal.

Quantum Tomography via Compressed Sensing: Error Bounds, Sample Complexity and Efficient Estimators

DTIC Science & Technology

2012-09-27

particular, we require no entangling gates or ancillary systems for the procedure. In contrast with [19], our method is not restricted to processes that are...of states, such as those recently developed for use with permutation-invariant states [60], matrix product states [61] or multi-scale entangled states...process tomography: first prepare the Jamiołkowski state ρE (by adjoining an ancilla, preparing the maximally entangled state |ψ0, and applying E); then

Effect of surface moisture on chemically bonded phosphor for thermographic phosphor thermometry

NASA Astrophysics Data System (ADS)

Cai, Tao; Kim, Dong; Kim, Mirae; Liu, Ying Zheng; Kim, Kyung Chun

2016-09-01

This study examined the effect of surface moisture on the calibration lifetime in chemically bonded phosphor paint preparation. Mg4FGeO6:Mn was used as a sensor material, which was excited by a pulsed UV LED. A high-speed camera with a frequency of 8000 Hz was used to conduct phosphor thermometry. Five samples with different degrees of surface moisture were selected during the preparation process, and each sample was calibrated 40 times at room temperature. A conventional post-processing method was used to acquire the phosphorescent lifetime for different samples with a 4  ×  4-pixel interrogation window. The measurement error and paint uniformity were also studied. The results showed that there was no obvious phosphorescence boundary between the wet parts and dry parts of phosphor paint. The lifetime increased by about 0.0345% per hour during the preparation process, showing the degree of surface moisture had almost no influence on the lifetime measurement. The lifetime changed only after annealing treatment. There was also no effect on the measurement error and uniformity. These results provide a reference for developing a real-time measurement method using thermographic phosphor thermometry. This study also provides a feasible basis for chemically bonded phosphor thermometry applications in humid and low-temperature environments.

Food adulteration analysis without laboratory prepared or determined reference food adulterant values.

PubMed

Kalivas, John H; Georgiou, Constantinos A; Moira, Marianna; Tsafaras, Ilias; Petrakis, Eleftherios A; Mousdis, George A

2014-04-01

Quantitative analysis of food adulterants is an important health and economic issue that needs to be fast and simple. Spectroscopy has significantly reduced analysis time. However, still needed are preparations of analyte calibration samples matrix matched to prediction samples which can be laborious and costly. Reported in this paper is the application of a newly developed pure component Tikhonov regularization (PCTR) process that does not require laboratory prepared or reference analysis methods, and hence, is a greener calibration method. The PCTR method requires an analyte pure component spectrum and non-analyte spectra. As a food analysis example, synchronous fluorescence spectra of extra virgin olive oil samples adulterated with sunflower oil is used. Results are shown to be better than those obtained using ridge regression with reference calibration samples. The flexibility of PCTR allows including reference samples and is generic for use with other instrumental methods and food products. Copyright © 2013 Elsevier Ltd. All rights reserved.

The low temperature synthesis, characterization and properties of ferroelectrics

NASA Astrophysics Data System (ADS)

Xu, Jie

2000-10-01

PZT 50:50 xerogels prepared by two different sol-gel routes crystallized in a similar fashion to give a mixture of tetragonal and rhombohedral at high temperature (1000°C). Both the diffraction and EXAFS data suggest that the compositional inhomogeneity of the samples prepared by the two routes is similar. The crystallization of CZT gels is complicated. Crystalline CaCO 3 was always detected in the dry gels regardless of the sample composition and preparation methods. At intermediate temperatures a fluorite related phase was always formed and it transformed to perovskite at higher temperatures. The EXAFS data suggest that perovskite CZT samples prepared using alkoxide sol-gel chemistry may not be random solid solutions. All the solution processed ZrTiO4 materials crystallized in the range 600--700°C. The KTN samples prepared using a conventional alkoxide sol-gel route crystallized completely to perovskite at lower temperatures than those prepared using prehydrolyzed precursors. The EXAFS data for the KTN samples prepared using a conventional alkoxide sol-gel route are consistent with a random distribution of tantalum and niobium in the solid solution. However, materials prepared using the inhomogeneous sol-gel route and by the direct reaction of mixed oxides were shown to be compositionally inhomogeneous. The heterogeneity could not be removed by regrinding and heating the mixed oxide samples several times. K2Ta4-xNbxO11 (x = 0, 2, 4) samples were prepared using alkoxide sol-gel chemistry and their crystallization was examined by powder X-ray diffraction. A Rietveld structure analysis of the pyrochlore formed from a gel with bulk composition K2Ta 2Nb2O11 indicated that it was rich in potassium relative to the bulk sample. On heating to high temperatures tetragonal tungsten bronzes were formed. A Rietveld analysis was also performed for K2Ta 2Nb2O11 with tetragonal tungsten bronze structure. The defect pyrochlores "AgTaO3" and GaTaO 3 were synthesized by ion-exchange using pyrochlore KTaO3 as a starting material. The structures of the pyrochlores were examined using the Rietveld method. The pyrochlore-to-perovskite transformations were also explored.

Using solvent-free sample preparation to promote protonation of poly(ethylene oxide)s with labile end-groups in matrix-assisted laser desorption/ionisation.

PubMed

Mazarin, Michael; Phan, Trang N T; Charles, Laurence

2008-12-01

Protonation is usually required to observe intact ions during matrix-assisted laser desorption/ionization (MALDI) of polymers containing fragile end-groups while cation adduction induces chain-end degradation. These polymers, generally obtained via living free radical polymerization techniques, are terminated with a functionality in which a bond is prone to homolytic cleavage, as required by the polymerization process. A solvent-free sample preparation method was used here to avoid salt contaminant from the solvent traditionally used in the dried-droplet MALDI procedure. Solvent-based and solvent-free sample preparations were compared for a series of three poly(ethylene oxide) polymers functionalized with a labile end-group in a nitroxide-mediated polymerization reaction, using 2,4,6-trihydroxyacetophenone (THAP) as the matrix without any added salt. Intact oligomer ions could only be produced as protonated molecules in solvent-free MALDI while sodium adducts of degraded polymers were formed from the dried-droplet samples. Although MALDI analysis was performed at the laser threshold, fragmentation of protonated macromolecules was still observed to occur. However, in contrast to sodiated molecules, dissociation of protonated oligomers does not involve the labile C--ON bond of the end-group. As the macromolecule size increased, protonation appeared to be less efficient and sodium adduction became the dominant ionization process, although no sodium salt was added in the preparation. Formation of sodiated degraded macromolecules would be dictated by increasing cation affinity as the size of the oligomers increases and would reveal the presence of salts at trace levels in the MALDI samples.

Effect of processing route for preparation of mullite from kaolinite and alumina

NASA Astrophysics Data System (ADS)

Behera, Pallavi Suhasinee; Bhattacharyya, Sunipa

2018-05-01

In current work, two different types of mullite ceramic powder were prepared using kaolinite and alumina by solid state and chemical precipitation route. The phases, bond types and microstructural evolution of the mullite powders were investigated by X-ray diffraction, infrared analysis, and field emission scanning electron microscopy to study the mullitisation behavior. The solid state method evident a pure mullite phase formation at 1550 °C. In case of chemical precipitation route small amount of alumina peak was noticed along with major phase of mullite which was also clearly apprehended from FESEM micrographs and IR spectra. Densification was more for the samples prepared by solid state process which may be correlated to the delayed mullitization process in chemical precipitation route.

Improvement of mechanical and thermal properties of high energy electron beam irradiated HDPE/hydroxyapatite nano-composite

NASA Astrophysics Data System (ADS)

Mohammadi, M.; Ziaie, F.; Majdabadi, A.; Akhavan, A.; Shafaei, M.

2017-01-01

In this research work, the nano-composites of high density polyethylene/hydroxyapatite samples were manufactured via two methods: In the first method, the granules of high density polyethylene and nano-structure hydroxyapatite were processed in an internal mixer to prepare the nano-composite samples with a different weight percentage of the reinforcement phase. As for the second one, high density polyethylene was prepared in nano-powder form in boiling xylene. During this procedure, the hydroxyapatite nano-powder was added with different weight percentages to the solvent to obtain the nano-composite. In both of the procedures, the used hydroxyapatite nano-powder was synthesized via hydrolysis methods. The samples were irradiated under 10 MeV electron beam in 70-200 kGy of doses. Mechanical, thermal and morphological properties of the samples were investigated and compared. The results demonstrate that the nano-composites which we have prepared using nano-polyethylene, show better mechanical and thermal properties than the composites prepared from normal polyethylene granules, due to the better dispersion of nano-particles in the polymer matrix.

SPAR 6 experiment report containerless processing of glass experiment 74-42

NASA Technical Reports Server (NTRS)

Happe, R. A.

1980-01-01

Pertinent portions of the ground based research are described, including experiments leading to the selection of the flight sample composition: a silica modified gallia-calcia glass. Included are details of the preparation of an approximately .25 in diameter flight sample.

Constructing a MoS₂ QDs/CdS Core/Shell Flowerlike Nanosphere Hierarchical Heterostructure for the Enhanced Stability and Photocatalytic Activity.

PubMed

Liang, Shijing; Zhou, Zhouming; Wu, Xiuqin; Zhu, Shuying; Bi, Jinhong; Zhou, Limin; Liu, Minghua; Wu, Ling

2016-02-15

MoS₂ quantum dots (QDs)/CdS core/shell nanospheres with a hierarchical heterostructure have been prepared by a simple microwave hydrothermal method. The as-prepared samples are characterized by XRD, TEM, SEM, UV-VIS diffuse reflectance spectra (DRS) and N₂-sorption in detail. The photocatalytic activities of the samples are evaluated by water splitting into hydrogen. Results show that the as-prepared MoS₂ QDs/CdS core/shell nanospheres with a diameter of about 300 nm are composed of the shell of CdS nanorods and the core of MoS₂ QDs. For the photocatalytic reaction, the samples exhibit a high stability of the photocatalytic activity and a much higher hydrogen evolution rate than the pure CdS, the composite prepared by a physical mixture, and the Pt-loaded CdS sample. In addition, the stability of CdS has also been greatly enhanced. The effect of the reaction time on the formations of nanospheres, the photoelectric properties and the photocatalytic activities of the samples has been investigated. Finally, a possible photocatalytic reaction process has also been proposed.

Wastewater Biosolid Composting Optimization Based on UV-VNIR Spectroscopy Monitoring

PubMed Central

Temporal-Lara, Beatriz; Melendez-Pastor, Ignacio; Gómez, Ignacio; Navarro-Pedreño, Jose

2016-01-01

Conventional wastewater treatment generates large amounts of organic matter–rich sludge that requires adequate treatment to avoid public health and environmental problems. The mixture of wastewater sludge and some bulking agents produces a biosolid to be composted at adequate composting facilities. The composting process is chemically and microbiologically complex and requires an adequate aeration of the biosolid (e.g., with a turner machine) for proper maturation of the compost. Adequate (near) real-time monitoring of the compost maturity process is highly difficult and the operation of composting facilities is not as automatized as other industrial processes. Spectroscopic analysis of compost samples has been successfully employed for compost maturity assessment but the preparation of the solid compost samples is difficult and time-consuming. This manuscript presents a methodology based on a combination of a less time-consuming compost sample preparation and ultraviolet, visible and short-wave near-infrared spectroscopy. Spectroscopic measurements were performed with liquid compost extract instead of solid compost samples. Partial least square (PLS) models were developed to quantify chemical fractions commonly employed for compost maturity assessment. Effective regression models were obtained for total organic matter (residual predictive deviation—RPD = 2.68), humification ratio (RPD = 2.23), total exchangeable carbon (RPD = 2.07) and total organic carbon (RPD = 1.66) with a modular and cost-effective visible and near infrared (VNIR) spectroradiometer. This combination of a less time-consuming compost sample preparation with a versatile sensor system provides an easy-to-implement, efficient and cost-effective protocol for compost maturity assessment and near-real-time monitoring. PMID:27854280

Wastewater Biosolid Composting Optimization Based on UV-VNIR Spectroscopy Monitoring.

PubMed

Temporal-Lara, Beatriz; Melendez-Pastor, Ignacio; Gómez, Ignacio; Navarro-Pedreño, Jose

2016-11-15

Conventional wastewater treatment generates large amounts of organic matter-rich sludge that requires adequate treatment to avoid public health and environmental problems. The mixture of wastewater sludge and some bulking agents produces a biosolid to be composted at adequate composting facilities. The composting process is chemically and microbiologically complex and requires an adequate aeration of the biosolid (e.g., with a turner machine) for proper maturation of the compost. Adequate (near) real-time monitoring of the compost maturity process is highly difficult and the operation of composting facilities is not as automatized as other industrial processes. Spectroscopic analysis of compost samples has been successfully employed for compost maturity assessment but the preparation of the solid compost samples is difficult and time-consuming. This manuscript presents a methodology based on a combination of a less time-consuming compost sample preparation and ultraviolet, visible and short-wave near-infrared spectroscopy. Spectroscopic measurements were performed with liquid compost extract instead of solid compost samples. Partial least square (PLS) models were developed to quantify chemical fractions commonly employed for compost maturity assessment. Effective regression models were obtained for total organic matter (residual predictive deviation-RPD = 2.68), humification ratio (RPD = 2.23), total exchangeable carbon (RPD = 2.07) and total organic carbon (RPD = 1.66) with a modular and cost-effective visible and near infrared (VNIR) spectroradiometer. This combination of a less time-consuming compost sample preparation with a versatile sensor system provides an easy-to-implement, efficient and cost-effective protocol for compost maturity assessment and near-real-time monitoring.

Automated processing of whole blood samples for the determination of immunosuppressants by liquid chromatography tandem-mass spectrometry.

PubMed

Vogeser, Michael; Spöhrer, Ute

2006-01-01

Liquid chromatography tandem-mass spectrometry (LC-MS/MS) is an efficient technology for routine determination of immunosuppressants in whole blood; however, time-consuming manual sample preparation remains a significant limitation of this technique. Using a commercially available robotic pipetting system (Tecan Freedom EVO), we developed an automated sample-preparation protocol for quantification of tacrolimus in whole blood by LC-MS/MS. Barcode reading, sample resuspension, transfer of whole blood aliquots into a deep-well plate, addition of internal standard solution, mixing, and protein precipitation by addition of an organic solvent is performed by the robotic system. After centrifugation of the plate, the deproteinized supernatants are submitted to on-line solid phase extraction, using column switching prior to LC-MS/MS analysis. The only manual actions within the entire process are decapping of the tubes, and transfer of the deep-well plate from the robotic system to a centrifuge and finally to the HPLC autosampler. Whole blood pools were used to assess the reproducibility of the entire analytical system for measuring tacrolimus concentrations. A total coefficient of variation of 1.7% was found for the entire automated analytical process (n=40; mean tacrolimus concentration, 5.3 microg/L). Close agreement between tacrolimus results obtained after manual and automated sample preparation was observed. The analytical system described here, comprising automated protein precipitation, on-line solid phase extraction and LC-MS/MS analysis, is convenient and precise, and minimizes hands-on time and the risk of mistakes in the quantification of whole blood immunosuppressant concentrations compared to conventional methods.

Design of gefitinib-loaded poly (l-lactic acid) microspheres via a supercritical anti-solvent process for dry powder inhalation.

PubMed

Lin, Qing; Liu, Guijin; Zhao, Ziyi; Wei, Dongwei; Pang, Jiafeng; Jiang, Yanbin

2017-10-30

To develop a safer, more stable and potent formulation of gefitinib (GFB), micro-spheres of GFB encapsulated into poly (l-lactic acid) (PLLA) have been prepared by supercritical anti-solvent (SAS) technology in this study. Operating factors were optimized using a selected OA 16 (4 5 ) orthogonal array design, and the properties of the raw material and SAS processed samples were characterized by different methods The results show that the GFB-loaded PLLA particles prepared were spherical, having a smaller and narrower particle size compared with raw GFB. The optimal GFB-loaded PLLA sample was prepared with less aggregation, highest GFB loading (15.82%) and smaller size (D 50 =2.48μm, which meets the size of dry powder inhalers). The results of XRD and DSC indicate that GFB is encapsulated into PLLA matrix in a polymorphic form different from raw GFB. FT-IR results show that the chemical structure of GFB does not change after the SAS process. The results of in vitro release show that the optimal sample release was slower compared with raw GFB particles. Moreover, the results of in vitro anti-cancer trials show that the optimal sample had a higher cytotoxicity than raw GFB. After blending with sieved lactose, the flowability and aerosolization performance of the optimal sample for DPI were improved, with angle of repose, emitted dose and fine particles fractions from 38.4° to 23°, 63.21% to >90%, 23.37% to >30%, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Development, validation, and application of a novel LC-MS/MS trace analysis method for the simultaneous quantification of seven iodinated X-ray contrast media and three artificial sweeteners in surface, ground, and drinking water.

PubMed

Ens, Waldemar; Senner, Frank; Gygax, Benjamin; Schlotterbeck, Götz

2014-05-01

A new method for the simultaneous determination of iodated X-ray contrast media (ICM) and artificial sweeteners (AS) by liquid chromatography-tandem mass spectrometry (LC-MS/MS) operated in positive and negative ionization switching mode was developed. The method was validated for surface, ground, and drinking water samples. In order to gain higher sensitivities, a 10-fold sample enrichment step using a Genevac EZ-2 plus centrifugal vacuum evaporator that provided excellent recoveries (90 ± 6 %) was selected for sample preparation. Limits of quantification below 10 ng/L were obtained for all compounds. Furthermore, sample preparation recoveries and matrix effects were investigated thoroughly for all matrix types. Considerable matrix effects were observed in surface water and could be compensated by the use of four stable isotope-labeled internal standards. Due to their persistence, fractions of diatrizoic acid, iopamidol, and acesulfame could pass the whole drinking water production process and were observed also in drinking water. To monitor the fate and occurrence of these compounds, the validated method was applied to samples from different stages of the drinking water production process of the Industrial Works of Basel (IWB). Diatrizoic acid was found as the most persistent compound which was eliminated by just 40 % during the whole drinking water treatment process, followed by iopamidol (80 % elimination) and acesulfame (85 % elimination). All other compounds were completely restrained and/or degraded by the soil and thus were not detected in groundwater. Additionally, a direct injection method without sample preparation achieving 3-20 ng/L limits of quantification was compared to the developed method.

An improved FIB sample preparation technique for site-specific plan-view specimens: A new cutting geometry.

PubMed

Li, Chen; Habler, Gerlinde; Baldwin, Lisa C; Abart, Rainer

2018-01-01

Focused ion beam (FIB) sample preparation technique in plan-view geometry allows direct correlations of the atomic structure study via transmission electron microscopy with micrometer-scale property measurements. However, one main technical difficulty is that a large amount of material must be removed underneath the specimen. Furthermore, directly monitoring the milling process is difficult unless very large material volumes surrounding the TEM specimen site are removed. In this paper, a new cutting geometry is introduced for FIB lift-out sample preparation with plan-view geometry. Firstly, an "isolated" cuboid shaped specimen is cut out, leaving a "bridge" connecting it with the bulk material. Subsequently the two long sides of the "isolated" cuboid are wedged, forming a triangular prism shape. A micromanipulator needle is used for in-situ transfer of the specimen to a FIB TEM grid, which has been mounted parallel with the specimen surface using a simple custom-made sample slit. Finally, the grid is transferred to the standard FIB grid holder for final thinning with standard procedures. This new cutting geometry provides clear viewing angles for monitoring the milling process, which solves the difficulty of judging whether the specimen has been entirely detached from the bulk material, with the least possible damage to the surrounding materials. With an improved success rate and efficiency, this plan-view FIB lift-out specimen preparation technique should have a wide application for material science. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

Poly (lactic-co-glycolic acid) particles prepared by microfluidics and conventional methods. Modulated particle size and rheology.

PubMed

Perez, Aurora; Hernández, Rebeca; Velasco, Diego; Voicu, Dan; Mijangos, Carmen

2015-03-01

Microfluidic techniques are expected to provide narrower particle size distribution than conventional methods for the preparation of poly (lactic-co-glycolic acid) (PLGA) microparticles. Besides, it is hypothesized that the particle size distribution of poly (lactic-co-glycolic acid) microparticles influences the settling behavior and rheological properties of its aqueous dispersions. For the preparation of PLGA particles, two different methods, microfluidic and conventional oil-in-water emulsification methods were employed. The particle size and particle size distribution of PLGA particles prepared by microfluidics were studied as a function of the flow rate of the organic phase while particles prepared by conventional methods were studied as a function of stirring rate. In order to study the stability and structural organization of colloidal dispersions, settling experiments and oscillatory rheological measurements were carried out on aqueous dispersions of PLGA particles with different particle size distributions. Microfluidics technique allowed the control of size and size distribution of the droplets formed in the process of emulsification. This resulted in a narrower particle size distribution for samples prepared by MF with respect to samples prepared by conventional methods. Polydisperse samples showed a larger tendency to aggregate, thus confirming the advantages of microfluidics over conventional methods, especially if biomedical applications are envisaged. Copyright © 2014 Elsevier Inc. All rights reserved.

Biomek 3000: the workhorse in an automated accredited forensic genetic laboratory.

PubMed

Stangegaard, Michael; Meijer, Per-Johan; Børsting, Claus; Hansen, Anders J; Morling, Niels

2012-10-01

We have implemented and validated automated protocols for a wide range of processes such as sample preparation, PCR setup, and capillary electrophoresis setup using small, simple, and inexpensive automated liquid handlers. The flexibility and ease of programming enable the Biomek 3000 to be used in many parts of the laboratory process in a modern forensic genetics laboratory with low to medium sample throughput. In conclusion, we demonstrated that sample processing for accredited forensic genetic DNA typing can be implemented on small automated liquid handlers, leading to the reduction of manual work as well as increased quality and throughput.

Effect of V-Nd co-doping on phase transformation and grain growth process of TiO2

NASA Astrophysics Data System (ADS)

Khatun, Nasima; Amin, Ruhul; Anita, Sen, Somaditya

2018-05-01

The pure and V-Nd co-doped TiO2 samples are prepared by the modified sol-gel process. The phase formation is confirmed by XRD spectrum. Phase transformation is delayed in V-Nd co-doped TiO2 (TVN) samples compared to pure TiO2. The particle size is comparatively small in TVN samples at both the temperature 450 °C and 900 °C. Hence the effect of Nd doping is dominated over V doping in both phase transformation and grain growth process of TiO2.

Immunosuppressant therapeutic drug monitoring by LC-MS/MS: workflow optimization through automated processing of whole blood samples.

PubMed

Marinova, Mariela; Artusi, Carlo; Brugnolo, Laura; Antonelli, Giorgia; Zaninotto, Martina; Plebani, Mario

2013-11-01

Although, due to its high specificity and sensitivity, LC-MS/MS is an efficient technique for the routine determination of immunosuppressants in whole blood, it involves time-consuming manual sample preparation. The aim of the present study was therefore to develop an automated sample-preparation protocol for the quantification of sirolimus, everolimus and tacrolimus by LC-MS/MS using a liquid handling platform. Six-level commercially available blood calibrators were used for assay development, while four quality control materials and three blood samples from patients under immunosuppressant treatment were employed for the evaluation of imprecision. Barcode reading, sample re-suspension, transfer of whole blood samples into 96-well plates, addition of internal standard solution, mixing, and protein precipitation were performed with a liquid handling platform. After plate filtration, the deproteinised supernatants were submitted for SPE on-line. The only manual steps in the entire process were de-capping of the tubes, and transfer of the well plates to the HPLC autosampler. Calibration curves were linear throughout the selected ranges. The imprecision and accuracy data for all analytes were highly satisfactory. The agreement between the results obtained with manual and those obtained with automated sample preparation was optimal (n=390, r=0.96). In daily routine (100 patient samples) the typical overall total turnaround time was less than 6h. Our findings indicate that the proposed analytical system is suitable for routine analysis, since it is straightforward and precise. Furthermore, it incurs less manual workload and less risk of error in the quantification of whole blood immunosuppressant concentrations than conventional methods. © 2013.

Enhanced 99 Tc retention in glass waste form using Tc(IV)-incorporated Fe minerals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Um, Wooyong; Luksic, Steven A.; Wang, Guohui

Technetium (99Tc) immobilization by doping into iron oxide mineral phases may alleviate the problems with Tc volatility during vitrification of nuclear waste. Reduced Tc, Tc(IV), substitutes for Fe(III) in the crystal structure by a process of Tc reduction from Tc(VII) to Tc(IV) followed by co-precipitation of Fe oxide minerals. Two Tc-incorporated Fe minerals (Tc-goethite and Tc-magnetite/maghemite) were prepared and tested for Tc retention in glass melt samples at temperatures between 600 – 1,000 oC. After being cooled, the solid glass specimens prepared at different temperatures were analyzed for Tc oxidation state using Tc K-edge XANES. In most samples, Tc wasmore » partially oxidized from Tc(IV) to Tc(VII) as the melt temperature increased. However, Tc retention in glass melt samples prepared using Tc-incorporated Fe minerals were moderately higher than in glass prepared using KTcO4 because of limited and delayed Tc volatilization.« less

From in situ coal to the final coal product: A case study of the Danville Coal Member (Indiana)

USGS Publications Warehouse

Mastalerz, Maria; Padgett, P.L.

1999-01-01

A surface coal mine operation and preparation plant in southwestern Indiana was sampled to examine variations in coal quality and coal petrography parameters for the Danville Coal Member of the Dugger Formation (Pennsylvanian-Desmoinesian, Westphalian D). Representative samples from in situ coal, preparation plant feeds, and a final coal product were collected in order to compare coal quality, coal petrography, trace element concentrations, and ash chemistry of the coal to those of the product. Coal quality parameters of the in situ samples and various feeds, coarse refuse, and final product were variable. The quality of the final coal product was best predicted by the coal quality of the clean coal feed (from the middle portions of the seam). Some trace element contents, especially lead and arsenic, varied between the coal feeds and the product. Lead contents increased in the feeds and product compared to the channel sample of the raw coal, possibly due to contamination in the handling process.A surface coal mine operation and preparation plant in southwestern Indiana was sampled to examine variations in coal quality and coal petrography parameters for the Danville Coal Member of the Dugger Formation (Pennsylvanian-Desmoinesian, Westphalian D). Representative samples from in situ coal, preparation plant feeds, and a final coal product were collected in order to compare coal quality, coal petrography, trace element concentrations, and ash chemistry of the coal to those of the product. Coal quality parameters of the in situ samples and various feeds, coarse refuse, and final product were variable. The quality of the final coal product was best predicted by the coal quality of the clean coal feed (from the middle portions of the seam). Some trace element contents, especially lead and arsenic, varied between the coal feeds and the product. Lead contents increased in the feeds and product compared to the channel sample of the raw coal, possibly due to contamination in the handling process.

PLE in the analysis of plant compounds. Part I. The application of PLE for HPLC analysis of caffeine in green tea leaves.

PubMed

Dawidowicz, Andrzej L; Wianowska, Dorota

2005-04-29

A broad spectrum of sample preparation methods is currently used for the isolation of pharmacologically active compounds from plant and herbal materials. The paper compares the effectiveness of infusion, microwave assisted solvent extraction (MASE), matrix solid-phase dispersion (MSPD) and pressurised liquid extraction (PLE) as sample preparation methods for the isolation of caffeine from green tea leaves. The effect of PLE variables, such as extraction temperature, pressure and time, on the yield of caffeine from the investigated matrix is discussed. The obtained results revealed that PLE, in comparison with other sample preparation methods applied, has significantly lower efficacy for caffeine isolation from green tea leaves. The evaluation of PLE conditions leads to the conclusion that elevated pressure applied in the PLE process is the factor hindering the extraction.

Removal of Non-metallic Inclusions from Nickel Base Superalloys by Electromagnetic Levitation Melting in a Slag

NASA Astrophysics Data System (ADS)

Manjili, Mohsen Hajipour; Halali, Mohammad

2018-02-01

Samples of INCONEL 718 were levitated and melted in a slag by the application of an electromagnetic field. The effects of temperature, time, and slag composition on the inclusion content of the samples were studied thoroughly. Samples were compared with the original alloy to study the effect of the process on inclusions. Size, shape, and chemical composition of remaining non-metallic inclusions were investigated. The samples were prepared by Standard Guide for Preparing and Evaluating Specimens for Automatic Inclusion Assessment of Steel (ASTM E 768-99) method and the results were reported by means of the Standard Test Methods for Determining the Inclusion Content of Steel (ASTM E 45-97). Results indicated that by increasing temperature and processing time, greater level of cleanliness could be achieved, and numbers and size of the remaining inclusions decreased significantly. It was also observed that increasing calcium fluoride content of the slag helped reduce inclusion content.

Preliminary physico-chemical profile of Brahmi Ghrita.

PubMed

Yadav, Kapil D; Reddy, Konduru R C; Agarwal, Alka

2013-07-01

Brahmi Ghrita was processed as per the process of Snehapaka procedure described in classics. It contained Brahmi (Bacopa monneri), Vacha (Acorus calamus), Kushtha (Sassurea lappa), Shankhapushpi (Convolvulos pluricalis), and Purana Ghrita. In the preparation of Brahmi Ghrita, Brahmi Swarasa, Kalka Dravya of Brahmi, Vacha, Kushtha, and Shankhapushpi were mixed in Purana Ghrita and heated for three hours at 110°C every day for three days. On the third day Ghrita was filtered to obtain the finished product. In this manner, three samples of Brahmi Ghrita were prepared. To understand the changes that occurred during the preparation, Brahmi Ghrita and Purana Ghrita were analyzed by using modern parameters such as Acid value, Saponification value, and so on. After the analysis, it was found that the Acid values of Sample A, B, and C of Brahmi Ghrita were 4.26, 4.03, and 4.03; the Saponification values of Samples A, B, and C of Brahmi Ghrita were 227.2, 230.01, and 230.01, and the Iodine values of Samples A, B, and C were 34.75, 35.88, and 35.88, respectively, and the Acid value, Saponification value, and Iodine value of Purana Ghrita were 1.57, 199.15, and 31.04, respectively. The present study revealed that, there was no significant variation in the analytical values among all three samples of Brahmi Ghrita.

Preliminary physico-chemical profile of Brahmi Ghrita

PubMed Central

Yadav, Kapil D.; Reddy, Konduru R. C.; Agarwal, Alka

2013-01-01

Brahmi Ghrita was processed as per the process of Snehapaka procedure described in classics. It contained Brahmi (Bacopa monneri), Vacha (Acorus calamus), Kushtha (Sassurea lappa), Shankhapushpi (Convolvulos pluricalis), and Purana Ghrita. In the preparation of Brahmi Ghrita, Brahmi Swarasa, Kalka Dravya of Brahmi, Vacha, Kushtha, and Shankhapushpi were mixed in Purana Ghrita and heated for three hours at 110°C every day for three days. On the third day Ghrita was filtered to obtain the finished product. In this manner, three samples of Brahmi Ghrita were prepared. To understand the changes that occurred during the preparation, Brahmi Ghrita and Purana Ghrita were analyzed by using modern parameters such as Acid value, Saponification value, and so on. After the analysis, it was found that the Acid values of Sample A, B, and C of Brahmi Ghrita were 4.26, 4.03, and 4.03; the Saponification values of Samples A, B, and C of Brahmi Ghrita were 227.2, 230.01, and 230.01, and the Iodine values of Samples A, B, and C were 34.75, 35.88, and 35.88, respectively, and the Acid value, Saponification value, and Iodine value of Purana Ghrita were 1.57, 199.15, and 31.04, respectively. The present study revealed that, there was no significant variation in the analytical values among all three samples of Brahmi Ghrita. PMID:24501526

Properties of Cu-Based Shape-Memory Alloys Prepared by Selective Laser Melting

NASA Astrophysics Data System (ADS)

Gustmann, T.; dos Santos, J. M.; Gargarella, P.; Kühn, U.; Van Humbeeck, J.; Pauly, S.

2017-03-01

Two shape-memory alloys with the nominal compositions (in wt.%) Cu-11.85Al-3.2Ni-3Mn and Cu-11.35Al-3.2Ni-3Mn-0.5Zr were prepared by selective laser melting (SLM). The parameters were optimised to identify the process window, in which almost fully dense samples can be obtained. Their microstructures were analysed and correlated with the shape-memory behaviour as well as the mechanical properties. Suction-cast specimens were also produced for comparison. Mainly, β 1' martensite forms in all samples, but 0.5 wt.% of Zr stabilises the Y phase (Cu2AlZr), and its morphology depends on the thermal history and cooling rate. After annealing, the Y phase is primarily found at the grain boundaries hampering grain coarsening. Due to the relative high cooling rates applied here, Zr is mostly dissolved in the martensite in the as-prepared samples and it has a grain-refining effect only up to a critical cooling rate. The Zr-containing samples have increased transformation temperatures, and the Y phase seems to be responsible for the jerky martensite-to-austenite transformation. All the samples are relatively ductile because they mostly fracture in a transgranular manner, exhibiting the typical double yielding. Selective laser melting allows the adjustment of the transformation temperatures and the mechanical properties already during processing without the need of a subsequent heat treatment.

The materials processing sciences glovebox

NASA Technical Reports Server (NTRS)

Traweek, Larry

1990-01-01

The Materials Processing Sciences Glovebox is a rack mounted workstation which allows on orbit sample preparation and characterization of specimens from various experiment facilities. It provides an isolated safe, clean, and sterile environment for the crew member to work with potentially hazardous materials. It has to handle a range of chemicals broader than even PMMS. The theme is that the Space Station Laboratory experiment preparation and characterization operations provide the fundamental glovebox design characteristics. Glovebox subsystem concepts and how internal material handling operations affect the design are discussed.

Burnishing rolling process of the surface prepared in the turning process

NASA Astrophysics Data System (ADS)

Kulakowska, Agnieszka; Kukielka, Leon; Kaldunski, Pawel; Bohdal, Lukasz; Patyk, Radoslaw; Chodor, Jaroslaw; Kukielka, Krzysztof

2018-05-01

The aim of this article is to demonstrate the possibility of using burnishing rolling process as the technology of product development. The experimental researches were carried out, showing the ability to form the surface layer of the product with the desired properties. First, during turning rolling the surfaces of the samples were prepared. Then, the surfaces were burnished. The influence of turning process on the state of the surface layer parameters of C45 steel shafts are shown. Among the examined aspects the surface roughness, nano-roughness, material bearing, surface microstructure, metallographic structure were considered. Numerical simulation were conducted. Conclusions from the experiments and simulation were given.

The optical properties of α-Fe2O3 nanostructures synthesized with different immersion time

NASA Astrophysics Data System (ADS)

Ahmad, W. R. W.; Mamat, M. H.; Zoolfakar, A. S.; Khusaimi, Z.; Yusof, M. M.; Ismail, A. S.; Saidi, S. A.; Rusop, M.

2018-05-01

In this study, nanostructured hematite (α-Fe2O3) thin films have been prepared successfully by sonicated immersion method on fluorine-doped tin oxide (FTO) coated glass substrate. The effect of the immersion time on the structural and optical properties of α-Fe2O3 nanostructure were investigated for a variation of immersion time ranging from 1 to 4 hour. From the characterization results, the surface morphology of the sample prepared in 4 hours immersion process has exhibited highest porosity, and the highest absorbance properties were found in the same sample. These results suggest that the different time duration during immersion process play important roles in optical properties of α-Fe2O3 nanostructures.

SrFe 12O 19 prepared by the proteic sol-gel process

NASA Astrophysics Data System (ADS)

Brito, P. C. A.; Gomes, R. F.; Duque, J. G. S.; Macêdo, M. A.

2006-10-01

Powders of strontium hexaferrite (SrFe 12O 19) were prepared by the proteic sol-gel process using coconut water as a precursor. X-ray diffraction (XRD) measurement showed the formation of SrFe 12O 19 with a small amount of the hematite for the sample calcined at 1000 °C with Fe/Sr=12. Rietveld refinement disclosed that this sample had 87.56% of the SrFe 12O 19 and 12.44% of Fe 2O 3 and the values for Rp, Rwp and χ2 were 4.28%, 5.93% and 1.71, respectively. The magnetic properties were Ms=64 emu/g, Mr/ Ms=0.55 and Hc=1.4 kOe for a crystallite size of 57 nm.

Band structure and visible light photocatalytic activity of multi-type nitrogen doped TiO(2) nanoparticles prepared by thermal decomposition.

PubMed

Dong, Fan; Zhao, Weirong; Wu, Zhongbiao; Guo, Sen

2009-03-15

Multi-type nitrogen doped TiO(2) nanoparticles were prepared by thermal decomposition of the mixture of titanium hydroxide and urea at 400 degrees C for 2h. The as-prepared photocatalysts were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), UV-vis diffuse reflectance spectra (UV-vis DRS), and photoluminescence (PL). The results showed that the as-prepared samples exhibited strong visible light absorption due to multi-type nitrogen doped in the form of substitutional (N-Ti-O and Ti-O-N) and interstitial (pi* character NO) states, which were 0.14 and 0.73 eV above the top of the valence band, respectively. A physical model of band structure was established to clarify the visible light photocatalytic process over the as-prepared samples. The photocatalytic activity was evaluated for the photodegradation of gaseous toluene under visible light irradiation. The activity of the sample prepared from wet titanium hydroxide and urea (TiO(2)-Nw, apparent reaction rate constant k = 0.045 min(-1)) was much higher than other samples including P25 (k = 0.0013 min(-1)). The high activity can be attributed to the results of the synergetic effects of strong visible light absorption, good crystallization, large surface hydroxyl groups, and enhanced separation of photoinduced carriers.

The effect of processing on the surface physical stability of amorphous solid dispersions.

PubMed

Yang, Ziyi; Nollenberger, Kathrin; Albers, Jessica; Moffat, Jonathan; Craig, Duncan; Qi, Sheng

2014-11-01

The focus of this study was to investigate the effect of processing on the surface crystallization of amorphous molecular dispersions and gain insight into the mechanisms underpinning this effect. The model systems, amorphous molecular dispersions of felodipine-EUDRAGIT® E PO, were processed both using spin coating (an ultra-fast solvent evaporation based method) and hot melt extrusion (HME) (a melting based method). Amorphous solid dispersions with drug loadings of 10-90% (w/w) were obtained by both processing methods. Samples were stored under 75% RH/room temperatures for up to 10months. Surface crystallization was observed shortly after preparation for the HME samples with high drug loadings (50-90%). Surface crystallization was characterized by powder X-ray diffraction (PXRD), ATR-FTIR spectroscopy and imaging techniques (SEM, AFM and localized thermal analysis). Spin coated molecular dispersions showed significantly higher surface physical stability than hot melt extruded samples. For both systems, the progress of the surface crystal growth followed zero order kinetics on aging. Drug enrichment at the surfaces of HME samples on aging was observed, which may contribute to surface crystallization of amorphous molecular dispersions. In conclusion it was found the amorphous molecular dispersions prepared by spin coating had a significantly higher surface physical stability than the corresponding HME samples, which may be attributed to the increased process-related apparent drug-polymer solubility and reduced molecular mobility due to the quenching effect caused by the rapid solvent evaporation in spin coating. Copyright © 2014 Elsevier B.V. All rights reserved.

Accelerating root system phenotyping of seedlings through a computer-assisted processing pipeline.

PubMed

Dupuy, Lionel X; Wright, Gladys; Thompson, Jacqueline A; Taylor, Anna; Dekeyser, Sebastien; White, Christopher P; Thomas, William T B; Nightingale, Mark; Hammond, John P; Graham, Neil S; Thomas, Catherine L; Broadley, Martin R; White, Philip J

2017-01-01

There are numerous systems and techniques to measure the growth of plant roots. However, phenotyping large numbers of plant roots for breeding and genetic analyses remains challenging. One major difficulty is to achieve high throughput and resolution at a reasonable cost per plant sample. Here we describe a cost-effective root phenotyping pipeline, on which we perform time and accuracy benchmarking to identify bottlenecks in such pipelines and strategies for their acceleration. Our root phenotyping pipeline was assembled with custom software and low cost material and equipment. Results show that sample preparation and handling of samples during screening are the most time consuming task in root phenotyping. Algorithms can be used to speed up the extraction of root traits from image data, but when applied to large numbers of images, there is a trade-off between time of processing the data and errors contained in the database. Scaling-up root phenotyping to large numbers of genotypes will require not only automation of sample preparation and sample handling, but also efficient algorithms for error detection for more reliable replacement of manual interventions.

Automated Drug Identification for Urban Hospitals

NASA Technical Reports Server (NTRS)

Shirley, Donna L.

1971-01-01

Many urban hospitals are becoming overloaded with drug abuse cases requiring chemical analysis for identification of drugs. In this paper, the requirements for chemical analysis of body fluids for drugs are determined and a system model for automated drug analysis is selected. The system as modeled, would perform chemical preparation of samples, gas-liquid chromatographic separation of drugs in the chemically prepared samples, infrared spectrophotometric analysis of the drugs, and would utilize automatic data processing and control for drug identification. Requirements of cost, maintainability, reliability, flexibility, and operability are considered.

Integrated Multi-process Microfluidic Systems for Automating Analysis

PubMed Central

Yang, Weichun; Woolley, Adam T.

2010-01-01

Microfluidic technologies have been applied extensively in rapid sample analysis. Some current challenges for standard microfluidic systems are relatively high detection limits, and reduced resolving power and peak capacity compared to conventional approaches. The integration of multiple functions and components onto a single platform can overcome these separation and detection limitations of microfluidics. Multiplexed systems can greatly increase peak capacity in multidimensional separations and can increase sample throughput by analyzing many samples simultaneously. On-chip sample preparation, including labeling, preconcentration, cleanup and amplification, can all serve to speed up and automate processes in integrated microfluidic systems. This paper summarizes advances in integrated multi-process microfluidic systems for automated analysis, their benefits and areas for needed improvement. PMID:20514343

Selected problems with boron determination in water treatment processes. Part I: comparison of the reference methods for ICP-MS and ICP-OES determinations.

PubMed

Kmiecik, Ewa; Tomaszewska, Barbara; Wątor, Katarzyna; Bodzek, Michał

2016-06-01

The aim of the study was to compare the two reference methods for the determination of boron in water samples and further assess the impact of the method of preparation of samples for analysis on the results obtained. Samples were collected during different desalination processes, ultrafiltration and the double reverse osmosis system, connected in series. From each point, samples were prepared in four different ways: the first was filtered (through a membrane filter of 0.45 μm) and acidified (using 1 mL ultrapure nitric acid for each 100 mL of samples) (FA), the second was unfiltered and not acidified (UFNA), the third was filtered but not acidified (FNA), and finally, the fourth was unfiltered but acidified (UFA). All samples were analysed using two analytical methods: inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES). The results obtained were compared and correlated, and the differences between them were studied. The results show that there are statistically significant differences between the concentrations obtained using the ICP-MS and ICP-OES techniques regardless of the methods of sampling preparation (sample filtration and preservation). Finally, both the ICP-MS and ICP-OES methods can be used for determination of the boron concentration in water. The differences in the boron concentrations obtained using these two methods can be caused by several high-level concentrations in selected whole-water digestates and some matrix effects. Higher concentrations of iron (from 1 to 20 mg/L) than chromium (0.02-1 mg/L) in the samples analysed can influence boron determination. When iron concentrations are high, we can observe the emission spectrum as a double joined and overlapping peak.

Rapid production of hollow SS316 profiles by extrusion based additive manufacturing

NASA Astrophysics Data System (ADS)

Rane, Kedarnath; Cataldo, Salvatore; Parenti, Paolo; Sbaglia, Luca; Mussi, Valerio; Annoni, Massimiliano; Giberti, Hermes; Strano, Matteo

2018-05-01

Complex shaped stainless steel tubes are often required for special purpose biomedical equipment. Nevertheless, traditional manufacturing technologies, such as extrusion, lack the ability to compete in a market of customized complex components because of associated expenses towards tooling and extrusion presses. To rapid manufacture few of such components with low cost and high precision, a new Extrusion based Additive Manufacturing (EAM) process, is proposed in this paper, and as an example, short stainless steel 316L complex shaped and sectioned tubes were prepared by EAM. Several sample parts were produced using this process; the dimensional stability, surface roughness and chemical composition of sintered samples were investigated to prove process competence. The results indicate that feedstock with a 316L particle content of 92.5 wt. % can be prepared with a sigma blade mixing, whose rheological behavior is fit for EAM. The green samples have sufficient strength to handle them for subsequent treatments. The sintered samples considerably shrunk to designed dimensions and have a homogeneous microstructure to impart mechanical strength. Whereas, maintaining comparable dimensional accuracy and chemical composition which are required for biomedical equipment still need iterations, a kinematic correction and modification in debinding cycle was proposed.

Upgrade Recycling of Cast Iron Scrap Chips towards β-FeSi₂ Thermoelectric Materials.

PubMed

Laila, Assayidatul; Nanko, Makoto; Takeda, Masatoshi

2014-09-04

The upgrade recycling of cast-iron scrap chips towards β-FeSi₂ thermoelectric materials is proposed as an eco-friendly and cost-effective production process. By using scrap waste from the machining process of cast-iron components, the material cost to fabricate β-FeSi₂ is reduced and the industrial waste is recycled. In this study, β-FeSi₂ specimens obtained from cast iron scrap chips were prepared both in the undoped form and doped with Al and Co elements. The maximum figure of merit ( ZT ) indicated a thermoelectric performance of approximately 70% in p-type samples and nearly 90% in n-type samples compared to β-FeSi₂ prepared from pure Fe and other published studies. The use of cast iron scrap chips to produce β-FeSi₂ shows promise as an eco-friendly and cost-effective production process for thermoelectric materials.

Simultaneous determination of 15 marker constituents in various radix Astragali preparations by solid-phase extraction and high-performance liquid chromatography.

PubMed

Qi, Lian-Wen; Yu, Qing-Tao; Yi, Ling; Ren, Mei-Ting; Wen, Xiao-Dong; Wang, Yu-Xia; Li, Ping

2008-01-01

An improved quality control method was developed to simultaneously determine 15 major constituents (eight flavonoids and seven saponins) in various radix Astragali preparations, using SPE for pretreatment of samples, HPLC with diode-array and evaporative light scattering detectors (DAD-ELSD) for quantification in one run, and HPLC-ESI-TOF/MS for definite identification of compounds in preparations. Optimum separations were obtained with a ZORBAX C(18) column, using a gradient elution with 0.3% aqueous formic acid and ACN. This established method was fully validated with respect to linearity, precision, repeatability, and accuracy, and was successfully applied to quantify the 15 compounds in 19 commercial samples, including 3 dosage forms, i. e., oral solution, injection, concentrated granule, and its processed products of radix Astragali. The results demonstrated that many factors might result in significant differences in quality of the final preparations, including crude drugs, pretreatment processes, manufacturing procedure, storage conditions, etc. Then the developed method provided a reasonable and powerful manner to ensure the efficacy, safety, and batch-to-batch uniformity of radix Astragali products by standardizing each procedure, and thus should be proposed as quality control for the clinical use and modernization of herbal preparations.

Mesoporous structured MIPs@CDs fluorescence sensor for highly sensitive detection of TNT.

PubMed

Xu, Shoufang; Lu, Hongzhi

2016-11-15

A facile strategy was developed to prepare mesoporous structured molecularly imprinted polymers capped carbon dots (M-MIPs@CDs) fluorescence sensor for highly sensitive and selective determination of TNT. The strategy using amino-CDs directly as "functional monomer" for imprinting simplify the imprinting process and provide well recognition sites accessibility. The as-prepared M-MIPs@CDs sensor, using periodic mesoporous silica as imprinting matrix, and amino-CDs directly as "functional monomer", exhibited excellent selectivity and sensitivity toward TNT with detection limit of 17nM. The recycling process was sustainable for 10 times without obvious efficiency decrease. The feasibility of the developed method in real samples was successfully evaluated through the analysis of TNT in soil and water samples with satisfactory recoveries of 88.6-95.7%. The method proposed in this work was proved to be a convenient and practical way to prepare high sensitive and selective fluorescence MIPs@CDs sensors. Copyright © 2016 Elsevier B.V. All rights reserved.

Detection of bacteria in platelet concentrates prepared from spiked single donations using cultural and molecular genetic methods.

PubMed

Störmer, M; Cassens, U; Kleesiek, K; Dreier, J

2007-02-01

Bacteria show differences in their growth kinetics depending on the type of blood component. On to storage at 22 degrees C, platelet concentrates (PCs) seem to be more prone to bacterial multiplication than red cell concentrates. Knowledge of the potential for bacterial proliferation in blood components, which are stored at a range of temperatures, is essential before considering implementation of a detection strategy. The efficacy of bacterial detection was determined, using real-time reverse transcriptase-polymerase chain reaction (RT-PCR), following bacterial growth in blood components obtained from a deliberately contaminated whole-blood (WB) unit. Cultivation was used as the reference method. WB was spiked with 2 colony-forming units mL(-1)Staphylococcus epidermidis or Klebsiella pneumoniae, kept for 15 h at room temperature and component preparation was processed. Samples were drawn, at intervals throughout the whole separation process, from each blood component. Nucleic acids were extracted using an automated high-volume extraction method. The 15-h storage revealed an insignificant increase in bacterial titre. No bacterial growth was detected in red blood cell or plasma units. K. pneumoniae showed rapid growth in the pooled PC and could be detected immediately after preparation using RT-PCR. S. epidermidis grew slowly and was detected 24 h after separation. These experiments show that sampling is indicative at 24 h after preparation of PCs at the earliest to minimize the sampling error.

Automated CD-SEM recipe creation technology for mass production using CAD data

NASA Astrophysics Data System (ADS)

Kawahara, Toshikazu; Yoshida, Masamichi; Tanaka, Masashi; Ido, Sanyu; Nakano, Hiroyuki; Adachi, Naokaka; Abe, Yuichi; Nagatomo, Wataru

2011-03-01

Critical Dimension Scanning Electron Microscope (CD-SEM) recipe creation needs sample preparation necessary for matching pattern registration, and recipe creation on CD-SEM using the sample, which hinders the reduction in test production cost and time in semiconductor manufacturing factories. From the perspective of cost reduction and improvement of the test production efficiency, automated CD-SEM recipe creation without the sample preparation and the manual operation has been important in the production lines. For the automated CD-SEM recipe creation, we have introduced RecipeDirector (RD) that enables the recipe creation by using Computer-Aided Design (CAD) data and text data that includes measurement information. We have developed a system that automatically creates the CAD data and the text data necessary for the recipe creation on RD; and, for the elimination of the manual operation, we have enhanced RD so that all measurement information can be specified in the text data. As a result, we have established an automated CD-SEM recipe creation system without the sample preparation and the manual operation. For the introduction of the CD-SEM recipe creation system using RD to the production lines, the accuracy of the pattern matching was an issue. The shape of design templates for the matching created from the CAD data was different from that of SEM images in vision. Thus, a development of robust pattern matching algorithm that considers the shape difference was needed. The addition of image processing of the templates for the matching and shape processing of the CAD patterns in the lower layer has enabled the robust pattern matching. This paper describes the automated CD-SEM recipe creation technology for the production lines without the sample preparation and the manual operation using RD applied in Sony Semiconductor Kyusyu Corporation Kumamoto Technology Center (SCK Corporation Kumamoto TEC).

Thermal Processing of PVP- and HPMC-Based Amorphous Solid Dispersions.

PubMed

LaFountaine, Justin S; Prasad, Leena Kumari; Brough, Chris; Miller, Dave A; McGinity, James W; Williams, Robert O

2016-02-01

Thermal processing technologies continue to gain interest in pharmaceutical manufacturing. However, the types and grades of polymers that can be utilized in common thermal processing technologies, such as hot-melt extrusion (HME), are often limited by thermal or rheological factors. The objectives of the present study were to compare and contrast two thermal processing methods, HME and KinetiSol® Dispersing (KSD), and investigate the influence of polymer type, polymer molecular weight, and drug loading on the ability to produce amorphous solid dispersions (ASDs) containing the model compound griseofulvin (GRIS). Dispersions were analyzed by a variety of imaging, solid-state, thermal, and solution-state techniques. Dispersions were prepared by both HME and KSD using polyvinylpyrrolidone (PVP) K17 or hydroxypropyl methylcellulose (HPMC) E5. Dispersions were only prepared by KSD using higher molecular weight grades of HPMC and PVP, as these could not be extruded under the conditions selected. Powder X-ray diffraction (PXRD) analysis showed that dispersions prepared by HME were amorphous at 10% and 20% drug load; however, it showed significant crystallinity at 40% drug load. PXRD analysis of KSD samples showed all formulations and drug loads to be amorphous with the exception of trace crystallinity seen in PVP K17 and PVP K30 samples at 40% drug load. These results were further supported by other analytical techniques. KSD produced amorphous dispersions at higher drug loads than could be prepared by HME, as well as with higher molecular weight polymers that were not processable by HME, due to its higher rate of shear and torque output.

Study of sample preparation for determination of endocannabinoids and analogous compounds in human serum by LC-MS/MS in MRM mode.

PubMed

Luque-Córdoba, D; Calderón-Santiago, M; Luque de Castro, M D; Priego-Capote, F

2018-08-01

Endocannabinoids are lipids with a key role in physiological processes such as the immune response or the metabolism. This involvement explains their association to pathologies such as cancer, obesity or multiple sclerosis. The determination of endocannabinoids constitutes a challenge for clinical laboratories due to the variety of biological matrices and the wide range of concentrations at which they can be found. This research deals with the comparison of three sample preparation strategies (viz., on-line SPE, off-line SPE for interferents removal, and protein precipitation) for subsequent LC-MS/MS analysis of 14 endocannabinoids and analogous compounds in serum. As a result, the on-line coupling between SPE and LC-MS/MS is proposed as the best approach for this determination. The proposed method allows full automation of the overall process, shortening of the analysis time, and avoidance of errors associated with sample preparation steps. The improvement in sensitivity and selectivity thus achieved allows obtaining quantification limits at the pg mL -1 level, which makes possible the application of the method for clinical studies. Copyright © 2018 Elsevier B.V. All rights reserved.

The planning and establishment of a sample preparation laboratory for drug discovery

PubMed Central

Dufresne, Claude

2000-01-01

Nature has always been a productive source of new drugs. With the advent of high-throughput screening, it has now become possible to rapidly screen large sample collections. In addition to seeking greater diversity from natural product sources (micro-organisms, plants, etc.), fractionation of the crude extracts prior to screening is becoming a more important part of our efforts. As sample preparation protocols become more involved, automation can help to achieve and maintain a desired sample throughput. To address the needs of our screening program, two robotic systems were designed. The first system processes crude extracts all the way to 96-well plates, containing solutions suitable for screening in biological and biochemical assays. The system can dissolve crude extracts, fractionate them on solid-phase extraction cartridges, dry and weigh each fraction, re-dissolve them to a known concentration, and prepare mother plates. The second system replicates mother plates into a number of daughter plates. PMID:18924691

Process dependent thermoelectric properties of EDTA assisted bismuth telluride

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kulsi, Chiranjit; Banerjee, Dipali, E-mail: dipalibanerjeebesu@gmail.com; Kargupta, Kajari

2016-04-13

Comparison between the structure and thermoelectric properties of EDTA (Ethylene-diamine-tetra-acetic acid) assisted bismuth telluride prepared by electrochemical deposition and hydrothermal route is reported in the present work. The prepared samples have been structurally characterized by high resolution X-ray diffraction spectra (HRXRD), field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopic images (HRTEM). Crystallite size and strain have been determined from Williamson-Hall plot of XRD which is in conformity with TEM images. Measurement of transport properties show sample in the pellet form (S{sub 1}) prepared via hydrothermal route has higher value of thermoelectric power (S) than the electrodepositedmore » film (S{sub 2}). But due to a substantial increase in the electrical conductivity (σ) of the film (S{sub 2}) over the pellet (S{sub 1}), the power factor and the figure of merit is higher for sample S{sub 2} than the sample S{sub 1} at room temperature.« less

Evaluation of two platelet-rich plasma processing methods and two platelet-activation techniques for use in llamas and alpacas.

PubMed

Semevolos, Stacy A; Youngblood, Cori D; Grissom, Stephanie K; Gorman, M Elena; Larson, Maureen K

2016-11-01

OBJECTIVE To evaluate 2 processing methods (commercial kit vs conical tube centrifugation) for preparing platelet rich plasma (PRP) for use in llamas and alpacas. SAMPLES Blood samples (30 mL each) aseptically collected from 6 healthy llamas and 6 healthy alpacas. PROCEDURES PRP was prepared from blood samples by use of a commercial kit and by double-step conical tube centrifugation. A CBC was performed for blood and PRP samples. Platelets in PRP samples were activated by means of a freeze-thaw method with or without 23mM CaCl 2 , and concentrations of platelet-derived growth factor-BB and transforming growth factor-β 1 were measured. Values were compared between processing methods and camelid species. RESULTS Blood CBC values for llamas and alpacas were similar. The commercial kit yielded a significantly greater degree of platelet enrichment (mean increase, 8.5 fold vs 2.8 fold) and WBC enrichment (mean increase, 3.7 fold vs 1.9 fold) than did conical tube centrifugation. Llamas had a significantly greater degree of platelet enrichment than alpacas by either processing method. No difference in WBC enrichment was identified between species. Concentrations of both growth factors were significantly greater in PRP samples obtained by use of the commercial kit versus those obtained by conical tube centrifugation. CONCLUSIONS AND CLINICAL RELEVANCE For blood samples from camelids, the commercial kit yielded a PRP product with a higher platelet and WBC concentration than achieved by conical tube centrifugation. Optimal PRP platelet and WBC concentrations for various applications need to be determined for llamas and alpacas.

Ayurvedic hydro-alcoholic anti-asthmatic medicine Vasarishta built upon Mritasanjeevani Sura: Development and evaluation

PubMed Central

Wele, Asmita A.; Pendse, Nikhil U.; Takle, Shrikant P.; Burase, Raghunath V.; Patil, Sanjay V.; Bhalerao, Supriya; Harsulkar, Abhay M.

2015-01-01

Introduction: Vasarishta built upon Mritasanjeevani Sura (MS) is a polyherbal hydro-alcoholic anti-asthmatic formulation which is administered in a dose of 1 ml instead of standard dose 40 ml, generally advocated for any “Asava–Arishta” in Ayurveda. Aim: The present study was aimed at finding out rationale for the peculiar distillation process to manufacture MS followed by Sthapana process to make Vasarishta. It was further aimed to find out difference in Vasarishta samples manufactured by purely fermentation process and the peculiar method mentioned above. Materials and Methods: Three batches of MS and subsequently three batches of Vasarishta were prepared. Basic standardization and development of standard operating procedure for the same were achieved by doing pH, percentage of alcohol and total reducing sugar, specific gravity on both MS and Vasarishta, during and after completion of process. Finally, MS and Vasarishta (built upon MS) made in laboratory were compared with marketed samples of MS and Vasarishta using gas chromatography. Results: The types of alcohols and volatile acids in MS and Vasarishta, prepared in laboratory, are similar but the proportions differ, which is taken as an indicator of process standardization. Values of furfural, ethyl acetate, and 1-butanol in lab samples are within permissible limits as against the values of the market samples. Conclusions: The textual process for the production of Vasarishta proved to produce organoleptically acceptable product which is virtually free of toxic compounds such as furfural. PMID:27313419

Advances in Software Tools for Pre-processing and Post-processing of Overset Grid Computations

NASA Technical Reports Server (NTRS)

Chan, William M.

2004-01-01

Recent developments in three pieces of software for performing pre-processing and post-processing work on numerical computations using overset grids are presented. The first is the OVERGRID graphical interface which provides a unified environment for the visualization, manipulation, generation and diagnostics of geometry and grids. Modules are also available for automatic boundary conditions detection, flow solver input preparation, multiple component dynamics input preparation and dynamics animation, simple solution viewing for moving components, and debris trajectory analysis input preparation. The second is a grid generation script library that enables rapid creation of grid generation scripts. A sample of recent applications will be described. The third is the OVERPLOT graphical interface for displaying and analyzing history files generated by the flow solver. Data displayed include residuals, component forces and moments, number of supersonic and reverse flow points, and various dynamics parameters.

32 CFR Appendix D to Part 1290 - Ticket Sample-A Nontraffic Violation

Code of Federal Regulations, 2010 CFR

2010-07-01

... 32 National Defense 6 2010-07-01 2010-07-01 false Ticket Sample-A Nontraffic Violation D Appendix D to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S...

32 CFR Appendix D to Part 1290 - Ticket Sample-A Nontraffic Violation

Code of Federal Regulations, 2014 CFR

2014-07-01

... 32 National Defense 6 2014-07-01 2014-07-01 false Ticket Sample-A Nontraffic Violation D Appendix D to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S...

32 CFR Appendix D to Part 1290 - Ticket Sample-A Nontraffic Violation

Code of Federal Regulations, 2012 CFR

2012-07-01

... 32 National Defense 6 2012-07-01 2012-07-01 false Ticket Sample-A Nontraffic Violation D Appendix D to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S...

32 CFR Appendix D to Part 1290 - Ticket Sample-A Nontraffic Violation

Code of Federal Regulations, 2011 CFR

2011-07-01

... 32 National Defense 6 2011-07-01 2011-07-01 false Ticket Sample-A Nontraffic Violation D Appendix D to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S...

32 CFR Appendix D to Part 1290 - Ticket Sample-A Nontraffic Violation

Code of Federal Regulations, 2013 CFR

2013-07-01

... 32 National Defense 6 2013-07-01 2013-07-01 false Ticket Sample-A Nontraffic Violation D Appendix D to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S...

Matrix effects in pesticide multi-residue analysis by liquid chromatography-mass spectrometry.

PubMed

Kruve, Anneli; Künnapas, Allan; Herodes, Koit; Leito, Ivo

2008-04-11

Three sample preparation methods: Luke method (AOAC 985.22), QuEChERS (quick, easy, cheap, effective, rugged and safe) and matrix solid-phase dispersion (MSPD) were applied to different fruits and vegetables for analysis of 14 pesticide residues by high-performance liquid chromatography with electrospray ionization-mass spectrometry (HPLC/ESI/MS). Matrix effect, recovery and process efficiency of the sample preparation methods applied to different fruits and vegetables were compared. The Luke method was found to produce least matrix effect. On an average the best recoveries were obtained with the QuEChERS method. MSPD gave unsatisfactory recoveries for some basic pesticide residues. Comparison of matrix effects for different apple varieties showed high variability for some residues. It was demonstrated that the amount of co-extracting compounds that cause ionization suppression of aldicarb depends on the apple variety as well as on the sample preparation method employed.

Abnormal externally guided movement preparation in recent-onset schizophrenia is associated with impaired selective attention to external input.

PubMed

Smid, Henderikus G O M; Westenbroek, Joanna M; Bruggeman, Richard; Knegtering, Henderikus; Van den Bosch, Robert J

2009-11-30

Several theories propose that the primary cognitive impairment in schizophrenia concerns a deficit in the processing of external input information. There is also evidence, however, for impaired motor preparation in schizophrenia. This provokes the question whether the impaired motor preparation in schizophrenia is a secondary consequence of disturbed (selective) processing of the input needed for that preparation, or an independent primary deficit. The aim of the present study was to discriminate between these hypotheses, by investigating externally guided movement preparation in relation to selective stimulus processing. The sample comprised 16 recent-onset schizophrenia patients and 16 controls who performed a movement-precuing task. In this task, a precue delivered information about one, two or no parameters of a movement summoned by a subsequent stimulus. Performance measures and measures derived from the electroencephalogram showed that patients yielded smaller benefits from the precues and showed less cue-based preparatory activity in advance of the imperative stimulus than the controls, suggesting a response preparation deficit. However, patients also showed less activity reflecting selective attention to the precue. We therefore conclude that the existing evidence for an impairment of externally guided motor preparation in schizophrenia is most likely due to a deficit in selective attention to the external input, which lends support to theories proposing that the primary cognitive deficit in schizophrenia concerns the processing of input information.

A Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for In-Situ Mars Surface Sample Analysis

NASA Technical Reports Server (NTRS)

Edmunson, J.; Gaskin, J. A.; Jerman, G. A.; Harvey, R. P.; Doloboff, I. J.; Neidholdt, E. L.

2016-01-01

The Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) project, funded by the NASA Planetary Instrument Concepts for the Advancement of Solar System Observations (PICASSO) Research Opportunities in Space and Earth Sciences (ROSES), will build upon previous miniaturized SEM designs and recent advancements in variable pressure SEM's to design and build a SEM to complete analyses of samples on the surface of Mars using the atmosphere as an imaging medium. This project is a collaboration between NASA Marshall Space Flight Center (MSFC), the Jet Propulsion Laboratory (JPL), electron gun and optics manufacturer Applied Physics Technologies, and small vacuum system manufacturer Creare. Dr. Ralph Harvery and environmental SEM (ESEM) inventor Dr. Gerry Danilatos serve as advisors to the team. Variable pressure SEMs allow for fine (nm-scale) resolution imaging and micron-scale chemical study of materials without sample preparation (e.g., carbon or gold coating). Charging of a sample is reduced or eliminated by the gas surrounding the sample. It is this property of ESEMs that make them ideal for locations where sample preparation is not yet feasible, such as the surface of Mars. In addition, the lack of sample preparation needed here will simplify the sample acquisition process and allow caching of the samples for future complementary payload use.

Determination of anti-inflammatory activities of standardised preparations of plant- and mushroom-based foods.

PubMed

Gunawardena, Dhanushka; Shanmugam, Kirubakaran; Low, Mitchell; Bennett, Louise; Govindaraghavan, Suresh; Head, Richard; Ooi, Lezanne; Münch, Gerald

2014-02-01

Chronic inflammatory processes contribute to the pathogenesis of many age-related diseases. In search of anti-inflammatory foods, we have systematically screened a variety of common dietary plants and mushrooms for their anti-inflammatory activity. A selection of 115 samples was prepared by a generic food-compatible processing method involving heating. These products were tested for their anti-inflammatory activity in murine N11 microglia and RAW 264.7 macrophages, using nitric oxide (NO) and tumour necrosis factor-α (TNF-α) as pro-inflammatory readouts. Ten food samples including lime zest, English breakfast tea, honey-brown mushroom, button mushroom, oyster mushroom, cinnamon and cloves inhibited NO production in N11 microglia, with IC50 values below 0.5 mg/ml. The most active samples were onion, oregano and red sweet potato, exhibiting IC50 values below 0.1 mg/ml. When these ten food preparations were retested in RAW 264.7 macrophages, they all inhibited NO production similar to the results obtained in N11 microglia. In addition, English breakfast tea leaves, oyster mushroom, onion, cinnamon and button mushroom preparations suppressed TNF-α production, exhibiting IC50 values below 0.5 mg/ml in RAW 264.7 macrophages. In summary, anti-inflammatory activity in these food samples survived 'cooking'. Provided that individual bioavailability allows active compounds to reach therapeutic levels in target tissues, these foods may be useful in limiting inflammation in a variety of age-related inflammatory diseases. Furthermore, these foods could be a source for the discovery of novel anti-inflammatory drugs.

Procedure for preparation for shipment of natural gas storage vessel

NASA Technical Reports Server (NTRS)

Amawd, A. M.

1974-01-01

A method for preparing a natural gas storage vessel for shipment is presented. The gas is stored at 3,000 pounds per square inch. The safety precautions to be observed are emphasized. The equipment and process for purging the tank and sampling the exit gas flow are described. A diagram of the pressure vessel and the equipment is provided.

The Role of Concurrent Chemical and Physical Processes in Determining the Maximum Use Temperature of Thermosetting Polymers for Aerospace Applications

DTIC Science & Technology

2011-04-04

ore purchased f rom Lonz a, AG and used a s-received. Copper(I I) acetoacetonate from R OC/RIC and nony lphenol (Technical Grade) fro m Aldrich...were combined to produce a liquid catalyst. Sample Preparation. Catalyst batc hes were prepared by blending 30 weight parts nony lphenol with

Determination of free sulfites (SO3-2) in dried fruits processed with sulfur dioxide by ion chromatography through anion exchange column and conductivity detection.

PubMed

Liao, Benjamin S; Sram, Jacqueline C; Files, Darin J

2013-01-01

A simple and effective anion ion chromatography (IC) method with anion exchange column and conductivity detector has been developed to determine free sulfites (SO3-2) in dried fruits processed with sulfur dioxide. No oxidation agent, such as hydrogen peroxide, is used to convert sulfites to sulfates for IC analysis. In addition, no stabilizing agent, such as formaldehyde, fructose or EDTA, is required during the sample extraction. This method uses aqueous 0.2 N NaOH as the solvent for standard preparation and sample extraction. The sulfites, either prepared from standard sodium sulfite powder or extracted from food samples, are presumed to be unbound SO3-2 in aqueous 0.2 N NaOH (pH > 13), because the bound sulfites in the sample matrix are released at pH > 10. In this study, sulfites in the standard solutions were stable at room temperature (i.e., 15-25 degrees C) for up to 12 days. The lowest standard of the linear calibration curve is set at 1.59 microg/mL SO3-2 (equivalent to 6.36 microg/g sample with no dilution) for analysis of processed dried fruits that would contain high levels (>1000 microg/g) of sulfites. As a consequence, this method typically requires significant dilution of the sample extract. Samples are prepared with a simple procedure of sample compositing, extraction with aqueous 0.2 N NaOH, centrifugation, dilution as needed, and filtration prior to IC. The sulfites in these sample extracts are stable at room temperature for up to 20 h. Using anion IC, the sulfites are eluted under isocratic conditions with 10 mM aqueous sodium carbonate solution as the mobile phase passing through an anion exchange column. The sulfites are easily separated, with an analysis run time of 18 min, regardless of the dried fruit matrix. Recoveries from samples spiked with sodium sulfites were demonstrated to be between 81 and 105% for five different fruit matrixes (apricot, golden grape, white peach, fig, and mango). Overall, this method is simple to perform and effective for the determination of high levels of sulfites in dried fruits.

Magnetic properties of Mn0.1Mg0.2TM0.7Fe2O4 (TM = Zn, Co, or Ni) prepared by hydrothermal processes: The effects of crystal size and chemical composition

NASA Astrophysics Data System (ADS)

Nhlapo, T. A.; Msomi, J. Z.; Moyo, T.

2018-02-01

Nano-crystalline Zn-, Co-, and Ni-substituted Mn-Mg ferrites were prepared by hydrothermal process and annealed at 1100 °C. Annealing conditions are critical on the crystalline phase. TEM and XRD data reveal particle sizes between 8 nm and 15 nm for the as-prepared fine powders, which increase to about 73 nm after sintering at 1100 °C. Mӧssbauer spectra show well resolved magnetic splitting in bulk samples. The as-prepared fine powders show weak hyperfine splitting and broad central doublets associated with fine particles. Magnetization data reveal a high coercive field at about 300 K of about 945 Oe in the Co-based nanosized oxide, which reduces to about 360 Oe after thermal annealing at 1100 °C. The magnetization curves of Zn- and Ni-based samples show much lower coercive fields indicative of superparamagnetic nanoparticles. The crystallite size and chemical composition have significant effects on the properties of Mn0.1Mg0.2(Zn,Co,Ni)0.7Fe2O4 investigated.

Preparation of Total RNA from Fission Yeast.

PubMed

Bähler, Jürg; Wise, Jo Ann

2017-04-03

Treatment with hot phenol breaks open fission yeast cells and begins to strip away bound proteins from RNA. Deproteinization is completed by multiple extractions with chloroform/isoamyl alcohol and separation of the aqueous and organic phases using MaXtract gel, an inert material that acts as a physical barrier between the phases. The final step is concentration of the RNA by ethanol precipitation. The protocol can be used to prepare RNA from several cultures grown in parallel, but it is important not to process too many samples at once because delays can be detrimental to RNA quality. A reasonable number of samples to process at once would be three to four for microarray or RNA sequencing analyses and six for preliminary investigations of mutants implicated in RNA metabolism. © 2017 Cold Spring Harbor Laboratory Press.

Antigen recovery and preservation using the microwave irradiation of biological samples for transmission electron microscopy analysis.

PubMed

Aïoun, Josiane; Chat, Sophie; Bordat, Christian; Péchoux, Christine

2013-01-01

Most studies using microwave irradiation (MWI) for the preparation of tissue samples have reported an improvement in structural integrity. However, there have been few studies on the effect of microwave (MW) on antigen preservation during sample preparation prior to immunolocalization. This report documents our experience of specimen preparation using an automatic microwave apparatus to obtain antigen preservation and retrieval. We tested the effects of MW processing vs. conventional procedures on the morphology and antigenicity of two different tissues: the brain and mammary gland, whose chemical composition and anatomical organization are quite different. We chose to locate the transcription factor PPARβ/δ using immunocytochemistry on brain tissue sections from hamsters. Antigen retrieval protocols involving MWI were used to restore immunoreactivity. We also studied the efficiency of the ultrastructural immunolocalization of both PPARγ and caveolin-1 following MWI vs. conventional treatment, on mammary gland tissue from mice at 10 days of lactation. Our findings showed that the treatment of tissue samples with MWI, in the context of a process lasting just a few hours from fixation to immunolocalization, enabled similar, or even better, results than conventional protocols. The quantification of immunolabeling for cav-1 indicated an increase in density of up to three-fold in tissues processed in the microwave oven. Furthermore, MW treatment permitted the localization of PPARβ/δ in glutaraldehyde-fixed specimens, which was impossible in the absence of MWI. This study thus showed that techniques involving the use of microwaves could largely improve both ultrastructure and immunodetection. Copyright © 2013 Elsevier Ltd. All rights reserved.

Microwave Processing of Crowns from Winter Cereals for Light Microscopy.

USDA-ARS?s Scientific Manuscript database

Microwave processing of tissue considerably shortens the time it takes to prepare samples for light and electron microscopy. However, plant tissues from different species and different regions of the plant respond differently making it impossible to use a single protocol for all plant tissue. The ...

Powdered hide model for vegetable tanning

USDA-ARS?s Scientific Manuscript database

Powdered hide samples for this initial study of vegetable tanning were prepared from hides that were dehaired by a typical sulfide or oxidative process, and carried through the delime/bate step of a tanning process. In this study, we report on interactions of the vegetable tannin, quebracho with th...

Evaluation of the Separability of Monodisperse Polystyrene Latex Microspheres in a Continuous Flow Electrophoresis System

NASA Technical Reports Server (NTRS)

Williams, G., Jr.

1983-01-01

The continuous flow electrophoresis system makes electrophoresis possible in a free flowing film of aqueous electrolyte medium. The sample is introduced at one end of the chamber and is subjected to a lateral dc field. This process separates the sample into fractions since each component has a distinctive electrophoric mobility. Evaluations were made of sample conductivity and buffer conductivity as they affect sample band spread and separation using the Continuous Particle Electrophoresis (CPE) system. Samples were prepared from mixtures of 5 percent and 1 percent polystyrene latex (PSL) microspheres which were .4, .56 and .7 microns in diameter. These were prepared in electrolyte media 1x and 3x the conductivity of the curtain buffer, approximately 150 and 450 micro mhos/cm. Samples with matched conductivities produced greater resolution and less band spread than those with 3x the conductivity of the curtain buffer.

Automation of laboratory testing for infectious diseases using the polymerase chain reaction-- our past, our present, our future.

PubMed

Jungkind, D

2001-01-01

While it is an extremely powerful and versatile assay method, polymerase chain reaction (PCR) can be a labor-intensive process. Since the advent of commercial test kits from Roche and the semi-automated microwell Amplicor system, PCR has become an increasingly useful and widespread clinical tool. However, more widespread acceptance of molecular testing will depend upon automation that allows molecular assays to enter the routine clinical laboratory. The forces driving the need for automated PCR are the requirements for diagnosis and treatment of chronic viral diseases, economic pressures to develop more automated and less expensive test procedures similar to those in the clinical chemistry laboratories, and a shortage in many areas of qualified laboratory personnel trained in the types of manual procedures used in past decades. The automated Roche COBAS AMPLICOR system has automated the amplification and detection process. Specimen preparation remains the most labor-intensive part of the PCR testing process, accounting for the majority of the hands-on-time in most of the assays. A new automated specimen preparation system, the COBAS AmpliPrep, was evaluated. The system automatically releases the target nucleic acid, captures the target with specific oligonucleotide probes, which become attached to magnetic beads via a biotin-streptavidin binding reaction. Once attached to the beads, the target is purified and concentrated automatically. Results of 298 qualitative and 57 quantitative samples representing a wide range of virus concentrations analyzed after the COBAS AmpliPrep and manual specimen preparation methods, showed that there was no significant difference in qualitative or quantitative hepatitis C virus (HCV) assay performance, respectively. The AmpliPrep instrument decreased the time required to prepare serum or plasma samples for HCV PCR to under 1 min per sample. This was a decrease of 76% compared to the manual specimen preparation method. Systems that can analyze more samples with higher throughput and that can answer more questions about the nature of the microbes that we can presently only detect and quantitate will be needed in the future.

Characterization Data Package for Containerized Sludge Samples Collected from Engineered Container SCS-CON-210

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fountain, Matthew S.; Fiskum, Sandra K.; Baldwin, David L.

This data package contains the K Basin sludge characterization results obtained by Pacific Northwest National Laboratory during processing and analysis of four sludge core samples collected from Engineered Container SCS-CON-210 in 2010 as requested by CH2M Hill Plateau Remediation Company. Sample processing requirements, analytes of interest, detection limits, and quality control sample requirements are defined in the KBC-33786, Rev. 2. The core processing scope included reconstitution of a sludge core sample distributed among four to six 4-L polypropylene bottles into a single container. The reconstituted core sample was then mixed and subsampled to support a variety of characterization activities. Additionalmore » core sludge subsamples were combined to prepare a container composite. The container composite was fractionated by wet sieving through a 2,000 micron mesh and a 500-micron mesh sieve. Each sieve fraction was sampled to support a suite of analyses. The core composite analysis scope included density determination, radioisotope analysis, and metals analysis, including the Waste Isolation Pilot Plant Hazardous Waste Facility Permit metals (with the exception of mercury). The container composite analysis included most of the core composite analysis scope plus particle size distribution, particle density, rheology, and crystalline phase identification. A summary of the received samples, core sample reconstitution and subsampling activities, container composite preparation and subsampling activities, physical properties, and analytical results are presented. Supporting data and documentation are provided in the appendices. There were no cases of sample or data loss and all of the available samples and data are reported as required by the Quality Assurance Project Plan/Sampling and Analysis Plan.« less

Comparison of mounting methods for the evaluation of fibers by phase contrast microscopy.

PubMed

Lee, Eun Gyung; Pang, Thomas W S; Nelson, John; Andrew, Mike; Harper, Martin

2011-07-01

The objectives of this study were to evaluate mounting methods for fiber examination of air sample filters by phase contrast microscopy (PCM) and to evaluate differences in fiber counts that might be due to fiber movement. Acetone/triacetin (AT) with various amounts of triacetin and acetone/Euparal (AE) where the mounting medium was placed between the cleared filter wedge and the coverslip were tested as a function of time. Field sample slides collected from a taconite iron-ore processing mill, a tremolitic talc-ore processing mill, and from around a crusher in a meta-basalt stone quarry were prepared with relocatable coverslips to revisit the same field areas on the slides. For each slide, three or four field areas were randomly selected and pictures were taken every 2 weeks to determine any sign of fiber movement over time. For 11 AT slides (named as AT-3.5) prepared with 3.5 μl of the mounting medium according to the NIOSH 7400 method, no fiber movements were detected over 59 weeks. On the other hand, AT slides prepared with larger quantities (10, 15, and 20 μl) of the mounting medium (named as AT-10) and AE slides prepared with ∼10 μl mounting medium showed fiber movement from the eighth day at the earliest. Fiber movement began earlier for the slides mounted with excess triacetin than for those mounted with Euparal. The sample slide storage method, either vertically or horizontally, did not seem to accelerate fiber movement. Additionally, two other modified methods, dimethylformamide solution/Euparal (mDE) and dimethylformamide solution/triacetin (mDT), were also prepared where the mounting medium was placed between the cleared filter wedge and the glass slide. The findings of fiber movements were similar; when 3.5 μl of triacetin was used for the mDT slides, fiber movements were not detected, while fibers on slides prepared with 10 μl triacetin (mDT-10) moved around. No fiber movements were observed for the mDE slides at any time during 59 weeks. Once fiber movement started, fibers moved over distances measured from 4 μm and up to >1000 μm within 22 weeks. However, since then, no further fiber movements have been observed in any field sample slides. Additional sample slides, two Amosite and two chrysotile, were prepared from Union for International Cancer Control (UICC) samples using the AT method with 5 μl triacetin mounting medium. Fiber movements were also observed in these samples; chrysotile fibers began to migrate in 3 weeks, while Amosite fiber movement started after 3 months. Although fiber movement was observed for the AT-10, AE, and mDT-10 sample slides, fiber counts were not significantly different from AT-3.5 and mDE samples that exhibited no fiber movement. Although fiber counts would not be significantly changed by fiber movement, the type and amount of mounting medium for sample slide preparation remains critical for issues such as quality assurance and training of analysts by revisiting the same fibers.

Nanostructured ZnO films with various morphologies prepared by ultrasonic spray pyrolysis and its growing process

NASA Astrophysics Data System (ADS)

Ma, H. L.; Liu, Z. W.; Zeng, D. C.; Zhong, M. L.; Yu, H. Y.; Mikmekova, E.

2013-10-01

Nanostructured ZnO films were prepared by the ultrasonic spray pyrolysis method using Zn(CH3COO)2·2H2O as a precursor. The effects of substrate temperature (Ts) on the morphology and properties were systematically studied. As the Ts increased from 430 °C to 610 °C, the morphology of the film transforms from closed packed nanosheets to dense nanocrystalline film and then to hexagonal nanorod array. The dense film formed at a temperature of 550 °C has the lowest electric resistivity and highest carrier concentration. The optical transmittance for all prepared samples was higher than 90%. The photoluminescence (PL) properties varied with the Ts due to the internal defect difference. The growth mechanism of ZnO film involves island growth and diffusion, which was evident by observing the samples prepared at various times.

Synthesis, characterization and application of ion imprinted polymeric nanobeads for highly selective preconcentration and spectrophotometric determination of Ni2 + ion in water samples

NASA Astrophysics Data System (ADS)

Rajabi, Hamid Reza; Razmpour, Saham

2016-01-01

Here, the researchers report on the synthesis of ion imprinted polymeric (IIP) nanoparticles using a thermal polymerization strategy, and their usage for the separation of Ni2 + ion from water samples. The prepared Ni-IIP was characterized by colorimetry, FT-IR spectroscopy, and scanning electron microscopy. It was found that the particle size of the prepared particle to be 50-70 nm in diameter with the highly selective binding capability for Ni2 + ion, with reasonable adsorption and desorption process. After preconcentration, bound ions can be eluted with an aqueous solution of hydrochloric acid, after their complexation with dimethylglyoxime, these ions can be quantified by UV-Vis absorption spectrophotometry. The effect of various parameters on the extraction efficiency including pH of sample solution, adsorption and leaching times, initial sample volume, concentration and volume of eluent were investigated. In selectivity study, it was found that imprinting causes increased affinity of the prepared IIP toward Ni2 + ion over other ions such as Na+, K+, Ag+, Co2 +, Cu2 +, Cd2 +, Hg2 +, Pb2 +, Zn2 +, Mn2 +, Mg2 +, Cr3 +, and Fe3 +. The prepared IIP can be used and regenerated for at least eight times without any significant decrease in binding affinities. The prepared IIP is considered to be promising and selective sorbent for solid-phase extraction and preconcentration of Ni2 + ion from different water samples.

The Resin-Embedded Cornea Prepared Via Rapid Processing Protocol : A Good Histomorphometric Target for Clinical Investigation in Ophthalmology and Optometry

PubMed Central

Cheah, Pike See; Mohidin, Norhani; Mohd Ali, Bariah; Maung, Myint; Latif, Azian Abdul

2008-01-01

This study illustrates and quantifies the changes on corneal tissue between the paraffin-embedded and resin-embedded blocks and thus, selects a better target in investigational ophthalmology and optometry via light microscopy. Corneas of two cynomolgus monkeys (Macaca fascicularis) were used in this study. The formalin-fixed cornea was prepared in paraffin block via the conventional tissue processing protocol (4-day protocol) and stained with haematoxylin and eosin. The glutaraldehyde-fixed cornea was prepared in resin block via the rapid and modified tissue processing procedure (1.2-day protocol) and stained with toluidine blue. The paraffin-embedded sample exhibits various undesired tissue damage and artifact such as thinner epithelium (due to the substantial volumic extraction from the tissue), thicker stroma layer (due to the separation of lamellae and the presence of voids) and the distorted endothelium. In contrast, the resin-embedded corneal tissue has demonstrated satisfactory corneal ultrastructural preservation. The rapid and modified tissue processing method for preparing the resin-embedded is particularly beneficial to accelerate the microscopic evaluation in ophthalmology and optometry. PMID:22570589

Simple Sodium Dodecyl Sulfate-Assisted Sample Preparation Method for LC-MS-based Proteomic Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhou, Jianying; Dann, Geoffrey P.; Shi, Tujin

2012-03-10

Sodium dodecyl sulfate (SDS) is one of the most popular laboratory reagents used for highly efficient biological sample extraction; however, SDS presents a significant challenge to LC-MS-based proteomic analyses due to its severe interference with reversed-phase LC separations and electrospray ionization interfaces. This study reports a simple SDS-assisted proteomic sample preparation method facilitated by a novel peptide-level SDS removal protocol. After SDS-assisted protein extraction and digestion, SDS was effectively (>99.9%) removed from peptides through ion substitution-mediated DS- precipitation with potassium chloride (KCl) followed by {approx}10 min centrifugation. Excellent peptide recovery (>95%) was observed for less than 20 {mu}g of peptides.more » Further experiments demonstrated the compatibility of this protocol with LC-MS/MS analyses. The resulting proteome coverage from this SDS-assisted protocol was comparable to or better than those obtained from other standard proteomic preparation methods in both mammalian tissues and bacterial samples. These results suggest that this SDS-assisted protocol is a practical, simple, and broadly applicable proteomic sample processing method, which can be particularly useful when dealing with samples difficult to solubilize by other methods.« less

Integrated massively parallel sequencing of 15 autosomal STRs and Amelogenin using a simplified library preparation approach.

PubMed

Xue, Jian; Wu, Riga; Pan, Yajiao; Wang, Shunxia; Qu, Baowang; Qin, Ying; Shi, Yuequn; Zhang, Chuchu; Li, Ran; Zhang, Liyan; Zhou, Cheng; Sun, Hongyu

2018-04-02

Massively parallel sequencing (MPS) technologies, also termed as next-generation sequencing (NGS), are becoming increasingly popular in study of short tandem repeats (STR). However, current library preparation methods are usually based on ligation or two-round PCR that requires more steps, making it time-consuming (about 2 days), laborious and expensive. In this study, a 16-plex STR typing system was designed with fusion primer strategy based on the Ion Torrent S5 XL platform which could effectively resolve the above challenges for forensic DNA database-type samples (bloodstains, saliva stains, etc.). The efficiency of this system was tested in 253 Han Chinese participants. The libraries were prepared without DNA isolation and adapter ligation, and the whole process only required approximately 5 h. The proportion of thoroughly genotyped samples in which all the 16 loci were successfully genotyped was 86% (220/256). Of the samples, 99.7% showed 100% concordance between NGS-based STR typing and capillary electrophoresis (CE)-based STR typing. The inconsistency might have been caused by off-ladder alleles and mutations in primer binding sites. Overall, this panel enabled the large-scale genotyping of the DNA samples with controlled quality and quantity because it is a simple, operation-friendly process flow that saves labor, time and costs. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nucleation of biomimetic apatite in synthetic body fluids: dense and porous scaffold development.

PubMed

Landi, Elena; Tampieri, Anna; Celotti, Giancarlo; Langenati, Ratih; Sandri, Monica; Sprio, Simone

2005-06-01

The effectiveness of synthetic body fluids (SBF) as biomimetic sources to synthesize carbonated hydroxyapatite (CHA) powder similar to the biological inorganic phase, in terms of composition and microstructure, was investigated. CHA apatite powders were prepared following two widely experimented routes: (1) calcium nitrate tetrahydrate and diammonium hydrogen phosphate and (2) calcium hydroxide and ortophosphoric acid, but using SBF as synthesis medium instead of pure water. The characteristics of the as-prepared powders were compared, also with the features of apatite powders synthesized via pure water-based classical methods. The powder thermal resistance and behaviour during densification were studied together with the mechanical properties of the dense samples. The sponge impregnation process was used to prepare porous samples having morphological and mechanical characteristics suitable for bone substitution. Using this novel synthesis was it possible to prepare nanosized (approximately equal to 20 nm), pure, carbonate apatite powder containing Mg, Na, K ions, with morphological and compositional features mimicking natural apatite and with improved thermal properties. After sintering at 1250 degrees C the carbonate-free apatite porous samples showed a surprising, high compressive strength together with a biomimetic morphology.

X-Ray Diffraction of different samples of Swarna Makshika Bhasma.

PubMed

Gupta, Ramesh Kumar; Lakshmi, Vijay; Jha, Chandra Bhushan

2015-01-01

Shodhana and Marana are a series of complex procedures that identify the undesirable effects of heavy metals/minerals and convert them into absorbable and assimilable forms. Study on the analytical levels is essential to evaluate the structural and chemical changes that take place during and after following such procedures as described in major classical texts to understand the mystery behind these processes. X-Ray Diffraction (XRD) helps to identify and characterize minerals/metals and fix up the particular characteristics pattern of prepared Bhasma. To evaluate the chemical changes in Swarna Makshika Bhasma prepared by using different media and methods. In this study, raw Swarna Makshika, purified Swarna Makshika and four types of Swarna Makshika Bhasma prepared by using different media and methods were analyzed by XRD study. XRD study of different samples revealed strongest peaks of iron oxide in Bhasma. Other phases of Cu2O, FeS2, Cu2S, FeSO4, etc., were also identified in many of the samples. XRD study revealed that Swarna Makshika Bhasma prepared by Kupipakwa method is better, convenient, and can save time.

Integrated process development-a robust, rapid method for inclusion body harvesting and processing at the microscale level.

PubMed

Walther, Cornelia; Kellner, Martin; Berkemeyer, Matthias; Brocard, Cécile; Dürauer, Astrid

2017-10-21

Escherichia coli stores large amounts of highly pure product within inclusion bodies (IBs). To take advantage of this beneficial feature, after cell disintegration, the first step to optimal product recovery is efficient IB preparation. This step is also important in evaluating upstream optimization and process development, due to the potential impact of bioprocessing conditions on product quality and on the nanoscale properties of IBs. Proper IB preparation is often neglected, due to laboratory-scale methods requiring large amounts of materials and labor. Miniaturization and parallelization can accelerate analyses of individual processing steps and provide a deeper understanding of up- and downstream processing interdependencies. Consequently, reproducible, predictive microscale methods are in demand. In the present study, we complemented a recently established high-throughput cell disruption method with a microscale method for preparing purified IBs. This preparation provided results comparable to laboratory-scale IB processing, regarding impurity depletion, and product loss. Furthermore, with this method, we performed a "design of experiments" study to demonstrate the influence of fermentation conditions on the performance of subsequent downstream steps and product quality. We showed that this approach provided a 300-fold reduction in material consumption for each fermentation condition and a 24-fold reduction in processing time for 24 samples.

A low energy muon spin rotation and point contact tunneling study of niobium films prepared for superconducting cavities

NASA Astrophysics Data System (ADS)

Junginger, Tobias; Calatroni, S.; Sublet, A.; Terenziani, G.; Prokscha, T.; Salman, Z.; Suter, A.; Proslier, T.; Zasadzinski, J.

2017-12-01

Point contact tunneling and low energy muon spin rotation are used to probe, on the same samples, the surface superconducting properties of micrometer thick niobium films deposited onto copper substrates using different sputtering techniques: diode, dc magnetron and HIPIMS. The combined results are compared to radio-frequency tests performances of RF cavities made with the same processes. Degraded surface superconducting properties are found to correlate to lower quality factors and stronger Q-slope. In addition, both techniques find evidence for surface paramagnetism on all samples and particularly on Nb films prepared by HIPIMS.

Enzymatic induction of supramolecular order and bioactivity

NASA Astrophysics Data System (ADS)

Yang, Chengbiao; Ren, Xinrui; Ding, Dan; Wang, Ling; Yang, Zhimou

2016-05-01

We showed in this study that enzymatic triggering is a totally different pathway for the preparation of self-assembling nanomaterials to the heating-cooling process. Because the molecules were under lower energy levels and the molecular conformation was more ordered during the enzymatic triggeration under mild conditions, nanomaterials with higher supramolecular order could be obtained through biocatalytic control. In this study, nanoparticles were obtained by an enzymatic reaction and nanofibers were observed through the heating-cooling process. We observed a distinct trough at 318 nm from the CD spectrum of a particle sample but not a fiber sample, suggesting the long range arrangement of molecules and helicity in the nanoparticles. The nanoparticles with higher supramolecular order possessed much better potency as a protein vaccine adjuvant because it accelerated the DC maturation and elicited stronger T-cells cytokine production than the nanofibers. Our study demonstrated that biocatalytic triggering is a useful method for preparing supramolecular nanomaterials with higher supramolecular order and probably better bioactivity.We showed in this study that enzymatic triggering is a totally different pathway for the preparation of self-assembling nanomaterials to the heating-cooling process. Because the molecules were under lower energy levels and the molecular conformation was more ordered during the enzymatic triggeration under mild conditions, nanomaterials with higher supramolecular order could be obtained through biocatalytic control. In this study, nanoparticles were obtained by an enzymatic reaction and nanofibers were observed through the heating-cooling process. We observed a distinct trough at 318 nm from the CD spectrum of a particle sample but not a fiber sample, suggesting the long range arrangement of molecules and helicity in the nanoparticles. The nanoparticles with higher supramolecular order possessed much better potency as a protein vaccine adjuvant because it accelerated the DC maturation and elicited stronger T-cells cytokine production than the nanofibers. Our study demonstrated that biocatalytic triggering is a useful method for preparing supramolecular nanomaterials with higher supramolecular order and probably better bioactivity. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr02330d

Time of flight secondary ion mass spectrometry of bone—Impact of sample preparation and measurement conditions

PubMed Central

Henss, Anja; Hild, Anne; Rohnke, Marcus; Wenisch, Sabine; Janek, Juergen

2015-01-01

Time of flight secondary ion mass spectrometry (ToF-SIMS) enables the simultaneous detection of organic and inorganic ions and fragments with high mass and spatial resolution. Due to recent technical developments, ToF-SIMS has been increasingly applied in the life sciences where sample preparation plays an eminent role for the quality of the analytical results. This paper focusses on sample preparation of bone tissue and its impact on ToF-SIMS analysis. The analysis of bone is important for the understanding of bone diseases and the development of replacement materials and new drugs for the cure of diseased bone. The main purpose of this paper is to find out which preparation process is best suited for ToF-SIMS analysis of bone tissue in order to obtain reliable and reproducible analytical results. The influence of the embedding process on the different components of bone is evaluated using principal component analysis. It is shown that epoxy resin as well as methacrylate based plastics (Epon and Technovit) as embedding materials do not infiltrate the mineralized tissue and that cut sections are better suited for the ToF-SIMS analysis than ground sections. In case of ground samples, a resin layer is smeared over the sample surface due to the polishing step and overlap of peaks is found. Beside some signals of fatty acids in the negative ion mode, the analysis of native, not embedded samples does not provide any advantage. The influence of bismuth bombardment and O2 flooding on the signal intensity of organic and inorganic fragments due to the variation of the ionization probability is additionally discussed. As C60 sputtering has to be applied to remove the smeared resin layer, its effect especially on the organic fragments of the bone is analyzed and described herein. PMID:26253108

Time of flight secondary ion mass spectrometry of bone-Impact of sample preparation and measurement conditions.

PubMed

Henss, Anja; Hild, Anne; Rohnke, Marcus; Wenisch, Sabine; Janek, Juergen

2015-06-07

Time of flight secondary ion mass spectrometry (ToF-SIMS) enables the simultaneous detection of organic and inorganic ions and fragments with high mass and spatial resolution. Due to recent technical developments, ToF-SIMS has been increasingly applied in the life sciences where sample preparation plays an eminent role for the quality of the analytical results. This paper focusses on sample preparation of bone tissue and its impact on ToF-SIMS analysis. The analysis of bone is important for the understanding of bone diseases and the development of replacement materials and new drugs for the cure of diseased bone. The main purpose of this paper is to find out which preparation process is best suited for ToF-SIMS analysis of bone tissue in order to obtain reliable and reproducible analytical results. The influence of the embedding process on the different components of bone is evaluated using principal component analysis. It is shown that epoxy resin as well as methacrylate based plastics (Epon and Technovit) as embedding materials do not infiltrate the mineralized tissue and that cut sections are better suited for the ToF-SIMS analysis than ground sections. In case of ground samples, a resin layer is smeared over the sample surface due to the polishing step and overlap of peaks is found. Beside some signals of fatty acids in the negative ion mode, the analysis of native, not embedded samples does not provide any advantage. The influence of bismuth bombardment and O2 flooding on the signal intensity of organic and inorganic fragments due to the variation of the ionization probability is additionally discussed. As C60 sputtering has to be applied to remove the smeared resin layer, its effect especially on the organic fragments of the bone is analyzed and described herein.

32 CFR Appendix B to Part 1290 - Ticket Sample-A Parking Violation

Code of Federal Regulations, 2010 CFR

2010-07-01

... 32 National Defense 6 2010-07-01 2010-07-01 false Ticket Sample-A Parking Violation B Appendix B to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S. DISTRICT COURTS Pt...

32 CFR Appendix C to Part 1290 - Ticket Sample-A Moving Violation

Code of Federal Regulations, 2010 CFR

2010-07-01

... 32 National Defense 6 2010-07-01 2010-07-01 false Ticket Sample-A Moving Violation C Appendix C to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S. DISTRICT COURTS Pt...

32 CFR Appendix B to Part 1290 - Ticket Sample-A Parking Violation

Code of Federal Regulations, 2014 CFR

2014-07-01

... 32 National Defense 6 2014-07-01 2014-07-01 false Ticket Sample-A Parking Violation B Appendix B to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S. DISTRICT COURTS Pt...

32 CFR Appendix C to Part 1290 - Ticket Sample-A Moving Violation

Code of Federal Regulations, 2014 CFR

2014-07-01

... 32 National Defense 6 2014-07-01 2014-07-01 false Ticket Sample-A Moving Violation C Appendix C to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S. DISTRICT COURTS Pt...

32 CFR Appendix B to Part 1290 - Ticket Sample-A Parking Violation

Code of Federal Regulations, 2013 CFR

2013-07-01

... 32 National Defense 6 2013-07-01 2013-07-01 false Ticket Sample-A Parking Violation B Appendix B to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S. DISTRICT COURTS Pt...

32 CFR Appendix B to Part 1290 - Ticket Sample-A Parking Violation

Code of Federal Regulations, 2012 CFR

2012-07-01

... 32 National Defense 6 2012-07-01 2012-07-01 false Ticket Sample-A Parking Violation B Appendix B to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S. DISTRICT COURTS Pt...

32 CFR Appendix C to Part 1290 - Ticket Sample-A Moving Violation

Code of Federal Regulations, 2012 CFR

2012-07-01

... 32 National Defense 6 2012-07-01 2012-07-01 false Ticket Sample-A Moving Violation C Appendix C to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S. DISTRICT COURTS Pt...

32 CFR Appendix B to Part 1290 - Ticket Sample-A Parking Violation

Code of Federal Regulations, 2011 CFR

2011-07-01

... 32 National Defense 6 2011-07-01 2011-07-01 false Ticket Sample-A Parking Violation B Appendix B to Part 1290 National Defense Other Regulations Relating to National Defense DEFENSE LOGISTICS AGENCY MISCELLANEOUS PREPARING AND PROCESSING MINOR OFFENSES AND VIOLATION NOTICES REFERRED TO U.S. DISTRICT COURTS Pt...

An Examination of the Space Weathering Patina of Lunar Rock 76015

NASA Technical Reports Server (NTRS)

Noble, S.; Chrisoffersen, R.; Rahman, Z.

2011-01-01

Space weathering discussions have generally centered around soils but exposed rocks will also incur the effects of weathering. Rocks have much longer surface lifetimes than an individual soil grain and thus record a longer history of exposure. By studying the weathering products which have built up on a rock surface, we can gain a deeper perspective on the weathering process and better assess the relative importance of various weathering components. The weathered coating, or patina, of the lunar rock 76015 has been previously studied under SEM and also by TEM using ultramicrotome sample preparation methods. However, to really understand the products involved in creating these coatings, it is helpful to examine the patina in cross section, something which is now possible though the use of Focused Ion Beam (FIB) sample prep techniques, which allows us to preserve intact the delicate stratigraphy of the patina coating and provides a unique cross-sectional view of the space weathering process. Several samples have been prepared from the rock and the coatings are found to be quite variable in thickness and composition from one sample to the next.

A Highly Flexible, Automated System Providing Reliable Sample Preparation in Element- and Structure-Specific Measurements.

PubMed

Vorberg, Ellen; Fleischer, Heidi; Junginger, Steffen; Liu, Hui; Stoll, Norbert; Thurow, Kerstin

2016-10-01

Life science areas require specific sample pretreatment to increase the concentration of the analytes and/or to convert the analytes into an appropriate form for the detection and separation systems. Various workstations are commercially available, allowing for automated biological sample pretreatment. Nevertheless, due to the required temperature, pressure, and volume conditions in typical element and structure-specific measurements, automated platforms are not suitable for analytical processes. Thus, the purpose of the presented investigation was the design, realization, and evaluation of an automated system ensuring high-precision sample preparation for a variety of analytical measurements. The developed system has to enable system adaption and high performance flexibility. Furthermore, the system has to be capable of dealing with the wide range of required vessels simultaneously, allowing for less cost and time-consuming process steps. However, the system's functionality has been confirmed in various validation sequences. Using element-specific measurements, the automated system was up to 25% more precise compared to the manual procedure and as precise as the manual procedure using structure-specific measurements. © 2015 Society for Laboratory Automation and Screening.

Mechanistic study of the influence of pyrolysis conditions on potassium speciation in biochar "preparation-application" process.

PubMed

Tan, Zhongxin; Liu, Liyun; Zhang, Limei; Huang, Qiaoyun

2017-12-01

Biochar samples produced from rice straw by pyrolysis at different temperatures (400°C and 800°C) and under different atmospheres (N 2 and CO 2 ) were applied to lettuce growth in a 'preparation-application' system. The conversion of potassium in the prepared biochar and the effect of the temperature used for pyrolysis on the bioavailability of potassium in the biochar were investigated. Root samples from lettuce plants grown with and without application of biochar were assayed by X-ray photoelectron spectroscopy (XPS). The optimal conditions for preparation of biochar to achieve the maximum bioavailability of potassium (i.e. for returning biochar to soil) were thus determined. Complex-K, a stable speciation of potassium in rice straw, was transformed into potassium sulfate, potassium nitrate, potassium nitrite, and potassium chloride after oxygen-limited pyrolysis. The aforementioned ionic-state potassium species can be directly absorbed and used by plants. Decomposition of the stable speciation of potassium during the pyrolysis process was more effective at higher temperature, whereas the pyrolysis atmosphere (CO 2 and N 2 ) had little effect on the quality of the biochar. Based on the potassium speciation in the biochar, the preparation cost, and the plant growth and rigor after the application of returning biochar to soil, 400°C and CO 2 atmosphere were the most appropriate conditions for preparation of biochar. Copyright © 2017. Published by Elsevier B.V.

Fabric phase sorptive extraction followed by UHPLC-MS/MS for the analysis of benzotriazole UV stabilizers in sewage samples.

PubMed

Montesdeoca-Esponda, Sarah; Sosa-Ferrera, Zoraida; Kabir, Abuzar; Furton, Kenneth G; Santana-Rodríguez, José Juan

2015-10-01

A fast and sensitive sample preparation strategy using fabric phase sorptive extraction followed by ultra-high-performance liquid chromatography and tandem mass spectrometry detection has been developed to analyse benzotriazole UV stabilizer compounds in aqueous samples. Benzotriazole UV stabilizer compounds are a group of compounds added to sunscreens and other personal care products which may present detrimental effects to aquatic ecosystems. Fabric phase sorptive extraction is a novel solvent minimized sample preparation approach that integrates the advantages of sol-gel derived hybrid inorganic-organic nanocomposite sorbents and the flexible, permeable and hydrophobic surface chemistry of polyester fabric. It is a highly sensitive, fast, efficient and inexpensive device that can be reused and does not suffer from coating damage, unlike SPME fibres or stir bars. In this paper, we optimized the extraction of seven benzotriazole UV filters evaluating the majority of the parameters involved in the extraction process, such as sorbent chemistry selection, extraction time, back-extraction solvent, back-extraction time and the impact of ionic strength. Under the optimized conditions, fabric phase sorptive extraction allows enrichment factors of 10 times with detection limits ranging from 6.01 to 60.7 ng L(-1) and intra- and inter-day % RSDs lower than 11 and 30 % for all compounds, respectively. The optimized sample preparation technique followed by ultra-high-performance liquid chromatography and tandem mass spectrometry detection was applied to determine the target analytes in sewage samples from wastewater treatment plants with different purification processes of Gran Canaria Island (Spain). Two UV stabilizer compounds were measured in ranges 17.0-60.5 ng mL(-1) (UV 328) and 69.3-99.2 ng mL(-1) (UV 360) in the three sewage water samples analysed.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Egorov, Oleg; O'Hara, Matthew J.; Grate, Jay W.

An automated fluidic instrument is described that rapidly determines the total 99Tc content of aged nuclear waste samples, where the matrix is chemically and radiologically complex and the existing speciation of the 99Tc is variable. The monitor links microwave-assisted sample preparation with an automated anion exchange column separation and detection using a flow-through solid scintillator detector. The sample preparation steps acidify the sample, decompose organics, and convert all Tc species to the pertechnetate anion. The column-based anion exchange procedure separates the pertechnetate from the complex sample matrix, so that radiometric detection can provide accurate measurement of 99Tc. We developed amore » preprogrammed spike addition procedure to automatically determine matrix-matched calibration. The overall measurement efficiency that is determined simultaneously provides a self-diagnostic parameter for the radiochemical separation and overall instrument function. Continuous, automated operation was demonstrated over the course of 54 h, which resulted in the analysis of 215 samples plus 54 hly spike-addition samples, with consistent overall measurement efficiency for the operation of the monitor. A sample can be processed and measured automatically in just 12.5 min with a detection limit of 23.5 Bq/mL of 99Tc in low activity waste (0.495 mL sample volume), with better than 10% RSD precision at concentrations above the quantification limit. This rapid automated analysis method was developed to support nuclear waste processing operations planned for the Hanford nuclear site.« less

Fluid control structures in microfluidic devices

DOEpatents

Mathies, Richard A.; Grover, William H.; Skelley, Alison; Lagally, Eric; Liu, Chung N.

2008-11-04

Methods and apparatus for implementing microfluidic analysis devices are provided. A monolithic elastomer membrane associated with an integrated pneumatic manifold allows the placement and actuation of a variety of fluid control structures, such as structures for pumping, isolating, mixing, routing, merging, splitting, preparing, and storing volumes of fluid. The fluid control structures can be used to implement a variety of sample introduction, preparation, processing, and storage techniques.

Fluid control structures in microfluidic devices

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mathies, Richard A.; Grover, William H.; Skelley, Alison

2017-05-09

Methods and apparatus for implementing microfluidic analysis devices are provided. A monolithic elastomer membrane associated with an integrated pneumatic manifold allows the placement and actuation of a variety of fluid control structures, such as structures for pumping, isolating, mixing, routing, merging, splitting, preparing, and storing volumes of fluid. The fluid control structures can be used to implement a variety of sample introduction, preparation, processing, and storage techniques.

Fluid control structures in microfluidic devices

NASA Technical Reports Server (NTRS)

Skelley, Alison (Inventor); Mathies, Richard A. (Inventor); Lagally, Eric (Inventor); Grover, William H. (Inventor); Liu, Chung N. (Inventor)

2008-01-01

Methods and apparatus for implementing microfluidic analysis devices are provided. A monolithic elastomer membrane associated with an integrated pneumatic manifold allows the placement and actuation of a variety of fluid control structures, such as structures for pumping, isolating, mixing, routing, merging, splitting, preparing, and storing volumes of fluid. The fluid control structures can be used to implement a variety of sample introduction, preparation, processing, and storage techniques.

Influence of growth temperature on bulk and surface defects in hybrid lead halide perovskite films

NASA Astrophysics Data System (ADS)

Peng, Weina; Anand, Benoy; Liu, Lihong; Sampat, Siddharth; Bearden, Brandon E.; Malko, Anton V.; Chabal, Yves J.

2016-01-01

The rapid development of perovskite solar cells has focused its attention on defects in perovskites, which are gradually realized to strongly control the device performance. A fundamental understanding is therefore needed for further improvement in this field. Recent efforts have mainly focused on minimizing the surface defects and grain boundaries in thin films. Using time-resolved photoluminescence spectroscopy, we show that bulk defects in perovskite samples prepared using vapor assisted solution process (VASP) play a key role in addition to surface and grain boundary defects. The defect state density of samples prepared at 150 °C (~1017 cm-3) increases by 5 fold at 175 °C even though the average grains size increases slightly, ruling out grain boundary defects as the main mechanism for the observed differences in PL properties upon annealing. Upon surface passivation using water molecules, the PL intensity and lifetime of samples prepared at 200 °C are only partially improved, remaining significantly lower than those prepared at 150 °C. Thus, the present study indicates that the majority of these defect states observed at elevated growth temperatures originates from bulk defects and underscores the importance to control the formation of bulk defects together with grain boundary and surface defects to further improve the optoelectronic properties of perovskites.The rapid development of perovskite solar cells has focused its attention on defects in perovskites, which are gradually realized to strongly control the device performance. A fundamental understanding is therefore needed for further improvement in this field. Recent efforts have mainly focused on minimizing the surface defects and grain boundaries in thin films. Using time-resolved photoluminescence spectroscopy, we show that bulk defects in perovskite samples prepared using vapor assisted solution process (VASP) play a key role in addition to surface and grain boundary defects. The defect state density of samples prepared at 150 °C (~1017 cm-3) increases by 5 fold at 175 °C even though the average grains size increases slightly, ruling out grain boundary defects as the main mechanism for the observed differences in PL properties upon annealing. Upon surface passivation using water molecules, the PL intensity and lifetime of samples prepared at 200 °C are only partially improved, remaining significantly lower than those prepared at 150 °C. Thus, the present study indicates that the majority of these defect states observed at elevated growth temperatures originates from bulk defects and underscores the importance to control the formation of bulk defects together with grain boundary and surface defects to further improve the optoelectronic properties of perovskites. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr06222e

Fully Automated Sample Preparation for Ultrafast N-Glycosylation Analysis of Antibody Therapeutics.

PubMed

Szigeti, Marton; Lew, Clarence; Roby, Keith; Guttman, Andras

2016-04-01

There is a growing demand in the biopharmaceutical industry for high-throughput, large-scale N-glycosylation profiling of therapeutic antibodies in all phases of product development, but especially during clone selection when hundreds of samples should be analyzed in a short period of time to assure their glycosylation-based biological activity. Our group has recently developed a magnetic bead-based protocol for N-glycosylation analysis of glycoproteins to alleviate the hard-to-automate centrifugation and vacuum-centrifugation steps of the currently used protocols. Glycan release, fluorophore labeling, and cleanup were all optimized, resulting in a <4 h magnetic bead-based process with excellent yield and good repeatability. This article demonstrates the next level of this work by automating all steps of the optimized magnetic bead-based protocol from endoglycosidase digestion, through fluorophore labeling and cleanup with high-throughput sample processing in 96-well plate format, using an automated laboratory workstation. Capillary electrophoresis analysis of the fluorophore-labeled glycans was also optimized for rapid (<3 min) separation to accommodate the high-throughput processing of the automated sample preparation workflow. Ultrafast N-glycosylation analyses of several commercially relevant antibody therapeutics are also shown and compared to their biosimilar counterparts, addressing the biological significance of the differences. © 2015 Society for Laboratory Automation and Screening.

Determination of Slake Durability Index (Sdi) Values on Different Shape of Laminated Marl Samples

NASA Astrophysics Data System (ADS)

Ankara, Hüseyin; Çiçek, Fatma; Talha Deniz, İsmail; Uçak, Emre; Yerel Kandemir, Süheyla

2016-10-01

The slake durability index (SDI) test is widely used to determine the disintegration characteristic of the weak and clay-bearing rocks in geo-engineering problems. However, due to the different shapes of sample pieces, such as, irregular shapes displayed mechanical breakages in the slaking process, the SDI test has some limitations that affect the index values. In addition, shape and surface roughness of laminated marl samples have a severe influence on the SDI. In this study, a new sample preparation method called Pasha Method was used to prepare spherical specimens from the laminated marl collected from Seyitomer collar (SLI). Moreover the SDI tests were performed on equal size and weight specimens: three sets with different shapes were used. The three different sets were prepared as the test samples which had sphere shape, parallel to the layers in irregular shape, and vertical to the layers in irregular shape. Index values were determined for the three different sets subjected to the SDI test for 4 cycles. The index values at the end of fourth cycle were found to be 98.43, 98.39 and 97.20 %, respectively. As seen, the index values of the sphere sample set were found to be higher than irregular sample sets.

MStern Blotting-High Throughput Polyvinylidene Fluoride (PVDF) Membrane-Based Proteomic Sample Preparation for 96-Well Plates.

PubMed

Berger, Sebastian T; Ahmed, Saima; Muntel, Jan; Cuevas Polo, Nerea; Bachur, Richard; Kentsis, Alex; Steen, Judith; Steen, Hanno

2015-10-01

We describe a 96-well plate compatible membrane-based proteomic sample processing method, which enables the complete processing of 96 samples (or multiples thereof) within a single workday. This method uses a large-pore hydrophobic PVDF membrane that efficiently adsorbs proteins, resulting in fast liquid transfer through the membrane and significantly reduced sample processing times. Low liquid transfer speeds have prevented the useful 96-well plate implementation of FASP as a widely used membrane-based proteomic sample processing method. We validated our approach on whole-cell lysate and urine and cerebrospinal fluid as clinically relevant body fluids. Without compromising peptide and protein identification, our method uses a vacuum manifold and circumvents the need for digest desalting, making our processing method compatible with standard liquid handling robots. In summary, our new method maintains the strengths of FASP and simultaneously overcomes one of the major limitations of FASP without compromising protein identification and quantification. © 2015 by The American Society for Biochemistry and Molecular Biology, Inc.

MStern Blotting–High Throughput Polyvinylidene Fluoride (PVDF) Membrane-Based Proteomic Sample Preparation for 96-Well Plates*

PubMed Central

Berger, Sebastian T.; Ahmed, Saima; Muntel, Jan; Cuevas Polo, Nerea; Bachur, Richard; Kentsis, Alex; Steen, Judith; Steen, Hanno

2015-01-01

We describe a 96-well plate compatible membrane-based proteomic sample processing method, which enables the complete processing of 96 samples (or multiples thereof) within a single workday. This method uses a large-pore hydrophobic PVDF membrane that efficiently adsorbs proteins, resulting in fast liquid transfer through the membrane and significantly reduced sample processing times. Low liquid transfer speeds have prevented the useful 96-well plate implementation of FASP as a widely used membrane-based proteomic sample processing method. We validated our approach on whole-cell lysate and urine and cerebrospinal fluid as clinically relevant body fluids. Without compromising peptide and protein identification, our method uses a vacuum manifold and circumvents the need for digest desalting, making our processing method compatible with standard liquid handling robots. In summary, our new method maintains the strengths of FASP and simultaneously overcomes one of the major limitations of FASP without compromising protein identification and quantification. PMID:26223766

The counting of native blood cells by digital microscopy

NASA Astrophysics Data System (ADS)

Torbin, S. O.; Doubrovski, V. A.; Zabenkov, I. V.; Tsareva, O. E.

2017-03-01

An algorithm for photographic images processing of blood samples in its native state was developed to determine the concentration of erythrocytes, leukocytes and platelets without individual separate preparation of cells' samples. Special "photo templates" were suggested to use in order to identify red blood cells. The effect of "highlighting" of leukocytes, which was found by authors, was used to increase the accuracy of this type of cells counting. Finally to raise the resolution of platelets from leukocytes the areas of their photo images were used, but not their sizes. It is shown that the accuracy of cells counting for native blood samples may be comparable with the accuracy of similar studies for smears. At the same time the proposed native blood analysis simplifies greatly the procedure of sample preparation in comparison to smear, permits to move from the detection of blood cells ratio to the determination of their concentrations in the sample.

Platinum adlayered ruthenium nanoparticles, method for preparing, and uses thereof

DOEpatents

Tong, YuYe; Du, Bingchen

2015-08-11

A superior, industrially scalable one-pot ethylene glycol-based wet chemistry method to prepare platinum-adlayered ruthenium nanoparticles has been developed that offers an exquisite control of the platinum packing density of the adlayers and effectively prevents sintering of the nanoparticles during the deposition process. The wet chemistry based method for the controlled deposition of submonolayer platinum is advantageous in terms of processing and maximizing the use of platinum and can, in principle, be scaled up straightforwardly to an industrial level. The reactivity of the Pt(31)-Ru sample was about 150% higher than that of the industrial benchmark PtRu (1:1) alloy sample but with 3.5 times less platinum loading. Using the Pt(31)-Ru nanoparticles would lower the electrode material cost compared to using the industrial benchmark alloy nanoparticles for direct methanol fuel cell applications.

Corrosion behavior of magnetic ferrite coating prepared by plasma spraying

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Yi; Wei, Shicheng, E-mail: wsc33333@163.com; Tong, Hui

Graphical abstract: The saturation magnetization (M{sub s}) of the ferrite coating is 34.417 emu/g while the M{sub s} value of the ferrite powder is 71.916 emu/g. It can be seen that plasma spray process causes deterioration of the room temperature soft magnetic properties. - Highlights: • Spinel ferrite coatings have been prepared by plasma spraying. • The coating consists of nanocrystalline grains. • The saturation magnetization of the ferrite coating is 34.417 emu/g. • Corrosion behavior of the ferrite coating was examined in NaCl solution. - Abstract: In this study, spray dried spinel ferrite powders were deposited on the surfacemore » of mild steel substrate through plasma spraying. The structure and morphological studies on the ferrite coatings were carried out using X-ray diffraction, scanning electron microscope and Raman spectroscopy. It was showed that spray dried process was an effective method to prepare thermal spraying powders. The coating showed spinel structure with a second phase of LaFeO{sub 3}. The magnetic property of the ferrite samples were measured by vibrating sample magnetometer. The saturation magnetization (M{sub s}) of the ferrite coating was 34.417 emu/g. The corrosion behavior of coating samples was examined by electrochemical impedance spectroscopy. EIS diagrams showed three corrosion processes as the coating immersed in 3.5 wt.% NaCl solution. The results suggested that plasma spraying was a promising technology for the production of magnetic ferrite coatings.« less

Processing study of high temperature superconducting Y-Ba-Cu-O ceramics

DOE Office of Scientific and Technical Information (OSTI.GOV)

Safari, A.; Wachtman, J.B. Jr.; Ward, C.

Processing of the YBa{sub 2}Cu{sub 3}O{sub 6+x} superconducting phase by employing different precursor powder preparation techniques (ball milling, attrition milling) and samples formed by different sintering conditions are discussed. The superconducting phase has been identified by powder x-ray diffraction. The effect of different powder processing and pressing conditions on the structure, density, resistivity and a.c. magnetic susceptibility were studied. Though there is no variation in T{sub c} for all the samples, attrition milled samples show a much lower resistance and less temperature dependence compared to ball milled samples above the superconducting transition temperature up to room temperature. Ball milled samplesmore » were loosely packed with more voids compared to attrition milled samples which are more densely packed with a needle-like structure.« less

Studies on the formation of hierarchical zeolite T aggregates with well-defined morphology in different template systems

NASA Astrophysics Data System (ADS)

Yin, Xiaoyan; Chu, Naibo; Lu, Xuewei; Li, Zhongfang; Guo, Hong

2016-01-01

In this paper, the disk-like and pumpkin-like hierarchical zeolite T aggregates consisted of primary nano-grains have been hydrothermally synthesized with and without the aid of the second template. The first template is used with tetramethylammonium hydroxide (TMAOH) and the second template is used with triethanolamine (TEA) or polyving akohol (PVA). A combination of characterization techniques, including XRD, SEM, TEM and N2 adsorption-desorption to examine the crystal crystallinity, morphology and surface properties of hierarchical zeolite T aggregates. In the single-template preparation process, the two-step varying-temperature treatment has been used to improve the meso-porosity of zeolite T aggregates. In the double-template preparation process, the amounts of PVA or TEA on the crystallinity, morphology and meso-porosity of zeolite T aggregates have been studied. It has been proved that the interstitial voids between the primary grains of aggregates are the origin of additional mesopores of samples. The micro- and meso-porosities of samples prepared with and without the second template have been contrasted in detail at last. In particular, the sample synthesized with the addition of PVA presents a hierarchical pore structure with the highest Sext value of 122 m2/g and Vmeso value of 0.255 cm3/g.

Solventless and solvent-minimized sample preparation techniques for determining currently used pesticides in water samples: a review.

PubMed

Tankiewicz, Maciej; Fenik, Jolanta; Biziuk, Marek

2011-10-30

The intensification of agriculture means that increasing amounts of toxic organic and inorganic compounds are entering the environment. The pesticides generally applied nowadays are regarded as some of the most dangerous contaminants of the environment. Their presence in the environment, especially in water, is hazardous because they cause human beings to become more susceptible to disease. For these reasons, it is essential to monitor pesticide residues in the environment with the aid of all accessible analytical methods. The analysis of samples for the presence of pesticides is problematic, because of the laborious and time-consuming operations involved in preparing samples for analysis, which themselves may be a source of additional contaminations and errors. To date, it has been standard practice to use large quantities of organic solvents in the sample preparation process; but as these solvents are themselves hazardous, solventless and solvent-minimized techniques are coming into use. This paper discusses the most commonly used over the last 15 years sample preparation techniques for monitoring organophosphorus and organonitrogen pesticides residue in water samples. Furthermore, a significant trend in sample preparation, in accordance with the principles of 'Green Chemistry' is the simplification, miniaturization and automation of analytical techniques. In view of this aspect, several novel techniques are being developed in order to reduce the analysis step, increase the sample throughput and to improve the quality and the sensitivity of analytical methods. The paper describes extraction techniques requiring the use of solvents - liquid-liquid extraction (LLE) and its modifications, membrane extraction techniques, hollow fibre-protected two-phase solvent microextraction, liquid phase microextraction based on the solidification of a floating organic drop (LPME-SFO), solid-phase extraction (SPE) and single-drop microextraction (SDME) - as well as solvent-free techniques - solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The advantages and drawbacks of these techniques are also discussed, and some solutions to their limitations are proposed. Copyright © 2011 Elsevier B.V. All rights reserved.

Differences in levels of platelet-derived microparticles in platelet components prepared using the platelet rich plasma, buffy coat, and apheresis procedures.

PubMed

Noulsri, Egarit; Udomwinijsilp, Prapaporn; Lerdwana, Surada; Chongkolwatana, Viroje; Permpikul, Parichart

2017-04-01

There has been an increased interest in platelet-derived microparticles (PMPs) in transfusion medicine. Little is known about PMP status during the preparation of platelet concentrates for transfusion. The aim of this study is to compare the PMP levels in platelet components prepared using the buffy coat (BC), platelet-rich plasma platelet concentrate (PRP-PC), and apheresis (AP) processes. Platelet components were prepared using the PRP-PC and BC processes. Apheresis platelets were prepared using the Trima Accel and Amicus instruments. The samples were incubated with annexin A5-FITC, CD41-PE, and CD62P-APC. At day 1 after processing, the PMPs and activated platelets were determined using flow cytometry. Both the percentage and number of PMPs were higher in platelet components prepared using the Amicus instrument (2.6±1.8, 32802±19036 particles/μL) than in platelet components prepared using the Trima Accel instrument (0.5±0.4, 7568±5298 particles/μL), BC (1.2±0.6, 12,920±6426 particles/μL), and PRP-PC (0.9±0.6, 10731±5514 particles/μL). Both the percentage and number of activated platelets were higher in platelet components prepared using the Amicus instrument (33.2±13.9, 427553±196965 cells/μL) than in platelet components prepared using the Trima Accel instrument (16.2±6.1, 211209±87706 cells/μL), BC (12.9±3.2, 140624±41003 cells/μL), and PRP-PC (21.1±6.3, 265210±86257 cells/μL). The study suggests high variability of PMPs and activated platelets in platelet components prepared using different processes. This result may be important in validating the instruments involved in platelet blood collection and processing. Copyright © 2016 Elsevier Ltd. All rights reserved.

Specimen preparation for high-resolution cryo-EM

PubMed Central

Passmore, Lori A.; Russo, Christopher J.

2016-01-01

Imaging a material with electrons at near-atomic resolution requires a thin specimen that is stable in the vacuum of the transmission electron microscope. For biological samples, this comprises a thin layer of frozen aqueous solution containing the biomolecular complex of interest. The process of preparing a high-quality specimen is often the limiting step in the determination of structures by single-particle electron cryomicroscopy (cryo-EM). Here we describe a systematic approach for going from a purified biomolecular complex in aqueous solution to high-resolution electron micrographs that are suitable for 3D structure determination. This includes a series of protocols for the preparation of vitrified specimens on various specimen supports, including all-gold and graphene. We also describe techniques for troubleshooting when a preparation fails to yield suitable specimens, and common mistakes to avoid during each part of the process. Finally, we include recommendations for obtaining the highest quality micrographs from prepared specimens with current microscope, detector and support technology. PMID:27572723

ICECAP: an integrated, general-purpose, automation-assisted IC50/EC50 assay platform.

PubMed

Li, Ming; Chou, Judy; King, Kristopher W; Jing, Jing; Wei, Dong; Yang, Liyu

2015-02-01

IC50 and EC50 values are commonly used to evaluate drug potency. Mass spectrometry (MS)-centric bioanalytical and biomarker labs are now conducting IC50/EC50 assays, which, if done manually, are tedious and error-prone. Existing bioanalytical sample preparation automation systems cannot meet IC50/EC50 assay throughput demand. A general-purpose, automation-assisted IC50/EC50 assay platform was developed to automate the calculations of spiking solutions and the matrix solutions preparation scheme, the actual spiking and matrix solutions preparations, as well as the flexible sample extraction procedures after incubation. In addition, the platform also automates the data extraction, nonlinear regression curve fitting, computation of IC50/EC50 values, graphing, and reporting. The automation-assisted IC50/EC50 assay platform can process the whole class of assays of varying assay conditions. In each run, the system can handle up to 32 compounds and up to 10 concentration levels per compound, and it greatly improves IC50/EC50 assay experimental productivity and data processing efficiency. © 2014 Society for Laboratory Automation and Screening.

Optimized Setup and Protocol for Magnetic Domain Imaging with In Situ Hysteresis Measurement.

PubMed

Liu, Jun; Wilson, John; Davis, Claire; Peyton, Anthony

2017-11-07

This paper elaborates the sample preparation protocols required to obtain optimal domain patterns using the Bitter method, focusing on the extra steps compared to standard metallographic sample preparation procedures. The paper proposes a novel bespoke rig for dynamic domain imaging with in situ BH (magnetic hysteresis) measurements and elaborates the protocols for the sensor preparation and the use of the rig to ensure accurate BH measurement. The protocols for static and ordinary dynamic domain imaging (without in situ BH measurements) are also presented. The reported method takes advantage of the convenience and high sensitivity of the traditional Bitter method and enables in situ BH measurement without interrupting or interfering with the domain wall movement processes. This facilitates establishing a direct and quantitative link between the domain wall movement processes-microstructural feature interactions in ferritic steels with their BH loops. This method is anticipated to become a useful tool for the fundamental study of microstructure-magnetic property relationships in steels and to help interpret the electromagnetic sensor signals for non-destructive evaluation of steel microstructures.

Analyzing Immunoglobulin Repertoires

PubMed Central

Chaudhary, Neha; Wesemann, Duane R.

2018-01-01

Somatic assembly of T cell receptor and B cell receptor (BCR) genes produces a vast diversity of lymphocyte antigen recognition capacity. The advent of efficient high-throughput sequencing of lymphocyte antigen receptor genes has recently generated unprecedented opportunities for exploration of adaptive immune responses. With these opportunities have come significant challenges in understanding the analysis techniques that most accurately reflect underlying biological phenomena. In this regard, sample preparation and sequence analysis techniques, which have largely been borrowed and adapted from other fields, continue to evolve. Here, we review current methods and challenges of library preparation, sequencing and statistical analysis of lymphocyte receptor repertoire studies. We discuss the general steps in the process of immune repertoire generation including sample preparation, platforms available for sequencing, processing of sequencing data, measurable features of the immune repertoire, and the statistical tools that can be used for analysis and interpretation of the data. Because BCR analysis harbors additional complexities, such as immunoglobulin (Ig) (i.e., antibody) gene somatic hypermutation and class switch recombination, the emphasis of this review is on Ig/BCR sequence analysis. PMID:29593723

Analysis of preparation of Chinese traditional medicine based on the fiber fingerprint drop trace

NASA Astrophysics Data System (ADS)

Zhang, Zhilin; Wang, Jialu; Sun, Weimin; Yan, Qi

2010-11-01

The purpose of the fiber micro-drop analyzing technique is to measure the characteristics of liquids using optical methods. The fiber fingerprint drop trace (FFDT) is a curve of light intensity vs. time. This curve indicates the forming, growing and dripping processes of the liquid drops. A pair of fibers was used to monitor the dripping process. The FFDTs are acquired and analyzed by a computer. Different liquid samples of many kinds of preparation of Chinese traditional medicines were tested by using the fiber micro-drop sensor in the experiments. The FFDTs of preparation of Chinese traditional medicines with different concentrations were analyzed in different ways. Considering the characters of the FFDTs, a novel method is proposed to measure the different preparation of Chinese traditional medicines and its concentration based on the corresponding relationship of FFDTs and the physical and chemical parameters of the liquids.

Improving ultraviolet photodetection of ZnO nanorods by Cr doped ZnO encapsulation process

NASA Astrophysics Data System (ADS)

Safa, S.; Mokhtari, S.; Khayatian, A.; Azimirad, R.

2018-04-01

Encapsulated ZnO nanorods (NRs) with different Cr concentration (0-4.5 at.%) were prepared in two different steps. First, ZnO NRs were grown by hydrothermal method. Then, they were encapsulated by dip coating method. The prepared samples were characterized by X-ray diffraction (XRD), scanning electron microscopy, and ultraviolet (UV)-visible spectrophotometer analyses. XRD analysis proved that Cr incorporated into the ZnO structure successfully. Based on optical analysis, band gap changes in the range of 2.74-3.84 eV. Finally, UV responses of all samples were deeply investigated. It revealed 0.5 at.% Cr doped sample had the most photocurrent (0.75 mA) and photoresponsivity (0.8 A/W) of all which were about three times greater than photocurrent and photoresponsivity of the undoped sample.

Preparation and characterization of molecularly homogeneous silica-titania film by sol-gel process with different synthetic strategies.

PubMed

Chen, Hsueh-Shih; Huang, Sheng-Hsin; Perng, Tsong-Pyng

2012-10-24

Three silica-titania thin films with various degrees of molecular homogeneity were synthesized by the sol-gel process with the same precursor formula but different reaction paths. The dried films prepared by a single spin-coating process have a thickness of 500-700 nm and displayed no cracks or pin holes. The transmittances and refractive indices of the samples are >97.8% in the range of 350-1800 nm and 1.62-1.65 at 500 nm, respectively. The in-plane and out-of-plane chemical homogeneities of the films were analyzed by X-ray photoelectron spectroscopy and Auger electron spectroscopy, respectively. For the film with the highest degree of homogeneity, the deviations of O, Si, and Ti atomic contents in both in-plane and out-of-plane directions are less than 1.5%, indicating that the film is highly molecularly homogeneous. It also possesses the highest transparency and the lowest refractive index among the three samples.

Quantitative Method for Simultaneous Analysis of Acetaminophen and 6 Metabolites.

PubMed

Lammers, Laureen A; Achterbergh, Roos; Pistorius, Marcel C M; Romijn, Johannes A; Mathôt, Ron A A

2017-04-01

Hepatotoxicity after ingestion of high-dose acetaminophen [N-acetyl-para-aminophenol (APAP)] is caused by the metabolites of the drug. To gain more insight into factors influencing susceptibility to APAP hepatotoxicity, quantification of APAP and metabolites is important. A few methods have been developed to simultaneously quantify APAP and its most important metabolites. However, these methods require a comprehensive sample preparation and long run times. The aim of this study was to develop and validate a simplified, but sensitive method for the simultaneous quantification of acetaminophen, the main metabolites acetaminophen glucuronide and acetaminophen sulfate, and 4 Cytochrome P450-mediated metabolites by using liquid chromatography with mass spectrometric (LC-MS) detection. The method was developed and validated for the human plasma, and it entailed a single method for sample preparation, enabling quick processing of the samples followed by an LC-MS method with a chromatographic run time of 9 minutes. The method was validated for selectivity, linearity, accuracy, imprecision, dilution integrity, recovery, process efficiency, ionization efficiency, and carryover effect. The method showed good selectivity without matrix interferences. For all analytes, the mean process efficiency was >86%, and the mean ionization efficiency was >94%. Furthermore, the accuracy was between 90.3% and 112% for all analytes, and the within- and between-run imprecision were <20% for the lower limit of quantification and <14.3% for the middle level and upper limit of quantification. The method presented here enables the simultaneous quantification of APAP and 6 of its metabolites. It is less time consuming than previously reported methods because it requires only a single and simple method for the sample preparation followed by an LC-MS method with a short run time. Therefore, this analytical method provides a useful method for both clinical and research purposes.

Improvement of High-throughput Genotype Analysis After Implementation of a Dual-curve Sybr Green I-based Quantification and Normalization Procedure

USDA-ARS?s Scientific Manuscript database

The ability to rapidly screen a large number of individuals is the key to any successful plant breeding program. One of the primary bottlenecks in high throughput screening is the preparation of DNA samples, particularly the quantification and normalization of samples for downstream processing. A ...

Using the Precaution Adoption Process Model to Describe a Disaster Preparedness Intervention among Low-Income Latinos

ERIC Educational Resources Information Center

Glik, Deborah C.; Eisenman, David P.; Zhou, Qiong; Tseng, Chi-Hong; Asch, Steven M.

2014-01-01

Only 40-50% of households in the United States are currently disaster prepared. In this intervention study, respondent-driven sampling was used to select a sample (n = 187) of low income, Latino residents of Los Angeles County, randomly assigned into two treatment conditions: (i) household preparedness education received through…

A novel sample preparation method to avoid influence of embedding medium during nano-indentation

NASA Astrophysics Data System (ADS)

Meng, Yujie; Wang, Siqun; Cai, Zhiyong; Young, Timothy M.; Du, Guanben; Li, Yanjun

2013-02-01

The effect of the embedding medium on the nano-indentation measurements of lignocellulosic materials was investigated experimentally using nano-indentation. Both the reduced elastic modulus and the hardness of non-embedded cell walls were found to be lower than those of the embedded samples, proving that the embedding medium used for specimen preparation on cellulosic material during nano-indentation can modify cell-wall properties. This leads to structural and chemical changes in the cell-wall constituents, changes that may significantly alter the material properties. Further investigation was carried out to detect the influence of different vacuum times on the cell-wall mechanical properties during the embedding procedure. Interpretation of the statistical analysis revealed no linear relationships between vacuum time and the mechanical properties of cell walls. The quantitative measurements confirm that low-viscosity resin has a rapid penetration rate early in the curing process. Finally, a novel sample preparation method aimed at preventing resin diffusion into lignocellulosic cell walls was developed using a plastic film to wrap the sample before embedding. This method proved to be accessible and straightforward for many kinds of lignocellulosic material, but is especially suitable for small, soft samples.

Purification and preparation of graphite oxide from natural graphite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Panatarani, C., E-mail: c.panatarani@phys.unpad.ac.id; Muthahhari, N.; Joni, I. Made

2016-03-11

Graphite oxide has attracted much interest as a possible route for preparation of natural graphite in the large-scale production and manipulation of graphene as a material with extraordinary electronic properties. Graphite oxide was prepared by modified Hummers method from purified natural graphite sample from West Kalimantan. We demonstrated that natural graphite is well-purified by acid leaching method. The purified graphite was proceed for intercalating process by modifying Hummers method. The modification is on the reaction time and temperature of the intercalation process. The materials used in the intercalating process are H{sub 2}SO{sub 4} and KMNO{sub 4}. The purified natural graphitemore » is analyzed by carbon content based on Loss on Ignition test. The thermo gravimetricanalysis and the Fouriertransform infrared spectroscopy are performed to investigate the oxidation results of the obtained GO which is indicated by the existence of functional groups. In addition, the X-ray diffraction and energy dispersive X-ray spectroscopy are also applied to characterize respectively for the crystal structure and elemental analysis. The results confirmed that natural graphite samples with 68% carbon content was purified into 97.68 % carbon content. While the intercalation process formed a formation of functional groups in the obtained GO. The results show that the temperature and reaction times have improved the efficiency of the oxidation process. It is concluded that these method could be considered as an important route for large-scale production of graphene.« less

Electrical field-induced extraction and separation techniques: promising trends in analytical chemistry--a review.

PubMed

Yamini, Yadollah; Seidi, Shahram; Rezazadeh, Maryam

2014-03-03

Sample preparation is an important issue in analytical chemistry, and is often a bottleneck in chemical analysis. So, the major incentive for the recent research has been to attain faster, simpler, less expensive, and more environmentally friendly sample preparation methods. The use of auxiliary energies, such as heat, ultrasound, and microwave, is one of the strategies that have been employed in sample preparation to reach the above purposes. Application of electrical driving force is the current state-of-the-art, which presents new possibilities for simplifying and shortening the sample preparation process as well as enhancing its selectivity. The electrical driving force has scarcely been utilized in comparison with other auxiliary energies. In this review, the different roles of electrical driving force (as a powerful auxiliary energy) in various extraction techniques, including liquid-, solid-, and membrane-based methods, have been taken into consideration. Also, the references have been made available, relevant to the developments in separation techniques and Lab-on-a-Chip (LOC) systems. All aspects of electrical driving force in extraction and separation methods are too specific to be treated in this contribution. However, the main aim of this review is to provide a brief knowledge about the different fields of analytical chemistry, with an emphasis on the latest efforts put into the electrically assisted membrane-based sample preparation systems. The advantages and disadvantages of these approaches as well as the new achievements in these areas have been discussed, which might be helpful for further progress in the future. Copyright © 2013 Elsevier B.V. All rights reserved.

Development of replicated optics for AXAF-1 XDA testing

NASA Technical Reports Server (NTRS)

Engelhaupt, Darell; Wilson, Michele; Martin, Greg

1995-01-01

Advanced optical systems for applications such as grazing incidence Wolter I x-ray mirror assemblies require extraordinary mirror surfaces in terms of fine finish and surface figure. The impeccable mirror surface is on the inside of the rotational mirror form. One practical method of producing devices with these requirements is to first fabricate an exterior surface for the optical device then replicate that surface to have the inverse component with lightweight characteristics. The replicated optic is not better than the master or mandrel from which it is made. This task identifies methods and materials for forming these extremely low roughness optical components. The objectives of this contract were to (1) prepare replication samples of electroless nickel coated aluminum, and determine process requirements for plating XDA test optic; (2) prepare and assemble plating equipment required to process a demonstration optic; (3) characterize mandrels, replicas and test samples for residual stress, surface contamination and surface roughness and figure using equipment at MSFC and; (4) provide technical expertise in establishing the processes, procedures, supplies and equipment needed to process the XDA test optics.

DC magnetron sputtered polyaniline-HCl thin films for chemical sensing applications.

PubMed

Menegazzo, Nicola; Boyne, Devon; Bui, Holt; Beebe, Thomas P; Booksh, Karl S

2012-07-03

Thin films of conducting polymers exhibit unique chemical and physical properties that render them integral parts in microelectronics, energy storage devices, and chemical sensors. Overall, polyaniline (PAni) doped in acidic media has shown metal-like electronic conductivity, though exact physical and chemical properties are dependent on the polymer structure and dopant type. Difficulties arising from poor processability render production of doped PAni thin films particularly challenging. In this contribution, DC magnetron sputtering, a physical vapor deposition technique, is applied to the preparation of conductive thin films of PAni doped with hydrochloric acid (PAni-HCl) in an effort to circumvent issues associated with conventional thin film preparation methods. Samples manufactured by the sputtering method are analyzed along with samples prepared by conventional drop-casting. Physical characterization (atomic force microscopy, AFM) confirm the presence of PAni-HCl and show that films exhibit a reduced roughness and potentially pinhole-free coverage of the substrate. Spectroscopic evidence (UV-vis, FT-IR, and X-ray photoelectron spectroscopy (XPS)) suggests that structural changes and loss of conductivity, not uncommon during PAni processing, does occur during the preparation process. Finally, the applicability of sputtered films to gas-phase sensing of NH(3) was investigated with surface plasmon resonance (SPR) spectroscopy and compared to previous contributions. In summary, sputtered PAni-HCl films exhibit quantifiable, reversible behavior upon exposure to NH(3) with a calculated LOD (by method) approaching 0.4 ppm NH(3) in dry air.

Osteoconductivity and Hydrophilicity of TiO2 Coatings on Ti Substrates Prepared by Different Oxidizing Processes

PubMed Central

Yamamoto, Dai; Kawai, Ikki; Kuroda, Kensuke; Ichino, Ryoichi; Okido, Masazumi; Seki, Azusa

2012-01-01

Various techniques for forming TiO2 coatings on Ti have been investigated for the improvement of the osteoconductivity of Ti implants. However, it is not clear how the oxidizing process affects this osteoconductivity. In this study, TiO2 coatings were prepared using the following three processes: anodizing in 0.1 M H3PO4 or 0.1 M NaOH aqueous solution; thermal oxidation at 673 K for 2 h in air; and a two-step process of anodizing followed by thermal oxidation. The oxide coatings were evaluated using SEM, XRD, and XPS. The water contact angle on the TiO2 coatings was measured as a surface property. The osteoconductivity of these samples was evaluated by measuring the contact ratio of formed hard tissue on the implanted samples (defined as the R B-I value) after 14 d implantation in rats' tibias. Anatase was formed by anodizing and rutile by thermal oxidation, but the difference in the TiO2 crystal structure did not influence the osteoconductivity. Anodized TiO2 coatings were hydrophilic, but thermally oxidized TiO2 coatings were less hydrophilic than anodized TiO2 coatings because they lacked in surface OH groups. The TiO2 coating process using anodizing without thermal oxidation gave effective improvement of the osteoconductivity of Ti samples. PMID:23316128

Preparation of amorphous solid dispersions by rotary evaporation and KinetiSol Dispersing: approaches to enhance solubility of a poorly water-soluble gum extract.

PubMed

Bennett, Ryan C; Brough, Chris; Miller, Dave A; O'Donnell, Kevin P; Keen, Justin M; Hughey, Justin R; Williams, Robert O; McGinity, James W

2015-03-01

Acetyl-11-keto-β-boswellic acid (AKBA), a gum resin extract, possesses poor water-solubility that limits bioavailability and a high melting point making it difficult to successfully process into solid dispersions by fusion methods. The purpose of this study was to investigate solvent and thermal processing techniques for the preparation of amorphous solid dispersions (ASDs) exhibiting enhanced solubility, dissolution rates and bioavailability. Solid dispersions were successfully produced by rotary evaporation (RE) and KinetiSol® Dispersing (KSD). Solid state and chemical characterization revealed that ASD with good potency and purity were produced by both RE and KSD. Results of the RE studies demonstrated that AQOAT®-LF, AQOAT®-MF, Eudragit® L100-55 and Soluplus with the incorporation of dioctyl sulfosuccinate sodium provided substantial solubility enhancement. Non-sink dissolution analysis showed enhanced dissolution properties for KSD-processed solid dispersions in comparison to RE-processed solid dispersions. Variances in release performance were identified when different particle size fractions of KSD samples were analyzed. Selected RE samples varying in particle surface morphologies were placed under storage and exhibited crystalline growth following solid-state stability analysis at 12 months in comparison to stored KSD samples confirming amorphous instability for RE products. In vivo analysis of KSD-processed solid dispersions revealed significantly enhanced AKBA absorption in comparison to the neat, active substance.

Synthesis and characterization of α-NaYF{sub 4}: Yb, Er nanoparticles by reverse microemulsion method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gunaseelan, M.; Senthilselvan, J., E-mail: jsselvan@hotmail.com

2016-05-06

A simple and cost effective reverse microemulsion system was newly designed to synthesis NaYF{sub 4}:20%Yb,2%Er upconverting luminescent nanoparticles. XRD results confirms the cubic structure of NaYF{sub 4} nanophosphor in the as prepared condition without any other impurity phases. The as-prepared sample itself having highly crystalline nanoparticle with well dispersed uniform morphology is the advantage of this reverse microemulsion process. HRTEM images of as prepared and calcined samples revealed spherical nanoclusters morphology with size of ~210 nm and ~245 nm respectively. The characteristic absorption wavelength that occurs at 980 nm due to transition of energy levels {sup 2}F{sub 5/2} to {sup 2}F{sub 7/2} formore » Yb{sup 3+} rare earth ion in as prepared and calcined upconversion nanoparticle confirms the presence of Yb{sup 3+} by UV-Visible spectroscopy which can act as a sensitizer for photonic upconversion. Therefore the absorption at NIR region and emission spectrum at visible region suggests that NaYF{sub 4}:20%Yb,2%Er is suitable for upcoversion process, due to its optical property and chemical stability this material also be useful for bio imaging applications.« less

Miniaturized Sample Preparation and Rapid Detection of Arsenite in Contaminated Soil Using a Smartphone.

PubMed

Siddiqui, Mohd Farhan; Kim, Soocheol; Jeon, Hyoil; Kim, Taeho; Joo, Chulmin; Park, Seungkyung

2018-03-04

Conventional methods for analyzing heavy metal contamination in soil and water generally require laboratory equipped instruments, complex procedures, skilled personnel and a significant amount of time. With the advancement in computing and multitasking performances, smartphone-based sensors potentially allow the transition of the laboratory-based analytical processes to field applicable, simple methods. In the present work, we demonstrate the novel miniaturized setup for simultaneous sample preparation and smartphone-based optical sensing of arsenic As(III) in the contaminated soil. Colorimetric detection protocol utilizing aptamers, gold nanoparticles and NaCl have been optimized and tested on the PDMS-chip to obtain the high sensitivity with the limit of detection of 0.71 ppm (in the sample) and a correlation coefficient of 0.98. The performance of the device is further demonstrated through the comparative analysis of arsenic-spiked soil samples with standard laboratory method, and a good agreement with a correlation coefficient of 0.9917 and the average difference of 0.37 ppm, are experimentally achieved. With the android application on the device to run the experiment, the whole process from sample preparation to detection is completed within 3 hours without the necessity of skilled personnel. The approximate cost of setup is estimated around 1 USD, weight 55 g. Therefore, the presented method offers the simple, rapid, portable and cost-effective means for onsite sensing of arsenic in soil. Combined with the geometric information inside the smartphones, the system will allow the monitoring of the contamination status of soils in a nation-wide manner.

Optical characterization of pure and Al-doped ZnO prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Belka, Radosław; Keczkowska, Justyna; Kasińska, Justyna

2016-09-01

In this paper the preparation process and optical characterization of pure and Al3+ doped zinc oxide (Al:ZnO) coatings will be presented. ZnO based materials have been studied extensively due to their potential applications in optoelectronic devices as conductive gas sensors, transparent conductive, electrodes, solar cell windows, varistors, UVfilters or photovoltaic cells. It is II-VI semiconductor with wide-band gap of 3.37 eV and large exciton binding energy of 60meV. It is possible to improve the conductivity of ZnO coating by intentionally doping ZnO with aluminium ions during preparation process. Such transparent and conducting thin films, known as AZO (Aluminium Zinc Oxide) films, are very good candidate for application as transparent conducting materials in many optoelectronic devices. The well-known sol-gel method is used for preparation of solution, coated on glass substrates by dip coating process. Prepared samples were investigated by Raman and UV-VIS spectroscopy. Transmittance as well as specular and diffuse reflectance spectroscopy methods were used for studies of optical parameters. We found that Al admixture influences on optical bandgap of ZnO.

Preparation and application of poly 3, 4-ethylenedioxythiophene (PEDOT) nanofibers in the pretreatment of samples before the determination of elements in children fingernails

NASA Astrophysics Data System (ADS)

Qiu, J. L.; Kang, X. J.; Ma, L.; Huang, W. Y.; Ge, Q. Y.

2015-07-01

Solid phase extraction (SPE) has been used widely for sample preparation in the analytical process. Many efforts have focused on developing novel adsorbents to enrich and purify the analytes effectively. In this study, poly-3, 4-ethylenedioxythiophene (PEDOT) nanofiber was prepared and used as the SPE adsorbent. The fiber performed good in extraction of metal ions, Cd, Sn, Hg, Pb, Al, and As, with the extraction recoveries ranged from 53.9% to 99.6% in the wet digested samples of fingernails. A PEDOT namofibers SPE column coupled with ICP-MS was established for assay of elements in fingernails. The levels of elements (Cd, Sn, Hg, Pb, Al, and As) in the fingernails of 77 healthy Chinese children (6-7 and 10-11 years) were determined. Independent t test shows that no significance has been found between boys and girls. On the contrary, there was obvious difference on the levels of most elements between the two grade groups.

[Developments in preparation and experimental method of solid phase microextraction fibers].

PubMed

Yi, Xu; Fu, Yujie

2004-09-01

Solid phase microextraction (SPME) is a simple and effective adsorption and desorption technique, which concentrates volatile or nonvolatile compounds from liquid samples or headspace of samples. SPME is compatible with analyte separation and detection by gas chromatography, high performance liquid chromatography, and other instrumental methods. It can provide many advantages, such as wide linear scale, low solvent and sample consumption, short analytical times, low detection limits, simple apparatus, and so on. The theory of SPME is introduced, which includes equilibrium theory and non-equilibrium theory. The novel development of fiber preparation methods and relative experimental techniques are discussed. In addition to commercial fiber preparation, different newly developed fabrication techniques, such as sol-gel, electronic deposition, carbon-base adsorption, high-temperature epoxy immobilization, are presented. Effects of extraction modes, selection of fiber coating, optimization of operating conditions, method sensitivity and precision, and systematical automation, are taken into considerations in the analytical process of SPME. A simple perspective of SPME is proposed at last.

Synchronous γ (Co60) photons and thermal processing induced insulator metal transition in amorphous chalcogenide As4Se3Te3 composition

NASA Astrophysics Data System (ADS)

El-Sayed, S. A.; Morsy, M. A.

2018-05-01

Amorphous chalcogenide composition AS4Se3Te3 is prepared by conventional quenching technique. The separate annealing or γ quanta irradiation not effect on the dc conductivity properties of the prepared composition. When the prepared samples are subjected to simultaneous annealing at temperature 413 K and γ quanta irradiation the dc conductivity increases. The dark dc conductivity increases by increasing the time of exposure to γ irradiation. At irradiation dose 1.47 × 104 Gy the dc conductivity starts to have metallic like conductivity character. These samples could be used as high temperature γ quanta dosimeter. By applying scaling theory on the samples irradiated with different dose of γ irradiation the critical exponents are determined and found to be < 2. The dark dc conductivity continuously decreases to 0 as temperature tends to zero. The steric value is low in the insulator side of conductivity, but high and almost saturated in the metallic side of conductivity.

Improvements to sample processing and measurement to enable more widespread environmental application of tritium.

PubMed

Moran, James; Alexander, Thomas; Aalseth, Craig; Back, Henning; Mace, Emily; Overman, Cory; Seifert, Allen; Freeburg, Wilcox

2017-08-01

Previous measurements have demonstrated the wealth of information that tritium (T) can provide on environmentally relevant processes. We present modifications to sample preparation approaches that enable T measurement by proportional counting on small sample sizes equivalent to 120mg of water and demonstrate the accuracy of these methods on a suite of standardized water samples. We identify a current quantification limit of 92.2 TU which, combined with our small sample sizes, correlates to as little as 0.00133Bq of total T activity. This enhanced method should provide the analytical flexibility needed to address persistent knowledge gaps in our understanding of both natural and artificial T behavior in the environment. Copyright © 2017. Published by Elsevier Ltd.

Improvements to sample processing and measurement to enable more widespread environmental application of tritium

DOE PAGES

Moran, James; Alexander, Thomas; Aalseth, Craig; ...

2017-01-26

Previous measurements have demonstrated the wealth of information that tritium (T) can provide on environmentally relevant processes. Here, we present modifications to sample preparation approaches that enable T measurement by proportional counting on small sample sizes equivalent to 120 mg of water and demonstrate the accuracy of these methods on a suite of standardized water samples. We also identify a current quantification limit of 92.2 TU which, combined with our small sample sizes, correlates to as little as 0.00133 Bq of total T activity. Furthermore, this enhanced method should provide the analytical flexibility needed to address persistent knowledge gaps inmore » our understanding of both natural and artificial T behavior in the environment.« less

Methods for producing silicon carbide architectural preforms

NASA Technical Reports Server (NTRS)

DiCarlo, James A. (Inventor); Yun, Hee (Inventor)

2010-01-01

Methods are disclosed for producing architectural preforms and high-temperature composite structures containing high-strength ceramic fibers with reduced preforming stresses within each fiber, with an in-situ grown coating on each fiber surface, with reduced boron within the bulk of each fiber, and with improved tensile creep and rupture resistance properties for each fiber. The methods include the steps of preparing an original sample of a preform formed from a pre-selected high-strength silicon carbide ceramic fiber type, placing the original sample in a processing furnace under a pre-selected preforming stress state and thermally treating the sample in the processing furnace at a pre-selected processing temperature and hold time in a processing gas having a pre-selected composition, pressure, and flow rate. For the high-temperature composite structures, the method includes additional steps of depositing a thin interphase coating on the surface of each fiber and forming a ceramic or carbon-based matrix within the sample.

Carbonate and silicate rock standards for cosmogenic 36Cl

NASA Astrophysics Data System (ADS)

Mechernich, Silke; Dunai, Tibor J.; Binnie, Steven A.; Goral, Tomasz; Heinze, Stefan; Dewald, Alfred; Benedetti, Lucilla; Schimmelpfennig, Irene; Phillips, Fred; Marrero, Shasta; Akif Sarıkaya, Mehmet; Gregory, Laura C.; Phillips, Richard J.; Wilcken, Klaus; Simon, Krista; Fink, David

2017-04-01

The number of studies using cosmogenic nuclides has increased multi-fold during the last two decades and several new dedicated target preparation laboratories and Accelerator Mass Spectrometry (AMS) facilities have been established. Each facility uses sample preparation and AMS measurement techniques particular to their needs. It is thus desirable to have community-accepted and well characterized rock standards available for routine processing using identical target preparation procedures and AMS measurement methods as carried out for samples of unknown cosmogenic nuclide concentrations. The usefulness of such natural standards is that they allow more rigorous quality control, for example, the long-term reproducibility of results and hence measurement precision, or the testing of new target preparation techniques or newly established laboratories. This is particularly pertinent for in-situ 36Cl studies due to the multiplicity of 36Cl production pathways that requires a variety of elemental and isotopic determinations in addition to AMS 36Cl assay. We have prepared two natural rock samples (denoted CoCal-N and CoFsp-N) to serve as standard material for in situ-produced cosmogenic 36Cl analysis. The sample CoCal-N is a pure limestone prepared from pebbles in a Namibian lag deposit, while the alkali-feldspar CoFsp-N is derived from a single crystal in a Namibian pegmatite. The sample preparation took place at the University of Cologne, where first any impurities were removed manually from both standards. CoCal-N was leached in 10 % HNO3 to remove the outer rim, and afterwards crushed and sieved to 250-500 μm size fractions. CoFsp-N was crushed, sieved to 250-500 μm size fractions and then leached in 1% HNO3 / 1% HF until 20% of the sample were removed. Both standards were thoroughly mixed using a rotating sample splitter before being distributed to other laboratories. To date, a total of 28 CoCal-N aliquots (between 2 and 16 aliquots per facility) and 31 CoFsp-N aliquots (between 2 and 20 aliquots per facility) have been analyzed by six target preparation laboratories employing five different AMS facilities. Currently, the internal reproducibility of the measurements underlines the homogeneity of both standards. The inter-laboratory comparison suggests low over-dispersion. Further measurements are pending and should allow meaningful statistical analysis. Both standard materials are freely available and can be obtained from Tibor Dunai tdunai@uni-koeln.de).

Description of the containerless melting of glass in low gravity

NASA Technical Reports Server (NTRS)

Ray, C. S.; Day, D. E.

1983-01-01

A brief description is given of a single-axis, acoustic levitator/furnace apparatus used to position, heat, melt, and quench multicomponent oxide, glass-forming compositions in low gravity. This apparatus is capable of processing eight approximately spherical samples (about 6 mm diameter) at temperatures up to 1550 C in a dry air atmosphere. Results are also presented for a containerless melting experiment conducted on SPAR VI where a ternary CaO-Ga2O3-SiO2 composition was levitated and quenched to a glass. Selected properties of the glass prepared on SPAR VI are compared with the properties of glass samples of identical composition prepared on earth.

Rapid microwave assisted synthesis of YIn1-xMnxO3 blue pigments: Synthesis, microstructure and optical properties

NASA Astrophysics Data System (ADS)

Zhou, Yuncheng; Jiang, Peng; Kuang, Jianlei; Yang, Xueshan; Cao, Wenbin

2018-07-01

The YIn1-xMnxO3 (0.1 ≤x ≤ 0.5) blue pigment samples are successfully prepared through a sol-gel process followed by microwave assisted sintering process. All the samples are shown single phases in the X-ray diffraction results. In the morphology study from scanning electronic microscope, the samples are composed of loosely connected small particles. The oxidation state of Mn is confirmed to be 3 + from the results of X-ray photonelectronic scan. The optical properties are characterized by UV-Visible spectrum and UV-visible-NIR spectrum. The samples exhibit intense blue color and they show small absorption in infrared region.

Fluoride glass: Crystallization, surface tension

NASA Technical Reports Server (NTRS)

Doremus, R. H.

1988-01-01

Fluoride glass was levitated acoustically in the ACES apparatus on STS-11, and the recovered sample had a different microstructure from samples cooled in a container. Further experiments on levitated samples of fluoride glass are proposed. These include nucleation, crystallization, melting observations, measurement of surface tension of molten glass, and observation of bubbles in the glass. Ground experiments are required on sample preparation, outgassing, and surface reactions. The results should help in the development and evaluation of containerless processing, especially of glass, in the development of a contaminent-free method of measuring surface tensions of melts, in extending knowledge of gas and bubble behavior in fluoride glasses, and in increasing insight into the processing and properties of fluoride glasses.

Anisotropic propagation imaging of elastic waves in oriented columnar thin films

NASA Astrophysics Data System (ADS)

Coffy, E.; Dodane, G.; Euphrasie, S.; Mosset, A.; Vairac, P.; Martin, N.; Baida, H.; Rampnoux, J. M.; Dilhaire, S.

2017-12-01

We report on the observation of strongly anisotropic surface acoustic wave propagation on nanostructured thin films. Two kinds of tungsten samples were prepared by sputtering on a silicon substrate: a conventional thin film with columns normal to the substrate surface, and an oriented columnar architecture using the glancing angle deposition (GLAD) process. Pseudo-Rayleigh waves (PRWs) were imaged as a function of time in x and y directions for both films thanks to a femtosecond heterodyne pump-probe setup. A strong anisotropic propagation as well as a high velocity reduction of the PRWs were exhibited for the GLAD sample. For the wavevector k/2π  =  3  ×  105 m-1 the measured group velocities v x and v y equal 2220 m s-1 for the sample prepared with conventional sputtering, whereas a strong anisotropy appears (v x   =  1600 m s-1 and v y   =  870 m s-1) for the sample prepared with the GLAD process. Using the finite element method, the anisotropy is related to the structural anisotropy of the thin film’s architecture. The drop of PRWs group velocities is mainly assigned to the porous microstructure, especially favored by atomic shadowing effects which appear during the growth of the inclined columns. Such GLAD thin films constitute a new tool for the control of the propagation of surface elastic waves and for the design of new devices with useful properties.

Preparation of C18 composite solid-phase microextraction fiber and its application to the determination of organochlorine pesticides in water samples.

PubMed

Li, Siyan; Lu, Chengwei; Zhu, Fang; Jiang, Ruifen; Ouyang, Gangfeng

2015-05-11

In this work, a C18 composite solid-phase microextraction (SPME) fiber was prepared with a new method and applied to the analysis of organochlorine pesticides (OCPs) in water sample. A stainless steel wire (o.d. 127 μm) was used as the substrate, and a mixture of the C18 particle (3.5 μm) and the 184 silicone was used as the coating material. During the process of fiber preparation, a section of capillary column was used to fix the mixture onto the stainless steel wire and to ensure the constant of coating thickness. The prepared fiber showed excellent thermal stability and solvent resistance. By coupling with gas chromatography-mass spectrometry (GC-MS), the fiber exhibited wide linearity (2-500 ng L(-1)) and good sensitivity for the determination of six OCPs in water samples, the OCPs tested included hexachlorobezene, trans-chlordane, cis-chlordane, o,p-DDT, p,p-DDT and mirex. Not only the extraction performance of the newly prepared fiber was more than seven times higher than those of commercial fibers, the limits of detections (LODs) (0.059-0.151 ng L(-1)) for OCPs achieved under optimized conditions were also lower than those of reported SPME methods. The fiber was successfully applied to the determination of OCPs in real water samples by using developed SPME-GC-MS method. Copyright © 2015 Elsevier B.V. All rights reserved.

Phytoplankton Enumeration and Evaluation Experiments

DTIC Science & Technology

2009-05-01

deballasted in another. The entrained organisms are generally discharged along with the ballast water. This process has been identified as a vector...ballasted in one port and deballasted in another. This process has been identified as a vector for the translocation of non- indigenous species (NIS...the probability that variable rates of cell survival from the irradiation process impacted NRLKW s ability to prepare samples with accurate numbers

Dielectrophoresis-Based Sample Handling in General-Purpose Programmable Diagnostic Instruments

PubMed Central

Gascoyne, Peter R. C.; Vykoukal, Jody V.

2009-01-01

As the molecular origins of disease are better understood, the need for affordable, rapid, and automated technologies that enable microscale molecular diagnostics has become apparent. Widespread use of microsystems that perform sample preparation and molecular analysis could ensure that the benefits of new biomedical discoveries are realized by a maximum number of people, even those in environments lacking any infrastructure. While progress has been made in developing miniaturized diagnostic systems, samples are generally processed off-device using labor-intensive and time-consuming traditional sample preparation methods. We present the concept of an integrated programmable general-purpose sample analysis processor (GSAP) architecture where raw samples are routed to separation and analysis functional blocks contained within a single device. Several dielectrophoresis-based methods that could serve as the foundation for building GSAP functional blocks are reviewed including methods for cell and particle sorting, cell focusing, cell ac impedance analysis, cell lysis, and the manipulation of molecules and reagent droplets. PMID:19684877

Bismuth molybdate thick films as ethanol sensor

NASA Astrophysics Data System (ADS)

Jain, Kiran; Kumar, Vipin; Gupta, H. P.; Rastogi, A. C.

2003-10-01

Ethanol sensitivity of bismuth molybdate thick films and sintered pellets were investigated. Sintered pellets were prepared by traditional ceramic processing. Thick films were prepared by metallorganic decomposition process. Ethanol gas sensitivity was measured at various temperatures and concentrations. Thick films of alpha phase bismuth molybdate prepared by spray pyrolysis showed a very fast response to ethanol detection. The response time for the bulk samples is about 40 sec which decreased to about 6 sec for thick films at an operating temperature of 300°C. An extremely low level approximately 10 ppm detection and fast response makes this technique ideal for sensor element fabrication for detection and estimation of alcohol in breath-analyzer. Unlike SnO2, the resistance of these sensors is not affected by humidity at the operating temperature.

Influence of CuO nanoparticle on palm oil based alkyd resin preparation and its antimicrobial activity

NASA Astrophysics Data System (ADS)

Ruey Ong, Huei; Maksudur Rahman Khan, Md.; Ramli, Ridzuan; Shein Hong, Chi; Yunus, Rosli Mohd

2018-03-01

An alkyd resin has been synthesized from palm oil that reacted with glycerol and phthalic anhydride by alcoholysis-polyesterification process and co-catalyzed by CuO nanoparticle. The CuO nanoparticle was pre-prepared in the glycerol via sol gel method, which creates a new reaction condition for resin preparation. The resins were characterized by fourier transform infrared spectroscopy (FTIR), where a new ester linkage bond (C-O-C) was noticed for resin sample. The antimicrobial activity and the curing behaviour of the resin were determined by Kirby-Bauer and differential scanning calorimeter technique. It was found that, the addition of CuO speeded up the reaction rate and played antimicrobial role. Moreover, it shortens the reaction time of alcoholysis and polyesterification process.

Quantitative LIBS analysis of vanadium in samples of hexagonal mesoporous silica catalysts.

PubMed

Pouzar, Miloslav; Kratochvíl, Tomás; Capek, Libor; Smoláková, Lucie; Cernohorský, Tomás; Krejcová, Anna; Hromádko, Ludek

2011-02-15

The method for the analysis of vanadium in hexagonal mesoporous silica (V-HMS) catalysts using Laser Induced Breakdown Spectrometry (LIBS) was suggested. Commercially available LIBS spectrometer was calibrated with the aid of authentic V-HMS samples previously analyzed by ICP OES after microwave digestion. Deposition of the sample on the surface of adhesive tape was adopted as a sample preparation method. Strong matrix effect connected with the catalyst preparation technique (1st vanadium added in the process of HMS synthesis, 2nd already synthesised silica matrix was impregnated by vanadium) was observed. The concentration range of V in the set of nine calibration standards was 1.3-4.5% (w/w). Limit of detection was 0.13% (w/w) and it was calculated as a triple standard deviation from five replicated determinations of vanadium in the real sample with a very low vanadium concentration. Comparable results of LIBS and ED XRF were obtained if the same set of standards was used for calibration of both methods and vanadium was measured in the same type of real samples. LIBS calibration constructed using V-HMS-impregnated samples failed for measuring of V-HMS-synthesized samples. LIBS measurements seem to be strongly influenced with different chemical forms of vanadium in impregnated and synthesised samples. The combination of LIBS and ED XRF is able to provide new information about measured samples (in our case for example about procedure of catalyst preparation). Copyright © 2010 Elsevier B.V. All rights reserved.

Enhanced 99Tc retention in glass waste form using Tc(IV)-incorporated Fe minerals

DOE PAGES

Um, Wooyong; Luksic, Steven A.; Wang, Guohui; ...

2017-09-07

We present that technetium ( 99Tc) immobilization by doping into iron oxide mineral phases may alleviate the problems with Tc volatility during vitrification of nuclear waste. Because reduced Tc, Tc(IV), substitutes for Fe(III) in the crystal structure by a process of Tc reduction from Tc(VII) to Tc(IV) followed by co-precipitation of Fe oxide minerals, two Tc-incorporated Fe minerals (Tc-goethite and Tc-magnetite/maghemite) were prepared and tested for Tc retention in glass melt samples at temperatures between 600 and 1000 °C. After being cooled, the solid glass specimens prepared at different temperatures at 600, 800, and 1000 °C were analyzed for Tcmore » oxidation state using Tc K-edge XANES. In most samples, Tc was partially (<60%) oxidized from Tc(IV) to Tc(VII) as the melt temperature increased up to 600 °C. However, most of Tc(IV) was completely (>95%) oxidized to Tc(VII) at temperature above 800 °C. Tc retention in glass melt samples prepared using Tc-incorporated Fe minerals were slightly higher (~10%) than in glass prepared using KTcO4 because of limited and delayed Tc volatilization.« less

Enhanced 99Tc retention in glass waste form using Tc(IV)-incorporated Fe minerals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Um, Wooyong; Luksic, Steven A.; Wang, Guohui

We present that technetium ( 99Tc) immobilization by doping into iron oxide mineral phases may alleviate the problems with Tc volatility during vitrification of nuclear waste. Because reduced Tc, Tc(IV), substitutes for Fe(III) in the crystal structure by a process of Tc reduction from Tc(VII) to Tc(IV) followed by co-precipitation of Fe oxide minerals, two Tc-incorporated Fe minerals (Tc-goethite and Tc-magnetite/maghemite) were prepared and tested for Tc retention in glass melt samples at temperatures between 600 and 1000 °C. After being cooled, the solid glass specimens prepared at different temperatures at 600, 800, and 1000 °C were analyzed for Tcmore » oxidation state using Tc K-edge XANES. In most samples, Tc was partially (<60%) oxidized from Tc(IV) to Tc(VII) as the melt temperature increased up to 600 °C. However, most of Tc(IV) was completely (>95%) oxidized to Tc(VII) at temperature above 800 °C. Tc retention in glass melt samples prepared using Tc-incorporated Fe minerals were slightly higher (~10%) than in glass prepared using KTcO4 because of limited and delayed Tc volatilization.« less

Improved electron transport properties of n-type naphthalenediimide polymers through refined molecular ordering and orientation induced by processing solvents.

PubMed

An, Yujin; Long, Dang Xuan; Kim, Yiho; Noh, Yong-Young; Yang, Changduk

2016-05-14

To determine the role played by the choice of processing solvents in governing the photophysics, microstructure, and charge carrier transport in naphthalenediimide (NDI)-based polymers, we have prepared two new NDI-bithiophene (T2)- and NDI-thienothiophene (TTh)-containing polymers with hybrid siloxane pentyl chains (SiC5) (P(NDI2SiC5-T2) and P(NDI2SiC5-TTh)). Among the various processing solvents studied here, the films prepared using chloroform exhibited far better electron mobilities (0.16 ± 0.1-0.21 ± 0.05 cm(2) V(-1) s(-1)) than the corresponding samples prepared from different solvents, exceeding one order of magnitude higher, indicating the significant influence of the processing solvent on the charge transport. Upon thin-film analysis using atomic force microscopy and grazing incidence X-ray diffraction, we discovered that molecular ordering and orientation are affected by the choice of the processing solvent, which is responsible for the change in the transport characteristics of this class of polymers.

Magnetoelectrets prepared by using temperature gradient method

NASA Astrophysics Data System (ADS)

Ojha, Pragya; Qureshi, M. S.; Malik, M. M.

2015-05-01

A novel Temperature Gradient method for preparation of magnetoelectret is proposed. Non uniform magnetic field and temperature gradient are expected to be the main cause for the formation of magnetoelectrets (MEs). Being bad conductors of heat, during their formation, there is a possibility for the existence of a temperature gradient along the dielectric electrode interface. In this condition, the motion of, molecules and charge carriers are dependent on Temperature Gradient in a preferred direction. To increase this temperature gradient on both sides of the sample novel method for the preparation of MEs is developed for the first time. For this method the special sample holders are designed in our laboratory. MEs are prepared in such a way that one surface is cooled and the other is heated, during the process. With the help of XRD analysis using Type-E orientation pattern and surface charge studies on magnetoelectrets, the two main causes Non uniform magnetic field and temperature gradient for the formation of magnetoelectrets (MEs), are authenticated experimentally.

Hydroxyapatite with Permanent Electrical Polarization: Preparation, Characterization, and Response against Inorganic Adsorbates.

PubMed

Rivas, Manuel; Del Valle, Luis J; Armelin, Elaine; Bertran, Oscar; Turon, Pau; Puiggalí, Jordi; Alemán, Carlos

2018-04-16

Permanently polarized hydroxyapatite (HAp) particles have been prepared by applying a constant DC of 500 V at 1000 °C for 1 h to the sintered mineral. This process causes important chemical changes, as the formation of OH - defects (vacancies), the disappearance of hydrogenophosphate ions at the mineral surface layer, and structural variations reflected by the increment of the crystallinity. As a consequence, the electrochemical properties and electrical conductivity of the polarized mineral increase noticeably compared with as-prepared and sintered samples. Moreover, these increments remain practically unaltered after several months. In addition, permanent polarization favours significantly the ability of HAp to adsorb inorganic bioadsorbates in comparison with as-prepared and sintered samples. The adsorbates cause a significant increment of the electrochemical stability and electrical conductivity with respect to bare polarized HAp, which may have many implications for biomedical applications of permanently polarized HAp. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Guidelines for Contracting Microfilming Services.

ERIC Educational Resources Information Center

Byrne, Sherry

1986-01-01

Outlines the process involved in selecting an outside filming agent for the purpose of preserving a library's or archive's holdings. Guidelines include project planning, selecting a filming agent, and contract preparation and maintenance. A sample contract is included. (Author/EM)

A highly sensitive and accurate gene expression analysis by sequencing ("bead-seq") for a single cell.

PubMed

Matsunaga, Hiroko; Goto, Mari; Arikawa, Koji; Shirai, Masataka; Tsunoda, Hiroyuki; Huang, Huan; Kambara, Hideki

2015-02-15

Analyses of gene expressions in single cells are important for understanding detailed biological phenomena. Here, a highly sensitive and accurate method by sequencing (called "bead-seq") to obtain a whole gene expression profile for a single cell is proposed. A key feature of the method is to use a complementary DNA (cDNA) library on magnetic beads, which enables adding washing steps to remove residual reagents in a sample preparation process. By adding the washing steps, the next steps can be carried out under the optimal conditions without losing cDNAs. Error sources were carefully evaluated to conclude that the first several steps were the key steps. It is demonstrated that bead-seq is superior to the conventional methods for single-cell gene expression analyses in terms of reproducibility, quantitative accuracy, and biases caused during sample preparation and sequencing processes. Copyright © 2014 Elsevier Inc. All rights reserved.

Preanalytics in lung cancer.

PubMed

Warth, Arne; Muley, Thomas; Meister, Michael; Weichert, Wilko

2015-01-01

Preanalytic sampling techniques and preparation of tissue specimens strongly influence analytical results in lung tissue diagnostics both on the morphological but also on the molecular level. However, in contrast to analytics where tremendous achievements in the last decade have led to a whole new portfolio of test methods, developments in preanalytics have been minimal. This is specifically unfortunate in lung cancer, where usually only small amounts of tissue are at hand and optimization in all processing steps is mandatory in order to increase the diagnostic yield. In the following, we provide a comprehensive overview on some aspects of preanalytics in lung cancer from the method of sampling over tissue processing to its impact on analytical test results. We specifically discuss the role of preanalytics in novel technologies like next-generation sequencing and in the state-of the-art cytology preparations. In addition, we point out specific problems in preanalytics which hamper further developments in the field of lung tissue diagnostics.

Containerless preparation of advanced optical glasses: Experiment 77F095

NASA Technical Reports Server (NTRS)

Happe, R. A.; Kim, K. S.

1982-01-01

Containerless processing of optical glasses was studied in preparation for space shuttle MEA flight experiments. Ground based investigation, experiment/hardware coordination activities and development of flight experiment and sample characterization plans were investigated. In the ground based investigation over 100 candidate glass materials for space processing were screened and promising compositions were identified. The system of Nb2O5-TiO2-CaO was found to be very rich with containerless glass compositions and as extensive number of the oxides combinations were tried resulting in a glass formation ternary phase diagram. The frequent occurrence of glass formation by containerless processing among the compositions for which no glass formations were previously reported indicated the possibility and an advantage of containerless processing in a terrestrial environment.

Recovery of Picloram and 2,4-Dichlorophenoxyacetic Acid from Aqueous Samples by Reversed-Phase Solid-Phase Extraction

Treesearch

Martha J.M. Wells; Jerry L. Michael

1987-01-01

Extensive preparation of samples before chromatographic analysis is usually the most time-consuming process in the determination of many organic compounds in environmental matrices. In the past, removal of some organic from aqueous solution was commonly done by liquid/liquid extraction. However, the introduction of stable, covalently bonded reversed-phase sorbents now...

All Plasma Products Are Not Created Equal: Characterizing Differences Between Plasma Products

DTIC Science & Technology

2015-06-01

2011;6(4):e18812. 24. Chandler WL. Microparticle counts in platelet - rich and platelet -free plasma , effect of centrifugation and sample-processing protocols...used throughout the article for this product. Laboratory Methods Platelet -Poor Plasma Preparation Platelet -poor plasma (PPP) was prepared by centrifuga... platelets , respectively. Flow cytometry was performed as described by Matijevic et al.4 Briefly, 10 KL of each plasma product was incubated with

Sample preparation for sequencing hits from one-bead-one-peptide combinatorial libraries by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry.

PubMed

Martínez-Ceron, María C; Giudicessi, Silvana L; Marani, Mariela M; Albericio, Fernando; Cascone, Osvaldo; Erra-Balsells, Rosa; Camperi, Silvia A

2010-05-15

Optimization of bead analysis by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) after the screening of one-bead-one-peptide combinatorial libraries was achieved, involving the fine-tuning of the whole process. Guanidine was replaced by acetonitrile (MeCN)/acetic acid (AcOH)/water (H(2)O), improving matrix crystallization. Peptide-bead cleavage with NH(4)OH was cheaper and safer than, yet as efficient as, NH(3)/tetrahydrofuran (THF). Peptide elution in microtubes instead of placing the beads in the sample plate yielded more sample aliquots. Successive dry layers deposit sample preparation was better than the dried droplet method. Among the matrices analyzed, alpha-cyano-4-hydroxycinnamic acid resulted in the best peptide ion yield. Cluster formation was minimized by the addition of additives to the matrix. Copyright 2010 Elsevier Inc. All rights reserved.

Direct PCR Offers a Fast and Reliable Alternative to Conventional DNA Isolation Methods for Gut Microbiomes.

PubMed

Videvall, Elin; Strandh, Maria; Engelbrecht, Anel; Cloete, Schalk; Cornwallis, Charlie K

2017-01-01

The gut microbiome of animals is emerging as an important factor influencing ecological and evolutionary processes. A major bottleneck in obtaining microbiome data from large numbers of samples is the time-consuming laboratory procedures required, specifically the isolation of DNA and generation of amplicon libraries. Recently, direct PCR kits have been developed that circumvent conventional DNA extraction steps, thereby streamlining the laboratory process by reducing preparation time and costs. However, the reliability and efficacy of direct PCR for measuring host microbiomes have not yet been investigated other than in humans with 454 sequencing. Here, we conduct a comprehensive evaluation of the microbial communities obtained with direct PCR and the widely used Mo Bio PowerSoil DNA extraction kit in five distinct gut sample types (ileum, cecum, colon, feces, and cloaca) from 20 juvenile ostriches, using 16S rRNA Illumina MiSeq sequencing. We found that direct PCR was highly comparable over a range of measures to the DNA extraction method in cecal, colon, and fecal samples. However, the two methods significantly differed in samples with comparably low bacterial biomass: cloacal and especially ileal samples. We also sequenced 100 replicate sample pairs to evaluate repeatability during both extraction and PCR stages and found that both methods were highly consistent for cecal, colon, and fecal samples ( r s > 0.7) but had low repeatability for cloacal ( r s = 0.39) and ileal ( r s = -0.24) samples. This study indicates that direct PCR provides a fast, cheap, and reliable alternative to conventional DNA extraction methods for retrieving 16S rRNA data, which can aid future gut microbiome studies. IMPORTANCE The microbial communities of animals can have large impacts on their hosts, and the number of studies using high-throughput sequencing to measure gut microbiomes is rapidly increasing. However, the library preparation procedure in microbiome research is both costly and time-consuming, especially for large numbers of samples. We investigated a cheaper and faster direct PCR method designed to bypass the DNA isolation steps during 16S rRNA library preparation and compared it with a standard DNA extraction method. We used both techniques on five different gut sample types collected from 20 juvenile ostriches and sequenced samples with Illumina MiSeq. The methods were highly comparable and highly repeatable in three sample types with high microbial biomass (cecum, colon, and feces), but larger differences and low repeatability were found in the microbiomes obtained from the ileum and cloaca. These results will help microbiome researchers assess library preparation procedures and plan their studies accordingly.

Thermal stability and magnetic properties of MgFe2O4@ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Mallesh, S.; Prabu, D.; Srinivas, V.

2017-05-01

Magnesium ferrite, MgFe2O4, (MgFO) nanoparticles (NPs) have been synthesized through sol-gel process. Subsequently, as prepared particles were coated with Zinc-oxide (ZnO) layer(s) through ultrasonication process. Thermal stability, structure and magnetic properties of as-prepared (AP) and annealed samples in the temperature range of 350 °C-1200 °C have been investigated. Structural data suggests that AP MgFO NPs and samples annealed below 500 °C in air exhibit stable ferrite phase. However, α-Fe2O3 and a small fraction of MgO secondary phases appear along with ferrite phase on annealing in the temperatures range 500 °C- 1000 °C. This results in significant changes in magnetic moment for AP NPs 0.77 μB increases to 0.92 μB for 1200 °C air annealed sample. The magnetic properties decreased at intermediate temperatures due to the presence of secondary phases. On the other hand, pure ferrite phase could be stabilized with an optimum amount of ZnO coated MgFO NPs for samples annealed in the temperature range 500 °C-1000 °C with improvement in magnetic behavior compared to that of MgFO samples.

SLUDGE WASHING AND DEMONSTRATION OF THE DWPF FLOWSHEET IN THE SRNL SHIELDED CELLS FOR SLUDGE BATCH 7A QUALIFICATION

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pareizs, J.; Billings, A.; Click, D.

2011-07-08

Waste Solidification Engineering (WSE) has requested that characterization and a radioactive demonstration of the next batch of sludge slurry (Sludge Batch 7a*) be completed in the Shielded Cells Facility of the Savannah River National Laboratory (SRNL) via a Technical Task Request (TTR). This characterization and demonstration, or sludge batch qualification process, is required prior to transfer of the sludge from Tank 51 to the Defense Waste Processing Facility (DWPF) feed tank (Tank 40). The current WSE practice is to prepare sludge batches in Tank 51 by transferring sludge from other tanks. Discharges of nuclear materials from H Canyon are oftenmore » added to Tank 51 during sludge batch preparation. The sludge is washed and transferred to Tank 40, the current DWPF feed tank. Prior to transfer of Tank 51 to Tank 40, SRNL simulates the Tank Farm and DWPF processes with a Tank 51 sample (referred to as the qualification sample). Sludge Batch 7a (SB7a) is composed of portions of Tanks 4, 7, and 12; the Sludge Batch 6 heel in Tank 51; and a plutonium stream from H Canyon. SRNL received the Tank 51 qualification sample (sample ID HTF-51-10-125) following sludge additions to Tank 51. This report documents: (1) The washing (addition of water to dilute the sludge supernate) and concentration (decanting of supernate) of the SB7a - Tank 51 qualification sample to adjust sodium content and weight percent insoluble solids to Tank Farm projections. (2) The performance of a DWPF Chemical Process Cell (CPC) simulation using the washed Tank 51 sample. The simulation included a Sludge Receipt and Adjustment Tank (SRAT) cycle, where acid was added to the sludge to destroy nitrite and reduce mercury, and a Slurry Mix Evaporator (SME) cycle, where glass frit was added to the sludge in preparation for vitrification. The SME cycle also included replication of five canister decontamination additions and concentrations. Processing parameters were based on work with a non-radioactive simulant. (3) Vitrification of a portion of the SME product and characterization and durability testing (as measured by the Product Consistency Test (PCT)) of the resulting glass. (4) Rheology measurements of the initial slurry samples and samples after each phase of CPC processing. This program was controlled by a Task Technical and Quality Assurance Plan (TTQAP), and analyses were guided by an Analytical Study Plan. This work is Technical Baseline Research and Development (R&D) for the DWPF. It should be noted that much of the data in this document has been published in interoffice memoranda. The intent of this technical report is bring all of the SB7a related data together in a single permanent record and to discuss the overall aspects of SB7a processing.« less

Stability of Mixed Preparations Consisting of Commercial Moisturizing Creams with an Ointment Base Investigated by Magnetic Resonance Imaging.

PubMed

Onuki, Yoshinori; Funatani, Chiaki; Yamamoto, Yoshihisa; Fukami, Toshiro; Koide, Tatsuo; Hayashi, Yoshihiro; Takayama, Kozo

2017-01-01

A moisturizing cream mixed with a steroid ointment is frequently prescribed to patients suffering from atopic dermatitis. However, there is a concern that the mixing operation causes destabilization. The present study was performed to investigate the stability of such preparations closely using magnetic resonance imaging (MRI). As sample preparations, five commercial moisturizing creams that are popular in Japan were mixed with an ointment base, a white petrolatum, at a volume ratio of 1 : 1. The mixed preparations were stored at 60°C to accelerate the destabilization processes. Subsequently, the phase separations induced by the storage test were monitored using MRI. Using advanced MR technologies including spin-spin relaxation time (T 2 ) mapping and MR spectroscopy, we successfully characterized the phase-separation behavior of the test samples. For most samples, phase separations developed by the bleeding of liquid oil components. From a sample consisting of an oil-in-water-type cream, Urepearl Cream 10%, a distinct phase-separation mode was observed, which was initiated by the aqueous component separating from the bottom part of the sample. The resultant phase separation was the most distinct among the test samples. To investigate the phase separation quantitatively and objectively, we conducted a histogram analysis on the acquired T 2 maps. The water-in-oil type creams were found to be much more stable after mixing with ointment base than those of oil-in-water type creams. This finding strongly supported the validity of the mixing operation traditionally conducted in pharmacies.

Comparative Evaluation of Small Molecular Additives and Their Effects on Peptide/Protein Identification.

PubMed

Gao, Jing; Zhong, Shaoyun; Zhou, Yanting; He, Han; Peng, Shuying; Zhu, Zhenyun; Liu, Xing; Zheng, Jing; Xu, Bin; Zhou, Hu

2017-06-06

Detergents and salts are widely used in lysis buffers to enhance protein extraction from biological samples, facilitating in-depth proteomic analysis. However, these detergents and salt additives must be efficiently removed from the digested samples prior to LC-MS/MS analysis to obtain high-quality mass spectra. Although filter-aided sample preparation (FASP), acetone precipitation (AP), followed by in-solution digestion, and strong cation exchange-based centrifugal proteomic reactors (CPRs) are commonly used for proteomic sample processing, little is known about their efficiencies at removing detergents and salt additives. In this study, we (i) developed an integrative workflow for the quantification of small molecular additives in proteomic samples, developing a multiple reaction monitoring (MRM)-based LC-MS approach for the quantification of six additives (i.e., Tris, urea, CHAPS, SDS, SDC, and Triton X-100) and (ii) systematically evaluated the relationships between the level of additive remaining in samples following sample processing and the number of peptides/proteins identified by mass spectrometry. Although FASP outperformed the other two methods, the results were complementary in terms of peptide/protein identification, as well as the GRAVY index and amino acid distributions. This is the first systematic and quantitative study of the effect of detergents and salt additives on protein identification. This MRM-based approach can be used for an unbiased evaluation of the performance of new sample preparation methods. Data are available via ProteomeXchange under identifier PXD005405.

High-density Bi-Pb-Sr-Ca-Cu-O superconductor prepared by rapid thermal melt processing

NASA Astrophysics Data System (ADS)

Moon, B. M.; Lalevic, B.; Kear, B. H.; McCandlish, L. E.; Safari, A.; Meskoob, M.

1989-10-01

A high quality, dense Bi-Pb-Sr-Ca-Cu-O superconductor has been successfully synthesized by rapid thermal melt processing. Conventionally sintered pellets were melted at 1200 °C, cooled rapidly, and then annealed. As-melted samples exhibited semiconductor behavior, which upon annealing became superconducting at 115 K [Tc(zero)=105 K]. A detailed study of various processing techniques has been carried out.

Novel Diffusion-Weighted MRI for High-Grade Prostate Cancer Detection

DTIC Science & Technology

2016-10-01

in image resolution and scale.This process is critical for evaluating new imaging modalities.Our initial findings illustrate the potential of the...eligible for analysis as determined by adequate pathologic processing and MR images deemed to be of adequate quality by the study team.  The...histology samples have been requested from the UIC biorepository for digitization  All MR images have been collected and prepared for image processing

Effect of preparation methods and doping on the structural and tunable emissions of CdS

NASA Astrophysics Data System (ADS)

Mohamed, Mohamed Bakr; Abdel-Kader, M. H.; Alhazime, Ali A.; Almarashi, Jamal Q. M.

2018-03-01

Fe, Mn and Mg doped CdS samples were prepared by thermolysis method in air and under flow of nitrogen. Structural, compositional and optical properties of the prepared samples were investigated using x-ray powder diffraction (XRD), scanning electron microscope (SEM/EDS mapping), Fourier transform infrared red (FTIR), UV-vis absorption and photoluminescence (PL) spectroscopes. Rietveld refinement of x-ray data showed that all the undoped and doped CdS samples prepared in air and under flow of nitrogen have both cubic and hexagonal structures. The percentages of hexagonal and cubic phases for all prepared samples were determined. The crystallite size increased for CdS prepared under flow of N2 compared with the sample prepared in air. The energy gap of all the samples was calculated using UV data. The intensity of PL emission changed according to the method of preparation and the kind of doping elements. PL emission revealed a blue shift for CdS prepared in air compared with CdS prepared under flow of nitrogen; also all doped samples showed a red shift of PL spectra compared with undoped samples. Undoped and doped CdS with Fe and Mg samples emitted violet and blue sub-spectra. Mn doped CdS prepared in air revealed violet, blue and yellow sub-spectra, while the sample prepared under flow of N2 emitted violet, blue and green sub-spectra.

Structural Channels and Atomic-Cluster Insertion in CsxBi4Te6 (1 ≤ x ≤ 1.25) As Observed by Aberration-Corrected Scanning Transmission Electron Microscopy.

PubMed

Zhang, Ruixin; Yang, Huaixin; Guo, Cong; Tian, Huanfang; Shi, Honglong; Chen, Genfu; Li, Jianqi

2016-12-19

Microstructural analyses based on aberration-corrected scanning transmission electron microscopy (STEM) observations demonstrate that low-dimensional Cs x Bi 4 Te 6 materials, known to be a novel thermoelectric and superconducting system, contain notable structural channels that go directly along the b axis, which can be partially filled by atom clusters depending on the thermal treatment process. We successfully prepared two series of Cs x Bi 4 Te 6 single-crystalline samples using two different sintering processes. The Cs x Bi 4 Te 6 samples prepared using an air-quenching method show superconductivity at approximately 4 K, while the Cs x Bi 4 Te 6 with the same nominal compositions prepared by slowly cooling are nonsuperconductors. Moreover, atomic structural investigations of typical samples reveal that the structural channels are often empty in superconducting materials; thus, we can represent the superconducting phase as Cs 1-y Bi 4 Te 6 with considering the point defects in the Cs layers. In addition, the channels in the nonsuperconducting crystals are commonly partially occupied by triplet Bi clusters. Moreover, the average structures for these two phases are also different in their monoclinic angles (β), which are estimated to be 102.3° for superconductors and 100.5° for nonsuperconductors.

Global metabolic profiling procedures for urine using UPLC-MS.

PubMed

Want, Elizabeth J; Wilson, Ian D; Gika, Helen; Theodoridis, Georgios; Plumb, Robert S; Shockcor, John; Holmes, Elaine; Nicholson, Jeremy K

2010-06-01

The production of 'global' metabolite profiles involves measuring low molecular-weight metabolites (<1 kDa) in complex biofluids/tissues to study perturbations in response to physiological challenges, toxic insults or disease processes. Information-rich analytical platforms, such as mass spectrometry (MS), are needed. Here we describe the application of ultra-performance liquid chromatography-MS (UPLC-MS) to urinary metabolite profiling, including sample preparation, stability/storage and the selection of chromatographic conditions that balance metabolome coverage, chromatographic resolution and throughput. We discuss quality control and metabolite identification, as well as provide details of multivariate data analysis approaches for analyzing such MS data. Using this protocol, the analysis of a sample set in 96-well plate format, would take ca. 30 h, including 1 h for system setup, 1-2 h for sample preparation, 24 h for UPLC-MS analysis and 1-2 h for initial data processing. The use of UPLC-MS for metabolic profiling in this way is not faster than the conventional HPLC-based methods but, because of improved chromatographic performance, provides superior metabolome coverage.

Preparation of nanobiochar as magnetic solid acid catalyst by pyrolysis-carbonization from oil palm empty fruit bunches

NASA Astrophysics Data System (ADS)

Jenie, S. N. Aisyiyah; Kristiani, Anis; Kustomo, Simanungkalit, Sabar; Mansur, Dieni

2017-11-01

Nanomaterials based on carbon exhibits unique properties, both physical and chemical, that can be utilized in various application, including catalyst. These nanomaterials were prepared through pyrolysis-carbonization process of biomass, oil palm empty fruit bunches. The effect of carbonization temperature in range of 500°C-600°C were also studied. The magnetic nanobiochar samples, MBC, were sulfonated by using sulfuric acid to increase their properties as solid acid catalyst. Their chemical and physical properties were characterized by Surface Area Analyzer and Porositymeter, X-Ray Diffraction, Scanning Electron Microscopy, Fourier Transform Infra-Red. The magnetic biochar samples obtained from carbonization at 873 K, MBC02-SO3H, was proven to have higher surface area, crystallinity properties and surface chemical composition after sulfonation process, which were confirmed by the BET, XRD and FT-IR analysis. Moreover, sample MBC02-SO3H exhibit promising catalytic acitivity in a catalysed esterification reaction, producing an ester yield of 64%. The result from this work opens new opportunities for the development of magnetic heterogenous acid catalyst from biomass waste.

A novel method for preparing histology slides to integrate the teaching of gross and microscopic anatomy.

PubMed

Provo-Klimek, Judy A; Troyer, Deryl L

2002-01-01

The authors have previously reported the development of a novel technique for sampling and preparing tissue slides for routine microscopic examination, without the use of a microtome. Termed "RAMP" (Rapid Adhesive Mediated Procedure), this simple, albeit somewhat crude, technique holds promise as a method that can be used in the field by veterinary practitioners for rapid microscopic evaluations to obtain early preliminary estimates of the nature of a mass or lesion. We incorporated the use of this method into a gross anatomy course in an attempt to gauge its utility for novices in tissue sampling and histology slide preparation. By having each group of students take a tissue sample from their cadaver, the activity simulated an actual necropsy situation in which practitioners in the field might use the technique. Because students were able to follow their specimen from sampling to microscopic examination, the activity provided a valuable integration of their learning of gross and microscopic anatomy. We conducted an evaluation of the process and the resulting slides with two successive classes of students. We conclude that the RAMP method is reasonably successful in the hands of individuals not trained in tissue preparation; was well received by the students as a valuable learning tool; and could potentially yield useful histological information for practicing veterinarians. Limitations of the method are also discussed.

Effect of drying temperatures on structural performance and photocatalytic activity of BiOCl synthesized by a soft chemical method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Guang, Lu, E-mail: lu_g@163.com; Hui, Wang; Xuejun, Zou

2016-07-15

A group of BiOCl photocatalysts with different drying temperatures were prepared by a soft chemical method. The effects of drying temperatures on the crystalline phase, morphology, surface area and optical property of as-prepared samples were investigated in detail by XRD, SEM, N{sub 2} absorption–desorption and DRS. Moreover, their photocatalytic activities on the degradation of rhodamine B were evaluated under visible light irradiation. It was found that the sample dried at 120 °C had the best photocatalytic activity, which was mainly attributed to the highest exposing proportion of {001} facets correspond to BiOCl, largest BET and minimum bandgap. The degradation mechanismmore » was explored that superoxide radicals were mainly contributed to the degradation of chromophore, however, holes and hydroxyl were mainly contributed to the photo degradation. Moreover, holes and hydroxyl dominated the degradation of RhB. - Graphical abstract: Holes, hydroxyl and superoxide radicals can attribute to the degradation process but take different degradation pathways. Superoxide radicals mainly contribute to the degradation of chromophore, however, holes and hydroxyl mainly contribute to the photo degradation. Display Omitted - Highlights: • BiOCl nanosheets were prepared by a soft chemical method. • Effect of drying temperatures on as-prepared BiOCl samples was studied. • The highest removal efficiency of RhB was obtained over the sample dried at 120 °C.« less

Development and optimization of a novel sample preparation method cored on functionalized nanofibers mat-solid-phase extraction for the simultaneous efficient extraction of illegal anionic and cationic dyes in foods.

PubMed

Qi, Feifei; Jian, Ningge; Qian, Liangliang; Cao, Weixin; Xu, Qian; Li, Jian

2017-09-01

A simple and efficient three-step sample preparation method was developed and optimized for the simultaneous analysis of illegal anionic and cationic dyes (acid orange 7, metanil yellow, auramine-O, and chrysoidine) in food samples. A novel solid-phase extraction (SPE) procedure based on nanofibers mat (NFsM) was proposed after solvent extraction and freeze-salting out purification. The preferred SPE sorbent was selected from five functionalized NFsMs by orthogonal experimental design, and the optimization of SPE parameters was achieved through response surface methodology (RSM) based on the Box-Behnken design (BBD). Under the optimal conditions, the target analytes could be completely adsorbed by polypyrrole-functionalized polyacrylonitrile NFsM (PPy/PAN NFsM), and the eluent was directly analyzed by high-performance liquid chromatography-diode array detection (HPLC-DAD). The limits of detection (LODs) were between 0.002 and 0.01 mg kg -1 , and satisfactory linearity with correlation coefficients (R > 0.99) for each dye in all samples was achieved. Compared with the Chinese standard method and the published methods, the proposed method was simplified greatly with much lower requirement of sorbent (5.0 mg) and organic solvent (2.8 mL) and higher sample preparation speed (10 min/sample), while higher recovery (83.6-116.5%) and precision (RSDs < 7.1%) were obtained. With this developed method, we have successfully detected illegal ionic dyes in three common representative foods: yellow croaker, soybean products, and chili seasonings. Graphical abstract Schematic representation of the process of the three-step sample preparation.

An overview of the main foodstuff sample preparation technologies for tetracycline residue determination.

PubMed

Pérez-Rodríguez, Michael; Pellerano, Roberto Gerardo; Pezza, Leonardo; Pezza, Helena Redigolo

2018-05-15

Tetracyclines are widely used for both the treatment and prevention of diseases in animals as well as for the promotion of rapid animal growth and weight gain. This practice may result in trace amounts of these drugs in products of animal origin, such as milk and eggs, posing serious risks to human health. The presence of tetracycline residues in foods can lead to the transmission of antibiotic-resistant pathogenic bacteria through the food chain. In order to ensure food safety and avoid exposure to these substances, national and international regulatory agencies have established tolerance levels for authorized veterinary drugs, including tetracycline antimicrobials. In view of that, numerous sensitive and specific methods have been developed for the quantification of these compounds in different food matrices. One will note, however, that the determination of trace residues in foods such as milk and eggs often requires extensive sample extraction and preparation prior to conducting instrumental analysis. Sample pretreatment is usually the most complicated step in the analytical process and covers both cleaning and pre-concentration. Optimal sample preparation can reduce analysis time and sources of error, enhance sensitivity, apart from enabling unequivocal identification, confirmation and quantification of target analytes. The development and implementation of more environmentally friendly analytical procedures, which involve the use of less hazardous solvents and smaller sample sizes compared to traditional methods, is a rapidly increasing trend in analytical chemistry. This review seeks to provide an updated overview of the main trends in sample preparation for the determination of tetracycline residues in foodstuffs. The applicability of several extraction and clean-up techniques employed in the analysis of foodstuffs, especially milk and egg samples, is also thoroughly discussed. Copyright © 2018 Elsevier B.V. All rights reserved.

Data on green tea flavor determinantes as affected by cultivars and manufacturing processes.

PubMed

Han, Zhuo-Xiao; Rana, Mohammad M; Liu, Guo-Feng; Gao, Ming-Jun; Li, Da-Xiang; Wu, Fu-Guang; Li, Xin-Bao; Wan, Xiao-Chun; Wei, Shu

2017-02-01

This paper presents data related to an article entitled "Green tea flavor determinants and their changes over manufacturing processes" (Han et al., 2016) [1]. Green tea samples were prepared with steaming and pan firing treatments from the tender leaves of tea cultivars 'Bai-Sang Cha' ('BAS') and 'Fuding-Dabai Cha' ('FUD'). Aroma compounds from the tea infusions were detected and quantified using HS-SPME coupled with GC/MS. Sensory evaluation was also made for characteristic tea flavor. The data shows the abundances of the detected aroma compounds, their threshold values and odor characteristics in the two differently processed tea samples as well as two different cultivars.

NASA and Deere to study effects of low-g on iron processing

NASA Technical Reports Server (NTRS)

1981-01-01

A technical exchange agreement to study the effects of processing iron alloys in microgravity is described. Alloy solidification experiments are to be performed in the low-g facilities at Marshall Space Center. Deere is to prepare and evaluate the samples, and perform thermal characterization studies of the furnace used for melting and solidifying the samples. Experiment planning and analysis are to be performed jointly and data shared between the two parties. The technical exchange concept, developed by NASA to involve the private sector in low gravity research programs, is described. Other low gravity processing fields in which industry is invited to participate are listed.

Synthesis and characterization of low-cost activated carbon prepared from Malawian baobab fruit shells by H3PO4 activation for removal of Cu(II) ions: equilibrium and kinetics studies

NASA Astrophysics Data System (ADS)

Vunain, Ephraim; Kenneth, Davie; Biswick, Timothy

2017-12-01

In this study, low-cost activated carbon (AC) prepared from baobab fruit shells by chemical activation using phosphoric acid was evaluated for the removal of Cu(II) ions from aqueous solution. The prepared activated carbon samples were characterized using N2-adsorption-desorption isotherms, SEM, FTIR, EDX and XRD analysis. The sample activated at 700 °C was chosen as our optimized sample because its physicochemical properties and BET results were similar to those of a commercial sample. The N2-adsorption-desorption results of the optimized sample revealed a BET surface area of 1089 m2/g, micropore volume of 0.3764 cm3/g, total pore volume of 0.4330 cm3/g and pore size of 1.45 nm. Operational parameters such as pH, initial copper concentration, contact time, adsorbent dosage and temperature were studied in a batch mode. Equilibrium data were obtained by testing the adsorption data using three different isotherm models: Langmuir, Freundlich and Dubinin-Radushkevish (D-R) models. It was found that the adsorption of copper correlated well with the Langmuir isotherm model with a maximum monolayer adsorption capacity of 3.0833 mg/g. The kinetics of the adsorption process was tested through pseudo-first-order and pseudo-second-order models. The pseudo-second-order kinetic model provided the best correlation for the experimental data studied. The adsorption followed chemisorption process. The study provided an effective use of baobab fruit shells as a valuable source of adsorbents for the removal of copper ions from aqueous solution. This study could add economic value to baobab fruit shells in Malawi, reduce disposal problems, and offer an economic source of AC to the AC users.

Improved chip design for integrated solid-phase microextraction in on-line proteomic sample preparation.

PubMed

Bergkvist, Jonas; Ekström, Simon; Wallman, Lars; Löfgren, Mikael; Marko-Varga, György; Nilsson, Johan; Laurell, Thomas

2002-04-01

A recently introduced silicon microextraction chip (SMEC), used for on-line proteomic sample preparation, has proved to facilitate the process of protein identification by sample clean up and enrichment of peptides. It is demonstrated that a novel grid-SMEC design improves the operating characteristics for solid-phase microextraction, by reducing dispersion effects and thereby improving the sample preparation conditions. The structures investigated in this paper are treated both numerically and experimentally. The numerical approach is based on finite element analysis of the microfluidic flow in the microchip. The analysis is accomplished by use of the computational fluid dynamics-module FLOTRAN in the ANSYS software package. The modeling and analysis of the previously reported weir-SMEC design indicates some severe drawbacks, that can be reduced by changing the microextraction chip geometry to the grid-SMEC design. The overall analytical performance was thereby improved and also verified by experimental work. Matrix-assisted laser desorption/ionization mass spectra of model peptides extracted from both the weir-SMEC and the new grid-SMEC support the numerical analysis results. Further use of numerical modeling and analysis of the SMEC structures is also discussed and suggested in this work.

Freezing of homogenized sputum samples for intermittent storage.

PubMed

Holz, O; Mücke, M; Zarza, P; Loppow, D; Jörres, R A; Magnussen, H

2001-08-01

Among the reasons that restrict the application of sputum induction in outpatient settings is the need for processing of samples within 2 h after induction. The aim of our study was to assess whether freezing is suitable for intermediate storage of sputum samples before processing. We compared differential cell counts between two sputum aliquots derived from the same sample. One aliquot was processed within 2 h after production and one, after it had been frozen under addition of dimethyl-sulfoxid (DMSO) and stored up to 10 days at -20 degrees C. Thirty-five samples were frozen immediately prior to preparation of cytospins, and 10 samples were frozen at an even earlier stage, directly after homogenization. In both sets of experiments we observed a significant relationship between frozen and native samples regarding macrophages, neutrophils and eosinophils, as indicated by respective intraclass correlation coefficients of 0.96, 0.96, and 0.93 in the first, and of 0.92, 0.96 and 0.77 in the second experiments. Our results indicate that the freezing of sputum samples at different stages of processing does not alter sputum morphology to an extent that affects the results of differential cell counts.

The Successful Diagnosis and Typing of Systemic Amyloidosis Using A Microwave-Assisted Filter-Aided Fast Sample Preparation Method and LC/MS/MS Analysis

PubMed Central

Zou, Lili; Shen, Kaini; Zhong, Dingrong; Zhou, Daobin; Sun, Wei; Li, Jian

2015-01-01

Laser microdissection followed by mass spectrometry has been successfully used for amyloid typing. However, sample contamination can interfere with proteomic analysis, and overnight digestion limits the analytical throughput. Moreover, current quantitative analysis methods are based on the spectrum count, which ignores differences in protein length and may lead to misdiagnoses. Here, we developed a microwave-assisted filter-aided sample preparation (maFASP) method that can efficiently remove contaminants with a 10-kDa cutoff ultrafiltration unit and can accelerate the digestion process with the assistance of a microwave. Additionally, two parameters (P- and D-scores) based on the exponentially modified protein abundance index were developed to define the existence of amyloid deposits and those causative proteins with the greatest abundance. Using our protocol, twenty cases of systemic amyloidosis that were well-typed according to clinical diagnostic standards (training group) and another twenty-four cases without subtype diagnoses (validation group) were analyzed. Using this approach, sample preparation could be completed within four hours. We successfully subtyped 100% of the cases in the training group, and the diagnostic success rate in the validation group was 91.7%. This maFASP-aided proteomic protocol represents an efficient approach for amyloid diagnosis and subtyping, particularly for serum-contaminated samples. PMID:25984759

Sample-to-answer palm-sized nucleic acid testing device towards low-cost malaria mass screening.

PubMed

Choi, Gihoon; Prince, Theodore; Miao, Jun; Cui, Liwang; Guan, Weihua

2018-05-19

The effectiveness of malaria screening and treatment highly depends on the low-cost access to the highly sensitive and specific malaria test. We report a real-time fluorescence nucleic acid testing device for malaria field detection with automated and scalable sample preparation capability. The device consists a compact analyzer and a disposable microfluidic reagent compact disc. The parasite DNA sample preparation and subsequent real-time LAMP detection were seamlessly integrated on a single microfluidic compact disc, driven by energy efficient non-centrifuge based magnetic field interactions. Each disc contains four parallel testing units which could be configured either as four identical tests or as four species-specific tests. When configured as species-specific tests, it could identify two of the most life-threatening malaria species (P. falciparum and P. vivax). The NAT device is capable of processing four samples simultaneously within 50 min turnaround time. It achieves a detection limit of ~0.5 parasites/µl for whole blood, sufficient for detecting asymptomatic parasite carriers. The combination of the sensitivity, specificity, cost, and scalable sample preparation suggests the real-time fluorescence LAMP device could be particularly useful for malaria screening in the field settings. Copyright © 2018 Elsevier B.V. All rights reserved.

High-throughput continuous hydrothermal synthesis of nanomaterials (part II): unveiling the as-prepared CexZryYzO2-δ phase diagram.

PubMed

Quesada-Cabrera, Raul; Weng, Xiaole; Hyett, Geoff; Clark, Robin J H; Wang, Xue Z; Darr, Jawwad A

2013-09-09

High-throughput continuous hydrothermal flow synthesis was used to manufacture 66 unique nanostructured oxide samples in the Ce-Zr-Y-O system. This synthesis approach resulted in a significant increase in throughput compared to that of conventional batch or continuous hydrothermal synthesis methods. The as-prepared library samples were placed into a wellplate for both automated high-throughput powder X-ray diffraction and Raman spectroscopy data collection, which allowed comprehensive structural characterization and phase mapping. The data suggested that a continuous cubic-like phase field connects all three Ce-Zr-O, Ce-Y-O, and Y-Zr-O binary systems together with a smooth and steady transition between the structures of neighboring compositions. The continuous hydrothermal process led to as-prepared crystallite sizes in the range of 2-7 nm (as determined by using the Scherrer equation).

Adsorptive removal of an anionic dye Congo red by flower-like hierarchical magnesium oxide (MgO)-graphene oxide composite microspheres

NASA Astrophysics Data System (ADS)

Xu, Jing; Xu, Difa; Zhu, Bicheng; Cheng, Bei; Jiang, Chuanjia

2018-03-01

Flower-like magnesium oxide (MgO) microspheres and MgO-graphene oxide (GO) composites with an average diameter of 500 nm and hierarchical structure were synthesized through an ethylene glycol-mediated self-assembly process. The adsorption of Congo red (CR) by the prepared samples was evaluated in water under ambient conditions. The equilibrium adsorption isotherms of CR on the as-prepared samples could be described by the Langmuir model. The MgO-GO microspheres prepared with 0.5 wt% GO showed higher adsorption capacity (237.0 mg/g) than the MgO microspheres (227.7 mg/g). Adsorption kinetics results of CR indicated that pseudo-second-order kinetic equation could well explain the adsorption kinetics behaviors of CR. These findings indicate that the MgO-GO composite microspheres are potential adsorbents for effective removal of Congo red from wastewater.

High-throughput sample processing and sample management; the functional evolution of classical cytogenetic assay towards automation.

PubMed

Ramakumar, Adarsh; Subramanian, Uma; Prasanna, Pataje G S

2015-11-01

High-throughput individual diagnostic dose assessment is essential for medical management of radiation-exposed subjects after a mass casualty. Cytogenetic assays such as the Dicentric Chromosome Assay (DCA) are recognized as the gold standard by international regulatory authorities. DCA is a multi-step and multi-day bioassay. DCA, as described in the IAEA manual, can be used to assess dose up to 4-6 weeks post-exposure quite accurately but throughput is still a major issue and automation is very essential. The throughput is limited, both in terms of sample preparation as well as analysis of chromosome aberrations. Thus, there is a need to design and develop novel solutions that could utilize extensive laboratory automation for sample preparation, and bioinformatics approaches for chromosome-aberration analysis to overcome throughput issues. We have transitioned the bench-based cytogenetic DCA to a coherent process performing high-throughput automated biodosimetry for individual dose assessment ensuring quality control (QC) and quality assurance (QA) aspects in accordance with international harmonized protocols. A Laboratory Information Management System (LIMS) is designed, implemented and adapted to manage increased sample processing capacity, develop and maintain standard operating procedures (SOP) for robotic instruments, avoid data transcription errors during processing, and automate analysis of chromosome-aberrations using an image analysis platform. Our efforts described in this paper intend to bridge the current technological gaps and enhance the potential application of DCA for a dose-based stratification of subjects following a mass casualty. This paper describes one such potential integrated automated laboratory system and functional evolution of the classical DCA towards increasing critically needed throughput. Published by Elsevier B.V.

Sample Results From The Extraction, Scrub, And Strip Test For The Blended NGS Solvent

DOE Office of Scientific and Technical Information (OSTI.GOV)

Washington, A. L. II; Peters, T. B.

This report summarizes the results of the extraction, scrub, and strip testing for the September 2013 sampling of the Next Generation Solvent (NGS) Blended solvent from the Modular Caustic Side-Solvent Extraction Unit (MCU) Solvent Hold Tank. MCU is in the process of transitioning from the BOBCalixC6 solvent to the NGS Blend solvent. As part of that transition, MCU has intentionally created a blended solvent to be processed using the Salt Batch program. This sample represents the first sample received from that blended solvent. There were two ESS tests performed where NGS blended solvent performance was assessed using either the Tankmore » 21 material utilized in the Salt Batch 7 analyses or a simulant waste material used in the V-5/V-10 contactor testing. This report tabulates the temperature corrected cesium distribution, or D Cs values, step recovery percentage, and actual temperatures recorded during the experiment. This report also identifies the sample receipt date, preparation method, and analysis performed in the accumulation of the listed values. The calculated extraction D Cs values using the Tank 21H material and simulant are 59.4 and 53.8, respectively. The DCs values for two scrub and three strip processes for the Tank 21 material are 4.58, 2.91, 0.00184, 0.0252, and 0.00575, respectively. The D-values for two scrub and three strip processes for the simulant are 3.47, 2.18, 0.00468, 0.00057, and 0.00572, respectively. These values are similar to previous measurements of Salt Batch 7 feed with lab-prepared blended solvent. These numbers are considered compatible to allow simulant testing to be completed in place of actual waste due to the limited availability of feed material.« less

The Synthesis and Photoluminescent Properties of CaMoO₄:Eu³⁺ Nanocrystals by a Soft Chemical Route.

PubMed

Li, Fuhai; Yu, Lixin; Sun, Jiaju; Li, Songchu; Wei, Shuilin

2017-04-01

In this paper, the CaMoO4:Eu3+ phosphors were prepared by a simple hydrothermal method assisted by the citric acid as the surfactant, and characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and fluorescent spectrophotometry. The results of XRD show that the as-prepared samples are single phase. The process of the Ostwald ripening is controlled by the content of the citric acid in the hydrothermal reaction. The pH value of the precursor affects the shift of the charge transition band (CTB) in the excitation spectra. The reaction condition can strongly affect the luminescent intensity of the samples.

Thermal reaction of sonochemically prepared amorphous Fe/C

NASA Astrophysics Data System (ADS)

Miyatani, R.; Kobayashi, Y.; Yamada, Y.

2017-11-01

An amorphous iron/carbon mixture was prepared by sonolysis of ferrocene in diphenylmethane. Heating of the amorphous mixture at 900 or 1200 °C produced nanoparticles, which were then analyzed using Mössbauer spectroscopy, X-ray diffraction, and transmission electron microscopy. The nanoparticles obtained after heating were spherical with diameters of about 50 nm. The sample obtained after heating at 900 °C consisted of α-Fe and Fe 3C, whereas the sample obtained after heating at 1200 °C consisted of α-Fe and γ-Fe. The reaction of the mixture during the heating process was accompanied by the formation of carbon nanotubes catalyzed by the iron or iron carbide nanoparticles.

Facile synthesis of SiO{sub 2} nanoparticles for biomedical applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Scano, A., E-mail: alescano80@tiscali.it; Pilloni, M., E-mail: alescano80@tiscali.it; Cabras, V., E-mail: alescano80@tiscali.it

Silica nanoparticles (SiO{sub 2} NPs) for biomedical applications have been prepared by using a facile modified Stöber-synthesis. Potassium borohydride (KBH{sub 4}) has been introduced in the synthesis procedure in order to control NP size. Several samples have been prepared varying tetraethylorthosilicate (TEOS) concentration, and using different process conditions (temperature, reaction time and atmosphere). In order to study the influence of the process conditions on the NP size, morphology and properties, several characterization techniques were used. Size and morphology of the as-prepared SiO{sub 2} NPs have been studied by using Transmission Electron Microscope (TEM) and Dynamic Light Scattering (DLS) techniques. Structuralmore » characterization was carried out by X-ray powder diffraction. To investigate the SiO{sub 2} NP fluorescence emission properties the fluorescence spectroscopy was also used.« less

Database of the United States Coal Pellet Collection of the U.S. Geological Survey Organic Petrology Laboratory

USGS Publications Warehouse

Deems, Nikolaus J.; Hackley, Paul C.

2012-01-01

The Organic Petrology Laboratory (OPL) of the U.S. Geological Survey (USGS) Eastern Energy Resources Science Center in Reston, Virginia, contains several thousand processed coal sample materials that were loosely organized in laboratory drawers for the past several decades. The majority of these were prepared as 1-inch-diameter particulate coal pellets (more than 6,000 pellets; one sample usually was prepared as two pellets, although some samples were prepared in as many as four pellets), which were polished and used in reflected light petrographic studies. These samples represent the work of many scientists from the 1970s to the present, most notably Ron Stanton, who managed the OPL until 2001 (see Warwick and Ruppert, 2005, for a comprehensive bibliography of Ron Stanton's work). The purpose of the project described herein was to organize and catalog the U.S. part of the petrographic sample collection into a comprehensive database (available with this report as a Microsoft Excel file) and to compile and list published studies associated with the various sample sets. Through this work, the extent of the collection is publicly documented as a resource and sample library available to other scientists and researchers working in U.S. coal basins previously studied by organic petrologists affiliated with the USGS. Other researchers may obtain samples in the OPL collection on loan at the discretion of the USGS authors listed in this report and its associated Web page.

A New Automated Method and Sample Data Flow for Analysis of Volatile Nitrosamines in Human Urine*

PubMed Central

Hodgson, James A.; Seyler, Tiffany H.; McGahee, Ernest; Arnstein, Stephen; Wang, Lanqing

2016-01-01

Volatile nitrosamines (VNAs) are a group of compounds classified as probable (group 2A) and possible (group 2B) carcinogens in humans. Along with certain foods and contaminated drinking water, VNAs are detected at high levels in tobacco products and in both mainstream and sidestream smoke. Our laboratory monitors six urinary VNAs—N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosopiperidine (NPIP), N-nitrosopyrrolidine (NPYR), and N-nitrosomorpholine (NMOR)—using isotope dilution GC-MS/MS (QQQ) for large population studies such as the National Health and Nutrition Examination Survey (NHANES). In this paper, we report for the first time a new automated sample preparation method to more efficiently quantitate these VNAs. Automation is done using Hamilton STAR™ and Caliper Staccato™ workstations. This new automated method reduces sample preparation time from 4 hours to 2.5 hours while maintaining precision (inter-run CV < 10%) and accuracy (85% - 111%). More importantly this method increases sample throughput while maintaining a low limit of detection (<10 pg/mL) for all analytes. A streamlined sample data flow was created in parallel to the automated method, in which samples can be tracked from receiving to final LIMs output with minimal human intervention, further minimizing human error in the sample preparation process. This new automated method and the sample data flow are currently applied in bio-monitoring of VNAs in the US non-institutionalized population NHANES 2013-2014 cycle. PMID:26949569

Fabrication of nano structural biphasic materials from phosphogypsum waste and their in vitro applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mohamed, Khaled R., E-mail: Kh_rezk966@yahoo.com; Mousa, Sahar M.; Inorganic Chemistry Department, National Research Centre, Dokki, P.O. Box 12622, 11787 Cairo

2014-02-01

Graphical abstract: (a) Schema of the process, (b) TEM of nano particles of biphasic materials and (c) SEM of post-immersion. - Highlights: • Ratio of HA and β-TCP phases were controlled by thermal treatment. • HA partially decomposed into β-TCP with other bioactive phases. • Calcined HA at 900 °C is the best for the bioactivity behavior. - Abstract: In this study, a novel process of preparing biphasic calcium phosphate (BCP) is proposed. Also its bioactivity for the utilization of the prepared BCP as a biomaterial is studied. A mixture of calcium hydroxyapatite (HAP) and tricalcium phosphate (β-TCP) could bemore » obtained by thermal treatment of HAP which was previously prepared from phosphogypsum (PG) waste. The chemical and phase composition, morphology and particle size of prepared samples was characterized by X-ray diffraction (XRD), Infrared spectroscopy (IR), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). The bioactivity was investigated by soaking of the calcined samples in simulated body fluid (SBF). Results confirmed that the calcination temperatures played an important role in the formation of calcium phosphate (CP) materials. XRD results indicated that HAP was partially decomposed into β-TCP. The in vitro data confirmed that the calcined HAP forming BCP besides other phases such as pyrophosphate and silica are bioactive materials. Therefore, BCP will be used as good biomaterials for medical applications.« less

Innovative Processing of Composites for Ultra-High Temperature Applications. Book 3

DTIC Science & Technology

1993-11-01

SiC Samples Prepared with Four Preceramic Polymer Infiltration / Pyrolysis (at 15750C) Cycles Figure 21 Scanning Electron...Micrograph of Large Pores near the Surface of Siliconized SIC Sample with Four Preceramic Polymer Infiltration / Pyrolysis (at 1575*C) Cycles II...In order to achieve dense, bulk composites with maximum SiC /Si ratio, two infiltration / pyrolysis cycles were used. S (4) After siliconization,

The role of mothers' and adolescents' perceptions of ethnic-racial socialization in shaping ethnic-racial identity among early adolescent boys and girls.

PubMed

Hughes, Diane; Hagelskamp, Carolin; Way, Niobe; Foust, Monica D

2009-05-01

The current study examined relationships between adolescents' and mothers' reports of ethnic-racial socialization and adolescents' ethnic-racial identity. The sample included 170 sixth graders (49% boys, 51% girls) and their mothers, all of whom identified as Black, Puerto Rican, Dominican, or Chinese. Two dimensions of ethnic-racial socialization (cultural socialization and preparation for bias) were evaluated alongside three dimensions of ethnic-racial identity (exploration, affirmation and belonging, and behavioral engagement). Mothers' reports of their cultural socialization predicted adolescents' reports, but only adolescents' reports predicted adolescents' ethnic-racial identity processes. Mothers' reports of preparation for bias predicted boys' but not girls' reports of preparation for bias. Again, only adolescents' reports of preparation for bias predicted their ethnic-racial identity. Thus, several gender differences in relationships emerged, with mothers' and adolescents' perceptions of cultural socialization, in particular, playing a more important role in girls' than in boys' identity processes. We discuss the implications of these findings for future research.

Anisotropy of mechanical and thermal properties of AZ31 sheets prepared using the ARB technique

NASA Astrophysics Data System (ADS)

Halmešová, K.; Trojanová, Z.; Džugan, J.; Drozd, Z.; Minárik, P.; Knapek, M.

2017-07-01

In the accumulative roll bonding (ARB) technique, repeated stacking of material followed by conventional roll-bonding is carried out. For this process the surfaces are cleaned with ethanol and then joined together by rolling. The rolled material is then cut into two halves, again surface treated and roll-bonded. This process may be repeated several times. For the magnesium alloy AZ31 (Mg-3Al-1Zn) rolling at an elevated temperature of 400 °C is necessary for ARB because of the low plasticity of hexagonal magnesium alloys at lower temperatures. Samples for this study were prepared using 1 to 3 ARB passes through the rolling mill. It was found that the ARB substantially refined the grain size of sheets to the micrometer scale. The microstructure and texture of the deformed samples were studied by light and electron microscopy. The mechanical properties of the ARB samples were explored using tensile test-pieces cut from the sheets with the tensile axis taken either parallel or perpendicular to the rolling direction, where a significant anisotropy in both mechanical properties and Young’s modulus was found. Anisotropy is explained on the basis of the specific microstructure and texture formed during the ARB process.

Application of mass spectrometry to process control for polymer material in autoclave curing

NASA Technical Reports Server (NTRS)

Smith, A. C.

1983-01-01

Mass spectrometer analysis of gas samples collected during a cure cycle of polymer materials can be used as a process control technique. This technique is particularly helpful in studying the various types of solvents and resin systems used in the preparation of polymer materials and characterizing the chemical composition of different resin systems and their mechanism of polymerization.

An EBIC study of dislocation networks in unprocessed and unprocessed web silicon ribbon. [for solar cells

NASA Technical Reports Server (NTRS)

Fieldler, F. S.; Ast, D.

1982-01-01

Experimental techniques for the preparation of electron beam induced current samples of Web-dentritic silicon are described. Both as grown and processed material were investigated. High density dislocation networks were found close to twin planes in the bulk of the material. The electrical activity of these networks is reduced in processed material.

Effect of Processing on Silk-Based Biomaterials: Reproducibility and Biocompatibility

PubMed Central

Wray, Lindsay S.; Hu, Xiao; Gallego, Jabier; Georgakoudi, Irene; Omenetto, Fiorenzo G.; Schmidt, Daniel; Kaplan, David L.

2012-01-01

Silk fibroin has been successfully used as a biomaterial for tissue regeneration. In order to prepare silk fibroin biomaterials for human implantation a series of processing steps are required to purify the protein. Degumming to remove inflammatory sericin is a crucial step related to biocompatibility and variability in the material. Detailed characterization of silk fibroin degumming is reported. The degumming conditions significantly affected cell viability on the silk fibroin material and the ability to form three-dimensional porous scaffolds from the silk fibroin, but did not affect macrophage activation or β-sheet content in the materials formed. Methods are also provided to determine the content of residual sericin in silk fibroin solutions and to assess changes in silk fibroin molecular weight. Amino acid composition analysis was used to detect sericin residuals in silk solutions with a detection limit between 1.0% and 10% wt/wt, while fluorescence spectroscopy was used to reproducibly distinguish between silk samples with different molecular weights. Both methods are simple and require minimal sample volume, providing useful quality control tools for silk fibroin preparation processes. PMID:21695778

Evaluation of the antifungal effects of bio-oil prepared with lignocellulosic biomass using fast pyrolysis technology.

PubMed

Kim, Kwang Ho; Jeong, Han Seob; Kim, Jae-Young; Han, Gyu Seong; Choi, In-Gyu; Choi, Joon Weon

2012-10-01

This study was performed to investigate the utility of bio-oil, produced via a fast pyrolysis process, as an antifungal agent against wood-rot fungi. Bio-oil solutions (25-100 wt.%) were prepared by diluting the bio-oil with EtOH. Wood block samples (yellow poplar and pitch pine) were treated with diluted bio-oil solutions and then subjected to a leaching process under hot water (70°C) for 72 h. After the wood block samples were thoroughly dried, they were subjected to a soil block test using Tyromyces palustris and Trametes versicolor. The antifungal effect of the 75% and 100% bio-oil solutions was the highest for both wood blocks. Scanning electron microscopy analysis indicated that some chemical components in the bio-oil solution could agglomerate together to form clusters in the inner part of the wood during the drying process, which could act as a wood preservative against fungal growth. According to GC/MS analysis, the components of the agglomerate were mainly phenolic compounds derived from lignin polymers. Copyright © 2012 Elsevier Ltd. All rights reserved.

Analysis of ultraviolet photo-response of ZnO nanostructures prepared by electrodeposition and atomic layer deposition

NASA Astrophysics Data System (ADS)

Makhlouf, Houssin; Karam, Chantal; Lamouchi, Amina; Tingry, Sophie; Miele, Philippe; Habchi, Roland; Chtourou, Radhouane; Bechelany, Mikhael

2018-06-01

In this work, ZnO nanowires (ZnO NWs) and urchin-like ZnO nanowires (U-ZnO NWs) based on self-assembled ordered polystyrene sphere (PS) were successfully prepared by combining atomic layer deposition (ALD) and electrochemical deposition (ECD) processes to build UV photosensors. The photo-response of the prepared samples was investigated and compared. The growth of the nanowires on self-assembled, ordered PS introduces a significant modification on the morphology, crystal orientation and grain size of U-ZnO NWs compared to randomly, vertically aligned ZnO NWs, and therefore improves the photo-response of U-ZnO NWs. The photocurrent may be produced by either a surface or bulk-related process. For ZnO NW-based photosensors, the photocurrent was monitored by a surface related process, whereas, it was mainly governed by a bulk related process for U-ZnO NWs, resulting in a higher and faster photo-response. The study of the rise and decay time constants for both materials showed that these parameters were strikingly sensitive to the optical properties.

7 CFR 27.21 - Preparation of samples of cotton.

Code of Federal Regulations, 2012 CFR

2012-01-01

... 7 Agriculture 2 2012-01-01 2012-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

7 CFR 27.21 - Preparation of samples of cotton.

Code of Federal Regulations, 2010 CFR

2010-01-01

... 7 Agriculture 2 2010-01-01 2010-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

7 CFR 27.21 - Preparation of samples of cotton.

Code of Federal Regulations, 2011 CFR

2011-01-01

... 7 Agriculture 2 2011-01-01 2011-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

Community-Level Physiological Profiling of Microbial Communities in Constructed Wetlands: Effects of Sample Preparation.

PubMed

Button, Mark; Weber, Kela; Nivala, Jaime; Aubron, Thomas; Müller, Roland Arno

2016-03-01

Community-level physiological profiling (CLPP) using BIOLOG® EcoPlates™ has become a popular method for characterizing and comparing the functional diversity, functional potential, and metabolic activity of heterotrophic microbial communities. The method was originally developed for profiling soil communities; however, its usage has expanded into the fields of ecotoxicology, agronomy, and the monitoring and profiling of microbial communities in various wastewater treatment systems, including constructed wetlands for water pollution control. When performing CLPP on aqueous samples from constructed wetlands, a wide variety of sample characteristics can be encountered and challenges may arise due to excessive solids, color, or turbidity. The aim of this study was to investigate the impacts of different sample preparation methods on CLPP performed on a variety of aqueous samples covering a broad range of physical and chemical characteristics. The results show that using filter paper, centrifugation, or settling helped clarify samples for subsequent CLPP analysis, however did not do so as effectively as dilution for the darkest samples. Dilution was able to provide suitable clarity for the darkest samples; however, 100-fold dilution significantly affected the carbon source utilization patterns (CSUPs), particularly with samples that were already partially or fully clear. Ten-fold dilution also had some effect on the CSUPs of samples which were originally clear; however, the effect was minimal. Based on these findings, for this specific set of samples, a 10-fold dilution provided a good balance between ease of use, sufficient clarity (for dark samples), and limited effect on CSUPs. The process and findings outlined here can hopefully serve future studies looking to utilize CLPP for functional analysis of microbial communities and also assist in comparing data from studies where different sample preparation methods were utilized.

Large-Scale Low-Cost NGS Library Preparation Using a Robust Tn5 Purification and Tagmentation Protocol

PubMed Central

Hennig, Bianca P.; Velten, Lars; Racke, Ines; Tu, Chelsea Szu; Thoms, Matthias; Rybin, Vladimir; Besir, Hüseyin; Remans, Kim; Steinmetz, Lars M.

2017-01-01

Efficient preparation of high-quality sequencing libraries that well represent the biological sample is a key step for using next-generation sequencing in research. Tn5 enables fast, robust, and highly efficient processing of limited input material while scaling to the parallel processing of hundreds of samples. Here, we present a robust Tn5 transposase purification strategy based on an N-terminal His6-Sumo3 tag. We demonstrate that libraries prepared with our in-house Tn5 are of the same quality as those processed with a commercially available kit (Nextera XT), while they dramatically reduce the cost of large-scale experiments. We introduce improved purification strategies for two versions of the Tn5 enzyme. The first version carries the previously reported point mutations E54K and L372P, and stably produces libraries of constant fragment size distribution, even if the Tn5-to-input molecule ratio varies. The second Tn5 construct carries an additional point mutation (R27S) in the DNA-binding domain. This construct allows for adjustment of the fragment size distribution based on enzyme concentration during tagmentation, a feature that opens new opportunities for use of Tn5 in customized experimental designs. We demonstrate the versatility of our Tn5 enzymes in different experimental settings, including a novel single-cell polyadenylation site mapping protocol as well as ultralow input DNA sequencing. PMID:29118030

Automation of dimethylation after guanidination labeling chemistry and its compatibility with common buffers and surfactants for mass spectrometry-based shotgun quantitative proteome analysis.

PubMed

Lo, Andy; Tang, Yanan; Chen, Lu; Li, Liang

2013-07-25

Isotope labeling liquid chromatography-mass spectrometry (LC-MS) is a major analytical platform for quantitative proteome analysis. Incorporation of isotopes used to distinguish samples plays a critical role in the success of this strategy. In this work, we optimized and automated a chemical derivatization protocol (dimethylation after guanidination, 2MEGA) to increase the labeling reproducibility and reduce human intervention. We also evaluated the reagent compatibility of this protocol to handle biological samples in different types of buffers and surfactants. A commercially available liquid handler was used for reagent dispensation to minimize analyst intervention and at least twenty protein digest samples could be prepared in a single run. Different front-end sample preparation methods for protein solubilization (SDS, urea, Rapigest™, and ProteaseMAX™) and two commercially available cell lysis buffers were evaluated for compatibility with the automated protocol. It was found that better than 94% desired labeling could be obtained in all conditions studied except urea, where the rate was reduced to about 92% due to carbamylation on the peptide amines. This work illustrates the automated 2MEGA labeling process can be used to handle a wide range of protein samples containing various reagents that are often encountered in protein sample preparation for quantitative proteome analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

In-vitro study of copper doped SiO2-CaO-P2O5 system for bioactivity and antimicrobial properties

NASA Astrophysics Data System (ADS)

Kaur, Kulwinder; Singh, K. J.; Anand, Vikas; Kaur, Harpreet; Arora, Daljit Singh

2015-08-01

Samples of the xCuO-(45-x)CaO-10P2O5-45SiO2 system (x varies from 0 to 4 mole%) have been synthesized for application as biomaterials to slow or inhibit the growth of living organisms (fungi and other pathogenic microorganisms) by the combination of sol-gel and co-precipitation processes. Prepared samples have been characterized by X-Ray Diffraction, Fourier Transform Infra-Red and Field Emission Scanning Electron Microscopy techniques before and after immersion in simulated body fluid. Antimicrobial activity of samples has been investigated against Staphylococcus aureus. Releasing of Cu2+and other ions in the simulated body fluid has been determined by Atomic Absorption Spectroscopy to ensure the use of prepared material as biomaterial with good antibacterial properties.

Heterogeneous sono-Fenton-like process using martite nanocatalyst prepared by high energy planetary ball milling for treatment of a textile dye.

PubMed

Dindarsafa, Mahsa; Khataee, Alireza; Kaymak, Baris; Vahid, Behrouz; Karimi, Atefeh; Rahmani, Amir

2017-01-01

High energy planetary ball milling was applied to prepare sono-Fenton nanocatalyst from natural martite (NM). The NM samples were milled for 2-6h at the speed of 320rpm for production of various ball milled martite (BMM) samples. The catalytic performance of the BMMs was greater than the NM for treatment of Acid Blue 92 (AB92) in heterogeneous sono-Fenton-like process. The NM and the BMM samples were characterized by XRD, FT-IR, SEM, EDX and BET analyses. The particle size distribution of the 6h-milled martite (BMM 3 ) was in the range of 10-90nm, which had the highest surface area compared to the other samples. Then, the impact of main operational parameters was investigated on the process. Complete removal of the dye was obtained at the desired conditions including initial pH 7, 2.5g/L BMM 3 dosage, 10mg/L AB92 concentration, and 150W ultrasonic power after 30min of treatment. The treatment process followed pseudo-first order kinetic. Environmentally-friendly modification of the NM, low leached iron amount and repeated application at milder pH were the significant benefits of the BMM 3 . The GC-MS was successfully used to identify the generated intermediates. Eventually, an artificial neural network (ANN) was applied to predict the AB92 removal efficiency based upon the experimental data with a proper correlation coefficient (R 2 =0.9836). Copyright © 2016 Elsevier B.V. All rights reserved.

Spark plasma sintering of bulk SrAl2O4-Sr3Al2O6 eutectic glass with wide-band optical window.

PubMed

Liu, Jiaxi; Lu, Nan; He, Gang; Li, Xiaoyu; Li, Jianqiang; Li, Jiangtao

2018-06-15

SrAl 2 O 4 -Sr 3 Al 2 O 6 eutectic glass was prepared by using an aerodynamic levitator equipped with a CO 2 laser device. A bulk transparent amorphous sample was obtained by the spark plasma sintering (SPS) of the prepared eutectic glass. XRD, a UV-vis-NIR spectrophotometer and FT-IR were employed to characterize the phase evolution and optical properties. The results show that the bulk SrAl 2 O 4 -Sr 3 Al 2 O 6 samples fabricated by the containerless process and SPS between 852 °C-857 °C were fully amorphous. The amorphous sample has a wide transparent window between 270 nm and 6.2 μm. The average refractive index in the visible light region is 1.680 and the Abbe number is 27.4. The prepared bulk SrAl 2 O 4 -Sr 3 Al 2 O 6 eutectic glass with the wide-band optical window may be a promising candidate for optical applications.

Evaluation of automated sample preparation, retention time locked gas chromatography-mass spectrometry and data analysis methods for the metabolomic study of Arabidopsis species.

PubMed

Gu, Qun; David, Frank; Lynen, Frédéric; Rumpel, Klaus; Dugardeyn, Jasper; Van Der Straeten, Dominique; Xu, Guowang; Sandra, Pat

2011-05-27

In this paper, automated sample preparation, retention time locked gas chromatography-mass spectrometry (GC-MS) and data analysis methods for the metabolomics study were evaluated. A miniaturized and automated derivatisation method using sequential oximation and silylation was applied to a polar extract of 4 types (2 types×2 ages) of Arabidopsis thaliana, a popular model organism often used in plant sciences and genetics. Automation of the derivatisation process offers excellent repeatability, and the time between sample preparation and analysis was short and constant, reducing artifact formation. Retention time locked (RTL) gas chromatography-mass spectrometry was used, resulting in reproducible retention times and GC-MS profiles. Two approaches were used for data analysis. XCMS followed by principal component analysis (approach 1) and AMDIS deconvolution combined with a commercially available program (Mass Profiler Professional) followed by principal component analysis (approach 2) were compared. Several features that were up- or down-regulated in the different types were detected. Copyright © 2011 Elsevier B.V. All rights reserved.

Spark plasma sintering of bulk SrAl2O4-Sr3Al2O6 eutectic glass with wide-band optical window

NASA Astrophysics Data System (ADS)

Liu, Jiaxi; Lu, Nan; He, Gang; Li, Xiaoyu; Li, Jianqiang; Li, Jiangtao

2018-06-01

SrAl2O4-Sr3Al2O6 eutectic glass was prepared by using an aerodynamic levitator equipped with a CO2 laser device. A bulk transparent amorphous sample was obtained by the spark plasma sintering (SPS) of the prepared eutectic glass. XRD, a UV–vis-NIR spectrophotometer and FT-IR were employed to characterize the phase evolution and optical properties. The results show that the bulk SrAl2O4-Sr3Al2O6 samples fabricated by the containerless process and SPS between 852 °C–857 °C were fully amorphous. The amorphous sample has a wide transparent window between 270 nm and 6.2 μm. The average refractive index in the visible light region is 1.680 and the Abbe number is 27.4. The prepared bulk SrAl2O4-Sr3Al2O6 eutectic glass with the wide-band optical window may be a promising candidate for optical applications.

Methods for Producing High-Performance Silicon Carbide Fibers, Architectural Preforms, and High-Temperature Composite Structures

NASA Technical Reports Server (NTRS)

Yun, Hee-Mann (Inventor); DiCarlo, James A. (Inventor)

2014-01-01

Methods are disclosed for producing architectural preforms and high-temperature composite structures containing high-strength ceramic fibers with reduced preforming stresses within each fiber, with an in-situ grown coating on each fiber surface, with reduced boron within the bulk of each fiber, and with improved tensile creep and rupture resistance properties tier each fiber. The methods include the steps of preparing an original sample of a preform formed from a pre-selected high-strength silicon carbide ceramic fiber type, placing the original sample in a processing furnace under a pre-selected preforming stress state and thermally treating the sample in the processing furnace at a pre-selected processing temperature and hold time in a processing gas having a pre-selected composition, pressure, and flow rate. For the high-temperature composite structures, the method includes additional steps of depositing a thin interphase coating on the surface of each fiber and forming a ceramic or carbon-based matrix within the sample.

Influence of growth temperature on bulk and surface defects in hybrid lead halide perovskite films.

PubMed

Peng, Weina; Anand, Benoy; Liu, Lihong; Sampat, Siddharth; Bearden, Brandon E; Malko, Anton V; Chabal, Yves J

2016-01-21

The rapid development of perovskite solar cells has focused its attention on defects in perovskites, which are gradually realized to strongly control the device performance. A fundamental understanding is therefore needed for further improvement in this field. Recent efforts have mainly focused on minimizing the surface defects and grain boundaries in thin films. Using time-resolved photoluminescence spectroscopy, we show that bulk defects in perovskite samples prepared using vapor assisted solution process (VASP) play a key role in addition to surface and grain boundary defects. The defect state density of samples prepared at 150 °C (∼10(17) cm(-3)) increases by 5 fold at 175 °C even though the average grains size increases slightly, ruling out grain boundary defects as the main mechanism for the observed differences in PL properties upon annealing. Upon surface passivation using water molecules, the PL intensity and lifetime of samples prepared at 200 °C are only partially improved, remaining significantly lower than those prepared at 150 °C. Thus, the present study indicates that the majority of these defect states observed at elevated growth temperatures originates from bulk defects and underscores the importance to control the formation of bulk defects together with grain boundary and surface defects to further improve the optoelectronic properties of perovskites.

Gravitational influences on the liquid-state homogenization and solidification of aluminum antimonide. [space processing of solar cell material

NASA Technical Reports Server (NTRS)

Ang, C.-Y.; Lacy, L. L.

1979-01-01

Typical commercial or laboratory-prepared samples of polycrystalline AlSb contain microstructural inhomogeneities of Al- or Sb-rich phases in addition to the primary AlSb grains. The paper reports on gravitational influences, such as density-driven convection or sedimentation, that cause microscopic phase separation and nonequilibrium conditions to exist in earth-based melts of AlSb. A triple-cavity electric furnace is used to homogenize the multiphase AlSb samples in space and on earth. A comparative characterization of identically processed low- and one-gravity samples of commercial AlSb reveals major improvements in the homogeneity of the low-gravity homogenized material.

Investigation of Zerodur material processing

NASA Technical Reports Server (NTRS)

Johnson, R. Barry

1993-01-01

The Final Report of the Center for Applied Optics (CAO), of The University of Alabama (UAH) study entitled 'Investigation of Zerodur Material Processing' is presented. The objectives of the effort were to prepare glass samples by cutting, grinding, etching, and polishing block Zerodur to desired specifications using equipment located in the optical shop located in the Optical System Branch at NASA/MSFC; characterize samples for subsurface damage and surface roughness; utilize Zerodur samples for coating investigations; and perform investigations into enhanced optical fabrication and metrology techniques. The results of this investigation will be used to support the Advanced X Ray Astrophysics Facility (AXAF) program as well as other NASA/MSFC research programs. The results of the technical effort are presented and discussed.

A solid-phase microextraction fiber with carbon nanoparticles as sorbent material prepared by a simple flame-based preparation process.

PubMed

Sun, Min; Feng, Juanjuan; Qiu, Huamin; Fan, Lulu; Li, Leilei; Luo, Chuannan

2013-07-26

A novel carbon nanoparticles-coated solid-phase microextraction (SPME) fiber was prepared via a simple and low-cost flame-based preparation process, with stainless steel wire as support. Surface characteristic of the fiber was studied with scanning electron microscope. A nano-scaled brushy structure was observed. Coupled to gas chromatography (GC), the fiber was used to extract phthalate esters (PAEs) and polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. Analytical performances of the proposed method were investigated under the optimum extraction conditions (extraction temperature, 40°C; content of KCl, 30% (w/v); extraction time, 50min for PAEs and 40min for PAHs) and compared with other reports for the same analytes. Calibration ranges were 0.06-500μgL(-1) for di-n-butyl phthalate (DBP), and 0.1-300μgL(-1) for di-cyclohexyl phthalate (DCHP) and di-(2-ethyl-hexyl) phthalate (DEHP). For the eight PAHs, good linearity was obtained ranging from 0.01 to 150μgL(-1). Limits of detection were 0.005μgL(-1) for three PAEs and 0.001-0.003μgL(-1) for eight PAHs. The fiber exhibited excellent stability. It can be used for 100 times with RSDs of extraction efficiency less than 22.4%. The as-established SPME-GC method was applied to determine PAEs in food-wrap and PAHs in cigarette ash and snow water, and satisfactory results were obtained. The carbon nanoparticles-coated SPME fiber was efficient for sampling of organic compounds from aqueous samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Changes in the Ginsenoside Content During Fermentation Using an Appliance for the Preparation of Red Ginseng.

PubMed

Lee, So Jin; Ha, Na; Kim, Yunjeong; Kim, Min-Gul

2016-01-01

The total amount of ginsenoside in fermented red ginseng (FRG) is increased by microbial fermentation. The aim of this study was to evaluate whether fermentation time and temperature affect the ginsenoside content during fermentation using an appliance for the preparation of red ginseng. The FRG and fermented red ginseng extracts (FRG-e) were prepared using an appliance for the preparation of red ginseng. The temperature was recorded and time points for sampling were scheduled at pre-fermentation (0[Formula: see text]h) and 18, 36, 48, 60 and 72[Formula: see text]h after the addition of the microbial strains. Samples of FRG and FRG-e were collected to identify changes in the ginsenoside contents at each time point during the fermentation process. The ginsenoside content was analyzed using high performance liquid chromatography (HPLC). The levels of ginsenoside Rh1, Rg3, and compound Y, which are known to have effective pharmacological properties, increased more than three-fold in the final products of FRG relative to samples prior to fermentation. Although the ginsenoside constituents of FRG-e decreased or increased and then decreased during fermentation, the total amount of ginsenoside in FRG-e was even higher than those in FRG; the total amounts of ginsenoside in FRG-e and FRG were 8282.8 and 738.0[Formula: see text]mg, respectively. This study examined the changes in composition of ginsenosides and suggests a method to manufacture high-content total ginsenosides according to the fermentation temperature and process time. Reducing the extraction time is expected to improve the decrease of ginsenosides in FRG-e as a function of the fermentation time.

[How to adapt to the requirements of "clinical value-oriented drug innovation" for pharmaceutical research in application process of new traditional Chinese medicine].

PubMed

Jin, Fang

2017-05-01

On August 9, 2015, the State Council promulgated the "Opinions of the State Council on the reform of drug and medical device review and approval system" (Guofa 2015 No. 44), and established the "clinical value-oriented drug innovation" model to encourage the research and development of new drugs. Following that, China Food and Drug Administration (CFDA) promulgated the "Notice on several policies for drug registration review and approval" (2015 No. 230 ) on November 11, 2015, clearly specifying that CFDA would "implement one-time approval for clinical trials application of the new drugs, and no longer take a phased declaration, review and approval system; for the new drugs that apply for clinical trials, mainly review the scientific natureof the clinical protocols and the risk control of the new drugs to guarantee the safety of subjects". Accordingly, the evaluation ideas and forms of new drug registration have also been adjusted greatly. For example, issues like the rationality of the drug manufacturing process, whether the scale can reflect the stability of the process, whether the preparation process is sufficient, and whether the choice of dosage form is reasonable are no longer the focus of evaluation before clinical trials. Issues regarding whether the preparation process design is reasonable, whether the effective components can be transferred to the preparation to a maximum extent, whether the process parameters determined in small and middle pilot trials can adapt to the requirements of mass production, no longer act as the reasons for refusing the clinical trials. The corresponding risks shall be borne by the applicant as the subject of liability. The focus in registration evaluation is mainly transferred to how to ensure the consistence of quality between clinical trial samples and the samples already available on market by guaranteeing stable sources of drug raw materials and stable quality of medicines as well as control of the whole preparation process. These issues run through the whole process of new drug development, but also have different focuses in different stages. According to the "Measures on communicating about drug research and development and technical review" (2016 No. 94) (On Trial) issued by CFDA on June 2, 2016, the applicants may communicate with the drug evaluation center in different phases in the process of new drugs registration in respects of medicine material problems, technological problems, and quality control of the preparations. In this paper, the transformation of Chinese medicine research model was described mainly in the following aspects: how to control the quality of medicines from origins, technology design of the preparation and technology process research, and how to establish whole-process quality system. The paper also reflects the concept that the quality of new Chinese drugs research and development comes from design. Copyright© by the Chinese Pharmaceutical Association.

Infrared spectroscopy and upconversion luminescence behaviour of erbium doped yttrium (III) oxide phosphor

NASA Astrophysics Data System (ADS)

Dubey, Vikas; Tiwari, Ratnesh; Tamrakar, Raunak Kumar; Rathore, Gajendra Singh; Sharma, Chitrakant; Tiwari, Neha

2014-11-01

The paper reports upconversion luminescence behaviour and infra-red spectroscopic pattern of erbium doped yttrium (III) oxide phosphor. Sample was synthesized by solid state reaction method with variable concentration or erbium (0.5-2.5 mol%). The conventional solid state method is suitable for large scale production and eco-friendly method. The prepared sample was characterized by X-ray diffraction (XRD) technique. From structural analysis by XRD technique shows cubic structure of prepared sample with variable concentration of erbium and no impurity phase were found when increase the concentration of Er3+. Particle size was calculated by Scherer's formula and it varies from 67 nm to 120 nm. The surface morphology of prepared phosphor was determined by field emission gun scanning electron microscopy (FEGSEM) technique. The surface morphology of the sample shows good connectivity with grains as well as some agglomerates formation occurs in sample. The functional group analysis was done by Fourier transform infra-red technique (FTIR) analysis which confirm the formation of Y2O3:Er3+ phosphor was prepared. The results indicated that the Y2O3:Er3+ phosphors might have high upconversion efficiency because of their low vibrational energy. Under 980 nm laser excitation sample shows intense green emission at 555 nm and orange emission at 590 nm wavelength. For green emission transition occurs 2H11/2 → 4I15/2, 4S3/2 → 4I15/2 for upconversion emissions. Excited state absorption and energy transfer process were discussed as possible upconversion mechanisms. The near infrared luminescence spectra was recorded. The upconversion luminescence intensity increase with increasing the concentration or erbium up to 2 mol% after that luminescence intensity decreases due to concentration quenching occurs. Spectrophotometric determinations of peaks are evaluated by Commission Internationale de I'Eclairage (CIE) technique. From CIE technique the dominant peak of from PL spectra shows intense green emission so the prepared phosphor is may be useful for green light emitting diode (GLED) application.

Effect of oxygen partial pressure during preparation of rutile-type FeNbTiO6 on electrical and dielectric properties, thermopower and Mössbauer spectra

NASA Astrophysics Data System (ADS)

Günther, A.; Hochleitner, R.; Lohringer, H.; Schmidbauer, E.; Schöttler-Himmel, A.; Volk, M.

2017-05-01

Electrical and dielectric properties were measured on rutile-type FeNbTiO6, sintered in air, CO2 or 5%H2/CO2 atmosphere between temperatures of 1423 and 1573 K. The individual samples show characteristic differences in DC and AC conductivity, dielectric constant ε(ω) (ω is angular frequency), dielectric loss and dissipation factor. Attempts were made to distinguish between bulk, grain boundary (GB) and sample-electrode (SE) processes. Samples show very high relaxor-like ε(ω) peaks at 500-600 K using Ag-paint contacts as expected from previous studies during preparation in air that is of interest for industrial application; utilizing Pt-paint and using slightly reducing sintering conditions, a clear variation was observed. These findings point to a notable influence of GB and/or SE effects on the experimental ε(ω), in addition to the intrinsic origin by polar nanoregions, as suggested earlier. Complex plane impedance plots are characterized by semicircular arcs due to bulk, GB and/or SE charge transport. The derived DC conductivity σDC shows Arrhenius behavior with activation energy of EA≈0.27-0.37 eV and σDC(300 K) ≈1×10-6-3×10-4 Ω-1cm-1 for the bulk, EA≈0.7-0.9 eV and σDC(300 K)≈5×10-10-1×10-4 Ω-1cm-1 for GB and/or SE processes, depending on the preparation conditions. The thermopower is small and negative, hence n-type conduction occurs and the charge carriers are electrons or electron polarons. 57Fe Mössbauer spectroscopy enabled to gain knowledge of local nonstoichiometry in the environment of Fe cations, presumably affecting electrical conduction in the bulk and GBs; after sample preparation in reducing conditions, apart from Fe3+ also the presence of Fe2+ ions was established.

40 Years of Processing Pieces of Space

NASA Technical Reports Server (NTRS)

Satterwhite, C. E.; Funk, R. C.; Righter, K.; Harrington, R. H.

2016-01-01

This year marks the 40th year anniversary for the Antarctic Search for Meteorite (ANSMET) program. In 1976, the ANSMET program led the first expedition to Antarctica. The ANSMET program is a US-led field-based science project that recovers meteorite samples from Antarctica. Once a year from late November to late January, a field team consisting of 8 to 12 people, spends 6-8 weeks camping on the ice and collecting meteorites. Since 1976, more than 22,000 meteorite samples have been recovered. These meteorites come from asteroids, planets and other bodies of the solar system. Once collected, the Antarctic meteorites are shipped to NASA/Johnson Space Center (JSC) Houston, TX. in a refrigerated truck and are kept frozen to minimize oxidation until they are ready for initial processing. In Antarctica each meteorite is given a field tag which consists of numbers, once in the lab, this is replaced by an official tag, consisting of the Antarctic field location and year collected. The types and numbers of meteorites that have been classified include 849 carbonaceous chondrites, 135 enstatites, 512 achondrites, 64 stony, 115 irons, 48 others (27 R chondrites, 7 ungrouped), 6,161 H chondrites, 7,668 L chondrites, and 4,589 LL chondrites. Although 80-85 percent of the collected meteorites fall in the ordinary chondrite group, the other approximately 15 percent represent rare types of achondrites and carbonaceous chondrites. These rare meteorites include 25 lunar meteorites, 15 Martian meteorites, scores of various types of carbonaceous chondrites, and unique achondrites. The Antarctic meteorites that have been collected are processed in the Meteorite Processing Lab at JSC in Houston, TX. Initial processing of the meteorites begins with thawing/drying the meteorites in a nitrogen glove box for 24 to 48 hours. The meteorites are then photographed, measured, weighed and a description of the interior and exterior of each meteorite is written. The meteorite is broken and a representative sample, either a 1-3 gram chip or thin section is sent to the Smithsonian Institution for classification. After Antarctic meteorites have been classified and approved by the Nomenclature Committee of the Meteoritical Society, they are announced in the Antarctic Meteorite Newsletter, which is published twice per year (fall and spring) so that scientists may review which meteorites are available to study. Requests for Antarctic Meteorite samples are welcomed from research scientists, regardless of their current state of funding for meteorite studies. Since its inception over 3,300 requests have been made for pieces of these meteorites and over 400 investigators worldwide are active in the study of meteorites.. Research on these samples has been published in more than1500 peer reviewed articles; a listing of papers for any meteorite sample can be generated by accessing http://curator.jsc.nasa.gov/antmet/referencesearch.cfm. Antarctic meteorite samples requested by scientists are prepared several different ways. Most samples are prepared as chips, either using a rock splitter or using a chisel and chipping bowl. In special situations, a researcher may request a meteorite slab in which case the samples are cut using a diamond-bladed bandsaw inside of a dry nitrogen glove box. The meteorites are always cut in a 100 percent liquid-free environment. Additionally, thin/thick sections of Antarctic meteorites are also prepared at JSC. The meteorite thin section lab at JSC can prepare standard 30-micron thin sections, thick sections of variable thickness (100 to 200 microns), or demountable sections using superglue, all section are prepared without using water. Although many of the techniques used back in the '70's are still used today, advances in computers, software, databases, available tools and instrumentation have helped to streamline and shorten the duration of the classification process. In conjunction with present day missions to asteroids and other planets, meteorite studies have not only led to a better understanding of the complex histories of these bodies but have also tied certain meteorite groups to particular asteroid bodies. New meteorite discoveries by the ANSMET program provide a cost effective method for obtaining samples of previously unsampled bodies, allowing scientists to learn more about the origin, composition, and evolution of the solar system. Preservation in our cleanrooms at NASA allows material to be archived for future generations and advances in instrumentation and analysis.

Acoustic Sample Deposition MALDI-MS (ASD-MALDI-MS): A Novel Process Flow for Quality Control Screening of Compound Libraries.

PubMed

Chin, Jefferson; Wood, Elizabeth; Peters, Grace S; Drexler, Dieter M

2016-02-01

In the early stages of drug discovery, high-throughput screening (HTS) of compound libraries against pharmaceutical targets is a common method to identify potential lead molecules. For these HTS campaigns to be efficient and successful, continuous quality control of the compound collection is necessary and crucial. However, the large number of compound samples and the limited sample amount pose unique challenges. Presented here is a proof-of-concept study for a novel process flow for the quality control screening of small-molecule compound libraries that consumes only minimal amounts of samples and affords compound-specific molecular data. This process employs an acoustic sample deposition (ASD) technique for the offline sample preparation by depositing nanoliter volumes in an array format onto microscope glass slides followed by matrix-assisted laser desorption/ionization mass spectrometric (MALDI-MS) analysis. An initial study of a 384-compound array employing the ASD-MALDI-MS workflow resulted in a 75% first-pass positive identification rate with an analysis time of <1 s per sample. © 2015 Society for Laboratory Automation and Screening.

Cytology Preparations of Formalin Fixative Aid Detection of Giardia in Duodenal Biopsy Samples.

PubMed

Panarelli, Nicole C; Gobara, Nariman; Hoda, Rana S; Chaump, Michael; Jessurun, Jose; Yantiss, Rhonda K

2017-04-01

Giardiasis is the most common intestinal parasitic infection in the United States. The organism elicits no, or minimal, inflammatory changes in duodenal biopsy samples, so it can be easily overlooked. We performed this study to determine whether Giardia could be isolated from the formalin fixative of biopsy samples, and to evaluate the value of fluid analysis in the assessment for potential infection. We prospectively evaluated duodenal biopsy samples from 92 patients with a clinical suspicion of giardiasis or symptoms compatible with that diagnosis (ie, diarrhea, bloating, or abdominal pain) Biopsy samples were routinely processed and stained with hematoxylin and eosin. Histologic diagnoses included giardiasis (5 cases, 4%), normal findings (64 cases, 70%), peptic injury/active duodenitis (12 cases, 13%), and intraepithelial lymphocytosis with villous blunting (10 cases, 12%). Fifteen cases (13%) showed detached degenerated epithelial cells or mucus droplets in the intervillous space that resembled Giardia. Cytology slides were prepared from formalin in the biopsy container using the standard Cytospin protocol and reviewed by a cytopathologist blinded to the biopsy findings. Cytologic evaluation revealed Giardia spp. in all 5 biopsy-proven cases, and identified an additional case that was not detected by biopsy analysis. Organisms were significantly more numerous (mean: 400 trophozoites; range, 120 to 810) and showed better morphologic features in cytology preparations compared with tissue sections (mean: 129 trophozoites; range, 37 to 253 organisms; P=0.05). Our findings suggest that cytology preparations from formalin fixative can resolve diagnostically challenging cases and even enhance Giardia detection in some cases.

Carbonaceous Chondrite Thin Section Preparation

NASA Technical Reports Server (NTRS)

Harrington, R.; Righter, K.

2017-01-01

Carbonaceous chondrite meteorites have long posed a challenge for thin section makers. The variability in sample hardness among the different types, and sometimes within individual sections, creates the need for an adaptable approach at each step of the thin section making process. This poster will share some of the procedural adjustments that have proven to be successful at the NASA JSC Meteorite Thin Section Laboratory. These adjustments are modifications of preparation methods that have been in use for decades and therefore do not require investment in new technology or materials.

In-situ XRD vs ex-situ vacuum annealing of tantalum oxynitride thin films: Assessments on the structural evolution

NASA Astrophysics Data System (ADS)

Cunha, L.; Apreutesei, M.; Moura, C.; Alves, E.; Barradas, N. P.; Cristea, D.

2018-04-01

The purpose of this work is to discuss the main structural characteristics of a group of tantalum oxynitride (TaNxOy) thin films, with different compositions, prepared by magnetron sputtering, and to interpret and compare the structural changes, by X-ray diffraction (XRD), when the samples are vacuum annealed under two different conditions: i) annealing, followed by ex-situ XRD: one sample of each deposition run was annealed at a different temperature, until a maximum of 800 °C, and the XRD patterns were obtained, at room temperature, after each annealing process; ii) annealing with in-situ XRD: the diffraction patterns are obtained, at certain temperatures, during the annealing process, using always the same sample. In-situ XRD annealing could be an interesting process to perform annealing, and analysing the evolution of the structure with the temperature, when compared to the classical process. A higher structural stability was observed in some of the samples, particularly on those with highest oxygen content, but also on the sample with non-metal (O + N) to metal (Ta) ratio around 0.5.

Initial Study on Thin Film Preparation of Carbon Nanodots Composites as Luminescence Material

NASA Astrophysics Data System (ADS)

Iskandar, F.; Aimon, A. H.; Akmaluddin, A. R.; Nuryadin, B. W.; Abdullah, M.

2016-08-01

Nowadays, the developments of phosphors materials require elements without noble metals and simple production process. Carbon nanodots (C-dots) are one of phosphor materials with wide range of emission band, and high biocompatibility. In this research thin film carbon nanodots composite have been prepared by spin coating method. Prior deposition, powder carbon nanodots were synthesized from a mixture of commercial urea as the nitrogen sources and citric acid as a carbon source by using hydrothermal and microwave-assisted heating method. The prepared powder was dispersed in transparent epoxy resin and then coated on glass substrate. The photoluminescence result for sample with 0.035 g citric acid exhibited an intense, single, homogeneous and broad spectrum with yellowish emission upon excitation at 365 nm. The Fourier Transform Infrared Spectroscopy (FTIR) result showed the existences of C=C, C-H, C=O, N-H and O-H functional groups which confirmed the quality of the sample. Further, based on UV-Vis measurement, the prepared thin film was highly transparent (transmittance 90%) with estimated film thickness around 764 nm. This result may open an opportunity for optoelectronic devices.

Results of Hg speciation testing on MCU strip effluent hold tank (SEHT) and decontaminated salt solution hold tank (DSSHT) materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.

2015-09-17

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team.i,ii The tenth shipment of samples was designated to include Modular Caustic Side Solvent Extraction Unit (MCU) Strip Effluent Hold Tank (SEHT) and MCU Decontaminated Salt Solution Hold Tank (DSSHT) materials from processing Salt Batch 7b. The MCU SEHT (MCU-15-722) and DSSHT (MCU-15-709) samples were pulled on June 15, 2015. All MCU samples were received at SRNL on June 16, 2015. The DSSHT sample wasmore » moved the same day to refrigeration, while the SEHT sample was placed in the Shielded Cells. On July 9, 2015 it was opened and an aliquot diluted 1:100 with Eurofins deionized water and a portion of the diluted sample transferred to a Teflon® bottle prior to moving it to refrigeration that same day. All samples were kept in the dark and refrigerated until final dilutions were prepared for shipment to Eurofins.« less

A novel platelet concentrate: titanium-prepared platelet-rich fibrin.

PubMed

Tunalı, Mustafa; Özdemir, Hakan; Küçükodacı, Zafer; Akman, Serhan; Yaprak, Emre; Toker, Hülya; Fıratlı, Erhan

2014-01-01

We developed a new product called titanium-prepared platelet-rich fibrin (T-PRF). The T-PRF method is based on the hypothesis that titanium may be more effective in activating platelets than the silica activators used with glass tubes in Chouckroun's leukocyte- and platelet-rich fibrin (L-PRF) method. In this study, we aimed to define the structural characteristics of T-PRF and compare it with L-PRF. Blood samples were collected from 10 healthy male volunteers. The blood samples were drawn using a syringe. Nine milliliters was transferred to a dry glass tube, and 9 mL was transferred to a titanium tube. Half of each clot (i.e., the blood that was clotted using T-PRF or L-PRF) was processed with a scanning electron microscope (SEM). The other half of each clot was processed for fluorescence microscopy analysis and light microscopy analysis. The T-PRF samples seemed to have a highly organized network with continuous integrity compared to the other L-PRF samples. Histomorphometric analysis showed that T-PRF fibrin network covers larger area than L-PRF fibrin network; also fibrin seemed thicker in the T-PRF samples. This is the first human study to define T-PRF as an autogenous leukocyte- and platelet-rich fibrin product. The platelet activation by titanium seems to offer some high characteristics to T-PRF.

Quantification of Parvovirus B19 DNA Using COBAS AmpliPrep Automated Sample Preparation and LightCycler Real-Time PCR

PubMed Central

Schorling, Stefan; Schalasta, Gunnar; Enders, Gisela; Zauke, Michael

2004-01-01

The COBAS AmpliPrep instrument (Roche Diagnostics GmbH, D-68305 Mannheim, Germany) automates the entire sample preparation process of nucleic acid isolation from serum or plasma for polymerase chain reaction analysis. We report the analytical performance of the LightCycler Parvovirus B19 Quantification Kit (Roche Diagnostics) using nucleic acids isolated with the COBAS AmpliPrep instrument. Nucleic acids were extracted using the Total Nucleic Acid Isolation Kit (Roche Diagnostics) and amplified with the LightCycler Parvovirus B19 Quantification Kit. The kit combination processes 72 samples per 8-hour shift. The lower detection limit is 234 IU/ml at a 95% hit-rate, linear range approximately 104-1010 IU/ml, and overall precision 16 to 40%. Relative sensitivity and specificity in routine samples from pregnant women are 100% and 93%, respectively. Identification of a persistent parvovirus B19-infected individual by the polymerase chain reaction among 51 anti-parvovirus B19 IgM-negative samples underlines the importance of additional nucleic acid testing in pregnancy and its superiority to serology in identifying the risk of parvovirus B19 transmission via blood or blood products. Combination of the Total Nucleic Acid Isolation Kit on the COBAS AmpliPrep instrument with the LightCycler Parvovirus B19 Quantification Kit provides a reliable and time-saving tool for sensitive and accurate detection of parvovirus B19 DNA. PMID:14736825

Assessment of the influence of different sample processing and cold storage duration on plant free proline content analyses.

PubMed

Teklić, Tihana; Spoljarević, Marija; Stanisavljević, Aleksandar; Lisjak, Miroslav; Vinković, Tomislav; Parađiković, Nada; Andrić, Luka; Hancock, John T

2010-01-01

A method which is widely accepted for the analysis of free proline content in plant tissues is based on the use of 3% sulfosalicylic acid as an extractant, followed by spectrophotometric quantification of a proline-ninhydrin complex in toluene. However, sample preparation and storage may influence the proline actually measured. This may give misleading or difficult to compare data. To evaluate free proline levels fresh and frozen strawberry (Fragaria × ananassa Duch.) leaves and soybean [Glycine max (L.) Merr.] hypocotyl tissues were used. These were ground with or without liquid nitrogen and proline extracted with sulfosalicylic acid. A particular focus was the influence of plant sample cold storage duration (1, 4 and 12 weeks at -20°C) on tissue proline levels measured. The free proline content analyses, carried out in leaves of Fragaria × ananassa Duch. as well as in hypocotyls of Glycine max (L.) Merr., showed a significant influence of the sample preparation method and cold storage period. Long-term storage of up to 12 weeks at -20°C led to a significant increase in the measured proline in all samples analysed. The observed changes in proline content in plant tissue samples stored at -20°C indicate the likelihood of the over-estimation of the proline content if the proline analyses are delayed. Plant sample processing and cold storage duration seem to have an important influence on results of proline analyses. Therefore it is recommended that samples should be ground fresh and analysed immediately. Copyright © 2010 John Wiley & Sons, Ltd.

Improved Dielectric Properties via Mechano-Chemical Activation in Ba0.80Pb0.20TiO3 Ceramics

NASA Astrophysics Data System (ADS)

Kumar, Parveen; Rani, Renu; Singh, Sangeeta; Juneja, J. K.; Prakash, Chandra; Raina, K. K.

2011-12-01

The present report is about the preparation and dielectric properties of commonly used Ba0.80Pb0.20TiO3 (BPT) ferroelectric ceramic via Mechano-Chemical Activation (MCA). Results were compared by the BPT sample prepared by conventional solid state method. The BPT sample prepared via MCA technique was found to have decreased tetragonality, dielectric constant value (ɛRT = 450 and ɛmax = 6170) approximately double the value for sample prepared by conventional method (ɛRT = 260 and ɛmax = 3275). Also, the sample prepared by MCA was found to be less frequency dependent. Thus, the BPT sample prepared via MCA is more suitable for capacitor applications requiring lesser frequency dependency than the conventionally prepared BPT sample.

SRB Processing Facilities Media Event

NASA Image and Video Library

2016-03-01

Inside the Booster Fabrication Facility (BFF) at NASA’s Kennedy Space Center in Florida, Jeff Cook, a thermal protection system specialist with Orbital ATK, displays a sample of the painted thermal protection system that is being applied to booster segments. Members of the news media toured the BFF. Orbital ATK is a contractor for NASA’s Marshall Space Flight Center in Alabama, and operates the BFF to prepare aft booster segments and hardware for the SLS rocket boosters. The SLS rocket and Orion spacecraft will launch on Exploration Mission-1 in 2018. The Ground Systems Development and Operations Program is preparing the infrastructure to process and launch spacecraft for deep-space missions and the journey to Mars.

[Standardization of cryopreservation process of Saccharomyces boulardii yeasts for usage in collections and banks of industrial microorganism strains].

PubMed

Gurina, T M; Vysekantsev, I P; Babinets, O M

2013-01-01

New implementation principle of freeze-thawing during cryopreservation of microorganisms, initiation of the process of crystal formation at cooling and thawing stage with the controlled rate of heating was experimentally substantiated. This allows increasing the cell viability, guaranteeing their equal number in each preparation, decreasing the contamination risk of the samples at thawing stage.

Recent advances in preparation and application of hybrid organic-silica monolithic capillary columns.

PubMed

Ou, Junjie; Lin, Hui; Zhang, Zhenbin; Huang, Guang; Dong, Jing; Zou, Hanfa

2013-01-01

Hybrid organic-silica monolithic columns, regarded as a second generation of silica-based monoliths, have received much interest due to their unique properties over the pure silica-based monoliths. This review mainly focuses on development in the fields of preparation of hybrid monolithic columns in a capillary and their application for CEC and capillary liquid chromatography separation, as well as for sample pretreatment of solid-phase microextraction and immobilized enzyme reactor since July 2010. The preparation approaches are comprehensively summarized with three routes: (i) general sol-gel process using trialkoxysilanes and tetraalkoxysilanes as coprecursors; (ii) "one-pot" process of alkoxysilanes and organic monomers concomitantly proceeding sol-gel chemistry and free radical polymerization; and (iii) other polymerization approaches of organic monomers containing silanes. The modification of hybrid monoliths containing reactive groups to acquire the desired surface functionality is also described. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Crystal nuclei templated nanostructured membranes prepared by solvent crystallization and polymer migration

NASA Astrophysics Data System (ADS)

Wang, Bo; Ji, Jing; Li, Kang

2016-09-01

Currently, production of porous polymeric membranes for filtration is predominated by the phase-separation process. However, this method has reached its technological limit, and there have been no significant breakthrough over the last decade. Here we show, using polyvinylidene fluoride as a sample polymer, a new concept of membrane manufacturing by combining oriented green solvent crystallization and polymer migration is able to obtain high performance membranes with pure water permeation flux substantially higher than those with similar pore size prepared by conventional phase-separation processes. The new manufacturing procedure is governed by fewer operating parameters and is, thus, easier to control with reproducible results. Apart from the high water permeation flux, the prepared membranes also show excellent stable flux after fouling and superior mechanical properties of high pressure load and better abrasion resistance. These findings demonstrate the promise of a new concept for green manufacturing nanostructured polymeric membranes with high performances.

Extraction, scrub, and strip test results for the solvent transfer to salt waste processing facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T.

The Savannah River National Laboratory (SRNL) prepared approximately 240 gallons of Caustic-Side Solvent Extraction (CSSX) solvent for use at the Salt Waste Processing Facility (SWPF). An Extraction, Scrub, and Strip (ESS) test was performed on a sample of the prepared solvent using a salt solution prepared by Parsons to determine cesium distribution ratios (D(Cs)), and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams. This data will be used by Parsons to help qualify the solvent for use at the SWPF. The ESS test showed acceptable performance of the solvent for extraction, scrub, and strip operations.more » The extraction D(Cs) measured 15.5, exceeding the required value of 8. This value is consistent with results from previous ESS tests using similar solvent formulations. Similarly, scrub and strip cesium distribution ratios fell within acceptable ranges.« less

Review of sample preparation strategies for MS-based metabolomic studies in industrial biotechnology.

PubMed

Causon, Tim J; Hann, Stephan

2016-09-28

Fermentation and cell culture biotechnology in the form of so-called "cell factories" now play an increasingly significant role in production of both large (e.g. proteins, biopharmaceuticals) and small organic molecules for a wide variety of applications. However, associated metabolic engineering optimisation processes relying on genetic modification of organisms used in cell factories, or alteration of production conditions remain a challenging undertaking for improving the final yield and quality of cell factory products. In addition to genomic, transcriptomic and proteomic workflows, analytical metabolomics continues to play a critical role in studying detailed aspects of critical pathways (e.g. via targeted quantification of metabolites), identification of biosynthetic intermediates, and also for phenotype differentiation and the elucidation of previously unknown pathways (e.g. via non-targeted strategies). However, the diversity of primary and secondary metabolites and the broad concentration ranges encompassed during typical biotechnological processes means that simultaneous extraction and robust analytical determination of all parts of interest of the metabolome is effectively impossible. As the integration of metabolome data with transcriptome and proteome data is an essential goal of both targeted and non-targeted methods addressing production optimisation goals, additional sample preparation steps beyond necessary sampling, quenching and extraction protocols including clean-up, analyte enrichment, and derivatisation are important considerations for some classes of metabolites, especially those present in low concentrations or exhibiting poor stability. This contribution critically assesses the potential of current sample preparation strategies applied in metabolomic studies of industrially-relevant cell factory organisms using mass spectrometry-based platforms primarily coupled to liquid-phase sample introduction (i.e. flow injection, liquid chromatography, or capillary electrophoresis). Particular focus is placed on the selectivity and degree of enrichment attainable, as well as demands of speed, absolute quantification, robustness and, ultimately, consideration of fully-integrated bioanalytical solutions to optimise sample handling and throughput. Copyright © 2016 Elsevier B.V. All rights reserved.

Recent advances in applications of nanomaterials for sample preparation.

PubMed

Xu, Linnan; Qi, Xiaoyue; Li, Xianjiang; Bai, Yu; Liu, Huwei

2016-01-01

Sample preparation is a key step for qualitative and quantitative analysis of trace analytes in complicated matrix. Along with the rapid development of nanotechnology in material science, numerous nanomaterials have been developed with particularly useful applications in analytical chemistry. Benefitting from their high specific areas, increased surface activities, and unprecedented physical/chemical properties, the potentials of nanomaterials for rapid and efficient sample preparation have been exploited extensively. In this review, recent progress of novel nanomaterials applied in sample preparation has been summarized and discussed. Both nanoparticles and nanoporous materials are evaluated for their unusual performance in sample preparation. Various compositions and functionalizations extended the applications of nanomaterials in sample preparations, and distinct size and shape selectivity was generated from the diversified pore structures of nanoporous materials. Such great variety make nanomaterials a kind of versatile tools in sample preparation for almost all categories of analytes. Copyright © 2015 Elsevier B.V. All rights reserved.

3D chemical mapping: application of scanning transmission (soft) X-ray microscopy (STXM) in combination with angle-scan tomography in bio-, geo-, and environmental sciences.

PubMed

Obst, Martin; Schmid, Gregor

2014-01-01

The identification of environmental processes and mechanisms often requires information on the organochemical and inorganic composition of specimens at high spatial resolution. X-ray spectroscopy (XAS) performed in the soft X-ray range (100-2,200 eV) provides chemical speciation information for elements that are of high biogeochemical relevance such as carbon, nitrogen, and oxygen but also includes transition metals such as iron, manganese, or nickel. Synchrotron-based scanning transmission X-ray microscopy (STXM) combines XAS with high resolution mapping on the 20-nm scale. This provides two-dimensional (2D) quantitative information about the distribution of chemical species such as organic macromolecules, metals, or mineral phases within environmental samples. Furthermore, the combination of STXM with angle-scan tomography allows for three-dimensional (3D) spectromicroscopic analysis of bio-, geo-, or environmental samples. For the acquisition of STXM tomography data, the sample is rotated around an axis perpendicular to the X-ray beam. Various sample preparation approaches such as stripes cut from TEM grids or the preparation of wet cells allow for preparing environmentally relevant specimens in a dry or in a fully hydrated state for 2D and 3D STXM measurements. In this chapter we give a short overview about the principles of STXM, its application to environmental sciences, different preparation techniques, and the analysis and 3D reconstruction of STXM tomography data.

Clostridium perfringens bacteriophages FCP39O and FCP26F: genomic organization and proteomic analysis of the virions

USDA-ARS?s Scientific Manuscript database

Initial screening for bacteriophages lytic for Clostridium perfringens was performed utilizing filtered samples obtained from poultry (intestinal material), soil, sewage and poultry processing drainage water. Lytic phage preparations were initially characterized by transmission electron microscopy ...

Preparing Protocols for Institutional Review Boards.

ERIC Educational Resources Information Center

Lyons, Charles M.

1983-01-01

Introduces the process by which Institutional Review Boards (IRBs) review proposals for research involving human subjects. Describes the composition of IRBs. Presents the Nuremberg code, the elements of informed consent, the judging criteria for proposals, and a sample protocol format. References newly published regulations governing research with…

A Preview of Coming Attractions: Classroom Teacher's Idea Notebook.

ERIC Educational Resources Information Center

Morin, Joy Ann

1995-01-01

Contends that it is important for students to be motivated and well prepared for class units and activities. Describes a "previews of coming attractions" instructional strategy that uses advance organizers to increase information processing efficiency. Includes a sample unit outline illustrating this approach. (CFR)

Pre-analytical issues in the haemostasis laboratory: guidance for the clinical laboratories.

PubMed

Magnette, A; Chatelain, M; Chatelain, B; Ten Cate, H; Mullier, F

2016-01-01

Ensuring quality has become a daily requirement in laboratories. In haemostasis, even more than in other disciplines of biology, quality is determined by a pre-analytical step that encompasses all procedures, starting with the formulation of the medical question, and includes patient preparation, sample collection, handling, transportation, processing, and storage until time of analysis. This step, based on a variety of manual activities, is the most vulnerable part of the total testing process and is a major component of the reliability and validity of results in haemostasis and constitutes the most important source of erroneous or un-interpretable results. Pre-analytical errors may occur throughout the testing process and arise from unsuitable, inappropriate or wrongly handled procedures. Problems may arise during the collection of blood specimens such as misidentification of the sample, use of inadequate devices or needles, incorrect order of draw, prolonged tourniquet placing, unsuccessful attempts to locate the vein, incorrect use of additive tubes, collection of unsuitable samples for quality or quantity, inappropriate mixing of a sample, etc. Some factors can alter the result of a sample constituent after collection during transportation, preparation and storage. Laboratory errors can often have serious adverse consequences. Lack of standardized procedures for sample collection accounts for most of the errors encountered within the total testing process. They can also have clinical consequences as well as a significant impact on patient care, especially those related to specialized tests as these are often considered as "diagnostic". Controlling pre-analytical variables is critical since this has a direct influence on the quality of results and on their clinical reliability. The accurate standardization of the pre-analytical phase is of pivotal importance for achieving reliable results of coagulation tests and should reduce the side effects of the influence factors. This review is a summary of the most important recommendations regarding the importance of pre-analytical factors for coagulation testing and should be a tool to increase awareness about the importance of pre-analytical factors for coagulation testing.

Two-Step Sintering Behavior of Sol-Gel Derived Dense and Submicron-Grained YIG Ceramics

NASA Astrophysics Data System (ADS)

Chen, Ruoyuan; Zhou, Jijun; Zheng, Liang; Zheng, Hui; Zheng, Peng; Ying, Zhihua; Deng, Jiangxia

2018-04-01

In this work, dense and submicron-grain yttrium iron garnet (YIG, Y3Fe5O12) ceramics were fabricated by a two-step sintering (TSS) method using nano-size YIG powder prepared by a citrate sol-gel method. The densification, microstructure, magnetic properties and ferromagnetic resonance (FMR) linewidth of the ceramics were investigated. The sample prepared at 1300°C in T 1, 1225°C in T 2 and 18 h holding time has a density higher than 98% of the theoretical value and exhibits a homogeneous microstructure with fine grain size (0.975 μm). In addition, the saturation magnetization ( M S) of this sample reaches 27.18 emu/g. High density and small grain size can also achieve small FMR linewidth. Consequently, these results show that the sol-gel process combined with the TSS process can effectively suppress grain-boundary migration while maintaining active grain-boundary diffusion to obtain dense and fine-grained YIG ceramics with appropriate magnetic properties.

Effects of Processing and Powder Size on Microstructure and Reactivity in Arrested Reactive Milled Al + Ni

DTIC Science & Technology

2012-05-01

reactive milled (RM) experiments forming nickel aluminides [3,4,6,8–10,12,15,16,18,19], titanium - based alloys [5] and combustion reactions in metal...highly heterogeneous and is refined during processing until reaction occurs. The refinement process consists of the cold welding of powder grains within... welding at the surface of deforming particles, which pro-Table 2 Sample preparation measurements corresponding to the designed exper- iments presented

Microbiological performance of a food safety management system in a food service operation.

PubMed

Lahou, E; Jacxsens, L; Daelman, J; Van Landeghem, F; Uyttendaele, M

2012-04-01

The microbiological performance of a food safety management system in a food service operation was measured using a microbiological assessment scheme as a vertical sampling plan throughout the production process, from raw materials to final product. The assessment scheme can give insight into the microbiological contamination and the variability of a production process and pinpoint bottlenecks in the food safety management system. Three production processes were evaluated: a high-risk sandwich production process (involving raw meat preparation), a medium-risk hot meal production process (starting from undercooked raw materials), and a low-risk hot meal production process (reheating in a bag). Microbial quality parameters, hygiene indicators, and relevant pathogens (Listeria monocytogenes, Salmonella, Bacillus cereus, and Escherichia coli O157) were in accordance with legal criteria and/or microbiological guidelines, suggesting that the food safety management system was effective. High levels of total aerobic bacteria (>3.9 log CFU/50 cm(2)) were noted occasionally on gloves of food handlers and on food contact surfaces, especially in high contamination areas (e.g., during handling of raw material, preparation room). Core control activities such as hand hygiene of personnel and cleaning and disinfection (especially in highly contaminated areas) were considered points of attention. The present sampling plan was used to produce an overall microbiological profile (snapshot) to validate the food safety management system in place.

Development and evaluation of a collection apparatus for recoil products for study of the deexcitation process of (235m)U.

PubMed

Shigekawa, Y; Kasamatsu, Y; Shinohara, A

2016-05-01

The nucleus (235m)U is an isomer with extremely low excitation energy (76.8 eV) and decays dominantly through the internal conversion (IC) process. Because outer-shell electrons are involved in the IC process, the decay constant of (235m)U depends on its chemical environment. We plan to study the deexcitation process of (235m)U by measuring the energy spectra of IC electrons in addition to the decay constants for various chemical forms. In this paper, the preparation method of (235m)U samples from (239)Pu by using alpha-recoil energy is reported. A Collection Apparatus for Recoil Products was fabricated, and then collection efficiencies under various conditions were determined by collecting (224)Ra recoiling out of (228)Th electrodeposited and precipitated sources. The pressure in the apparatus (vacuum or 1 atm of N2 gas) affected the variations of the collection efficiencies depending on the negative voltage applied to the collector. The maximum values of the collection efficiencies were mainly affected by the thickness of the (228)Th sources. From these results, the suitable conditions of the (239)Pu sources for preparation of (235m)U were determined. In addition, dissolution efficiencies were determined by washing collected (224)Ra with solutions. When (224)Ra was collected in 1 atm of N2 gas and dissolved with polar solutions such as water, the dissolution efficiencies were nearly 100%. The method of rapid dissolution of recoil products would be applicable to rapid preparation of short-lived (235m)U samples for various chemical forms.

Space processing of composite materials

NASA Technical Reports Server (NTRS)

Steurer, W. H.; Kaye, S.

1975-01-01

Materials and processes for the testing of aluminum-base fiber and particle composites, and of metal foams under extended-time low-g conditions were investigated. A wetting and dispersion technique was developed, based on the theory that under the absence of a gas phase all solids are wetted by liquids. The process is characterized by a high vacuum environment and a high temperature cycle. Successful wetting and dispersion experiments were carried out with sapphire fibers, whiskers and particles, and with fibers of silicon carbide, pyrolytic graphite and tungsten. The developed process and facilities permit the preparation of a precomposite which serves as sample material for flight experiments. Low-g processing consists then merely in the uniform redistribution of the reinforcements during a melting cycle. For the preparation of metal foams, gas generation by means of a thermally decomposing compound was found most adaptable to flight experiments. For flight experiments, the use of compacted mixture of the component materials limits low-g processing to a simple melt cycle.

A laboratory information management system for the analysis of tritium (3H) in environmental waters.

PubMed

Belachew, Dagnachew Legesse; Terzer-Wassmuth, Stefan; Wassenaar, Leonard I; Klaus, Philipp M; Copia, Lorenzo; Araguás, Luis J Araguás; Aggarwal, Pradeep

2018-07-01

Accurate and precise measurements of low levels of tritium ( 3 H) in environmental waters are difficult to attain due to complex steps of sample preparation, electrolytic enrichment, liquid scintillation decay counting, and extensive data processing. We present a Microsoft Access™ relational database application, TRIMS (Tritium Information Management System) to assist with sample and data processing of tritium analysis by managing the processes from sample registration and analysis to reporting and archiving. A complete uncertainty propagation algorithm ensures tritium results are reported with robust uncertainty metrics. TRIMS will help to increase laboratory productivity and improve the accuracy and precision of 3 H assays. The software supports several enrichment protocols and LSC counter types. TRIMS is available for download at no cost from the IAEA at www.iaea.org/water. Copyright © 2018 Elsevier Ltd. All rights reserved.

Influence of the sintering temperature on the electrical properties of Ce-doped WO3 ceramics prepared from nano-powders

NASA Astrophysics Data System (ADS)

Dong, Liang; Chen, Han-Jun; Wang, Yu; Li, De-Zhu; Li, Tong-Ye; Zhao, Yong

2007-04-01

Using a nm-level powder fabricated by a wet chemical method as precursor, the CeO2-doped WO3 ceramics were prepared by the conventional solid state reaction at sintering temperatures from 600 to 1100 °C. The x-ray diffraction analysis reveals the coexistence of different WO3 phases in the samples sintered at temperatures below 900 °C, whereas a single phase appears in the samples sintered above 1000 °C. No new Ce-W compound appears. As the sintering temperature increases, the electrical properties of the samples display an interesting transformation from linear to nonlinear behaviour. The measurements of scanning electron microscope, complex impedance and electrical stability indicate that a lot of grain boundary regions in the samples sintered at low temperatures strongly influences the electrical transportation. Therefore, the electrical nonlinearity is due to a basic process controlled by the back-to-back Schottky barriers at grain boundaries with suitable thickness as well as the coexistence of phases.

Synthesis of crystalline Ce-activated garnet phosphor powders and technique to characterize their scintillation light yield

NASA Astrophysics Data System (ADS)

Gordienko, E.; Fedorov, A.; Radiuk, E.; Mechinsky, V.; Dosovitskiy, G.; Vashchenkova, E.; Kuznetsova, D.; Retivov, V.; Dosovitskiy, A.; Korjik, M.; Sandu, R.

2018-04-01

This work reports on a process of preparation of garnet phosphor powders and a technique for light yield evaluation of strongly light scattering samples. Powders of scintillation compounds could be used as individual materials or as samples for express tests of scintillation properties. However, estimation of their light yield (LY) is complicated by strong light scattering of this kind of materials. Ce3+-activated yttrium-aluminum and gallium-gadolinium-aluminum garnet phosphor powders, Y3Al5O12 (YAG:Ce) and Gd3Ga3Al2O12 (GGAG:Ce), were obtained using a modified coprecipitation technique. Ga tends to residue in mother liquor in ammonia media, but the modification allows to avoid the loss of components. We propose an approach for sample preparation and LY measurement setup with alpha particles excitation, allowing to decrease light scattering influence and to estimate a light yield of powder samples. This approach is used to evaluate the obtained powders.

Thermal Stress Effect on Density Changes of Hemp Hurds Composites

NASA Astrophysics Data System (ADS)

Schwarzova, Ivana; Cigasova, Julia; Stevulova, Nadezda

2016-12-01

The aim of this article is to study the behavior of prepared biocomposites based on hemp hurds as a filling agent in composite system. In addition to the filler and water, an alternative binder, called MgO-cement was used. For this objective were prepared three types of samples; samples based on untreated hemp hurds as a referential material and samples based on chemically (with NaOH solution) and physically (by ultrasonic procedure) treated hemp hurds. The thermal stress effect on bulk density changes of hemp hurds composites was monitored. Gradual increase in temperature led to composites density reduction of 30-40 %. This process is connected with mass loss of the adsorbed moisture and physically bound water and also with degradation of organic compounds present in hemp hurds aggregates such as pectin, hemicelluloses and cellulose. Therefore the changes in the chemical composition of treated hemp hurds in comparison to original sample and its thermal decomposition were also studied.

Evaporator Feed Qualification Analysis Of Tank 38H And 43H Samples: January 2010 Through April 2013

DOE Office of Scientific and Technical Information (OSTI.GOV)

Martino, C. J.; Coleman, C. J.

2013-08-21

This report provides the results of analyses that focused on the chemical species that pertain to the sodium aluminosilicate formation potential for archived Tank 38H and 43H subsurface samples from January 2010 through April 2013. Analyses included warm acid strike preparation followed by analysis of silicon, aluminum, and sodium and water dilution preparation followed by analysis for anions. The Tank 43H and 38H supernatant liquid silicon measurements for the January 2010 through April 2013 time period exhibit a slight increasing trend. Over this time period, the silicon concentration in the Tank 43H and Tank 38H samples averaged 179 mg/L andmore » 235 mg/L, respectively. Comparison of Tank 43H sample results from 2005 through April 2013 to the previously developed process control models indicates that the current formation of sodium aluminosilicate in the 2H system is due to the seeded direct precipitation of cancrinite and sodalite.« less

Effects of preparation methods on the structure and mechanical properties of wet conditioned starch/montmorillonite nanocomposite films.

PubMed

Müller, Péter; Kapin, Éva; Fekete, Erika

2014-11-26

TPS/Na-montmorillonite nanocomposite films were prepared by solution and melt blending. Clay content changed between 0 and 25 wt% based on the amount of dry starch. Structure, tensile properties, and water content of wet conditioned films were determined as a function of clay content. Intercalated structure and VH-type crystallinity of starch were found for all the nanocomposites independently of clay and plasticizer content or preparation method, but at larger than 10 wt% clay content nanocomposites prepared by melt intercalation contained aggregated particles as well. In spite of the incomplete exfoliation clay reinforces TPS considerably. Preparation method has a strong influence on mechanical properties of wet conditioned films. Mechanical properties of the conditioned samples prepared by solution homogenization are much better than those of nanocomposites prepared by melt blending. Water, which was either adsorbed or bonded in the composites in conditioning or solution mixing process, respectively, has different effect on mechanical properties. Copyright © 2014 Elsevier Ltd. All rights reserved.

EVALUATION OF ARG-1 SAMPLES PREPARED BY CESIUM CARBONATE DISSOLUTION DURING THE ISOLOK SME ACCEPTABILITY TESTING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T.; Hera, K.; Coleman, C.

2011-12-05

Evaluation of Defense Waste Processing Facility (DWPF) Chemical Process Cell (CPC) cycle time identified several opportunities to improve the CPC processing time. The Mechanical Systems & Custom Equipment Development (MS&CED) Section of the Savannah River National Laboratory (SRNL) recently completed the evaluation of one of these opportunities - the possibility of using an Isolok sampling valve as an alternative to the Hydragard valve for taking DWPF process samples at the Slurry Mix Evaporator (SME). The use of an Isolok for SME sampling has the potential to improve operability, reduce maintenance time, and decrease CPC cycle time. The SME acceptability testingmore » for the Isolok was requested in Task Technical Request (TTR) HLW-DWPF-TTR-2010-0036 and was conducted as outlined in Task Technical and Quality Assurance Plan (TTQAP) SRNLRP-2011-00145. RW-0333P QA requirements applied to the task, and the results from the investigation were documented in SRNL-STI-2011-00693. Measurement of the chemical composition of study samples was a critical component of the SME acceptability testing of the Isolok. A sampling and analytical plan supported the investigation with the analytical plan directing that the study samples be prepared by a cesium carbonate (Cs{sub 2}CO{sub 3}) fusion dissolution method and analyzed by Inductively Coupled Plasma - Optical Emission Spectroscopy (ICP-OES). The use of the cesium carbonate preparation method for the Isolok testing provided an opportunity for an additional assessment of this dissolution method, which is being investigated as a potential replacement for the two methods (i.e., sodium peroxide fusion and mixed acid dissolution) that have been used at the DWPF for the analysis of SME samples. Earlier testing of the Cs{sub 2}CO{sub 3} method yielded promising results which led to a TTR from Savannah River Remediation, LLC (SRR) to SRNL for additional support and an associated TTQAP to direct the SRNL efforts. A technical report resulting from this work was issued that recommended that the mixed acid method be replaced by the Cs{sub 2}CO{sub 3} method for the measurement of magnesium (Mg), sodium (Na), and zirconium (Zr) with additional testing of the method by DWPF Laboratory being needed before further implementation of the Cs{sub 2}CO{sub 3} method at that laboratory. While the SME acceptability testing of the Isolok does not address any of the open issues remaining after the publication of the recommendation for the replacement of the mixed acid method by the Cs{sub 2}CO{sub 3} method (since those issues are to be addressed by the DWPF Laboratory), the Cs{sub 2}CO{sub 3} testing associated with the Isolok testing does provide additional insight into the performance of the method as conducted by SRNL. The performance is to be investigated by looking to the composition measurement data generated by the samples of a standard glass, the Analytical Reference Glass - 1 (ARG-1), that were prepared by the Cs{sub 2}CO{sub 3} method and included in the SME acceptability testing of the Isolok. The measurements of these samples were presented as part of the study results, but no statistical analysis of these measurements was conducted as part of those results. It is the purpose of this report to provide that analysis, which was supported using JMP Version 7.0.2.« less

In-vitro study of copper doped SiO{sub 2}-CaO-P{sub 2}O{sub 5} system for bioactivity and antimicrobial properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaur, Kulwinder; Singh, K. J., E-mail: kanwarjitsingh@yahoo.com; Anand, Vikas

Samples of the xCuO-(45-x)CaO-10P{sub 2}O{sub 5}-45SiO{sub 2} system (x varies from 0 to 4 mole%) have been synthesized for application as biomaterials to slow or inhibit the growth of living organisms (fungi and other pathogenic microorganisms) by the combination of sol-gel and co-precipitation processes. Prepared samples have been characterized by X-Ray Diffraction, Fourier Transform Infra-Red and Field Emission Scanning Electron Microscopy techniques before and after immersion in simulated body fluid. Antimicrobial activity of samples has been investigated against Staphylococcus aureus. Releasing of Cu{sup 2+}and other ions in the simulated body fluid has been determined by Atomic Absorption Spectroscopy to ensuremore » the use of prepared material as biomaterial with good antibacterial properties.« less

Laboratory investigations

NASA Technical Reports Server (NTRS)

Russell, Ray W.

1988-01-01

Laboratory studies related to cometary grains and the nuclei of comets can be broken down into three areas which relate to understanding the spectral properties, the formation mechanisms, and the evolution of grains and nuclei: (1) Spectral studies to be used in the interpretation of cometary spectra; (2) Sample preparation experiments which may shed light on the physical nature and history of cometary grains and nuclei by exploring the effects on grain emissivities resulting from the ways in which the samples are created; and (3) Grain processing experiments which should provide insight on the interaction of cometary grains with the environment in the immediate vicinity of the cometary nucleus as the comet travels from the Oort cloud through perihelion, and perhaps even suggestions regarding the relationship between interstellar grains and cometary matter. A summary is presented with a different view of lab experiments than is found in the literature, concentrating on measurement techniques and sample preparations especially relevant to cometary dust.

Evaluation of Microstructure and Mechanical Properties of Al-TiC Metal Matrix Composite Prepared by Conventional, Microwave and Spark Plasma Sintering Methods

PubMed Central

Ghasali, Ehsan; Fazili, Ali; Alizadeh, Masoud; Shirvanimoghaddam, Kamyar; Ebadzadeh, Touradj

2017-01-01

In this research, the mechanical properties and microstructure of Al-15 wt % TiC composite samples prepared by spark plasma, microwave, and conventional sintering were investigated. The sintering process was performed by the speak plasma sintering (SPS) technique, microwave and conventional furnaces at 400 °C, 600 °C, and 700 °C, respectively. The results showed that sintered samples by SPS have the highest relative density (99% of theoretical density), bending strength (291 ± 12 MPa), and hardness (253 ± 23 HV). The X-ray diffraction (XRD) investigations showed the formation of TiO2 from the surface layer decomposition of TiC particles. Scanning electron microscopy (SEM) micrographs demonstrated uniform distribution of reinforcement particles in all sintered samples. The SEM/EDS analysis revealed the formation of TiO2 around the porous TiC particles. PMID:29088114

Fabrication and thermoelectric properties of n-type (Sr0.9Gd0.1)TiO3 oxides

NASA Astrophysics Data System (ADS)

Li, Liangliang; Qin, Xiaoying; Liu, Yongfei; Xin, Hongxing; Zhang, Jian; Li, Di; Song, Chunjun; Guo, Guanglei; Dou, Yunchen; Zou, Tianhua

2014-02-01

The n-type oxides (Sr0.9Gd0.1)TiO3 (SGTO) have been successfully prepared via a sol-gel process followed by solid-state sintering. The effects of sintering temperature on the thermoelectric (TE) properties of the SGTO samples have been investigated. The Seebeck coefficient showed no obvious difference, while the electrical conductivity increased with increasing sintering temperature, benefiting from an enhancement of densification. The maximum power factor (PF) value, 20.5μW/K2cm at 370 K in the metallic region, was observed for the sample sintered at 1748 K. As a result, the peak figure of merit (ZT) values for the samples sintered at higher than 1673 K were in the range of 0.28-0.30. All the results indicate that such synthetic method provides a simple and effective way to prepare TE oxides.

In Vitro Evaluation and Mechanism Analysis of the Fiber Shedding Property of Textile Pile Debridement Materials

PubMed Central

Fu, Yijun; Xie, Qixue; Lao, Jihong; Wang, Lu

2016-01-01

Fiber shedding is a critical problem in biomedical textile debridement materials, which leads to infection and impairs wound healing. In this work, single fiber pull-out test was proposed as an in vitro evaluation for the fiber shedding property of a textile pile debridement material. Samples with different structural design (pile densities, numbers of ground yarns and coating times) were prepared and estimated under this testing method. Results show that single fiber pull-out test offers an appropriate in vitro evaluation for the fiber shedding property of textile pile debridement materials. Pull-out force for samples without back-coating exhibited a slight escalating trend with the supplement in pile density and number of ground yarn plies, while back-coating process significantly raised the single fiber pull-out force. For fiber shedding mechanism analysis, typical pull-out behavior and failure modes of the single fiber pull-out test were analyzed in detail. Three failure modes were found in this study, i.e., fiber slippage, coating point rupture and fiber breakage. In summary, to obtain samples with desirable fiber shedding property, fabric structural design, preparation process and raw materials selection should be taken into full consideration. PMID:28773428

Processing, Mechanical and Optical Properties of Additive-Free ZrC Ceramics Prepared by Spark Plasma Sintering.

PubMed

Musa, Clara; Licheri, Roberta; Orrù, Roberto; Cao, Giacomo; Sciti, Diletta; Silvestroni, Laura; Zoli, Luca; Balbo, Andrea; Mercatelli, Luca; Meucci, Marco; Sani, Elisa

2016-06-18

In the present study, nearly fully dense monolithic ZrC samples are produced and broadly characterized from microstructural, mechanical and optical points of view. Specifically, 98% dense products are obtained by Spark Plasma Sintering (SPS) after 20 min dwell time at 1850 °C starting from powders preliminarily prepared by Self-propagating High-temperature Synthesis (SHS) followed by 20 min ball milling. A prolonged mechanical treatment up to 2 h of SHS powders does not lead to appreciable benefits. Vickers hardness of the resulting samples (17.5 ± 0.4 GPa) is reasonably good for monolithic ceramics, but the mechanical strength (about 250 MPa up to 1000 °C) could be further improved by suitable optimization of the starting powder characteristics. The very smoothly polished ZrC specimen subjected to optical measurements displays high absorption in the visible-near infrared region and low thermal emittance at longer wavelengths. Moreover, the sample exhibits goodspectral selectivity (2.1-2.4) in the 1000-1400 K temperature range. These preliminary results suggest that ZrC ceramics produced through the two-step SHS/SPS processing route can be considered as attractive reference materials for the development of innovative solar energy absorbers.

Irradiation effect of low-energy ion on polyurethane nanocoating containing metal oxide nanoparticles

NASA Astrophysics Data System (ADS)

Verma, Jaya; Nigam, Subhasha; Sinha, Surbhi; Sikarwar, B. S.; Bhattacharya, Arpita

2017-12-01

Irradiation effect of low-energy ion beam has been investigated on nanocoating developed with silica, titania and silica-titania core-shell nanoparticles embedded in an organic binder for nanopaint application. In this work, we have taken polyurethane as a model organic binder. Silica nanoparticles have been prepared through sol-gel synthesis with a particle size of 85 nm. Titania and core-shell nanoparticles have been prepared through both sol-gel and peptization process. Particle sizes obtained were 107 nm for titania and 240 nm for core-shell nanoparticles prepared through sol-gel process and 75 nm for TiO2 and 144 nm for core-shell nanoparticles prepared through peptization process. The coating formulations were developed with the above nanoparticles individually and nanoparticle concentration was varied from 1 to 6 wt% and the best performance in terms of hydrophobicity was obtained with 4 wt % of the nanoparticles in polyurethane coating formulation. All the coating formulations prepared were applied on a glass substrate and dried at 100°C. The dry film thickness obtained was around 100 µm in each case. These films dried on glass substrate were irradiated by nitrogen and argon ion beam with energy of 26 keV at fluences of 1014 to 1016 ions/cm2. The anti-algal property of the irradiated samples was improved and hydrophobicity was reduced.

Laser Induced Breakdown Spectroscopy of Glass and Crystal Samples

NASA Astrophysics Data System (ADS)

Sharma, Prakash; Sandoval, Alejandra; Carter, Michael; Kumar, Akshaya

2015-03-01

Different types of quartz crystals and rare earth ions doped glasses have been identified using the laser induced breakdown spectroscopy (LIBS) technique. LIBS is a real time technique, can be used to identify samples in solid, liquid and gas phases. The advantage of LIBS technique is that no sample preparation is required and laser causes extremely minimal damage to the sample surface. The LIBS spectrum of silicate glasses, prepared by sol-gel method and doped with different concentration of rare earth ions, has been recorded. The limit of detection of rare earth ions in glass samples has been calculated. Total 10 spectrums of each sample were recorded and then averaged to get a final spectrum. The ocean optics LIBS2500 plus spectrometer along with a Q- switched Nd: YAG laser (Quantel, Big Sky) were used to record the LIBS spectrum. This spectrometer can analyze the sample in the spectral range of 200 nm to 980 nm. The spectrum was processed by OOILIBS-plus (v1.0) software. This study has application in the industry where different crystals can be easily identified before they go for shaping and polishing. Also, concentration of rare earth ions in glass can be monitored in real time for quality control.

Effect of polyaniline on MWCNTs supercapacitor properties prepared by electrophoretic deposition

NASA Astrophysics Data System (ADS)

Razak, Rozelia Azila Abd; Eleas, Nor Hamizah; Mohammad, Nurul Nazwa; Yusof, Azmi Mohamed; Zaine, Intan Syaffinazzilla

2017-08-01

Multi-walled carbon nanotubes (MWCNTs) is widely used as supercapacitor electrode material. However, the specific capacitance of MWCNTs cannot achieve optimum value to facilitate required demand. Conducting polymers have been introduced to achieve optimum energy density and power density of supercapacitor electrode material. Previous work had demonstrated the effects of adding conducting polymer into carbon base material to get pseudocapacitance effect. Nevertheless the effects specifically of polyaniline (PANi) to MWCNTs were significantly low. This work describes the effect of PANi adding on MWCNTs film prepared by electrophoretic deposition (EPD) technique in order to increase the specific capacitance of MWCNTs. The commercial MWCNTs is dispersed in deionized water by using crystal violet. The admixtures without PANi (sample A), 5wt.% of PANi (sample B) and 10wt.% of PANi (sample C) have been prepared by ex-situ polymerization. The voltage supplied for film deposition is 8 V for 5 minutes. The morphology, functional group and electrochemical properties of MWCNTs due to the presence of PANi had been studied. From FESEM analysis, the presence of PANi can be clearly observed for sample B and sample C while FTIR analysis, proves PANi structure on MWCNTs with its functional group presence in sample B and sample C through the absorbtion band which obviously shifted to higher value compare to sample A. Cyclic voltammogram (CV) analysis shown redox activity occurred in sample B and sample C with identical anodic and cathodic peaks. Sample B hold the higher specific capacitance and higher energy density compared than sample A and sample B. From galvanostatic charge-discharge (CD) measurement, the charge and discharge process for sample B is longer than sample A and sample C which consequently lower its power density. The presence of PANi at 5wt.% is able to increase specific capacitance as well as energy density to optimum value.

Accelerating sample preparation through enzyme-assisted microfiltration of Salmonella in chicken extract

USDA-ARS?s Scientific Manuscript database

Microfiltration of chicken extracts has the potential to significantly decrease the time required to detect Salmonella, as long as the extract can be efficiently filtered and the pathogenic microorganisms kept in a viable state during this process. We present conditions that enable microfiltration ...

Evaporation-based method for preparing gelatin foams with aligned tubular pore structures.

PubMed

Frazier, Shane D; Srubar, Wil V

2016-05-01

Gelatin-based foams with aligned tubular pore structures were prepared via liquid-to-gas vaporization of tightly bound water in dehydrated gelatin hydrogels. This study elucidates the mechanism of the foaming process by investigating the secondary (i.e., helical) structure, molecular interactions, and water content of gelatin films before and after foaming using X-ray diffraction, Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry and thermogravimetric analysis (TGA), respectively. Experimental data from gelatin samples prepared at various gelatin-to-water concentrations (5-30 wt.%) substantiate that resulting foam structures are similar in pore diameter (approximately 350 μm), shape, and density (0.05-0.22 g/cm(3)) to those fabricated using conventional methods (e.g., freeze-drying). Helical structures were identified in the films but were not evident in the foamed samples after vaporization (~150 °C), suggesting that the primary foaming mechanism is governed by the vaporization of water that is tightly bound in secondary structures (i.e., helices, β-turns, β-sheets) that are present in dehydrated gelatin films. FTIR and TGA data show that the foaming process leads to more disorder and reduced hydrogen bonding to hydroxyl groups in gelatin and that no thermal degradation of gelatin occurs before or after foaming. Copyright © 2016 Elsevier B.V. All rights reserved.

Tracking sources of Clostridium botulinum type E contamination in seal meat.

PubMed

Leclair, Daniel; Farber, Jeffrey M; Pagotto, Franco; Suppa, Sandy; Doidge, Bill; Austin, John W

2017-01-01

Botulism in Nunavik, Quebec is associated with the consumption of aged marine mammal meat and fat. The objective was to identify meat handling practices presenting a risk of contamination of seal meat with C. botulinum. Potential sources of contamination were assessed through interviews with igunaq producers from five communities of Nunavik. These sources were verified by detection and isolation of C. botulinum from igunaq prepared in the field from seal carcasses. Interviews indicated practices presenting a risk for contamination included: placing meat or fat on coastal rocks, using seawater for rinsing, and ageing meat in inverted seal skin pouches. Although the presence of C. botulinum type E spores was detected in only two of 32 (6.3%) meat or fat samples collected during the butchering process, two of four igunaq preparations from these samples contained type E botulinum toxin. Analysis of C. botulinum type E isolates recovered from these preparations indicated that shoreline soil may be a source of contamination. Seal meat and fat may be contaminated with C. botulinum type E during the butchering process. Measures can be adopted to reduce the risks of contamination in the field and possibly decrease the incidence of type E botulism in Nunavik.

Effect of surface modification on photoluminescence properties of Y3Al5O12:Ce3+, Gd3+ nano-phosphors.

PubMed

Li, Jie; Zhao, Junfu; Zhou, Hefeng; Liang, Jian; Liu, Xuguang; Xu, Bingshe

2011-04-01

In this study, a series of Y(3)Al(5)O(12):Ce(3+), Gd(3+) nano-phosphors were prepared using a simply wet chemical process with polyvinyl pyrrolidone as a modifier. The crystal and bonding structures of Y(3)Al(5)O(12):Ce(3+), Gd(3+) nano-phosphors prepared with different weight percentages of polyvinyl pyrrolidone were characterized by X-ray diffractometry and infrared spectrometry. The decomposition process of dried precursor gel with adding 1.37 wt% polyvinyl pyrrolidone was investigated by differential thermal and thermogravimetric analysis. The effect of surface modification on photoluminescence properties for the samples was studied. The results show that the steric hindrance effect of polyvinyl pyrrolidone leads to high dispersion and good crystallinity of Y(3)Al(5)O(12):Ce(3+), Gd(3+) nano-phosphors prepared with adding a proper weight percentages of polyvinyl pyrrolidone. Adding polyvinyl pyrrolidone is beneficial for the photoluminescence enhancement of the samples, which is attributed to the promotion of the incorporation of Ce(3+) and Gd(3+) into the Y(3)Al(5)O(12) nanocrystal and the surface passivation of the nano-particles by the polyvinyl pyrrolidone molecules. Copyright © 2011 Elsevier B.V. All rights reserved.

Filtration of water-sediment samples for the determination of organic compounds

USGS Publications Warehouse

Sandstrom, Mark W.

1995-01-01

This report describes the equipment and procedures used for on-site filtration of surface-water and ground-water samples for determination of organic compounds. Glass-fiber filters and a positive displacement pumping system are suitable for processing most samples for organic analyses. An optional system that uses disposable in-line membrane filters is suitable for a specific gas chromatography/mass spectrometry, selected-ion monitoring analytical method for determination of organonitrogen herbicides. General procedures to minimize contamination of the samples include preparing a clean workspace at the site, selecting appropriate sample-collection materials, and cleaning of the equipment with detergent, tap water, and methanol.

Commander Bowersox Tends to Zeolite Crystal Samples Aboard Space Station

NASA Technical Reports Server (NTRS)

2003-01-01

Expedition Six Commander Ken Bowersox spins Zeolite Crystal Growth sample tubes to eliminate bubbles that could affect crystal formation in preparation of a 15 day experiment aboard the International Space Station (ISS). Zeolites are hard as rock, yet are able to absorb liquids and gases like a sponge. By using the ISS microgravity environment to grow better, larger crystals, NASA and its commercial partners hope to improve petroleum manufacturing and other processes.

Science of Decision Making: A Data-Modeling Approach

DTIC Science & Technology

2013-10-01

were separated on a capillary column using the Dionex UltiMate 3000 (Sunnyvale, CA). The resolved peptides were then sprayed into a linear ion trap...database (3–5). These algorithms assign a peptide sequence, along with a matching score of the experimental ion product mass spectrum, to a theoretical ion ...Bacterial Sample Processing Samples were prepared for liquid chromatography (LC) tandem MS (LC– MS/MS) in a similar manner to that previously reported

Influenza A Virus Isolation, Culture and Identification

PubMed Central

Eisfeld, Amie J.; Neumann, Gabriele; Kawaoka, Yoshihiro

2017-01-01

SUMMARY Influenza A viruses (IAV) cause epidemics and pandemics that result in considerable financial burden and loss of human life. To manage annual IAV epidemics and prepare for future pandemics, improved understanding of how IAVs emerge, transmit, cause disease, and acquire pandemic potential is urgently needed. Fundamental techniques essential for procuring such knowledge are IAV isolation and culture from experimental and surveillance samples. Here, we present a detailed protocol for IAV sample collection and processing, amplification in chicken eggs and mammalian cells, and identification from samples containing unknown pathogens. This protocol is robust, and allows for generation of virus cultures that can be used for downstream analyses. Once experimental or surveillance samples are obtained, virus cultures can be generated and the presence of IAV can be verified in 3–5 days. Increased time-frames may be required for less experienced laboratory personnel, or when large numbers of samples will be processed. PMID:25321410

Devitrification of amorphous celecoxib.

PubMed

Gupta, Piyush; Bansal, Arvind K

2005-09-30

The purpose of this research was to analyze the devitrification of amorphous celecoxib (CEL) in the presence of different stressors (temperature, pressure, and/or humidity) encountered during processing of solid dosage forms. Amorphous CEL was prepared in situ in the analytical instruments, as well as in laboratory, by quench-cooling of melt process, and analyzed by dynamic mechanical thermal analysis, differential scanning calorimetry, microscopy, and Fourier-transform infrared spectroscopy. Amorphous CEL prepared in situ in the analytical instruments was resistant to crystallization under the influence of temperature and/or pressure, because of its protection from the external environment during preparation. These samples exhibited structural relaxation during annealing at 25 degrees C/0% relative humidity (RH) for 16 hours. Generation of amorphous CEL in the laboratory resulted in partially crystalline samples, because of exposure to environmental temperature and humidity, resulting in incomplete vitrification. Subjection to thermal stress favored crystallization of amorphous CEL into metastable polymorphic forms, which were not obtained by solvent recrystallization approach. Temperature and humidity were identified as the major factors promoting devitrification of amorphous CEL, leading to loss of solubility advantage. Exposure to International Conference on Harmonization-specified accelerated stability storage conditions (40 degrees C/75% RH) resulted in complete devitrification of amorphous CEL within 15 days. The phase-transformation process of amorphous CEL along the temperature scale was examined visually, as well as spectrally. This propensity for devitrification of amorphous CEL seemed to depend on the strength of differential molecular interactions between the amorphous and crystalline form.

Process Research of Polycrystalline Silicon Material (PROPSM)

NASA Technical Reports Server (NTRS)

Culik, J. S.

1984-01-01

A passivation process (hydrogenation) that will improve the power generation of solar cells fabricated from presently produced, large grain, cast polycrystalline silicon (Semix), a potentially low cost material are developed. The first objective is to verify the operation of a DC plasma hydrogenation system and to investigate the effect of hydrogen on the electrical performance of a variety of polycrystalline silicon solar cells. The second objective is to parameterize and optimize a hydrogenation process for cast polycrystalline silicon, and will include a process sensitivity analysis. The sample preparation for the first phase is outlined. The hydrogenation system is described, and some early results that were obtained using the hydrogenation system without a plasma are summarized. Light beam induced current (LBIC) measurements of minicell samples, and their correlation to dark current voltage characteristics, are discussed.

Results of Hg speciation testing on DWPF SMECT-8, OGCT-1, AND OGCT-2 samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C.

2016-02-22

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team. The sixteenth shipment of samples was designated to include a Defense Waste Processing Facility (DWPF) Slurry Mix Evaporator Condensate Tank (SMECT) sample from Sludge Receipt and Adjustment Tank (SRAT) Batch 738 processing and two Off-Gas Condensate Tank (OGCT) samples, one following Batch 736 and one following Batch 738. The DWPF sample designations for the three samples analyzed are provided. The Batch 738 ‘End ofmore » SME Cycle’ SMECT sample was taken at the conclusion of Slurry Mix Evaporator (SME) operations for this batch and represents the fourth SMECT sample examined from Batch 738. Batch 738 experienced a sludge slurry carryover event, which introduced sludge solids to the SMECT that were particularly evident in the SMECT-5 sample, but less evident in the ‘End of SME Cycle’ SMECT-8 sample.« less

Drug loaded silica coated MnFe2O4 ferromagnetic biomaterials for targeted cancer treatment

NASA Astrophysics Data System (ADS)

Anand, Vikas; Singh, K. J.; Kaur, Kulwinder; Bhatia, Gaurav

2017-05-01

Magnetically attracted silica coated MnFe2O4 samples have been prepared by using co-precipitation method. Structural changes have been confirmed from XRD spectra. Ferromagnetic behavior of samples has been studied by using vibration sample magnetometer. Cytotoxicity and cell culture of samples have been investigated by using human MG63 cell line and found that sample provide a healthy environment to the growth of cell lines. Drug carrier ability of sample has been checked with gentamycin as an antibiotic and results show that sample can be used as excellent drug carriers. Drug loaded samples can be easily targeted to specific area due to their attractive nature towards external magnetic field. Moreover, magnetic nanoparticles can also be used to kill the cancer cells by using hyperthermia technique. Hyperthermia is a process to raise the temperature of surrounding cells in the presence of external AC magnetic field above the maximum temperature limit for surviving of the cancer cells. Cancer cell can survive only up to 47°C. After that cancer cells start to die, but healthy cells can easily survive up to higher temperature. Our results indicate that prepared samples possess good drug carrier ability and hence, can be potential candidates for cancer cell treatment.

Preparation of 'near' homogeneous samples for the analysis of matrix-assisted laser desorption/ionisation processes

NASA Astrophysics Data System (ADS)

Allwood, D. A.; Perera, I. K.; Perkins, J.; Dyer, P. E.; Oldershaw, G. A.

1996-11-01

Highly uniform thin films of samples for matrix-assisted laser desorption/ionisation (MALDI) have been fabricated by depositing a saturated solution of ferulic acid onto a soda lime glass disc and crushing with polished aluminium, the films covering large areas of the substrate and having a thickness between 45-60 μm. The effects that different substrates and crushing materials as well as sample concentration and sample recrystallisation have on these films has been examined by scanning electron microscopy. Such films have been shown to have a lower threshold fluence for matrix ion detection than standard dried-droplet samples, the reduction being approximately 15% for three of the five matrices analysed. An explanation for this is proposed in terms of crushed samples possessing a greater average energy per unit volume coupled to them by the laser due to their improved surface uniformity. Furthermore, samples that are dried at refrigerated temperatures (˜ 2.25°C) are shown to have a much improved macroscopic uniformity over samples dried at room temperature. Refrigerated and crushed MALDI samples yield analyte ions with good spot-to-spot and pulse-to-pulse reproducibility and both preparation steps appear to improve the resolution of spectra obtained with a time-of-flight mass spectrometer.

Analysis of coke beverages by total-reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Fernández-Ruiz, Ramón; von Bohlen, Alex; Friedrich K, E. Josue; Redrejo, M. J.

2018-07-01

The influence of the organic content, sample preparation process and the morphology of the depositions of two types of Coke beverage, traditional and light Coke, have been investigated by mean of Total-reflection X-ray Fluorescence (TXRF) spectrometry. Strong distortions of the nominal concentration values, up to 128% for P, have been detected in the analysis of traditional Coke by different preparation methods. These differences have been correlated with the edge X-ray energies of the elements analyzed being more pronounced for the lighter elements. The influence of the organic content (mainly sugar) was evaluated comparing traditional and light Coke analytical TXRF results. Three sample preparation methods have been evaluated as follows: direct TXRF analysis of the sample only adding internal standard, TXRF analysis after open vessel acid digestion and TXRF analysis after high pressure and temperature microwave-assisted acid digestion. Strong correlations were detected between quantitative results, methods of preparation and energies of the X-ray absorption edges of quantified elements. In this way, a decay behavior for the concentration differences between preparation methods and the energies of the X-ray absorption edges of each element were observed. The observed behaviors were modeled with exponential decay functions obtaining R2 correlation coefficients from 0.989 to 0.992. The strong absorption effect observed, and even possible matrix effect, can be explained by the inherent high organic content of the evaluated samples and also by the morphology and average thickness of the TXRF depositions observed. As main conclusion of this work, the analysis of light elements in samples with high organic content by TXRF, i.e. medical, biological, food or any other organic matrixes should be taken carefully. In any case, the direct analysis is not recommended and a previous microwave-assisted acid digestion, or similar, is mandatory, for the correct elemental quantification by TXRF.

In vivo Degradation of Three-Dimensional Silk Fibroin Scaffolds

PubMed Central

Wang, Yongzhong; Rudym, Darya D.; Walsh, Ashley; Abrahamsen, Lauren; Kim, Hyeon-Joo; Kim, Hyun Suk; Kirker-Head, Carl; Kaplan, David L.

2011-01-01

Three-dimensional porous scaffolds prepared from regenerated silk fibroin using either an all aqueous process or a process involving an organic solvent, hexafluoroisopropanol (HFIP) have shown promise in cell culture and tissue engineering applications. However, their biocompatibility and in vivo degradation has not been fully established. The present study was conducted to systematically investigate how processing method (aqueous vs. organic solvent) and processing variables (silk fibroin concentration and pore size) affect the short-term (up to 2 months) and long-term (up to 1 year) in vivo behavior of the protein scaffolds in both nude and Lewis rats. The samples were analyzed by histology for scaffold morphological changes and tissue ingrowth, and by real-time RT-PCR and immunohistochemistry for immune responses. Throughout the period of implantation, all scaffolds were well-tolerated by the host animals and immune responses to the implants were mild. Most scaffolds prepared from the all aqueous process degraded to completion between two and six months, while those prepared from organic solvent (hexafluoroisopropanol (HFIP)) process persisted beyond one year. Due to widespread cellular invasion throughout the scaffold, the degradation of aqueous-derived scaffolds appears to be more homogeneous than that of HFIP-derived scaffolds. In general and especially for the HFIP-derived scaffolds, a higher original silk fibroin concentration (e.g. 17%) and smaller pore size (e.g. 100–200 µm) resulted in lower levels of tissue ingrowth and slower degradation. These results demonstrate that the in vivo behavior of the three-dimensional silk fibroin scaffolds is related to the morphological and structural features that resulted from different scaffold preparation processes. The insights gained in this study can serve as a guide for processing scenarios to match desired morphological and structural features and degradation time with tissue-specific applications. PMID:18502501

Enhanced spot preparation for liquid extractive sampling and analysis

DOEpatents

Van Berkel, Gary J.; King, Richard C.

2015-09-22

A method for performing surface sampling of an analyte, includes the step of placing the analyte on a stage with a material in molar excess to the analyte, such that analyte-analyte interactions are prevented and the analyte can be solubilized for further analysis. The material can be a matrix material that is mixed with the analyte. The material can be provided on a sample support. The analyte can then be contacted with a solvent to extract the analyte for further processing, such as by electrospray mass spectrometry.

Niche and neutral processes both shape community structure in parallelized, aerobic, single carbon-source enrichments

DOE Data Explorer

Flynn, Theodore M.; Koval, Jason C.; Greenwald, Stephanie M.; Owens, Sarah M.; Kemner, Kenneth M.; Antonopoulos, Dionysios A.

2017-01-01

We present DNA sequence data in FASTA-formatted files from aerobic environmental microcosms inoculated with a sole carbon source. DNA sequences are of 16S rRNA genes present in DNA extracted from each microcosm along with the environmental samples (soil, water) used to inoculate them. These samples were sequenced using the Illumina MiSeq platform at the Environmental Sample Preparation and Sequencing Facility at Argonne National Laboratory. This data is compatible with standard microbiome analysis pipelines (e.g., QIIME, mothur, etc.).

Insights into Regolith Dynamics from the Irradiation Record Preserved in Hayabusa Samples

NASA Technical Reports Server (NTRS)

Keller, Lindsay P.; Berger, E. L.

2014-01-01

The rates of space weathering processes are poorly constrained for asteroid surfaces, with recent estimates ranging over 5 orders of magnitude. The return of the first surface samples from a space-weathered asteroid by the Hayabusa mission and their laboratory analysis provides "ground truth" to anchor the timescales for space weathering. We determine the rates of space weathering on Itokawa by measuring solar flare track densities and the widths of solar wind damaged rims on grains. These measurements are made possible through novel focused ion beam (FIB) sample preparation methods.

One-Step Preparation of Large Area Films of Oriented MoS2 Nanoparticles on Multilayer Graphene and Its Electrocatalytic Activity for Hydrogen Evolution

PubMed Central

He, Jinbao; Fernández, Cristina; Primo, Ana

2018-01-01

MoS2 is a promising material to replace Pt-based catalysts for the hydrogen evolution reaction (HER), due to its excellent stability and high activity. In this work, MoS2 nanoparticles supported on graphitic carbon (about 20 nm) with a preferential 002 facet orientation have been prepared by pyrolysis of alginic acid films on quartz containing adsorbed (NH4)2MoS4 at 900 °C under Ar atmosphere. Although some variation of the electrocatalytic activity has been observed from batch to batch, the MoS2 sample exhibited activity for HER (a potential onset between 0.2 and 0.3 V vs. SCE), depending on the concentrations of (NH4)2MoS4 precursor used in the preparation process. The loading and particle size of MoS2, which correlate with the amount of exposed active sites in the sample, are the main factors influencing the electrocatalytic activity. PMID:29361756

TiO2 nanocomposites: Preparation, characterization, mechanical and biological properties

NASA Astrophysics Data System (ADS)

Koşarsoy, Gözde; Şen, Elif Hilal; Aksöz, Nilüfer; İde, Semra; Aksoy, Hüsnü

2014-11-01

Some novel nanocomposites, which contain different concentrations of TiO2 nanopowders, were firstly prepared by using marble dust with convenient chemical components. Their nano structures characterized and distributions of the nano-aggregations related with internal structural content of the samples have been determined by X-ray Scattering Methods (SAXS and WAXS) and mechanical properties were determined by using strain-stress measurements to increase their potential usage possibility as building materials in health and research centers. In the last and important part of the study, Candida albicans and Aspergillus niger which are a significant risk to medical patients were used to investigate originally prepared nanostructured samples' photocatalyst effect. During the last part of the study, effect of UV and visible light on photocatalyst nanocomposites were also researched. Heterogeneous photocatalysts can carry out advanced oxidation processes used for an antimicrobial effect on microorganisms. TiO2 nanoparticles as one of heterogeneous photocatalysts have been shown to exhibit strong cytotoxicity when exposed to UV and visible light.

Borax as flux on sintering of iron Ancor Steel 1000® under glow discharge

NASA Astrophysics Data System (ADS)

Ariza Suarez, H. G.; Sarmiento Santos, A.; Ortiz Otálora, C. A.

2016-02-01

This work studies the flux effect of borax (di sodium tetraborate decahydrate) on sintering of iron Ancor Steel 1000® in abnormal glow discharge. The incidence of the percentage by weight of borax and the sintering temperature in the process were observed. Samples of powder metallurgical iron were prepared with proportions of 0.50%, 2.0%, 4.0% and 6.0% by weight of borax using the procedures of powder metallurgy. The samples were sintered at 800 and 1100°C for 30min, by glow discharge at low pressure in a reducing atmosphere composed of 20% H2+80% Ar. The samples in compact green-state were analyzed by TGA-DSC to determine the fusion process and mass loss during sintering. The analysis of microhardness and density, shows that at a sintering temperature of 800°C the sample density decreases and the sample microhardness increases with respect to sintered samples without borax. Sintered samples were analysed by DRX showing the absence of precipitates.

An instrument for automated purification of nucleic acids from contaminated forensic samples

PubMed Central

Broemeling, David J; Pel, Joel; Gunn, Dylan C; Mai, Laura; Thompson, Jason D; Poon, Hiron; Marziali, Andre

2008-01-01

Forensic crime scene sample analysis, by its nature, often deals with samples in which there are low amounts of nucleic acids, on substrates that often lead to inhibition of subsequent enzymatic reactions such as PCR amplification for STR profiling. Common substrates include denim from blue jeans, which yields indigo dye as a PCR inhibitor, and soil, which yields humic substances as inhibitors. These inhibitors frequently co-extract with nucleic acids in standard column or bead-based preps, leading to frequent failure of STR profiling. We present a novel instrument for DNA purification of forensic samples that is capable of highly effective concentration of nucleic acids from soil particulates, fabric, and other complex samples including solid components. The novel concentration process, known as SCODA, is inherently selective for long charged polymers such as DNA, and therefore is able to effectively reject known contaminants. We present an automated sample preparation instrument based on this process, and preliminary results based on mock forensic samples. PMID:18438455

Preparation and characterization of resistant starch III from elephant foot yam (Amorphophallus paeonifolius) starch.

PubMed

Reddy, Chagam Koteswara; Haripriya, Sundaramoorthy; Noor Mohamed, A; Suriya, M

2014-07-15

The purpose of this study was to assess the properties of resistant starch (RS) III prepared from elephant foot yam starch using pullulanase enzyme. Native and gelatinized starches were subjected to enzymatic hydrolysis (pullulanase, 40 U/g per 10h), autoclaved (121°C/30 min), stored under refrigeration (4°C/24h) and then lyophilized. After preparation of resistant starch III, the morphological, physical, chemical and functional properties were assessed. The enzymatic and retrogradation process increased the yield of resistant starch III from starch with a concomitant increase increase in its water absorption capacity and water solubility index. A decrease in swelling power was observed due to the hydrolysis and thermal process. Te reduced pasting properties and hardness of resistant starch III were associated with the disintegration of starch granules due to the thermal process. The viscosity was found to be inversely proportional to the RS content in the sample. The thermal properties of RS increased due to retrogradation and recrystallization (P<0.05). Copyright © 2014 Elsevier Ltd. All rights reserved.

Clean and Cold Sample Curation

NASA Technical Reports Server (NTRS)

Allen, C. C.; Agee, C. B.; Beer, R.; Cooper, B. L.

2000-01-01

Curation of Mars samples includes both samples that are returned to Earth, and samples that are collected, examined, and archived on Mars. Both kinds of curation operations will require careful planning to ensure that the samples are not contaminated by the instruments that are used to collect and contain them. In both cases, sample examination and subdivision must take place in an environment that is organically, inorganically, and biologically clean. Some samples will need to be prepared for analysis under ultra-clean or cryogenic conditions. Inorganic and biological cleanliness are achievable separately by cleanroom and biosafety lab techniques. Organic cleanliness to the <50 ng/sq cm level requires material control and sorbent removal - techniques being applied in our Class 10 cleanrooms and sample processing gloveboxes.

Preparation and thermoelectric properties of sulfur doped Ag2Te nanoparticles via solvothermal methods.

PubMed

Zhou, Wenwen; Zhao, Weiyun; Lu, Ziyang; Zhu, Jixin; Fan, Shufen; Ma, Jan; Hng, Huey Hoon; Yan, Qingyu

2012-07-07

In this work, n-type Ag(2)Te nanoparticles are prepared by a solvothermal approach with uniform and controllable sizes, e.g. 5-15 nm. The usage of dodecanethiol during the synthesis effectively introduces sulfur doping into the sample, which optimizes the charge carrier concentration of the nanoparticles to >1 × 10(20) cm(-3). This allows us to achieve the desired electrical resistivities of <5 × 10(-6)Ω m. It is demonstrated that Ag(2)Te particles prepared by this solvothermal process can exhibit high ZT values, e.g. 15 nm Ag(2)Te nanoparticles with effective sulphur doping show a maximum ZT value of ~0.62 at 550 K.

Full genome virus detection in fecal samples using sensitive nucleic acid preparation, deep sequencing, and a novel iterative sequence classification algorithm.

PubMed

Cotten, Matthew; Oude Munnink, Bas; Canuti, Marta; Deijs, Martin; Watson, Simon J; Kellam, Paul; van der Hoek, Lia

2014-01-01

We have developed a full genome virus detection process that combines sensitive nucleic acid preparation optimised for virus identification in fecal material with Illumina MiSeq sequencing and a novel post-sequencing virus identification algorithm. Enriched viral nucleic acid was converted to double-stranded DNA and subjected to Illumina MiSeq sequencing. The resulting short reads were processed with a novel iterative Python algorithm SLIM for the identification of sequences with homology to known viruses. De novo assembly was then used to generate full viral genomes. The sensitivity of this process was demonstrated with a set of fecal samples from HIV-1 infected patients. A quantitative assessment of the mammalian, plant, and bacterial virus content of this compartment was generated and the deep sequencing data were sufficient to assembly 12 complete viral genomes from 6 virus families. The method detected high levels of enteropathic viruses that are normally controlled in healthy adults, but may be involved in the pathogenesis of HIV-1 infection and will provide a powerful tool for virus detection and for analyzing changes in the fecal virome associated with HIV-1 progression and pathogenesis.

Full Genome Virus Detection in Fecal Samples Using Sensitive Nucleic Acid Preparation, Deep Sequencing, and a Novel Iterative Sequence Classification Algorithm

PubMed Central

Cotten, Matthew; Oude Munnink, Bas; Canuti, Marta; Deijs, Martin; Watson, Simon J.; Kellam, Paul; van der Hoek, Lia

2014-01-01

We have developed a full genome virus detection process that combines sensitive nucleic acid preparation optimised for virus identification in fecal material with Illumina MiSeq sequencing and a novel post-sequencing virus identification algorithm. Enriched viral nucleic acid was converted to double-stranded DNA and subjected to Illumina MiSeq sequencing. The resulting short reads were processed with a novel iterative Python algorithm SLIM for the identification of sequences with homology to known viruses. De novo assembly was then used to generate full viral genomes. The sensitivity of this process was demonstrated with a set of fecal samples from HIV-1 infected patients. A quantitative assessment of the mammalian, plant, and bacterial virus content of this compartment was generated and the deep sequencing data were sufficient to assembly 12 complete viral genomes from 6 virus families. The method detected high levels of enteropathic viruses that are normally controlled in healthy adults, but may be involved in the pathogenesis of HIV-1 infection and will provide a powerful tool for virus detection and for analyzing changes in the fecal virome associated with HIV-1 progression and pathogenesis. PMID:24695106

Advancing microwave technology for dehydration processing of biologics.

PubMed

Cellemme, Stephanie L; Van Vorst, Matthew; Paramore, Elisha; Elliott, Gloria D

2013-10-01

Our prior work has shown that microwave processing can be effective as a method for dehydrating cell-based suspensions in preparation for anhydrous storage, yielding homogenous samples with predictable and reproducible drying times. In the current work an optimized microwave-based drying process was developed that expands upon this previous proof-of-concept. Utilization of a commercial microwave (CEM SAM 255, Matthews, NC) enabled continuous drying at variable low power settings. A new turntable was manufactured from Ultra High Molecular Weight Polyethylene (UHMW-PE; Grainger, Lake Forest, IL) to provide for drying of up to 12 samples at a time. The new process enabled rapid and simultaneous drying of multiple samples in containment devices suitable for long-term storage and aseptic rehydration of the sample. To determine sample repeatability and consistency of drying within the microwave cavity, a concentration series of aqueous trehalose solutions were dried for specific intervals and water content assessed using Karl Fischer Titration at the end of each processing period. Samples were dried on Whatman S-14 conjugate release filters (Whatman, Maidestone, UK), a glass fiber membrane used currently in clinical laboratories. The filters were cut to size for use in a 13 mm Swinnex(®) syringe filter holder (Millipore(™), Billerica, MA). Samples of 40 μL volume could be dehydrated to the equilibrium moisture content by continuous processing at 20% with excellent sample-to-sample repeatability. The microwave-assisted procedure enabled high throughput, repeatable drying of multiple samples, in a manner easily adaptable for drying a wide array of biological samples. Depending on the tolerance for sample heating, the drying time can be altered by changing the power level of the microwave unit.

C18-coated stir bar sorptive extraction combined with high performance liquid chromatography-electrospray tandem mass spectrometry for the analysis of sulfonamides in milk and milk powder.

PubMed

Yu, Chunhe; Hu, Bin

2012-02-15

A simple, rapid, sensitive, inexpensive and less sample consuming method of C(18)-stir bar sorptive extraction (SBSE)-high performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) was proposed for the determination of six sulfonamides in milk and milk powder samples. C(18) silica particles coated stir bar was prepared by adhesion method, and two kinds of adhesive glue, polydimethylsiloxane (PDMS) sol and epoxy glue were tried. It was found that the C(18)-coated stir bar prepared by PDMS sol as adhesive glue is more robust than that prepared by epoxy glue when liquid desorption was employed, in terms of both lifetime and organic solvent tolerance. The preparation of C(18) stir bar was simple with good mechanic strength and the stir bar could be reused for more than 20 times. Granular coating has relatively high specific surface area and is propitious to sorptive extraction based process. Compared to conventional PDMS SBSE coating, C(18) coating shows good affinity to the target polar/weak polar sulfonamides. To achieve optimum SBSE extraction performance, several parameters including extraction and desorption time, ionic strength, sample pH and stirring speed were investigated. The detection limits of the proposed method for six sulfonamides were in the range of 0.9-10.5 μg/L for milk and 2.7-31.5 μg/kg for milk powder. Good linearities were obtained for sulfonamides with the correlation coefficients (R) above 0.9922. Finally, the proposed method was successfully applied to the determination of sulfonamides in milk and milk powder samples and satisfied recoveries of spiked target compounds in real samples were obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

Standardized Sample Preparation Using a Drop-on-Demand Printing Platform

DTIC Science & Technology

2013-05-07

successful and robust methodology for energetic sample preparation. Keywords: drop-on-demand; inkjet printing; sample preparation OPEN ACCESS...on a similar length scale. Recently, drop-on-demand inkjet printing technology has emerged as an effective approach to produce test materials to...which most of the material is concentrated along the edges, samples prepared using drop-on-demand inkjet technology demonstrate excellent uniform

Preparation and characterization of sorghum flour with increased resistant starch content

USDA-ARS?s Scientific Manuscript database

The primary objective of this research was to develop an effective process to increase the resistant starch content of sorghum flour. A secondary objective was to investigate the role of the sorghum proteins on starch digestibility. Samples of white sorghum flour (28.9% amylose content) with differe...

Protocol for Initial Purification of Bacteriocin

DTIC Science & Technology

2015-10-01

lysate/extract preparation, column purification, and a desalting . The peptide was tracked throughout the process using a soft agar overlay activity...tris PAGE. It is necessary to desalt those samples for 150-mM and 1-M fractions, by using dialysis or G10 sephadex columns, in order to prevent

Facile preparation of nitrogen-doped porous carbon from waste tobacco by a simple pre-treatment process and their application in electrochemical capacitor and CO{sub 2} capture

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sha, Yunfei; Lou, Jiaying; Bai, Shizhe

2015-04-15

Highlights: • A pre-treatment process is used to prepared N-doped carbon from waste biomass. • Waste tobaccos, which are limited for the disposal, are used as the raw materials. • The product shows a specific surface area and nitrogen content. • Its electrochemical performance is better than commercial activated carbon. • Its CO{sub 2} sorption performance is also better than commercial activated carbon. - Abstract: Preparing nitrogen-doped porous carbons directly from waste biomass has received considerable interest for the purpose of realizing the atomic economy. In this study, N-doped porous carbons have been successfully prepared from waste tobaccos (WT) bymore » a simple pre-treatment process. The sample calcinated at 700 °C (WT-700) shows a micro/meso-porous structures with a BET surface area of 1104 m{sup 2} g{sup −1} and a nitrogen content of ca. 19.08 wt.% (EDS). Performance studies demonstrate that WT-700 displays 170 F g{sup −1} electrocapacitivity at a current density of 0.5 A g{sup −1} (in 6 M KOH), and a CO{sub 2} capacity of 3.6 mmol g{sup −1} at 0 °C and 1 bar, and a selectivity of ca. 32 for CO{sub 2} over N{sub 2} at 25 °C. Our studies indicate that it is feasible to prepare N-enriched porous carbons from waste natural crops by a pre-treatment process for potential industrial application.« less

Australia's evolving food practices: a risky mix of continuity and change.

PubMed

Venn, Danielle; Banwell, Cathy; Dixon, Jane

2017-10-01

To investigate trends in five key aspects of Australian food practice which have been implicated in diet-related health risks, specifically energy intake. They are: the replacement of home-prepared foods by commercially prepared foods; consumer reliance on ultra-processed foods; de-structured dining; increased pace of eating; and a decline in commensal eating. Data were from repeated cross-sections from the national Household Expenditure and Time Use Surveys. Trends in food practice aspects were examined using indicators of food expenditure across different food groups and time spent eating and cooking, including where, when and with whom eating activities took place. Australia, 1989-2010. Nationally representative samples of Australian households. The share of the total food budget spent on food away from home rose steadily from 22·8 % in 1989 to 26·5 % in 2010, while spending on ultra-processed foods increased. The basic patterning of meals and the pace of eating changed little, although people spent more time eating alone and at restaurants. Cooking time declined considerably, particularly for women. These changes have occurred over the same time that obesity and diet-related, non-communicable diseases have increased rapidly in Australia. Some aspects are implicated more than others: particularly the shift from domestic cooking to use of pre-prepared and ultra-processed foods, a reduction in time spent in food preparation and cooking, as well as an upsurge in time and money devoted to eating away from home. These are all likely to operate through the higher energy content of commercially prepared, compared with unprocessed or lightly processed, foods.

Determination of epichlorohydrin and 1,3-dichloro-2-propanol in synthesis of cationic etherifying reagent by headspace gas chromatography.

PubMed

Tao, Zheng-Yi; Chai, Xin-Sheng; Wu, Shu-Bin

2011-09-16

This study demonstrates a headspace gas chromatographic(HS-GC) technique for the determination of residual epichlorohydrin (ECH) and generated 1,3-dichloro-2-propanol (DCP) in synthesis process of 3-chloro-2-hydroxypropyltrimethylammonium chloride (CHTAC). By a weight-based sampling method, coupled with significant dilution in 15.8% sodium sulfate and 0.1% silver nitrate mixed solution rapidly, the sample for HS-GC analysis is prepared. Based on the reaction stoichiometry, the conversion (R) of CHTAC during the synthesis process can be calculated from sampling weight and GC peak area. The results showed that the method has a good measurement precision (RSD<2.5%) and accuracy (recovery=101-104%) for the quantification of both ECH and DCP in the process samples. The present method is simple and accurate, which can be used for the efficient determination of the CHTAC conversion in the synthesis research. Copyright © 2011 Elsevier B.V. All rights reserved.

Levitation force of melt-textured YBCO superconductors under non-quasi-static situation

NASA Astrophysics Data System (ADS)

Zhao, Z. M.; Xu, J. M.; Yuan, X. Y.; Zhang, C. P.

2018-06-01

The superconducting levitation force of a simple superconductor-magnet system under non-quasi-static situation is investigated experimentally. Two yttrium barium copper oxide (YBCO) samples with different performances are chosen from two small batches of samples prepared by the top-seeded melt-textured growth process. The residual carbon content of the precursor powders of the two batches is different due to different heat treatment processes. During the experimental process for measuring the levitation force, the value of the relative speed between the YBCO sample and the permanent magnet is higher than that in conventional studies. The variation characteristics of the superconducting levitation force are analyzed and a crossing phenomenon in the force-displacement hysteresis curves is observed. The results indicate that the superconducting levitation force is different due to the different residual carbon contents. As residual carbon contents reduce, the crossing phenomenon is more obvious accordingly.

The Effect of Multiple Surface Treatments on Biological Properties of Ti-6Al-4V Alloy

NASA Astrophysics Data System (ADS)

Parsikia, Farhang; Amini, Pupak; Asgari, Sirous

2014-09-01

In this research, the effect of various surface treatments including laser processing, grit blasting and anodizing on chemical structure, surface topography, and bioactivity of Ti-6Al-4V was investigated. Six groups of samples were prepared by a combination of two alternative laser processes, grit blasting and anodizing. Selected samples were first evaluated using microanalysis techniques and contact roughness testing and were then exposed to in vitro environment. Scanning electron microscopy was used to characterize the corresponding final surface morphologies. Weight measurement and atomic absorption tests were employed for determination of bioactivity limits of different surface conditions. Based on the data obtained in this study, low-energy laser processing generally yields a better biological response. The maximum bioactivity was attained in those samples exposed to a three step treatment including low-energy laser treatment followed by grit blasting and anodizing.

Summary Report for the Environmental Protection Agency MERL/FRMAC/RAP Mission Alignment Exercise held at the Savannah River Site on June 9-13 2014

DOE Office of Scientific and Technical Information (OSTI.GOV)

Allen, Mark B.; Shanks, Sonoya Toyoko; Fournier, Sean Donovan

From June 9th thru June 13th 2014, members of the Federal Radiological Monitoring and Assessment Center (FRMAC), the Environmental Protection Agency (EPA) and the Department of Energy Radiological Assistance Program (DOE RAP) Region-3 participated in a joint nuclear incident emergency response exercise at the Savannah River Site (SRS) near Aiken, South Carolina. The purpose of this exercise was to strengthen the interoperability relationship between the FRMAC, RAP, and the EPA Mobile Environmental Radiation Laboratory (MERL) stationed in Montgomery, Alabama. The exercise was designed to allowed members of the DOE RAP Region-3 team to collect soil, water, vegetation and air samplesmore » from SRS and submit them through an established FRMAC hotline. Once received and processed through the hotline, FRMAC delivered the samples to the EPA MERL for sample preparation and laboratory radiological analysis. Upon completion of laboratory analysis, data was reviewed and submitted back to FRMAC via an electronic data deliverable (EDD). As part of the exercise, an evaluation was conducted to identify gaps and potential improvements in each step of the processes. Additionally, noteworthy practices and potential future areas of interoperability between FRMAC and EPA were acknowledged. The exercise also provided a unique opportunity for FRMAC personnel to observe EPA sample receipt and sample preparation processes and to gain familiarity with the MERL laboratory instrumentation and radiation detection capabilities. The observations and lessons-learned from this exercise will be critical for developing a more efficient, integrated response for future interactions between the FRMAC and EPA assets.« less

Crystallinity as a tunable switch of poly(L-lactide) shape memory effects.

PubMed

Sobota, Michał; Jurczyk, Sebastian; Kwiecień, Michał; Smola-Dmochowska, Anna; Musioł, Marta; Domański, Marian; Janeczek, Henryk; Kawalec, Michał; Kurcok, Piotr

2017-02-01

Materials with shape memory effect (SME) have already been widely used in the medical field. The interesting part of this group is represented by double function materials. The bioresorption and SME ability are common in polyesters implants. The first information about vascular stent made of bioresorbable polyester with SME was published in 2000. However, there are not many investigations about SME control of elements in the aspect of material processing. In the present work, the ability to control the shape memory (SM) of bioresorbable and semicrystalline poly(L-lactide) (PLLA) is investigated. The studies are based on the unexpected effect of material orientation which was demonstrated even at low percentage deformation in crystallized mould injected material. The presented studies revealed that the different degrees of crystallinity obtained during processing might be a useful switch to create a tailored SME for a specific application. The prepared samples of variable morphology revealed a possibility to control the value of material stress during permanent shape recovery. The degree of shape recovery of the prepared samples was also controlable. The highest stress value observed during permanent shape recovery reached 10MPa for the sample annealed 60min at 115°C even when the sample was only deformed in 8%. The other significant aspect of this work is to present the problem of slow crystallization of the material during and after processing (cooling rate) as well as the possibility of negative SME change during the shelf life of the fabric. Copyright © 2016 Elsevier Ltd. All rights reserved.

Stardust Interstellar Preliminary Examination II: Curating the Interstellar Dust Collector, Picokeystones, and Sources of Impact Tracks

NASA Technical Reports Server (NTRS)

Frank, David R.; Westphal, Andrew J.; Zolensky, Michael E.; Gainsforth, Zack; Butterworth, Anna L.; Bastien, Ronald K.; Allen, Carlton; Anderson, David; Bechtel, Hans A.; Sandford, Scott A.

2013-01-01

We discuss the inherent difficulties that arise during "ground truth" characterization of the Stardust interstellar dust collector. The challenge of identifying contemporary interstellar dust impact tracks in aerogel is described within the context of background spacecraft secondaries and possible interplanetary dust particles and beta-meteoroids. In addition, the extraction of microscopic dust embedded in aerogel is technically challenging. Specifically, we provide a detailed description of the sample preparation techniques developed to address the unique goals and restrictions of the Interstellar Preliminary Exam. These sample preparation requirements and the scarcity of candidate interstellar impact tracks exacerbate the difficulties. We also illustrate the role of initial optical imaging with critically important examples, and summarize the overall processing of the collection to date.

Improved microautoradiographic method to determine individual microorganisms active in substrate uptake in natural waters.

PubMed

Tabor, P S; Neihof, R A

1982-10-01

We report a method which combines epifluorescence microscopy and microautoradiography to determine both the total number of microorganisms in natural water populations and those individual organisms active in the uptake of specific substrates. After incubation with H-labeled substrate, the sample is filtered and, while still on the filter, mounted directly in a film of autoradiographic emulsion on a microscope slide. The microautoradiogram is processed and stained with acridine orange, and, subsequently, the filter is removed before microscopic observation. This novel preparation resulted in increased accuracy in direct counts made from the autoradiogram, improved sensitivity in the recognition of uptake-active (H-labeled) organisms, and enumeration of a significantly greater number of labeled organisms compared with corresponding samples prepared by a previously reported method.

Improved Microautoradiographic Method to Determine Individual Microorganisms Active in Substrate Uptake in Natural Waters

PubMed Central

Tabor, Paul S.; Neihof, Rex A.

1982-01-01

We report a method which combines epifluorescence microscopy and microautoradiography to determine both the total number of microorganisms in natural water populations and those individual organisms active in the uptake of specific substrates. After incubation with 3H-labeled substrate, the sample is filtered and, while still on the filter, mounted directly in a film of autoradiographic emulsion on a microscope slide. The microautoradiogram is processed and stained with acridine orange, and, subsequently, the filter is removed before microscopic observation. This novel preparation resulted in increased accuracy in direct counts made from the autoradiogram, improved sensitivity in the recognition of uptake-active (3H-labeled) organisms, and enumeration of a significantly greater number of labeled organisms compared with corresponding samples prepared by a previously reported method. Images PMID:16346120

Microextraction by Packed Sorbent (MEPS) and Solid-Phase Microextraction (SPME) as Sample Preparation Procedures for the Metabolomic Profiling of Urine

PubMed Central

Silva, Catarina; Cavaco, Carina; Perestrelo, Rosa; Pereira, Jorge; Câmara, José S.

2014-01-01

For a long time, sample preparation was unrecognized as a critical issue in the analytical methodology, thus limiting the performance that could be achieved. However, the improvement of microextraction techniques, particularly microextraction by packed sorbent (MEPS) and solid-phase microextraction (SPME), completely modified this scenario by introducing unprecedented control over this process. Urine is a biological fluid that is very interesting for metabolomics studies, allowing human health and disease characterization in a minimally invasive form. In this manuscript, we will critically review the most relevant and promising works in this field, highlighting how the metabolomic profiling of urine can be an extremely valuable tool for the early diagnosis of highly prevalent diseases, such as cardiovascular, oncologic and neurodegenerative ones. PMID:24958388

Magnetic properties of Ni nanoparticles dispersed in silica prepared by high-energy ball milling

NASA Astrophysics Data System (ADS)

González, E. M.; Montero, M. I.; Cebollada, F.; de Julián, C.; Vicent, J. L.; González, J. M.

1998-04-01

We analyze the magnetic properties of mechanically ground nanosized Ni particles dispersed in a SiO2 matrix. Our magnetic characterization of the as-milled samples show the occurrence of two blocking processes and that of non-monotonic milling time evolutions of the magnetic-order temperature, the high-field magnetization and the saturation coercivity. The measured coercivities exhibit giant values and a uniaxial-type temperature dependence. Thermal treatment carried out in the as-prepared samples result in a remarkable coercivity reduction and in an increase of the high-field magnetization. We conclude, on the basis of the consideration of a core (pure Ni) and shell (Ni-Si inhomogeneous alloy) particle structure, that the magnetoelastic anisotropy plays the dominant role in determining the magnetic properties of our particles.

Development of low fat potato chips through microwave processing.

PubMed

Joshi, A; Rudra, S G; Sagar, V R; Raigond, P; Dutt, S; Singh, B; Singh, B P

2016-08-01

Since snacks high in fats are known to be a significant source of fat and energy intake, these have been put in high dietary restraint category. Therefore, an attempt was made to process potato chips through microwave processing without incorporation of any oil in potato chips. Microwave processing of potato chips was done using microwave power varying from 180 to 600 W using constant sample size. Among eleven different drying models, Parabolic model was found to be the best fit through non-linear regression analysis to illustrate drying kinetics of potato chips. The structural, textural and colour attributes of microwaved potato chips were similar to commercial fried potato chips. It was found that at 600 W after 2.5-3.0 min of processing, potato chips gained the fracturability and crispiness index as that of commercial fried chips. Microwave processing was found suitable for processing of potato chips with low fat content (~3.09 vs 35.5 % in commercial preparation) and with acceptable sensory scores (≥7.6 on 9.0 point on hedonic scale vs 8.0 of control preparation).

Chars from gasification of coal and pine activated with K2CO3: acetaminophen and caffeine adsorption from aqueous solutions.

PubMed

Galhetas, Margarida; Mestre, Ana S; Pinto, Moisés L; Gulyurtlu, Ibrahim; Lopes, Helena; Carvalho, Ana P

2014-11-01

The high carbon contents and low toxicity levels of chars from coal and pine gasification provide an incentive to consider their use as precursors of porous carbons obtained by chemical activation with K2CO3. Given the chars characteristics, previous demineralization and thermal treatments were made, but no improvement on the solids properties was observed. The highest porosity development was obtained with the biomass derived char (Pi). This char sample produced porous materials with preparation yields near 50% along with high porosity development (ABET≈1500m(2)g(-1)). For calcinations at 800°C, the control of the experimental conditions allowed the preparation of samples with a micropore system formed almost exclusively by larger micropores. A mesopore network was developed only for samples calcined at 900°C. Kinetic and equilibrium acetaminophen and caffeine adsorption data, showed that the processes obey to a pseudo-second order kinetic equation and to the Langmuir model, respectively. The results of sample Pi/1:3/800/2 outperformed those of the commercial carbons. Acetaminophen adsorption process was ruled by the micropore size distribution of the carbons. The caffeine monolayer capacities suggest a very efficient packing of this molecule in samples presenting monomodal micropore size distribution. The surface chemistry seems to be the determinant factor that controls the affinity of caffeine towards the carbons. Copyright © 2014 Elsevier Inc. All rights reserved.

Fluorinated Graphene Prepared by Direct Fluorination of N, O-Doped Graphene Aerogel at Different Temperatures for Lithium Primary Batteries.

PubMed

Bi, Xu; Li, Yanyan; Qiu, Zhipeng; Liu, Chao; Zhou, Tong; Zhuo, Shuping; Zhou, Jin

2018-06-25

Fluorinated graphene (FG) has been a star material as a new derivative of graphene. In this paper, a series of fluorinated graphene materials are prepared by using N, O-doped graphene aerogel as precursor via a direct fluorination method, and the effect of fluorination temperature on the FG structure is investigated. The prepared FG samples are systematically characterized by scanning and transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and Raman spectroscopy. It is found that the structure of FG, including features such as layer size, chemical composition, chemical bond state of the component elements, etc., is significantly related to the fluorination temperature. With the change of the fluorination temperature, fluorine atoms enter the graphene framework by a substitution process of the N, O-containing groups, including residual phenol, ether, carbonyl groups, or C⁻N groups, and the addition to CC bonds, subsequently forming a fluoride with different fluorine contents. The fluorine content increases as the fluorination temperature increases from 200 °C to 300 °C, but decreases at a fluorination temperature of 350 °C due to the decomposition of the fluorinated graphene. The prepared FG samples are used as cathode material for lithium primary batteries. The FG sample prepared at 300 °C gives a high specific capacity of 632 mAh g −1 and a discharge plateau of 2.35 V at a current density of 10 mA g −1 , corresponding to a high energy density of 1485 Wh kg −1 .

Efficiency of organic acid preparations for the elimination of naturally occurring Salmonella in feed material.

PubMed

Axmann, Sonja; Kolar, Veronika; Adler, Andreas; Strnad, Irmengard

2017-11-01

Salmonella can enter animal stocks via feedstuffs, thus posing not only an infection risk for animals, but also threatening to contaminate food of animal origin and finally humans. Salmonella contamination in feedstuffs is still a recurring and serious issue in animal production (especially for the poultry sector), and is regularly detected upon self-monitoring by feed companies (self-checks) and official inspections authorities. Operators within the feed chain in certain cases need to use hygienic condition enhancers, such as organic acids, to improve the quality of feed for animal nutrition, providing additional guarantees for the protection of animal and public health. The present study investigated the efficiencies of five organic acid preparations. The acid products were added to three different feed materials contaminated with Salmonella (contamination occurred by recontamination in the course of the production process) at seven different inclusion rates (1-7%) and analysed after 1, 2, and 7 days' exposure time using culture method (tenfold analysis). A reliable standard was established for defining a successful decontamination under the prevailing test conditions: 10 Salmonella-negative results out of 10 tested samples (0/10: i.e. 0 positive samples and 10 negative samples). The results demonstrated that the tested preparations showed significant differences with regard to the reduction in Salmonella contamination. At an inclusion rate of 7% of the feed materials, two out of five acid preparations showed an insufficient, very small, decontamination effect, whereas two others had a relatively large partial effect. Reliable decontamination was demonstrated only for one acid preparation, however, subject to the use of the highest acid concentration.

Lack of latex allergen contamination of solutions withdrawn from vials with natural rubber stoppers.

PubMed

Thomsen, D J; Burke, T G

2000-01-01

The effect on latex allergen contamination and microbial growth of a latex-allergy precaution technique for preparing injectable products was studied. The study consisted of three parts: (1) preparation of 20 samples from vials with latex-containing stoppers in accordance with conventional guidelines, (2) preparation of 20 samples in accordance with latex-allergy precaution guidelines, and (3) preparation of 5 latex-free samples and 1 latex-contaminated sample as negative and positive controls, respectively. The conventional method involved swabbing a vial top with an alcohol prep pad, puncturing the dry natural rubber stopper with an 18-gauge needle attached to a latex-free syringe, and withdrawing the contents of the vial into the syringe. The latex-allergy precaution preparation technique was similar, except that the stopper was removed before the vial contents were withdrawn. There was essentially no difference in latex allergen concentrations between the two drug preparation methods. None of the samples prepared with the standard method supported any microbial growth. One sample prepared with the latex-allergy precaution method grew bacteria. Removal of the dry rubber stopper from vials did not yield solutions with less latex allergen than solutions prepared according to conventional guidelines.

Sample registration software for process automation in the Neutron Activation Analysis (NAA) Facility in Malaysia nuclear agency

NASA Astrophysics Data System (ADS)

Rahman, Nur Aira Abd; Yussup, Nolida; Salim, Nazaratul Ashifa Bt. Abdullah; Ibrahim, Maslina Bt. Mohd; Mokhtar, Mukhlis B.; Soh@Shaari, Syirrazie Bin Che; Azman, Azraf B.; Ismail, Nadiah Binti

2015-04-01

Neutron Activation Analysis (NAA) had been established in Nuclear Malaysia since 1980s. Most of the procedures established were done manually including sample registration. The samples were recorded manually in a logbook and given ID number. Then all samples, standards, SRM and blank were recorded on the irradiation vial and several forms prior to irradiation. These manual procedures carried out by the NAA laboratory personnel were time consuming and not efficient. Sample registration software is developed as part of IAEA/CRP project on `Development of Process Automation in the Neutron Activation Analysis (NAA) Facility in Malaysia Nuclear Agency (RC17399)'. The objective of the project is to create a pc-based data entry software during sample preparation stage. This is an effective method to replace redundant manual data entries that needs to be completed by laboratory personnel. The software developed will automatically generate sample code for each sample in one batch, create printable registration forms for administration purpose, and store selected parameters that will be passed to sample analysis program. The software is developed by using National Instruments Labview 8.6.

Microbial safety and overall quality of cantaloupe fresh-cut pieces prepared from whole fruit after wet steam treatment.

PubMed

Ukuku, Dike O; Geveke, David J; Chau, Lee; Niemira, Brendan A

2016-08-16

Fresh-cut cantaloupes have been associated with outbreaks of Salmonellosis. Minimally processed fresh-cut fruits have a limited shelf life because of deterioration caused by spoilage microflora and physiological processes. The objectives of this study were to use a wet steam process to 1) reduce indigenous spoilage microflora and inoculated populations of Salmonella, Escherichia coli O157:H7 and Listeria monocytogenes on the surface of cantaloupes, and 2) reduce the populations counts in cantaloupe fresh-cut pieces after rind removal and cutting. The average inocula of Salmonella, E. coli O157:H7 and Listeria monocytogenes was 10(7)CFU/ml and the populations recovered on the cantaloupe rind surfaces after inoculation averaged 4.5, 4.8 and 4.1logCFU/cm(2), respectively. Whole cantaloupes were treated with a wet steam processing unit for 180s, and the treated melons were stored at 5°C for 29days. Bacterial populations in fresh-cut pieces prepared from treated and control samples stored at 5 and 10°C for up to 12days were determined and changes in color (CIE L*, a*, and b*) due to treatments were measured during storage. Presence and growth of aerobic mesophilic bacteria and Salmonella, E. coli O157:H7 and L. monocytogenes were determined in fresh-cut cantaloupe samples. There were no visual signs of physical damage on all treated cantaloupe surfaces immediately after treatments and during storage. All fresh-cut pieces from treated cantaloupes rind surfaces were negative for bacterial pathogens even after an enrichment process. Steam treatment significantly (p<0.05) changed the color of the fresh-cut pieces. Minimal wet steam treatment of cantaloupes rind surfaces designated for fresh-cut preparation will enhance the microbial safety of fresh-cut pieces, by reducing total bacterial populations. This process holds the potential to significantly reduce the incidence of foodborne illness associated with fresh-cut fruits. Published by Elsevier B.V.

Three-phase molecularly imprinted sol-gel based hollow fiber liquid-phase microextraction combined with liquid chromatography-tandem mass spectrometry for enrichment and selective determination of a tentative lung cancer biomarker.

PubMed

Moein, Mohammad Mahdi; Javanbakht, Mehran; Karimi, Mohammad; Akbari-Adergani, Behrouz; Abdel-Rehim, Mohamed

2015-07-15

In the present study, the modification of a polysulfone hollow fiber membrane with in situ molecularly imprinted sol-gel process (as a novel and one-step method) was prepared and investigated. 3-(propylmethacrylate)trimethoxysilane (3PMTMOS) as an inorganic precursor was used for preparation of molecularly imprinted sol-gel. The modified molecularly imprinted sol-gel hollow fiber membrane (MSHM) was used for the liquid-phase microextraction (LPME) of hippuric acid (HA) in human plasma and urine samples. MSHM as a selective, robust, and durable tool was used for at least 50 extractions without significant decrease in the extraction efficiency. The non-molecularly imprinted sol-gel hollow fiber membrane (NSHM) as blank hollow fiber membrane was prepared by the same process, only without HA. To achieve the best condition, influential parameters on the extraction efficiency were thoroughly investigated. The capability of this robust, green, and simple method for extraction of HA was successfully accomplished with LC/MS/MS. The limits of detection (LOD) and quantification (LOQ) in human plasma and urine samples were 0.3 and 1.0nmolL(-1), respectively. The standard calibration curves were obtained within the concentration range 1-2000nmolL(-1) for HA in human plasma and urine. The coefficients of determination (r(2)) were ≥0.998. The obtained data exhibited recoveries were higher than 89% for the extraction of HA in human plasma and urine samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Fast determination of diphenhydramine hydrochloride in reconstitutable syrups by CWT, PLS AND PCR methods.

PubMed

Devrim, Burcu; Dinç, Erdal; Bozkir, Asuman

2014-01-01

Diphenhydramine hydrochloride (DPH), a histamine H1-receptor antagonist, is widely used as antiallergic, antiemetic and antitussive drug found in many pharmaceutical preparations. In this study, a new reconstitutable syrup formulation of DPH was prepared because it is more stable in solid form than that in liquid form. The quantitative estimation of the DPH content of a reconstitutable syrup formulation in the presence of pharmaceutical excipients, D-sorbitol, sodium citrate, sodium benzoate and sodium EDTA is not possible by the direct absorbance measurement. Therefore, a signal processing approach based on continuous wavelet transform was used to determine the DPH in the reconstitutable syrup formulations and to eliminate the effect of excipients on the analysis. The absorption spectra of DPH in the range of 5.0-40.0 μg/mL were recorded between 200-300 nm. Various wavelet families were tested and Biorthogonal1.1 continuous wavelet transform (BIOR1.1-CWT) was found to be optimal signal processing family to get fast and desirable determination results and to overcome excipient interference effects. For a comparison of the experimental results obtained by partial least squares (PLS) and principal component regression (PCR) methods were applied to the quantitative prediction of DPH in the mentioned samples. The validity of the proposed BIOR1.1-CWT, PLS and PCR methods were achieved analyzing the prepared samples containing the mentioned excipients and using standard addition technique. It was observed that the proposed graphical and numerical approaches are suitable for the quantitative analysis of DPH in samples including excipients.

Metabolomic analysis using porcine skin: a pilot study of analytical techniques.

PubMed

Wu, Julie; Fiehn, Oliver; Armstrong, April W

2014-06-15

Metabolic byproducts serve as indicators of the chemical processes and can provide valuable information on pathogenesis by measuring the amplified output. Standardized techniques for metabolome extraction of skin samples serve as a critical foundation to this field but have not been developed. We sought to determine the optimal cell lysage techniques for skin sample preparation and to compare GC-TOF-MS and UHPLC-QTOF-MS for metabolomic analysis. Using porcine skin samples, we pulverized the skin via various combinations of mechanical techniques for cell lysage. After extraction, the samples were subjected to GC-TOF-MS and/or UHPLC-QTOF-MS. Signal intensities from GC-TOF-MS analysis showed that ultrasonication (2.7x107) was most effective for cell lysage when compared to mortar-and-pestle (2.6x107), ball mill followed by ultrasonication (1.6x107), mortar-and-pestle followed by ultrasonication (1.4x107), and homogenization (trial 1: 8.4x106; trial 2: 1.6x107). Due to the similar signal intensities, ultrasonication and mortar-and-pestle were applied to additional samples and subjected to GC-TOF-MS and UHPLC-QTOF-MS. Ultrasonication yielded greater signal intensities than mortar-and-pestle for 92% of detected metabolites following GC-TOF-MS and for 68% of detected metabolites following UHPLC-QTOF-MS. Overall, ultrasonication is the preferred method for efficient cell lysage of skin tissue for both metabolomic platforms. With standardized sample preparation, metabolomic analysis of skin can serve as a powerful tool in elucidating underlying biological processes in dermatological conditions.

High-throughput simultaneous analysis of RNA, protein, and lipid biomarkers in heterogeneous tissue samples.

PubMed

Reiser, Vladimír; Smith, Ryan C; Xue, Jiyan; Kurtz, Marc M; Liu, Rong; Legrand, Cheryl; He, Xuanmin; Yu, Xiang; Wong, Peggy; Hinchcliffe, John S; Tanen, Michael R; Lazar, Gloria; Zieba, Renata; Ichetovkin, Marina; Chen, Zhu; O'Neill, Edward A; Tanaka, Wesley K; Marton, Matthew J; Liao, Jason; Morris, Mark; Hailman, Eric; Tokiwa, George Y; Plump, Andrew S

2011-11-01

With expanding biomarker discovery efforts and increasing costs of drug development, it is critical to maximize the value of mass-limited clinical samples. The main limitation of available methods is the inability to isolate and analyze, from a single sample, molecules requiring incompatible extraction methods. Thus, we developed a novel semiautomated method for tissue processing and tissue milling and division (TMAD). We used a SilverHawk atherectomy catheter to collect atherosclerotic plaques from patients requiring peripheral atherectomy. Tissue preservation by flash freezing was compared with immersion in RNAlater®, and tissue grinding by traditional mortar and pestle was compared with TMAD. Comparators were protein, RNA, and lipid yield and quality. Reproducibility of analyte yield from aliquots of the same tissue sample processed by TMAD was also measured. The quantity and quality of biomarkers extracted from tissue prepared by TMAD was at least as good as that extracted from tissue stored and prepared by traditional means. TMAD enabled parallel analysis of gene expression (quantitative reverse-transcription PCR, microarray), protein composition (ELISA), and lipid content (biochemical assay) from as little as 20 mg of tissue. The mean correlation was r = 0.97 in molecular composition (RNA, protein, or lipid) between aliquots of individual samples generated by TMAD. We also demonstrated that it is feasible to use TMAD in a large-scale clinical study setting. The TMAD methodology described here enables semiautomated, high-throughput sampling of small amounts of heterogeneous tissue specimens by multiple analytical techniques with generally improved quality of recovered biomolecules.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Scheele, R.D.

In 1995, available subsegment samples of wastes taken from the Hanford Site underground radioactive waste storage tanks 241-C-112 (C-112) and 241-C-109 (C-109) were reanalyzed to determine the nickel concentrations in the samples and to determine whether the use of a nickel crucible in the analytical sample preparation biased the reported nickel concentrations reported by Simpson and coworkers and in the original report that this report supplements. The reanalysis strategy to determine nickel was to use a sodium peroxide flux in a zirconium crucible instead of the previously used potassium hydroxide flux in a nickel crucible. This supplemental report provides themore » results of the reanalyses and updates tables from the original report which reflect the new nickel analyses. Nickel is important with respect to management of the potentially reactive ferrocyanide wastes as it is one of the key defining characteristics of the solids that resulted from scavenging radiocesium using ferrocyanides. In Hanford Site wastes, few other processes introduced nickel into the wastes other than radiocobalt scavenging, which was often coupled with the ferrocyanide-scavenging process. Thus the presence of nickel in a waste provides strong evidence that the original waste was or contained ferrocyanide waste at one time. Given the potential import of nickel as a defining characteristic and marker for ferrocyanide wastes, the Pacific Northwest Laboratory`s (PNL) Analytical Chemistry Laboratory (ACL) reanalyzed available samples from tanks C-112 and C-109 using inductively coupled argon plasma/atomic emission spectrometry (ICP/AES) and an alternative sample preparation method which precluded contamination of the analytical samples with nickel.« less

Investigation of the influence of vanadium, iron and nickel dopants on the morphology, and crystal structure and photocatalytic properties of titanium dioxide based nanopowders.

PubMed

Shao, Godlisten N; Jeon, Sun-Jeong; Haider, M Salman; Abbass, Nadir; Kim, Hee Taik

2016-07-15

Photoactive V, Fe and Ni doped TiO2 (M-TiO2) nanopowders were synthesized by a modified two-step sol-gel process in the absence of additives. Titanium oxychloride, which is a rarely-used TiO2 precursor was used to yield M-TiO2 photocatalysts with preferential photochemical performance in the presence of natural solar irradiation. The obtained samples were calcined at different calcination temperatures ranging from 450 to 800°C to evaluate the influence of the sintering on the physicochemical properties. The properties of the obtained samples were examined by XRF, XRD, Raman spectroscopy, UV-visible DRS, XPS, nitrogen gas physisorption studies, SEM-EDAX and HRTEM analyses. Structural characterization of the samples revealed the incorporation of these transition metal element into TiO2. It was also depicted that the morphology, crystal structure, optical and photochemical properties of the obtained samples were largely dependent on the calcination temperature and the type of dopant used during the preparation process. The photochemical performance of the samples was investigated in the photodegradation of methylene blue in the presence of natural sunlight. The experimental results indicated that the VT600 sample possessed the highest activity due to its superior properties. This study provides a systematic preparation and selection of the precursor, dopant and calcination temperature that are suitable for the formation of TiO2-based heterogeneous photocatalysts with appealing morphology, crystal structure, optical and photochemical properties for myriad of applications. Copyright © 2016 Elsevier Inc. All rights reserved.

Comparing paraffined and deparaffinized breast cancer tissue samples and an analysis of Raman spectroscopy and infrared methods

NASA Astrophysics Data System (ADS)

Depciuch, J.; Kaznowska, E.; Szmuc, K.; Zawlik, I.; Cholewa, M.; Heraud, P.; Cebulski, J.

2016-05-01

Breast cancer makes up a quarter of all cancer in women, which is why research into new diagnostic methods and sample preparations need to be developed at an accelerated pace. Researchers are looking for diagnostic tools to detect when an individual has cancer cells and use that information to see what measurements and approaches can be used to take further diagnostic steps. The most common method of sample preparation is the imbibing of tumor tissue in paraffin, which can produce a background for spectroscopic measurements in the range of 500-3500 cm-1. In this study we demonstrated that proper preparation of paraffin-embedded specimens and the measurement methodology can eliminate paraffin vibration, as was done in the work Depciuch et al. 2015. Thanks to this spectroscopic technique there may become a reliable and accurate method of diagnosing breast cancer based on the evidence found from the prepared samples. The study compared the results obtained through Raman spectroscopy and FTIR (Fourier Transform Infrared) measurements of healthy and cancerous breast tissues that were either embedded in paraffin or deparaffinized. The resulting spectrum and accurate analysis led to the conclusion that the appropriate measurement of the background and the elimination of peaks from the paraffin had the greatest impact on the reliability of results. Furthermore, after the accurate, detailed studies FTIR and Raman spectroscopy on samples of breast tissue that were deparaffinized or embedded in paraffin, including a complete analysis of the peak after transformation Kramers-Kröning (KK), it was found that sample preparation did not affect the result obtained by measuring the reflectance in the mid-infrared range, and that this only had a minimal effect relating to the intensity obtained by the measurement of the Raman peak. Only in special cases, when Raman spectroscopic methods are used for research to find the peculiarities of the spectra, are deparaffinization recommended, in order to attain more detailed results that could be crucial in understanding the process of carcinogenesis.

Effect of resin infiltration on the thermal and mechanical properties of nano-sized silica-based thermal insulation.

PubMed

Lee, Jae Chun; Kim, Yun-Il; Lee, Dong-Hun; Kim, Won-Jun; Park, Sung; Lee, Dong Bok

2011-08-01

Several kinds of nano-sized silica-based thermal insulation were prepared by dry processing of mixtures consisting of fumed silica, ceramic fiber, and a SiC opacifier. Infiltration of phenolic resin solution into the insulation, followed by hot-pressing, was attempted to improve the mechanical strength of the insulation. More than 22% resin content was necessary to increase the strength of the insulation by a factor of two or more. The structural integrity of the resin-infiltrated samples could be maintained, even after resin burn-out, presumably due to reinforcement from ceramic fibers. For all temperature ranges and similar sample bulk density values, the thermal conductivities of the samples after resin burn-out were consistently higher than those of the samples obtained from the dry process. Mercury intrusion curves indicated that the median size of the nanopores formed by primary silica aggregates in the samples after resin burn-out is consistently larger than that of the sample without resin infiltration.

The annealing investigation on morphology and photoluminescence properties of In2O3 1-D nanostructures in resistive evaporation mechanism

NASA Astrophysics Data System (ADS)

Shariati, Mohsen; Ghafouri, Vahid

2014-02-01

Synthesis of In2O3 nanostructures grown on Si substrate by the resistive evaporation of metallic indium granules followed by dry oxidation process has been articulated. To prepare nucleation growth sites, selected samples pre-annealed around indium melting point in free-oxygen atmosphere and then to fabricate 1-D nanostructures, they annealed in a horizontal thermal furnace in presence of argon and oxygen. For comparison, one sample, the same origin as initially pre-annealed samples, was excluded in pre-annealing process but presented in annealing step. Characterization of the products with FESEM revealed that the pre-annealed obtained nanostructures are mostly nanorod and nanowire with different morphologies. For the comparative sample, no 1-D structures achieved. X-ray diffraction (XRD) patterns for pre-annealed samples indicated that they are crystalline and the comparative one is polycrystalline. Photoluminescence (PL) measurements carried out at room temperature revealed that emission band shifted to shorter wavelength from pre-annealed samples to comparative one.

Small RNA Library Preparation Method for Next-Generation Sequencing Using Chemical Modifications to Prevent Adapter Dimer Formation.

PubMed

Shore, Sabrina; Henderson, Jordana M; Lebedev, Alexandre; Salcedo, Michelle P; Zon, Gerald; McCaffrey, Anton P; Paul, Natasha; Hogrefe, Richard I

2016-01-01

For most sample types, the automation of RNA and DNA sample preparation workflows enables high throughput next-generation sequencing (NGS) library preparation. Greater adoption of small RNA (sRNA) sequencing has been hindered by high sample input requirements and inherent ligation side products formed during library preparation. These side products, known as adapter dimer, are very similar in size to the tagged library. Most sRNA library preparation strategies thus employ a gel purification step to isolate tagged library from adapter dimer contaminants. At very low sample inputs, adapter dimer side products dominate the reaction and limit the sensitivity of this technique. Here we address the need for improved specificity of sRNA library preparation workflows with a novel library preparation approach that uses modified adapters to suppress adapter dimer formation. This workflow allows for lower sample inputs and elimination of the gel purification step, which in turn allows for an automatable sRNA library preparation protocol.

Quantitative determination of allergenic 5-alk(en)ylresorcinols in mango (Mangifera indica L.) peel, pulp, and fruit products by high-performance liquid chromatography.

PubMed

Knödler, Matthias; Reisenhauer, Katharina; Schieber, Andreas; Carle, Reinhold

2009-05-13

Despite a number of serious case reports of mango dermatitis, no attempts at the identification and quantification of allergenic 5-alk(en)ylresorcinols in mango fruits have so far been made. Therefore, total alk(en)ylresorcinol content and relative homologue composition in 13 mango peel samples and 7 samples of mango pulp were determined by HPLC and LC-MS/MS analyses. Furthermore, mango puree and nectar prepared on pilot plant scale were also analyzed and compared with commercially available thermally preserved products. Depending on cultivar, alk(en)ylresorcinol contents ranged from 79.3 to 1850.5 mg/kg of dry matter (DM) in mango peels and from 4.9 to 187.3 mg/kg of DM in samples of mango pulp. The profile of alk(en)ylresorcinols was found to be highly characteristic, with an average homologue composition of C15:0 (6.1%), C15:1 (1.7%), C17:0 (1.1%), C17:1 (52.5%), C17:2 (33.4%), C17:3 (2.4%), C19:1 (2.1%), and C19:2 (0.8%). Mango puree samples prepared from peeled and unpeeled fruits revealed contents of 3.8 and 12.3 mg/kg of fresh weight, respectively. Content and homologue composition were not significantly affected during puree processing and thermal preservation. In nectar samples prepared from peeled and unpeeled fruits, contents of 1.4 and 4.6 mg/L, respectively, were found.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Souza, Douglas F., E-mail: souzadf@outlook.com; Nunes, Eduardo H.M., E-mail: eduardohmn@gmail.com; Pimenta, Daiana S.

In this work we fabricated alumina samples by the freeze-casting technique using tert-butanol as the solvent. The prepared materials were examined by scanning electron microscopy and X-ray microtomography. Next, they were coated with sol–gel silica films by dip-coating. Permeability tests were carried out in order to assess the permeation behavior of the materials processed in this study. We observed that the sintering time and alumina loading showed a remarkable effect on both the structural properties and flexural strength of the freeze-cast samples. Nitrogen adsorption tests revealed that the silica prepared in this study exhibited a microporous structure. It was observedmore » that the presence of silica coatings on the alumina surface decreased the CO{sub 2} permeance by about one order of magnitude. Because of the similar kinetic diameters of nitrogen and carbon dioxide, the CO{sub 2}/N{sub 2} system showed a separation efficiency that was lower than that observed for the He/CO{sub 2} and He/N{sub 2} systems. We noticed that increasing the feed pressure improved the separation capacity of the obtained materials. - Highlights: • Porous alumina samples obtained by the freeze-casting technique • Microporous silica coating prepared by a simple sol–gel dip-coating methodology • Samples examined by SEM, μ-CT, and nitrogen sorption tests • Mechanical tests were carried out in the freeze-cast samples. • The presence of silica coatings on the alumina surface decreased the CO{sub 2} permeance.« less

Methods for the preparation and analysis of solids and suspended solids for total mercury

USGS Publications Warehouse

Olund, Shane D.; DeWild, John F.; Olson, Mark L.; Tate, Michael T.

2004-01-01

The methods documented in this report are utilized by the Wisconsin District Mercury Lab for analysis of total mercury in solids (soils and sediments) and suspended solids (isolated on filters). Separate procedures are required for the different sample types. For solids, samples are prepared by room-temperature acid digestion and oxidation with aqua regia. The samples are brought up to volume with a 5 percent bromine monochloride solution to ensure complete oxidation and heated at 50?C in an oven overnight. Samples are then analyzed with an automated flow injection system incorporating a cold vapor atomic fluorescence spectrometer. A method detection limit of 0.3 ng of mercury per digestion bomb was established using multiple analyses of an environmental sample. Based on the range of masses processed, the minimum sample reporting limit varies from 0.6 ng/g to 6 ng/g. Suspended solids samples are oxidized with a 5 percent bromine monochloride solution and held at 50?C in an oven for 5 days. The samples are then analyzed with an automated flow injection system incorporating a cold vapor atomic fluorescence spectrometer. Using a certified reference material as a surrogate for an environmental sample, a method detection limit of 0.059 ng of mercury per filter was established. The minimum sample reporting limit varies from 0.059 ng/L to 1.18 ng/L, depending on the volume of water filtered.

Preview of the NASA NNWG NDE Sample Preparation Handbook

NASA Technical Reports Server (NTRS)

2010-01-01

This viewgraph presents a step-by-step how-to fabrication documentation of every kind of sample that is fabricated for MSFC by UA Huntsville, including photos and illustrations. The tabulation of what kind of samples are being fabricated for what NDE method, detailed instructions/documentation of the inclusion/creation of defects, detailed specifications for materials, processes, and equipment, case histories and/or experiences with the different fabrication methods and defect inclusion techniques, discussion of pitfalls and difficulties associated with sample fabrication and defect inclusion techniques, and a discussion of why certain fabrication techniques are needed as related to the specific NDE methods are included in this presentation.

Analysis of IAEA Environmental Samples for Plutonium and Uranium by ICP/MS in Support Of International Safeguards

DOE Office of Scientific and Technical Information (OSTI.GOV)

Farmer, Orville T.; Olsen, Khris B.; Thomas, May-Lin P.

2008-05-01

A method for the separation and determination of total and isotopic uranium and plutonium by ICP-MS was developed for IAEA samples on cellulose-based media. Preparation of the IAEA samples involved a series of redox chemistries and separations using TRU® resin (Eichrom). The sample introduction system, an APEX nebulizer (Elemental Scientific, Inc), provided enhanced nebulization for a several-fold increase in sensitivity and reduction in background. Application of mass bias (ALPHA) correction factors greatly improved the precision of the data. By combining the enhancements of chemical separation, instrumentation and data processing, detection levels for uranium and plutonium approached high attogram levels.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

This volume contains the interim change notice for sample preparation methods. Covered are: acid digestion for metals analysis, fusion of Hanford tank waste solids, water leach of sludges/soils/other solids, extraction procedure toxicity (simulate leach in landfill), sample preparation for gamma spectroscopy, acid digestion for radiochemical analysis, leach preparation of solids for free cyanide analysis, aqueous leach of solids for anion analysis, microwave digestion of glasses and slurries for ICP/MS, toxicity characteristic leaching extraction for inorganics, leach/dissolution of activated metal for radiochemical analysis, extraction of single-shell tank (SST) samples for semi-VOC analysis, preparation and cleanup of hydrocarbon- containing samples for VOCmore » and semi-VOC analysis, receiving of waste tank samples in onsite transfer cask, receipt and inspection of SST samples, receipt and extrusion of core samples at 325A shielded facility, cleaning and shipping of waste tank samplers, homogenization of solutions/slurries/sludges, and test sample preparation for bioassay quality control program.« less

Effects of Sample Preparation on the Infrared Reflectance Spectra of Powders

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brauer, Carolyn S.; Johnson, Timothy J.; Myers, Tanya L.

2015-05-22

While reflectance spectroscopy is a useful tool in identifying molecular compounds, laboratory measurement of solid (particularly powder) samples often is confounded by sample preparation methods. For example, both the packing density and surface roughness can have an effect on the quantitative reflectance spectra of powdered samples. Recent efforts in our group have focused on developing standard methods for measuring reflectance spectra that accounts for sample preparation, as well as other factors such as particle size and provenance. In this work, the effect of preparation method on sample reflectivity was investigated by measuring the directional-hemispherical spectra of samples that were hand-packedmore » as well as pressed into pellets using an integrating sphere attached to a Fourier transform infrared spectrometer. The results show that the methods used to prepare the sample have a substantial effect on the measured reflectance spectra, as do other factors such as particle size.« less

Effects of sample preparation on the infrared reflectance spectra of powders

NASA Astrophysics Data System (ADS)

Brauer, Carolyn S.; Johnson, Timothy J.; Myers, Tanya L.; Su, Yin-Fong; Blake, Thomas A.; Forland, Brenda M.

2015-05-01

While reflectance spectroscopy is a useful tool for identifying molecular compounds, laboratory measurement of solid (particularly powder) samples often is confounded by sample preparation methods. For example, both the packing density and surface roughness can have an effect on the quantitative reflectance spectra of powdered samples. Recent efforts in our group have focused on developing standard methods for measuring reflectance spectra that accounts for sample preparation, as well as other factors such as particle size and provenance. In this work, the effect of preparation method on sample reflectivity was investigated by measuring the directional-hemispherical spectra of samples that were hand-loaded as well as pressed into pellets using an integrating sphere attached to a Fourier transform infrared spectrometer. The results show that the methods used to prepare the sample can have a substantial effect on the measured reflectance spectra, as do other factors such as particle size.

Paint Analysis

NASA Technical Reports Server (NTRS)

1994-01-01

Lewis Research Center (LEW) has assisted The Cleveland Museum of Art (CMA) in analyzing the museum's paintings. Because of the many layers of paint that are often involved, this is a complex process. The cross-section of a paint chip must be scanned with a microscope to determine whether a paint layer is original or a restoration. The paint samples, however, are rarely flat enough for high magnification viewing and are frequently scratched. LEW devised an automated method that produces intact, flat, polished paint cross-sections. A sophisticated microprocessor-controlled grinding and polishing machine was manually employed in preparation of exotic samples for aerospace research was a readily adaptable technique. It produced perfectly flat samples with clearly defined layers. The process has been used successfully on a number of paintings, and LEW and CMA are considering additional applications.

The effect of different composition of ternary mixtures of emulsifying salts on the consistency of processed cheese spreads manufactured from Swiss-type cheese with different degrees of maturity.

PubMed

Salek, R N; Černíková, M; Maděrová, S; Lapčík, L; Buňka, F

2016-05-01

The scope of this work was to investigate the dependence of selected textural (texture profile analysis, TPA) and viscoelastic properties of processed cheese on the composition of ternary mixtures of emulsifying salts [disodium hydrogenphosphate, DSP; tetrasodium diphosphate, TSPP; sodium salt of polyphosphate (with mean length n ≈ 20), P20; and trisodium citrate, TSC] during a 60-d storage period (6±2°C). The processed cheese samples [40% wt/wt dry matter (DM) content, 50% wt/wt fat in DM content] were manufactured using Swiss-type cheese (as the main raw material) with 4 different maturity degrees (4, 8, 12, and 16 wk of ripening). Moreover, the pH of the samples was adjusted (the target values within the range of 5.60-5.80), corresponding to the standard pH values of spreadable processed cheese. With respect to the individual application of emulsifying salts (regardless of the maturity degree of the Swiss-type cheese applied), the samples prepared with P20 were the hardest, followed by those prepared with TSPP, TSC, and DSP. Furthermore, a specific ratio of DSP:TSPP (1:1) led to a significant increase in the hardness of the samples. On the whole, the hardness of all processed cheese samples increased with the prolonging storage period, whereas their hardness significantly dropped with the rising ripening stage of the raw material utilized. In all of the cases, the trends of hardness development remained analogous, and only the absolute values differed significantly. Moreover, the findings of TPA were in accordance with those of the rheological analysis. In particular, the specific ratio of DSP:TSPP (1:1) resulted in the highest gel strength and interaction factor values, followed by P20, TSPP, TSC, and DSP (used individually), reporting the same trend which was demonstrated by TPA. The monitored values of the gel strength and interaction factor decreased with the increasing maturity degree of the Swiss-type cheese used. The intensity of the rigidity of the samples showed an analogous relationship to the intensity of the gel strength; the higher the gel strength of the sample, the more inflexible the product is expected to be. Copyright © 2016 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Phase Segregation and Superior Thermoelectric Properties of Mg2Si(1-x)Sb(x) (0 ≤ x ≤ 0.025) Prepared by Ultrafast Self-Propagating High-Temperature Synthesis.

PubMed

Zhang, Qiang; Su, Xianli; Yan, Yonggao; Xie, Hongyao; Liang, Tao; You, Yonghui; Tang, Xinfeng; Uher, Ctirad

2016-02-10

A series of Sb-doped Mg2Si(1-x)Sb(x) compounds with the Sb content x within 0 ≤ x ≤ 0.025 were prepared by self-propagating high-temperature synthesis (SHS) combined with plasma activated sintering (PAS) method in less than 20 min. Thermodynamic parameters of the SHS process, such as adiabatic temperature, ignition temperature, combustion temperature, and propagation speed of the combustion wave, were determined for the first time. Nanoprecipitates were observed for the samples doped with Sb. Thermoelectric properties were characterized in the temperature range of 300-875 K. With the increasing content of Sb, the electrical conductivity σ rises markedly while the Seebeck coefficient α decreases, which is attributed to the increase in carrier concentration. The carrier mobility μ(H) decreases slightly with the increasing carrier concentration but remains larger than the Sb-doped samples prepared by other methods, which is ascribed to the self-purification process associated with the SHS synthesis. In spite of the increasing electrical conductivity with the increasing Sb content x, the overall thermal conductivity κ decreases on account of a significantly falled lattice thermal conductivity κ(L) due to the strong point defect scattering on Sb impurities and possibly enhanced interface scattering on nanoprecipitates. As a result, the sample with x = 0.02 achieves the thermoelectric figure of merit ZT ∼ 0.65 at 873 K, one of the highest values for the Sb-doped binary Mg2Si compounds investigated so far. A subsequent annealing treatment on the sample with x = 0.02 at 773 K for 7 days has resulted in no noticeble changes in the thermoelectric transport properties, indicating an excellent thermal stability of the compounds prepared by the SHS method. Therefore, SHS method can serve as an effective alternative fabrication route to synthesize Mg-Si based themoelectrics and some other functional materials due to the resulting high performance, perfect thermal stability, and feasible production in large scale for commercial application.

Online reverse phase-high-performance liquid chromatography-fluorescence detection-electrospray ionization-mass spectrometry separation and characterization of heparan sulfate, heparin, and low-molecular weight-heparin disaccharides derivatized with 2-aminoacridone.

PubMed

Galeotti, Fabio; Volpi, Nicola

2011-09-01

A high-resolution online reverse-phase-high-performance liquid chromatography (RP-HPLC)-fluorescence detector (Fd)-electrospray ionization-mass spectrometry (ESI-MS) separation and structural characterization of disaccharides prepared from heparin (Hep), heparan sulfate (HS), and various low-molecular-weight (LMW)-Hep using heparin lyases and derivatization with 2-aminoacridone (AMAC) are described. A total of 12 commercially available Hep/HS-derived unsaturated disaccharides were separated and unambiguously identified on the basis of their retention times and mass spectra. The constituent disaccharides of various samples, including unfractionated Hep/HS, fast-moving and slow-moving Hep components, and several marketed products, were characterized. Furthermore, for the first time, the saturated trisulfated disaccharide belonging to the nonreducing end of Heps was detected as being approximately 2% in unfractionated samples and ~15-21% in LMW-Heps prepared by nitrous acid depolymerization. No desalting of the commercial products prior to enzymatic digestion or prepurification steps to eliminate any excess of AMAC reagent or interference from proteins, peptides, and other sample impurities before RP-HPLC-Fd-ESI-MS injection were necessary. This method has applicability for the rapid differentiation of pharmaceutical Heps and LMW-Heps prepared by means of different depolymerization processes and for compositional analysis of small amounts of samples derived from biological sources by using the highly sensitive fluorescence detector.

An automated multidimensional preparative gas chromatographic system for isolation and enrichment of trace amounts of xenon from ambient air.

PubMed

Larson, Tuula; Östman, Conny; Colmsjö, Anders

2011-04-01

The monitoring of radioactive xenon isotopes is one of the principal methods for the detection of nuclear explosions in order to identify clandestine nuclear testing. In this work, a miniaturized, multiple-oven, six-column, preparative gas chromatograph was constructed in order to isolate trace quantities of radioactive xenon isotopes from ambient air, utilizing nitrogen as the carrier gas. The multidimensional chromatograph comprised preparative stainless steel columns packed with molecular sieves, activated carbon, and synthetic carbon adsorbents (e.g., Anasorb®-747 and Carbosphere®). A combination of purification techniques--ambient adsorption, thermal desorption, back-flushing, thermal focusing, and heart cutting--was selectively optimized to produce a well-defined xenon peak that facilitated reproducible heart cutting and accurate quantification. The chromatographic purification of a sample requires approximately 4 h and provides complete separation of xenon from potentially interfering components (such as water vapor, methane, carbon dioxide, and radon) with recovery and accuracy close to 100%. The preparative enrichment process isolates and concentrates a highly purified xenon gas fraction that is suitable for subsequent ultra-low-level γ-, ß/γ-spectroscopic or high-resolution mass spectrometric measurement (e.g., to monitor the gaseous fission products of nuclear explosions at remote locations). The Xenon Processing Unit is a free-standing, relatively lightweight, and transportable system that can be interfaced to a variety of sampling and detection systems. It has a relatively inexpensive, rugged, and compact modular (19-inch rack) design that provides easy access to all parts for maintenance and has a low power requirement.

Assessment of household preparedness through training exercises--two metropolitan counties, Tennessee, 2011.

PubMed

2012-09-14

Public health emergency preparedness involves improving both workforce and household capacity to manage disasters. To improve preparedness at both levels, the Tennessee Department of Health (TDH) formed a Rapid Assessment of Populations Impacted by Disasters (RAPID) team. In 2011, the team used Community Assessment for Public Health Emergency Response (CASPER) two-stage cluster sampling methodology to measure household preparedness for disasters or emergencies in two metropolitan counties. In the two counties, 23% and 31% of households reported being "well-prepared" to handle disasters or emergencies, 43% and 44% reported being "somewhat prepared," and 25% and 20% reported being "not at all prepared." As a result of this experience, RAPID teams were able to improve their methods, streamline processes, and create a better community assessment toolkit. To increase preparedness at both the community and workforce levels, public health departments should assess community preparedness to inform the planning process and provide field training and exercise opportunities for public health workers.

Preparation of Pd supported on La(Sr)-Mn-O Perovskite by microwave Irradiation Method and Its Catalytic Performances for the Methane Combustion

PubMed Central

Wang, Wei; Yuan, Fulong; Niu, Xiaoyu; Zhu, Yujun

2016-01-01

In this work, a series of palladium supported on the La0.8Sr0.2MnO3.15 perovskite catalysts (Pd/LSM-x) with different Pd loading were prepared by microwave irradiation processing plus incipient wetness impregnation method and characterized by XRD, TEM, H2-TPR and XPS. These catalysts were evaluated on the lean CH4 combustion. The results show that the Pd/LSM-x samples prepared by microwave irradiation processing possess relative higher surface areas than LSM catalyst. The addition of Pd to the LSM leads to the increase in the oxygen vacancy content and the enhancement in the mobility of lattice oxygen which play an important role on the methane combustion. The Pd/LSM-3 catalysts with 4.2wt% Pd loading exhibited the best performance for CH4 combustion that temperature for 10% and 90% of CH4 conversion is 315 and 520 °C. PMID:26781628

A Surface Plasmon Resonance-Based Optical Fiber Probe Fabricated with Electropolymerized Molecular Imprinting Film for Melamine Detection

PubMed Central

Zheng, Yongping; Zhang, Tingwei; Wu, Songjie; Zhang, Jue; Fang, Jing

2018-01-01

Molecularly imprinted polymer (MIP) films prepared by bulk polymerization suffer from numerous deficiencies, including poor mass transfer ability and difficulty in controlling reaction rate and film thickness, which usually result in poor repeatability. However, polymer film synthesized by electropolymerization methods benefit from high reproducibility, simplicity and rapidity of preparation. In the present study, an Au film served as the refractive index-sensitive metal film to couple with the light leaked out from optical fiber core and the electrode for electropolymerizing MIP film simultaneously. The manufactured probe exhibited satisfactory sensitivity and specificity. Furthermore, the surface morphology and functional groups of the synthesized MIP film were characterized by Atomic Force Microscopy (AFM) and Fourier transform infrared microspectroscopy (FTIR) for further insights into the adsorption and desorption processes. Given the low cost, label-free test, simple preparation process and fast response, this method has a potential application to monitor substances in complicated real samples for out-of-lab test in the future. PMID:29522472

Central composite design with the help of multivariate curve resolution in loadability optimization of RP-HPLC to scale-up a binary mixture.

PubMed

Taheri, Mohammadreza; Moazeni-Pourasil, Roudabeh Sadat; Sheikh-Olia-Lavasani, Majid; Karami, Ahmad; Ghassempour, Alireza

2016-03-01

Chromatographic method development for preparative targets is a time-consuming and subjective process. This can be particularly problematic because of the use of valuable samples for isolation and the large consumption of solvents in preparative scale. These processes could be improved by using statistical computations to save time, solvent and experimental efforts. Thus, contributed by ESI-MS, after applying DryLab software to gain an overview of the most effective parameters in separation of synthesized celecoxib and its co-eluted compounds, design of experiment software that relies on multivariate modeling as a chemometric approach was used to predict the optimized touching-band overloading conditions by objective functions according to the relationship between selectivity and stationary phase properties. The loadability of the method was investigated on the analytical and semi-preparative scales, and the performance of this chemometric approach was approved by peak shapes beside recovery and purity of products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A novel approach to TEM preparation with a (7-axis stage) triple-beam FIB-SEM system

NASA Astrophysics Data System (ADS)

Clarke, Jamil J.

2015-10-01

Preparation of lamellae from bulk to grid for Cs-corrected Transmission Electron Microscope (TEM) observation has mostly become routine work on the latest FIB-SEM systems, with standardized techniques that often are left to automation for the initial steps. The finalization of lamellae however, has mostly become, non-routine, non-repeatable and often driven by user experience level in most cases to produce high quality damage-less cross section. Materials processing of the latest technologies, with ever-shrinking Nano-sized structures pose challenges to modern FIB-SEM systems. This can often lead to specialized techniques and hyper-specific functions for producing ultra-thin high quality lamellae that often are lab specific, preventing practical use of such techniques across multiple materials and applications. Several factors that should be incorporated in processing fine structured materials successfully include how the use of electron and ion scan conditions can affect a thin section during ion milling, the type of ion species applied for material processing during the finalization of lamellae with gallium ions or of a smaller ion species type such as Ar/Xe, sample orientation of the lamella during the thinning process which is linked to ion beam incident angle as a direct relationship in the creation of waterfall effects or curtain effects, and how software can be employed to aid in the reduction of these artifacts with reproducible results regardless of FIB-SEM experience for site-specific lift outs. A traditional TEM preparation was performed of a fine structure specimen in pursuit of a process technique to produce a high quality TEM lamella which would address all of the factors mentioned. These new capabilities have been refined and improved upon during the FIB-SEM design and development stages with an end result of a new approach that yields an improvement in quality by the reduction of common ion milling artifacts such as curtain effects, amorphous material, and better pin pointing of the area of interest while reducing overall processing time for the TEM sample preparation process and enhancing repeatability through ease of use via software controls. The development of these new technologies, incorporating a third Ar/Xe ion beam column in conjunction with the electron and gallium ion beam column, a 7-axis stage for enhanced sample orientation with tilt functions in two axes and automated swing control along with a host of additional functions which address the factors aforementioned such as electron and ion scan techniques and curtain effect removal by the use of hardware and software components that are key to reduce typical FIB related artifacts, all of which are called "ACE [Anti Curtaining Effect] Technologies" are explained. The overall developments of these technologies are to address a significant point that productivity, throughput and repeatability are comprised by synergy between the user, application, software and hardware within a FIB-SEM system. The latest Hitachi FIB-SEM platform offers these innovations for reliability, repeatability and high quality lamella preparation for Cs-corrected (S)TEMs.

Potential artifacts associated with historical preparation of joint compound samples and reported airborne asbestos concentrations.

PubMed

Brorby, G P; Sheehan, P J; Berman, D W; Bogen, K T; Holm, S E

2011-05-01

Airborne samples collected in the 1970s for drywall workers using asbestos-containing joint compounds were likely prepared and analyzed according to National Institute of Occupational Safety and Health Method P&CAM 239, the historical precursor to current Method 7400. Experimentation with a re-created, chrysotile-containing, carbonate-based joint compound suggested that analysis following sample preparation by the historical vs. current method produces different fiber counts, likely because of an interaction between the different clearing and mounting chemicals used and the carbonate-based joint compound matrix. Differences were also observed during analysis using Method 7402, depending on whether acetic acid/dimethylformamide or acetone was used during preparation to collapse the filter. Specifically, air samples of sanded chrysotile-containing joint compound prepared by the historical method yielded fiber counts significantly greater (average of 1.7-fold, 95% confidence interval: 1.5- to 2.0-fold) than those obtained by the current method. In addition, air samples prepared by Method 7402 using acetic acid/dimethylformamide yielded fiber counts that were greater (2.8-fold, 95% confidence interval: 2.5- to 3.2-fold) than those prepared by this method using acetone. These results indicated (1) there is an interaction between Method P&CAM 239 preparation chemicals and the carbonate-based joint compound matrix that reveals fibers that were previously bound in the matrix, and (2) the same appeared to be true for Method 7402 preparation chemicals acetic acid/dimethylformamide. This difference in fiber counts is the opposite of what has been reported historically for samples of relatively pure chrysotile dusts prepared using the same chemicals. This preparation artifact should be considered when interpreting historical air samples for drywall workers prepared by Method P&CAM 239. Copyright © 2011 JOEH, LLC

Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging

NASA Astrophysics Data System (ADS)

Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

2017-08-01

Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed.

Results Of Hg Speciation Testing On DWPF SMECT-1, SMECT-3, And SMECT-5 Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C.

2016-01-07

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team. The thirteenth shipment of samples was designated to include Defense Waste Processing Facility (DWPF) Slurry Mix Evaporator Condensate Tank (SMECT) from Sludge Receipt and Adjustment Tank (SRAT) Batch 736 and 738 samples. Triplicate samples of each material were prepared for this shipment. Each replicate was analyzed for seven Hg species: total Hg, total soluble (dissolved) Hg, elemental Hg [Hg(0)], ionic (inorganic) Hg [Hg(I) andmore » Hg(II)], methyl Hg [CH 3Hg-X, where X is a counter anion], ethyl Hg [CH 3CH 2-Hg-X, where X is a counter anion], and dimethyl Hg [(CH 3) 2Hg]. The difference between the total Hg and total soluble Hg measurements gives the particulate Hg concentration, i.e. Hg adsorbed to the surface of particulate matter in the sample but without resolution of the specific adsorbed species. The average concentrations of Hg species in the aqueous samples derived from Eurofins reported data corrected for dilutions performed by SRNL are tabulated.« less

Al2O3-TiC Composite Prepared by Spark Plasma Sintering Process: Evaluation of Mechanical and Tribological Properties

NASA Astrophysics Data System (ADS)

Kumar, Rohit; Chaubey, A. K.; Bathula, Sivaiah; Prashanth, K. G.; Dhar, Ajay

2018-03-01

Al2O3-10TiC composites were synthesized by spark plasma sintering (SPS) process. Microstructural and mechanical properties of the composite reveal homogeneous distribution of the fine TiC particles in the matrix. The samples were produced with different sintering temperature, and it shows that the hardness and density gradually increases with increasing sintering temperature. Abrasion wear test result reveals that the composite sintered at 1500 °C shows high abrasion resistance (wt. loss 0.016 g) and the lowest abrasion resistance was observed for the composite sample sintered at 1100 °C (wt. loss 1.459 g). The profilometry surface roughness study shows that sample sintered at 1100 °C shows maximum roughness ( R a = 6.53 µm) compared to the sample sintered at 1500 °C ( R a = 0.66 µm) corroborating the abrasion wear test results.

Biocompatibility of metal injection molded versus wrought ASTM F562 (MP35N) and ASTM F1537 (CCM) cobalt alloys.

PubMed

Chen, Hao; Sago, Alan; West, Shari; Farina, Jeff; Eckert, John; Broadley, Mark

2011-01-01

We present a comparative analysis between biocompatibility test results of wrought and Metal Injection Molded (MIM) ASTM F562-02 UNS R30035 (MP35N) and F1537 UNS R31538 (CCM) alloy samples that have undergone the same generic orthopedic implant's mechanical, chemical surface pre-treatment, and a designed pre-testing sample preparation method. Because the biocompatibility properties resulting from this new MIM cobalt alloy process are not well understood, we conducted tests to evaluate cytotoxicity (in vitro), hemolysis (in vitro), toxicity effects (in vivo), tissue irritation level (in vivo), and pyrogenicity count (in vitro) on such samples. We show that our developed MIM MP35N and CCM materials and treatment processes are biocompatible, and that both the MIM and wrought samples, although somewhat different in microstructure and surface, do not show significant differences in biocompatibility.

Research on laser-induced damage resistance of fused silica optics by the fluid jet polishing method.

PubMed

Lv, Liang; Ma, Ping; Huang, Jinyong; He, Xiang; Cai, Chao; Zhu, Heng

2016-03-20

Laser-induced damage threshold (LIDT) is one important evaluation index for optical glasses applied in large laser instruments which are exposed to high light irradiation flux. As a new kind of precise polishing technology, fluid jet polishing (FJP) has been widely used in generating planar, spherical, and aspherical optics with high-accuracy surfaces. Laser damage resistances of fused silica optics by the FJP process are studied in this paper. Fused silica samples with various FJP parameters are prepared, and laser damage experiments are performed with 351 nm wavelength and a 5.5 ns pulse width laser. Experimental results demonstrate that the LIDT of the samples treated with FJP processes did not increase, compared to their original state. The surface quality of the samples is one factor for the decrease of LIDT. For ceria solution polished samples, the cerium element remaining is another factor of the lower LIDT.

Can an inadequate cervical cytology sample in ThinPrep be converted to a satisfactory sample by processing it with a SurePath preparation?

PubMed

Sørbye, Sveinung Wergeland; Pedersen, Mette Kristin; Ekeberg, Bente; Williams, Merete E Johansen; Sauer, Torill; Chen, Ying

2017-01-01

The Norwegian Cervical Cancer Screening Program recommends screening every 3 years for women between 25 and 69 years of age. There is a large difference in the percentage of unsatisfactory samples between laboratories that use different brands of liquid-based cytology. We wished to examine if inadequate ThinPrep samples could be satisfactory by processing them with the SurePath protocol. A total of 187 inadequate ThinPrep specimens from the Department of Clinical Pathology at University Hospital of North Norway were sent to Akershus University Hospital for conversion to SurePath medium. Ninety-one (48.7%) were processed through the automated "gynecologic" application for cervix cytology samples, and 96 (51.3%) were processed with the "nongynecological" automatic program. Out of 187 samples that had been unsatisfactory by ThinPrep, 93 (49.7%) were satisfactory after being converted to SurePath. The rate of satisfactory cytology was 36.6% and 62.5% for samples run through the "gynecology" program and "nongynecology" program, respectively. Of the 93 samples that became satisfactory after conversion from ThinPrep to SurePath, 80 (86.0%) were screened as normal while 13 samples (14.0%) were given an abnormal diagnosis, which included 5 atypical squamous cells of undetermined significance, 5 low-grade squamous intraepithelial lesion, 2 atypical glandular cells not otherwise specified, and 1 atypical squamous cells cannot exclude high-grade squamous intraepithelial lesion. A total of 2.1% (4/187) of the women got a diagnosis of cervical intraepithelial neoplasia 2 or higher at a later follow-up. Converting cytology samples from ThinPrep to SurePath processing can reduce the number of unsatisfactory samples. The samples should be run through the "nongynecology" program to ensure an adequate number of cells.

MARS: bringing the automation of small-molecule bioanalytical sample preparations to a new frontier.

PubMed

Li, Ming; Chou, Judy; Jing, Jing; Xu, Hui; Costa, Aldo; Caputo, Robin; Mikkilineni, Rajesh; Flannelly-King, Shane; Rohde, Ellen; Gan, Lawrence; Klunk, Lewis; Yang, Liyu

2012-06-01

In recent years, there has been a growing interest in automating small-molecule bioanalytical sample preparations specifically using the Hamilton MicroLab(®) STAR liquid-handling platform. In the most extensive work reported thus far, multiple small-molecule sample preparation assay types (protein precipitation extraction, SPE and liquid-liquid extraction) have been integrated into a suite that is composed of graphical user interfaces and Hamilton scripts. Using that suite, bioanalytical scientists have been able to automate various sample preparation methods to a great extent. However, there are still areas that could benefit from further automation, specifically, the full integration of analytical standard and QC sample preparation with study sample extraction in one continuous run, real-time 2D barcode scanning on the Hamilton deck and direct Laboratory Information Management System database connectivity. We developed a new small-molecule sample-preparation automation system that improves in all of the aforementioned areas. The improved system presented herein further streamlines the bioanalytical workflow, simplifies batch run design, reduces analyst intervention and eliminates sample-handling error.

A Sample WebQuest Applicable in Teaching Topological Concepts

ERIC Educational Resources Information Center

Yildiz, Sevda Goktepe; Korpeoglu, Seda Goktepe

2016-01-01

In recent years, WebQuests have received a great deal of attention and have been used effectively in teaching-learning process in various courses. In this study, a WebQuest that can be applicable in teaching topological concepts for undergraduate level students was prepared. A number of topological concepts, such as countability, infinity, and…

Solvent Extraction of Copper: An Extractive Metallurgy Exercise for Undergraduate Teaching Laboratories

ERIC Educational Resources Information Center

Smellie, Iain A.; Forgan, Ross S.; Brodie, Claire; Gavine, Jack S.; Harris, Leanne; Houston, Daniel; Hoyland, Andrew D.; McCaughan, Rory P.; Miller, Andrew J.; Wilson, Liam; Woodhall, Fiona M.

2016-01-01

A multidisciplinary experiment for advanced undergraduate students has been developed in the context of extractive metallurgy. The experiment serves as a model of an important modern industrial process that combines aspects of organic/inorganic synthesis and analysis. Students are tasked to prepare a salicylaldoxime ligand and samples of the…

Effect of sample preparation on the discrimination of bacterial isolates cultured in liquid nutrient media using laser induced breakdown spectroscopy

USDA-ARS?s Scientific Manuscript database

Laser induced breakdown spectroscopy (LIBS) is used as the basis for discrimination between 2 genera of gram-negative bacteria and 2 genera of gram-positive bacteria representing pathogenic threats commonly found in poultry processing rinse waters. Because LIBS-based discrimination relies primarily ...

Strategic development of a multivariate calibration model for the uniformity testing of tablets by transmission NIR analysis.

PubMed

Sasakura, D; Nakayama, K; Sakamoto, T; Chikuma, T

2015-05-01

The use of transmission near infrared spectroscopy (TNIRS) is of particular interest in the pharmaceutical industry. This is because TNIRS does not require sample preparation and can analyze several tens of tablet samples in an hour. It has the capability to measure all relevant information from a tablet, while still on the production line. However, TNIRS has a narrow spectrum range and overtone vibrations often overlap. To perform content uniformity testing in tablets by TNIRS, various properties in the tableting process need to be analyzed by a multivariate prediction model, such as a Partial Least Square Regression modeling. One issue is that typical approaches require several hundred reference samples to act as the basis of the method rather than a strategically designed method. This means that many batches are needed to prepare the reference samples; this requires time and is not cost effective. Our group investigated the concentration dependence of the calibration model with a strategic design. Consequently, we developed a more effective approach to the TNIRS calibration model than the existing methodology.

Electrical transport property, thermal stability and oxidation resistance of single crystalline β-Zn4Sb3 prepared using the Bi-Sn mixed-flux method

NASA Astrophysics Data System (ADS)

Deng, Shuping; Li, Decong; Chen, Zhong; Tang, Yu; Shen, Lanxian; Deng, Shukang

2017-12-01

Single crystal samples β-Zn4Sb3 have been prepared by using Bi-Sn mixed-flux method. The obtained crystals exhibit p-type conduction behavior with carrier concentration varying from 4.40 × 1019 to 18.12 × 1019 cm-3 as carrier mobility changes from 25.8 to 61.5 cm2 V-1 s-1 at room temperature. Electrical transport properties of the samples were optimized by Bi-Sn co-doped, which brought by Bi-Sn mixed-flux. And the maximal power factor of 1.45 × 10-3 W m-1 K-2 is achieved at 510 K for the sample with Bi flux content x = 0.5. Consequently, the oxidation resistance of the sample was determined by exploring the effects of heat treatment in air on electrical transport properties and thermal stability, which the single crystalline β-Zn4Sb3 still possess an excellent oxidation resistance and thermal stability after the heat treatment process.

Quantum Dots obtained by LPE from under-saturated In-As liquid phases on GaAs substrates

NASA Astrophysics Data System (ADS)

Ortiz, F. E.; Mishurnyi, V.; Gorbatchev, A.; De Anda, F.; Prutskij, T.

2011-01-01

In this work we inform about quantum dots (QD) obtained by Liquid Phase Epitaxy (LPE) on GaAs substrates from under-saturated In-As liquid phases. In our processes, we have prepared saturated In-rich liquid phases by dissolving an InAs wafer at one of the temperatures interval from 450 to 414 C for 60 minutes. The contact between In-As liquid phase and the GaAs substrate was always done at a constant temperature of 444 C for 5 seconds. Thus, the growth temperature for most of the samples was higher than the liquidus temperature. We think that the growth driving force is related to a transient process that occurs when the system is trying to reach equilibrium. Under the atom force microscope (AFM) we have observed nano-islands on the surfaces of the samples obtained from under-saturated liquid phases prepared at 438, 432 and 426 C. The 25 K photoluminescence spectrum shows a peak at a 1.33 eV, in addition to the GaAs related line.

Investigation of Physically and Chemically Ionic Liquid Confinement in Nanoporous Materials by a Combination of SANS, Contrast-Matching SANS, XRD and Nitrogen Adsorption

NASA Astrophysics Data System (ADS)

Romanos, G. E.; Stefanopoulos, K. L.; Vangeli, O. C.; Mergia, K.; Beltsios, K. G.; Kanellopoulos, N. K.; Lairez, D.

2012-02-01

In the present study, [bmim][PF6] ionic liquid (IL) was introduced into the pores of two ordered mesoporous silicas (MCM-41 and SBA-15) having different pore sizes by means of two different processes: a) with physical imbibition from a methanol solution under high vacuum and b) by chemically immobilising the IL with silanisation of the pore surface followed by reaction with butyl-methyl imidazolium chloride and anion exchange with PF6, the process termed as the "grafting to" method. Both the extent of IL entrapment and the structural properties of the IL phase under confinement were investigated by SANS, contrast-matching SANS, XRD and nitrogen adsorption measurements. The results show that the pores of chemically prepared samples are not totally filled by IL and also suggest for ordering of the silylated IL phase. On the other hand, the physically prepared samples are almost or totally filled with IL whereas no evidence for ordering of the confined IL phase was observed.

Synthesis of surface molecular imprinted polymers based on carboxyl-modified silica nanoparticles with the selective detection of dibutyl phthalate from tap water samples

NASA Astrophysics Data System (ADS)

Xu, Wanzhen; Zhang, Xiaoming; Huang, Weihong; Luan, Yu; Yang, Yanfei; Zhu, Maiyong; Yang, Wenming

2017-12-01

In this work, the molecular imprinted polymers were synthesized with the low monomer concentrations for dibutyl phthalate (DBP). The polymers were prepared over carboxyl-modified silica nanoparticle, which used methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linker agent and azoisobutyronitrile as the initiator in the process of preparation. Various measures were used to characterize the structure and morphology in order to get the optimal polymer. The characterization results show that the optimal polymer has suitable features for further adsorption process. And adsorption capacity experiments were evaluated to analyze its adsorption performance, through adsorption isotherms/kinetics, selectivity adsorption and desorption and regeneration experiments. These results showed that the molecular imprinted polymers had a short equilibrium time about 60 min and high stability with 88% after six cycles. Furthermore, the molecular imprinted polymers were successfully applied to remove dibutyl phthalate. The concentration range was 5.0-30.0 μmol L-1, and the limit of detection was 0.06 μmol L-1 in tap water samples.

Coal technology program progress report, February 1976

DOE Office of Scientific and Technical Information (OSTI.GOV)

None

Final testing of the 20-atm bench-scale system is underway in preparation for experiments with hydrogen. Laboratory-scale testing of a number of inexpensive pure compounds to improve the settling rate of solids in Solvent Refined Coal (SRC) unfiltered oil (UFO), bench-scale testing of the effect of the Tretolite additive on settling, and characterization tests on a new sample of UFO from the PAMCO-SRC process are reported. Experimental engineering support of an in situ gasification process include low-temperature pyrolyses at exceptionally low heating rates (0.3/sup 0/C/min). Highly pyrophoric chars were consistently produced. Aqueous by-products from coal conversion technologies and oil shale retortingmore » have been analyzed directly to determine major organic components. A report is being prepared discussing various aspects of the engineering evaluations of nuclear process heat for coal. A bench-scale test program on thermochemical water splitting for hydrogen production is under consideration. In the coal-fueled MIUS program, preparations for procurement of tubing for the matrix in the fluidized-bed furnace and for fabrication of the furnace continued. Analyses of the AiResearch gas turbine and recuperator under coal-fueled MIUS operating conditions are near completion. Process flow diagrams and heat and material balances were completed for most of the units in the synthoil process. Overall utilities requirements were calculated and the coal preparation flowsheets were finalized. For hydrocarbonization, the flowsheet was revised to include additional coal data. Flowsheets were finalized for the acid gas separation and recycle, and the oil-solids separation. (LTN)« less

Stability of Drugs of Abuse in Urine Samples at Room Temperature by Use of a Salts Mixture.

PubMed

Pellegrini, Manuela; Graziano, Silvia; Mastrobattista, Luisa; Minutillo, Adele; Busardo, Francesco Paolo; Scarsella, Gianfranco

2017-01-01

It has long been recognized that ensuring analyte stability is of crucial importance in the use of any quantitative bioanalytical method. As analyses are usually not performed directly after collection of the biological samples, but after these have been processed and stored, it is essential that analyte stability can be maintained at storage conditions to ensure that the obtained concentration results adequately reflect those directly after sampling. The conservation of urine samples in refrigerated/ frozen conditions is strongly recommended; but not always feasible. The aim of this study was to assess the stability of some well-known drugs of abuse methamphetamine (MA), 11-nor-9-carboxy-Δ9- tetrahydrocannabinol (THC-COOH), benzoylecgonine (BE), and morphine (MOR) in urine samples kept at room temperature by adding a salt mixture (sodium citrate, sodium ascorbate, borax). Two different urine samples were prepared with and without salt mixture, stored at room temperature and then analyzed by gas chromatography-mass spectrometry at 0, 1, 7, 15, and 30 days after collection/preparation to look for eventual analyte degradation. Methamphetamine showed no significant changes with respect to the time of collection/ preparation (T0) up to 7 days later (T7), with or without salt mixture addiction. Then a significant degradation occurred in both salted and non salted urine. BE decrease was observed starting from day 1 after sample collection in salted and not salted samples, respectively. Salt addition seemed to reduce at least the initial BE degradation, with a significant difference (p<0.001) at 7 and 15 days of storage. However, the degradation was not more prevented in salted samples at 30 days of storage. A 20% decrease of MOR concentration was observed starting from day 1 after collection/preparation, both in salted and not salted samples with no subsequent decrease. With regard to THCCOOH, a significant decrease was observed starting from 7 days after collection/preparation, with of without adding the salt mixture. However, when comparing salted versus non salted samples at each time point, a statistically significant difference was observed at 7 and 30 days of storage. The results obtained indicate that the degradation of MA, THC-COOH and BE in urine samples kept at room temperature can be slowed by the addition of the salt mixture, whereas it seems to be ineffective in samples containing MOR. This evidence has to be taken into account, in the eventuality of using salted urine to prevent in a certain extent abuse of above-reported drugs of abuse. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Processing, Mechanical and Optical Properties of Additive-Free ZrC Ceramics Prepared by Spark Plasma Sintering

PubMed Central

Musa, Clara; Licheri, Roberta; Orrù, Roberto; Cao, Giacomo; Sciti, Diletta; Silvestroni, Laura; Zoli, Luca; Balbo, Andrea; Mercatelli, Luca; Meucci, Marco; Sani, Elisa

2016-01-01

In the present study, nearly fully dense monolithic ZrC samples are produced and broadly characterized from microstructural, mechanical and optical points of view. Specifically, 98% dense products are obtained by Spark Plasma Sintering (SPS) after 20 min dwell time at 1850 °C starting from powders preliminarily prepared by Self-propagating High-temperature Synthesis (SHS) followed by 20 min ball milling. A prolonged mechanical treatment up to 2 h of SHS powders does not lead to appreciable benefits. Vickers hardness of the resulting samples (17.5 ± 0.4 GPa) is reasonably good for monolithic ceramics, but the mechanical strength (about 250 MPa up to 1000 °C) could be further improved by suitable optimization of the starting powder characteristics. The very smoothly polished ZrC specimen subjected to optical measurements displays high absorption in the visible-near infrared region and low thermal emittance at longer wavelengths. Moreover, the sample exhibits goodspectral selectivity (2.1–2.4) in the 1000–1400 K temperature range. These preliminary results suggest that ZrC ceramics produced through the two-step SHS/SPS processing route can be considered as attractive reference materials for the development of innovative solar energy absorbers. PMID:28773611

Preparation of Sm-doped ceria (SDC) nanowires and tubes by gas-liquid co-precipitation at room temperature

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gu Lina; School of Chemistry and Chemical Engineering, Anhui University, 230039 Hefei; Meng Guangyao

Sm-doped cerium dioxide (SDC) with fcc structure was formed using a gas-liquid chemical co-precipitation process at room temperature. Morphology and structure of the as-prepared samples were characterized using TG, XRD, TEM, HRTEM and SAED techniques. Under our specific experimental conditions, two kinds of 1D nano-structures SDC have been mainly obtained. SDC nanowires are 0.3-1.2 {mu}m in lengths and 5-20 nm in diameters. SDC nanotubes have outer diameters in 10-40 nm with lengths up to 2 {mu}m. The as-prepared SDC shows very strong UV absorption ability and the maximum absorption peak redshifts compared with that of SDC nanoparticles.

Molecular epidemiology biomarkers-Sample collection and processing considerations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Holland, Nina T.; Pfleger, Laura; Berger, Eileen

2005-08-07

Biomarker studies require processing and storage of numerous biological samples with the goals of obtaining a large amount of information and minimizing future research costs. An efficient study design includes provisions for processing of the original samples, such as cryopreservation, DNA isolation, and preparation of specimens for exposure assessment. Use of standard, two-dimensional and nanobarcodes and customized electronic databases assure efficient management of large sample collections and tracking results of data analyses. Standard operating procedures and quality control plans help to protect sample quality and to assure validity of the biomarker data. Specific state, federal and international regulations are inmore » place regarding research with human samples, governing areas including custody, safety of handling, and transport of human samples. Appropriate informed consent must be obtained from the study subjects prior to sample collection and confidentiality of results maintained. Finally, examples of three biorepositories of different scale (European Cancer Study, National Cancer Institute and School of Public Health Biorepository, University of California, Berkeley) are used to illustrate challenges faced by investigators and the ways to overcome them. New software and biorepository technologies are being developed by many companies that will help to bring biological banking to a new level required by molecular epidemiology of the 21st century.« less

The enhancement of beneficial effects following audio feedback by cognitive preparation in the treatment of social anxiety: a single-session experiment.

PubMed

Nilsson, Jan-Erik; Lundh, Lars-Gunnar; Faghihi, Shahriar; Roth-Andersson, Gun

2011-12-01

According to cognitive models, negatively biased processing of the publicly observable self is an important aspect of social phobia; if this is true, effective methods for producing corrective feedback concerning the public self should be strived for. Video feedback is proven effective, but since one's voice represents another aspect of the self, audio feedback should produce equivalent results. This is the first study to assess the enhancement of audio feedback by cognitive preparation in a single-session randomized controlled experiment. Forty socially anxious participants were asked to give a speech, then to listen to and evaluate a taped recording of their performance. Half of the sample was given cognitive preparation prior to the audio feedback and the remainder received audio feedback only. Cognitive preparation involved asking participants to (1) predict in detail what they would hear on the audiotape, (2) form an image of themselves giving the speech and (3) listen to the audio recording as though they were listening to a stranger. To assess generalization effects all participants were asked to give a second speech. Audio feedback with cognitive preparation was shown to produce less negative ratings after the first speech, and effects generalized to the evaluation of the second speech. More positive speech evaluations were associated with corresponding reductions of state anxiety. Social anxiety as indexed by the Implicit Association Test was reduced in participants given cognitive preparation. Small sample size; analogue study. Audio feedback with cognitive preparation may be utilized as a treatment intervention for social phobia. Copyright © 2011 Elsevier Ltd. All rights reserved.

A New Technique for Preparation of High-Grade Titanium Slag from Titanomagnetite Concentrate by Reduction-Melting-Magnetic Separation Processing

NASA Astrophysics Data System (ADS)

Lv, Chao; Yang, Kun; Wen, Shu-ming; Bai, Shao-jun; Feng, Qi-cheng

2017-10-01

This paper proposes a new technique for preparation of high-grade titanium slag from Panzhihua vanadium titanomagnetite concentrate by reduction-melting-magnetic separation processing. Chemical analysis, x-ray diffraction, and scanning electron microscopy in conjunction with energy-dispersive spectroscopy were used to characterize the samples. The effective separation of iron and titanium slag could be realized by melting metallized pellets at 1550°C for 60 min with the addition of 1% CaO (basicity of 1.1) and 2% graphite powder. The small iron particles embedded in the slag could be removed by fine grinding and magnetic separation process. The grade of TiO2 in the obtained high-grade titanium slag reached 60.68% and the total recovery of TiO2 was 91.25%, which could be directly applied for producing titanium white by the sulfuric acid process. This technique provides an alternative method to use vanadium titanomagnetite concentrate of the Panzhihua area in China.

Cross-sectional TEM specimen preparation for W/B{sub 4}C multilayer sample using FIB

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mondal, Puspen, E-mail: puspen@rrcat.gov.in; Pradhan, P. C.; Tiwari, Pragya

2016-05-23

A recent emergence of a cross-beam scanning electron microscopy (SEM)/focused-ion-beam (FIB) system have given choice to fabricate cross-sectional transmission electron microscopy (TEM) specimen of thin film multilayer sample. A 300 layer pair thin film multilayer sample of W/B{sub 4}C was used to demonstrate the specimen lift-out technique in very short time as compared to conventional cross-sectional sample preparation technique. To get large area electron transparent sample, sample prepared by FIB is followed by Ar{sup +} ion polishing at 2 kV with grazing incident. The prepared cross-sectional sample was characterized by transmission electron microscope.

Rapid Microbial Sample Preparation from Blood Using a Novel Concentration Device

PubMed Central

Boardman, Anna K.; Campbell, Jennifer; Wirz, Holger; Sharon, Andre; Sauer-Budge, Alexis F.

2015-01-01

Appropriate care for bacteremic patients is dictated by the amount of time needed for an accurate diagnosis. However, the concentration of microbes in the blood is extremely low in these patients (1–100 CFU/mL), traditionally requiring growth (blood culture) or amplification (e.g., PCR) for detection. Current culture-based methods can take a minimum of two days, while faster methods like PCR require a sample free of inhibitors (i.e., blood components). Though commercial kits exist for the removal of blood from these samples, they typically capture only DNA, thereby necessitating the use of blood culture for antimicrobial testing. Here, we report a novel, scaled-up sample preparation protocol carried out in a new microbial concentration device. The process can efficiently lyse 10 mL of bacteremic blood while maintaining the microorganisms’ viability, giving a 30‑μL final output volume. A suite of six microorganisms (Staphylococcus aureus, Streptococcus pneumoniae, Escherichia coli, Haemophilus influenzae, Pseudomonas aeruginosa, and Candida albicans) at a range of clinically relevant concentrations was tested. All of the microorganisms had recoveries greater than 55% at the highest tested concentration of 100 CFU/mL, with three of them having over 70% recovery. At the lowest tested concentration of 3 CFU/mL, two microorganisms had recoveries of ca. 40–50% while the other four gave recoveries greater than 70%. Using a Taqman assay for methicillin-sensitive S. aureus (MSSA)to prove the feasibility of downstream analysis, we show that our microbial pellets are clean enough for PCR amplification. PCR testing of 56 spiked-positive and negative samples gave a specificity of 0.97 and a sensitivity of 0.96, showing that our sample preparation protocol holds great promise for the rapid diagnosis of bacteremia directly from a primary sample. PMID:25675242

System for autonomous monitoring of bioagents

DOEpatents

Langlois, Richard G.; Milanovich, Fred P.; Colston, Jr, Billy W.; Brown, Steve B.; Masquelier, Don A.; Mariella, Jr., Raymond P.; Venkateswaran, Kodomudi

2015-06-09

An autonomous monitoring system for monitoring for bioagents. A collector gathers the air, water, soil, or substance being monitored. A sample preparation means for preparing a sample is operatively connected to the collector. A detector for detecting the bioagents in the sample is operatively connected to the sample preparation means. One embodiment of the present invention includes confirmation means for confirming the bioagents in the sample.

Electro-Chemical-Mechanical, Low Stress, Automatic Polishing (ECMP) Device (Preprint)

DTIC Science & Technology

2010-01-01

into models that predict mechanical response [ 4 - 6 ]. In addition, surface preparation steps are critical to the imaging of ceramic and hybrid...2p 3/2 peak in the spectral data found in Figure 4 . The Ti 2p 3/2 peak is initially observed at 458.4 eV indicating that titanium is present in its...above 6 acceptable limits for both (average IQ values were higher than 2000). For the titanium samples, the samples processed without applied

Spectroscopy and photochemistry of humic acids

NASA Astrophysics Data System (ADS)

Sokolova, I. V.; Vershinin, N. O.; Skobczova, K. A.; Tchaikovskaya, O. N.; Mayer, G. V.

2018-04-01

Spectroscopy and photochemistry of humic acids are discussed. The samples of HAs fractions were obtained from Fluka Chemical Co and prepared from peat of Western Siberia region. The comparative analysis of these acids with the sample of humic acids allocated from brown coal is carried out. A specific feature of the reactor is the use of barrier discharge excilamp (KrCl) with radiation wavelength λ = 222 nm. Influence of the received humic acids on process of photodegradation of herbicide - 2.4-dichlorophenoxyacetic acid is considered.

Analysis of defect structure in silicon. Characterization of samples from UCP ingot 5848-13C

NASA Technical Reports Server (NTRS)

Natesh, R.; Guyer, T.; Stringfellow, G. B.

1982-01-01

Statistically significant quantitative structural imperfection measurements were made on samples from ubiquitous crystalline process (UCP) Ingot 5848 - 13 C. Important trends were noticed between the measured data, cell efficiency, and diffusion length. Grain boundary substructure appears to have an important effect on the conversion efficiency of solar cells from Semix material. Quantitative microscopy measurements give statistically significant information compared to other microanalytical techniques. A surface preparation technique to obtain proper contrast of structural defects suitable for QTM analysis was perfected.

Non-destructive Determination of Disintegration Time and Dissolution in Immediate Release Tablets by Terahertz Transmission Measurements.

PubMed

Markl, Daniel; Sauerwein, Johanna; Goodwin, Daniel J; van den Ban, Sander; Zeitler, J Axel

2017-05-01

The aim of this study was to establish the suitability of terahertz (THz) transmission measurements to accurately measure and predict the critical quality attributes of disintegration time and the amount of active pharmaceutical ingredient (API) dissolved after 15, 20 and 25 min for commercial tablets processed at production scale. Samples of 18 batches of biconvex tablets from a production-scale design of experiments study into exploring the design space of a commercial tablet manufacturing process were used. The tablet production involved the process steps of high-shear wet granulation, fluid-bed drying and subsequent compaction. The 18 batches were produced using a 4 factor split plot design to study the effects of process changes on the disintegration time. Non-destructive and contactless terahertz transmission measurements of the whole tablets without prior sample preparation were performed to measure the effective refractive index and absorption coefficient of 6 tablets per batch. The disintegration time (R 2  = 0.86) and API dissolved after 15 min (R 2  = 0.96) linearly correlates with the effective refractive index, n eff , measured at terahertz frequencies. In contrast, no such correlation could be established from conventional hardness measurements. The magnitude of n eff represents the optical density of the sample and thus it reflects both changes in tablet porosity as well as granule density. For the absorption coefficient, α eff , we observed a better correlation with dissolution after 20 min (R 2  = 0.96) and a weaker correlation with disintegration (R 2  = 0.83) compared to n eff . The measurements of n eff and α eff provide promising predictors for the disintegration and dissolution time of tablets. The high penetration power of terahertz radiation makes it possible to sample a significant volume proportion of a tablet without any prior sample preparation. Together with the short measurement time (seconds), the potential to measure content uniformity and the fact that the method requires no chemometric models this technology shows clear promise to be established as a process analyser to non-destructively predict critical quality attributes of tablets.

Single hair analysis of small molecules using MALDI-triple quadrupole MS imaging and LC-MS/MS: investigations on opportunities and pitfalls.

PubMed

Poetzsch, Michael; Steuer, Andrea E; Roemmelt, Andreas T; Baumgartner, Markus R; Kraemer, Thomas

2014-12-02

Single hair analysis normally requires extensive sample preparation microscale protocols including time-consuming steps like segmentation and extraction. Matrix assisted laser desorption and ionization mass spectrometric imaging (MALDI-MSI) was shown to be an alternative tool in single hair analysis, but still, questions remain. Therefore, an investigation of MALDI-MSI in single hair analysis concerning the extraction process, usage of internal standard (IS), and influences on the ionization processes were systematically investigated to enable the reliable application to hair analysis. Furthermore, single dose detection, quantitative correlation to a single hair, and hair strand LC-MS/MS results were performed, and the performance was compared to LC-MS/MS single hair monitoring. The MALDI process was shown to be independent from natural hair color and not influenced by the presence of melanin. Ionization was shown to be reproducible along and in between different hair samples. MALDI image intensities in single hair and hair snippets showed good semiquantitative correlation to zolpidem hair concentrations obtained from validated routine LC-MS/MS methods. MALDI-MSI is superior to LC-MS/MS analysis when a fast, easy, and cheap sample preparation is necessary, whereas LC-MS/MS showed higher sensitivity with the ability of single dose detection for zolpidem. MALDI-MSI and LC-MS/MS segmental single hair analysis showed good correlation, and both are suitable for consumption monitoring of drugs of abuse with a high time resolution.

Effect of sample inhomogeneity in KAr dating

USGS Publications Warehouse

Engels, J.C.; Ingamells, C.O.

1970-01-01

Error in K-Ar ages is often due more to deficiencies in the splitting process, whereby portions of the sample are taken for potassium and for argon determination, than to imprecision in the analytical methods. The effect of the grain size of a sample and of the composition of a contaminating mineral can be evaluated, and this provides a useful guide in attempts to minimize error. Rocks and minerals should be prepared for age determination with the effects of contaminants and grain size in mind. The magnitude of such effects can be much larger than intuitive estimates might indicate. ?? 1970.

X-ray diffraction and TGA kinetic analyses for chemical looping combustion applications.

PubMed

Tijani, Mansour Mohammedramadan; Aqsha, Aqsha; Mahinpey, Nader

2018-04-01

Synthesis and characterization of supported metal-based oxygen carriers were carried out to provide information related to the use of oxygen carriers for chemical looping combustion processes. The Cu, Co, Fe, Ni metals supported with Al 2 O 3 , CeO 2 , TiO 2 , ZrO 2 were prepared using the wetness impregnation technique. Then, the X-ray Diffraction (XRD) characterization of oxidized and reduced samples was obtained and presented. The kinetic analysis using Thermogravimetric analyzer (TGA) of the synthesized samples was conducted. The kinetics of reduction reaction of all samples were estimated and explained.

Characterization of fission gas bubbles in irradiated U-10Mo fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Casella, Andrew M.; Burkes, Douglas E.; MacFarlan, Paul J.

2017-09-01

Irradiated U-10Mo fuel samples were prepared with traditional mechanical potting and polishing methods with in a hot cell. They were then removed and imaged with an SEM located outside of a hot cell. The images were then processed with basic imaging techniques from 3 separate software packages. The results were compared and a baseline method for characterization of fission gas bubbles in the samples is proposed. It is hoped that through adoption of or comparison to this baseline method that sample characterization can be somewhat standardized across the field of post irradiated examination of metal fuels.

Current Technical Approaches for the Early Detection of Foodborne Pathogens: Challenges and Opportunities.

PubMed

Cho, Il-Hoon; Ku, Seockmo

2017-09-30

The development of novel and high-tech solutions for rapid, accurate, and non-laborious microbial detection methods is imperative to improve the global food supply. Such solutions have begun to address the need for microbial detection that is faster and more sensitive than existing methodologies (e.g., classic culture enrichment methods). Multiple reviews report the technical functions and structures of conventional microbial detection tools. These tools, used to detect pathogens in food and food homogenates, were designed via qualitative analysis methods. The inherent disadvantage of these analytical methods is the necessity for specimen preparation, which is a time-consuming process. While some literature describes the challenges and opportunities to overcome the technical issues related to food industry legal guidelines, there is a lack of reviews of the current trials to overcome technological limitations related to sample preparation and microbial detection via nano and micro technologies. In this review, we primarily explore current analytical technologies, including metallic and magnetic nanomaterials, optics, electrochemistry, and spectroscopy. These techniques rely on the early detection of pathogens via enhanced analytical sensitivity and specificity. In order to introduce the potential combination and comparative analysis of various advanced methods, we also reference a novel sample preparation protocol that uses microbial concentration and recovery technologies. This technology has the potential to expedite the pre-enrichment step that precedes the detection process.

Extended Investigation on the Delicate Correlations Between Thermal Behavior and Physical Characteristics of Multi-component Blends

NASA Astrophysics Data System (ADS)

Shokoohi, Shirin

2015-11-01

Polypropylene (PP)/polyamide6 (PA6)/ethylene propylene diene rubber (EPDM) (70/15/15) ternary polymer blends compatibilized with maleic anhydride-grafted EPDM (EPDM-g-MA) were prepared under various processing parameters (barrel temperature, screw speed, and blending sequence). Thermal studies on the prepared blend samples were carried out using differential scanning calorimetry and dynamic mechanical thermal analysis. According to the results, heterogeneous nucleation phenomenon was observed due to the solidification of the PA6 particles dispersed within the PP melt leading to a significant increase in the crystallinity degree and exotherm crystallization peak temperature of PP compared to the pure homopolymer. This was suppressed in the samples with core-shell morphology due to the reduced PP/PA6 interfacial contact. Fractionated crystallization was observed when PA6 droplets dispersed too fine within the matrix (in this case bar{d}_M˜ 0.3 \\upmu {m}). Scanning electron microscopy micrographs were consistent with the melting and crystallization behavior of the blend samples.

First evidence of tyre debris characterization at the nanoscale by focused ion beam

DOE Office of Scientific and Technical Information (OSTI.GOV)

Milani, M.; Pucillo, F.P.; Ballerini, M.

2004-07-15

In this paper, we present a novel technique for the nanoscale characterization of the outer and inner structure of tyre debris. Tyre debris is produced by the normal wear of tyres. In previous studies, the microcharacterization and identification were performed by analytical electron microscopy. This study is a development of the characterization of surface and microstructure of tyre debris. For the first time, tyre debris was analysed by focused ion beam (FIB), a technique with 2- to 5-nm resolution that does not require any sample preparation. We studied tyre debris produced in the laboratory. We made electron and ionic imagingmore » of the surface of the material, and after a ionic cut, we studied the internal microstructure of the same sample. The tyre debris was analysed by FIB without any sample preparations unlike the case of scanning and transmission electron microscopy (SEM and TEM). Useful information was derived to improve detection and monitoring techniques of pollution by tyre degradation processes.« less

Ultrasonic-assisted in-situ fabrication of BiOBr modified Bi2O2CO3 microstructure with enhanced photocatalytic performance.

PubMed

Cheng, Lijun; Hu, Xumin; Hao, Liang

2018-06-01

Via an ultrasonic-assisted in-situ etching method, BiOBr modified Bi 2 O 2 CO 3 microstructures were fabricated in short time. The samples were characterized by XRD, SEM, TEM, BET, UV-Vis, XPS and PL spectra methods. Rhodamine B (RhB) aqueous solution was applied to evaluate the photocatalytic activities of the as-prepared samples. The results showed that the sample prepared at pH of 2 in which the molar ratio of BiOBr and Bi 2 O 2 CO 3 was 0.69:1 had the largest specific surface area, the best utilization for ultraviolet and visible light and efficient separation efficiency of charge carriers, contributing to its best photocatalytic activity. O 2 - was proved to be main active species in RhB photodegradation process. Last, the photocatalytic mechanism of the composite was discussed in detail. Copyright © 2018 Elsevier B.V. All rights reserved.

Rheology and stability kinetics of bare silicon nanoparticle inks for low-cost direct printing

DOE Office of Scientific and Technical Information (OSTI.GOV)

More, Priyesh V.; Jeong, Sunho; Seo, Yeong-Hui

2013-12-16

Highly dispersed and stable silicon nanoparticles ink is formulated for its application in direct printing or printable electronics. These dispersions are prepared from free-standing silicon nanoparticles which are not capped with any organic ligand, making it suitable for electronic applications. Silicon nanoparticles dispersions are prepared by suspending the nanoparticles in benzonitrile or ethanol by using polypropylene glycol (PPG) as a binder. All the samples show typical shear thinning behavior while the dispersion samples show low viscosities signifying good quality dispersion. Such thinning behavior favors in fabrication of dense films with spin-coating or patterns with drop casting. The dispersion stability ismore » monitored by turbiscan measurements showing good stability for one week. A low-cost direct printing method for dispersion samples is also demonstrated to obtain micro-sized patterns. Low electrical resistivity of resulting patterns, adjustable viscosity and good stability makes these silicon nanoparticles dispersions highly applicable for direct printing process.« less

Analysis of microstructure and mechanical properties of aluminium-copper joints welded by FSW process

NASA Astrophysics Data System (ADS)

Iordache, M.; Sicoe, G.; Iacomi, D.; Niţu, E.; Ducu, C.

2017-08-01

The research conducted in this article aimed to check the quality of joining some dissimilar materials Al-Cu by determining the mechanical properties and microstructure analysis. For the experimental measurements there were used tin alloy Al - EN-AW-1050A with a thickness of 2 mm and Cu99 sheet with a thickness of 2 mm, joined by FSW weld overlay. The main welding parameters were: rotating speed of the rotating element 1400 rev/min, speed of the rotating element 50 mm/min. The experimental results were determined on samples specially prepared for metallographic analysis. In order to prepare samples for their characterization, there was designed and built a device that allowed simultaneous positioning and fixing for grinding. The characteristics analyzed in the joint welded samples were mictrostructure, microhardness and residual stresses. The techniques used to determine these characteristics were optical microscopy, electron microscopy with fluorescence radioactive elemental analysis (EDS), Vickers microhardness line - HV0.3 and X-ray diffractometry.

The XRD Study of the Effect of Slight Change in Structure on the Superconductivity of Y-Ba-Cu-O System Material

NASA Astrophysics Data System (ADS)

Huaqin, Wang; Shiyuan, Zhang; Tongzheng, Jin; Shiying, Han; Dirong, Qiu; Hao, Wang; Ningsheng, Zhou

In this paper the differences in diffraction intensities from some crystal planes in the X-ray diffraction patterns of high Tc Y-Ba-Cu-O system superconductors prepared by different processing conditions and the difference among various structure cells in references are interpreted using computer fitting. The results suggest that there exists two structure cells in the single phase YBa2Cu3O7-x samples. Both structure cells have the same crystal symmetry and almost the same lattice parameters, a=3.821Å, b=3.892Å and c=11.676Å, but the different distortion degree of Cu2-O plane. According to EPR spectra measured on the same samples, it is considered that the improvement of superconductivity for the samples prepared by two-step annealing in flowing oxygen may be related to concentration of the structure cell with more serious distortion on the Cu2-O plane.

Quantum dots assisted laser desorption/ionization mass spectrometric detection of carbohydrates: qualitative and quantitative analysis.

PubMed

Bibi, Aisha; Ju, Huangxian

2016-04-01

A quantum dots (QDs) assisted laser desorption/ionization mass spectrometric (QDA-LDI-MS) strategy was proposed for qualitative and quantitative analysis of a series of carbohydrates. The adsorption of carbohydrates on the modified surface of different QDs as the matrices depended mainly on the formation of hydrogen bonding, which led to higher MS intensity than those with conventional organic matrix. The effects of QDs concentration and sample preparation method were explored for improving the selective ionization process and the detection sensitivity. The proposed approach offered a new dimension to the application of QDs as matrices for MALDI-MS research of carbohydrates. It could be used for quantitative measurement of glucose concentration in human serum with good performance. The QDs served as a matrix showed the advantages of low background, higher sensitivity, convenient sample preparation and excellent stability under vacuum. The QDs assisted LDI-MS approach has promising application to the analysis of carbohydrates in complex biological samples. Copyright © 2016 John Wiley & Sons, Ltd.

Template-Free Synthesis and Enhanced Photocatalytic Performance of Uniform BiOCI Flower-Like Microspheres.

PubMed

Chang, Fei; Xie, Yunchao; Chen, Juan; Luo, Jieru; Li, Chenlu; Hu, Xuefeng; Xu, Bin

2015-02-01

Preparation of uniform BiOCI flower-like microspheres was facilely accomplished through a sim- ple protocol involving regulation of pH value in aqueous with sodium hydroxide in the presence of n-propanol. The as-prepared samples were characterized by a collection of techniques, such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), UV-vis diffuse reflectance spectroscopy (UV-vis DRS), and nitrogen adsorption-desorption isotherms. Based upon the SEM analyses, uniform microspheres could be formed with coexistence of some fragments of BiOCI nanosheets without n-propanol. The addition of appropriate amount of n-propanol was beneficial to provide BiOCI samples containing only flower-like microspheres, which were further subjected to the photocatalytic measurements towards Rhodamine B in aqueous under visible light irradiation and exhibited the best catalytic performance among all samples tested. In addition, the photocatalytic process was confirmed to undergo through a photosensitization pathway, in which superoxide radicals (.O-) played critical roles.